CN116355282B - Antibacterial material and preparation method and application thereof - Google Patents
Antibacterial material and preparation method and application thereof Download PDFInfo
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- CN116355282B CN116355282B CN202310440020.XA CN202310440020A CN116355282B CN 116355282 B CN116355282 B CN 116355282B CN 202310440020 A CN202310440020 A CN 202310440020A CN 116355282 B CN116355282 B CN 116355282B
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- antibacterial material
- glass beads
- microbeads
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 165
- 239000000463 material Substances 0.000 title claims abstract description 140
- 238000002360 preparation method Methods 0.000 title claims abstract description 60
- 239000011521 glass Substances 0.000 claims abstract description 114
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000004332 silver Substances 0.000 claims abstract description 75
- 229910052709 silver Inorganic materials 0.000 claims abstract description 75
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 239000002861 polymer material Substances 0.000 claims abstract description 47
- 239000011325 microbead Substances 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 38
- -1 silver amine Chemical class 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- 239000002243 precursor Substances 0.000 claims description 33
- 150000001412 amines Chemical class 0.000 claims description 28
- 239000003446 ligand Substances 0.000 claims description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 13
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 12
- MFEIKQPHQINPRI-UHFFFAOYSA-N 3-Ethylpyridine Chemical compound CCC1=CC=CN=C1 MFEIKQPHQINPRI-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 7
- 125000003277 amino group Chemical group 0.000 claims description 7
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 6
- 229940071536 silver acetate Drugs 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 6
- NJBCRXCAPCODGX-UHFFFAOYSA-N 2-methyl-n-(2-methylpropyl)propan-1-amine Chemical compound CC(C)CNCC(C)C NJBCRXCAPCODGX-UHFFFAOYSA-N 0.000 claims description 5
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 5
- LMEWRZSPCQHBOB-UHFFFAOYSA-M silver;2-hydroxypropanoate Chemical compound [Ag+].CC(O)C([O-])=O LMEWRZSPCQHBOB-UHFFFAOYSA-M 0.000 claims description 5
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229940071575 silver citrate Drugs 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 8
- 239000002131 composite material Substances 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000011324 bead Substances 0.000 description 92
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 27
- 230000000845 anti-microbial effect Effects 0.000 description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- 238000001746 injection moulding Methods 0.000 description 17
- 230000009286 beneficial effect Effects 0.000 description 14
- 239000004033 plastic Substances 0.000 description 14
- 229920003023 plastic Polymers 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 9
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 8
- 239000004743 Polypropylene Substances 0.000 description 7
- 229920001155 polypropylene Polymers 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 230000001954 sterilising effect Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000004599 antimicrobial Substances 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 241000208818 Helianthus Species 0.000 description 3
- 235000003222 Helianthus annuus Nutrition 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000002952 polymeric resin Substances 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000008156 Ringer's lactate solution Substances 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明提供了一种抗菌材料及其制备方法和应用。根据本发明的抗菌材料，包括玻璃微珠，所述玻璃微珠表面附着有银胺络合物。本发明的抗菌材料，玻璃微珠表面附着有银胺络合物，将该抗菌材料添加到高分子材料中时，在高分子材料的制备成型过程中，银胺络合物受热分解成纳米银颗粒，纳米银颗粒附着在玻璃微珠表面，可以为玻璃微珠及以其为原料制备的复合材料提供高效的杀菌能力，无需大量添加即可发挥高效的抗菌效果，降低了成本，利于大规模普及应用。本发明还提供了抗菌材料的制备方法和应用。
The present invention provides an antibacterial material and a preparation method and application thereof. The antibacterial material according to the present invention comprises glass microbeads, and a silver amine complex is attached to the surface of the glass microbeads. The antibacterial material of the present invention has a silver amine complex attached to the surface of the glass microbeads. When the antibacterial material is added to a polymer material, during the preparation and molding process of the polymer material, the silver amine complex is decomposed into nano silver particles by heat. The nano silver particles are attached to the surface of the glass microbeads, which can provide efficient bactericidal ability for the glass microbeads and the composite materials prepared with the glass microbeads as raw materials. The efficient antibacterial effect can be exerted without a large amount of addition, which reduces the cost and is conducive to large-scale popularization and application. The present invention also provides a preparation method and application of the antibacterial material.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to an antibacterial material and a preparation method and application thereof.
Background
Diseases caused by bacterial infection have long been a threat to human health and safety. Nano silver has been widely used in antibacterial goods due to its high heat resistance, safety and broad-spectrum antibacterial property. Plastic related articles are also important as an important component in daily life to improve the antimicrobial properties of such articles.
In the related art, the technical proposal related to the nano silver antibacterial composite material and the preparation thereof is to add nano silver particles into polymer resin, on one hand, the method can not ensure the uniform distribution of nano silver in the material, and on the other hand, a large amount of nano silver particles are needed to be added for enabling the plastic product to reach the antibacterial standard, so that the cost is high and the large-scale popularization and application are difficult.
Thus, there remains a need to develop a new antimicrobial material.
Disclosure of Invention
The present invention aims to solve at least one of the above technical problems in the prior art. Therefore, the antibacterial material provided by the invention can be uniformly distributed in the high polymer material, can exert antibacterial effect without adding a large amount, is easy to prepare and low in cost, and is beneficial to large-scale popularization and application.
The invention also provides a preparation method of the antibacterial material.
The invention also provides an antibacterial microbead.
The invention also provides a modified polymer material.
The invention also provides a household appliance.
The first aspect of the invention provides an antibacterial material, which comprises glass beads, wherein silver amine complexes are attached to the surfaces of the glass beads.
The invention relates to one of the technical schemes of antibacterial materials, which has at least the following beneficial effects:
When the antibacterial material is added into a high polymer material, the silver amine complex is heated and decomposed into nano silver particles in the preparation process of the high polymer material, and the nano silver particles are attached to the surfaces of the glass beads, so that the antibacterial material has high-efficiency sterilization capability. When the antibacterial material is used as a raw material to prepare the modified polymer material, a large amount of antibacterial material is not required to be added, so that the efficient antibacterial effect can be exerted, the cost is reduced, and the large-scale popularization and application are facilitated.
The antibacterial material provided by the invention takes the glass beads as a matrix, is easy to prepare, can be used for modifying a high polymer material, has the characteristics of light weight and antibacterial property, and has wide application prospects in industries such as household appliances, automobiles and the like.
The use cost of the antibacterial material is obviously lower than that of nano silver particles.
According to the antibacterial material disclosed by the invention, the silver-amine complex is attached to the surfaces of the glass beads, and the decomposition temperature of the silver-amine complex can be distributed between 90 ℃ and 150 ℃ according to the difference of silver precursors and amine ligands which are raw materials for preparing the silver-amine complex, so that the antibacterial material better fits the processing forming temperature of most high polymer materials, and the application range is wide.
According to some embodiments of the invention, the glass beads have a particle size in the range of 10 μm to 80 μm.
According to some embodiments of the invention, the glass beads are hollow glass beads, which are beneficial to further realizing light weight.
According to some embodiments of the invention, the antimicrobial material is prepared from raw materials including glass beads, silver precursors, amine ligands, silane coupling agents, and solvents.
The silver precursor is decomposed to form nano silver, which is attached to the surface of glass microsphere.
The amine ligand has the function of reducing the decomposition temperature of the silver precursor and controlling the growth rate and the grain diameter of the nano silver.
The silane coupling agent has the function of carrying out surface modification on the glass beads and increasing the compatibility of the glass beads and the polymer resin.
The solvent has the function of providing a reaction environment for the silver precursor, the amine ligand and the silane coupling agent, and is convenient for fully mixing and stirring the raw materials.
According to some embodiments of the invention, the mass ratio of the glass beads in the preparation raw materials of the antibacterial material is 5-15 wt%.
According to some embodiments of the invention, the molar ratio of the silver precursor to the amine groups in the amine ligand is 1:1-5.
According to some embodiments of the invention, the molar ratio of the silver precursor to the amine groups in the amine ligand is 1:2-5.
According to some embodiments of the invention, the molar ratio of amine groups in the silver precursor and amine ligand is 1:2.
According to some embodiments of the invention, the silver precursor comprises at least one of silver acetate, silver oxalate, silver citrate, and silver lactate.
According to some embodiments of the invention, the silver precursor is silver oxalate.
According to some embodiments of the invention, the silver precursor is 20wt% to 50wt% in the preparation raw material of the antibacterial material.
According to some embodiments of the invention, the amine ligand comprises at least one of 2-amino-2-methyl-1-propanol, diisobutylamine, propylenediamine, octylamine, sunflower amine, and 3-ethylpyridine.
According to some embodiments of the invention, the amine ligand is 2-amino-2-methyl-1-propanol.
According to some embodiments of the invention, the silane coupling agent comprises at least one of 3-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane.
According to some embodiments of the invention, the silane coupling agent comprises at least one of KH-550, KH-540, and KH-551.
According to some embodiments of the invention, the mass ratio of the silane coupling agent in the preparation raw material of the antibacterial material is 5-10 wt%.
According to some embodiments of the invention, the solvent comprises at least one of water, ethanol, ethylene glycol, glycerol, and t-butanol.
According to some embodiments of the invention, the solvent is deionized water.
According to some embodiments of the invention, the solvent is present in the antimicrobial material in a preparation raw material in a mass ratio of 25wt% to 70wt%.
The second aspect of the invention provides a method for preparing the antibacterial material, which comprises the steps of mixing raw materials for preparing the antibacterial material, heating, stirring and drying to obtain the antibacterial material.
The invention relates to a technical scheme in a preparation method of an antibacterial material, which at least has the following beneficial effects:
According to the preparation method of the antibacterial material, the preparation raw materials of the antibacterial material are mixed, namely the glass beads are mixed with the preparation raw materials of the silver-amine complex, the preparation raw materials of the silver-amine complex specifically comprise a silver precursor, an amine ligand, a silane coupling agent and a solvent, the preparation raw materials of the silver-amine complex react to form the silver-amine complex in the heating and stirring process, the silver-amine complex is attached to the surfaces of the glass beads, and then the solution is dried, so that the antibacterial material can be obtained.
According to some embodiments of the invention, the method further comprises pre-treating the glass beads.
According to some embodiments of the invention, the pretreatment method may be to ultrasonically clean glass beads by sequentially using acetone, acetic acid aqueous solution and ethanol.
The pretreatment is used for removing impurities and grease on the surfaces of the glass beads, and is favorable for the adhesion of silver-amine complexes and the adhesion of nano silver particles.
According to some embodiments of the invention, the temperature of the heating and stirring is 60 ℃ to 90 ℃.
According to some embodiments of the invention, the temperature of the heating and stirring is 80-90 ℃.
According to some embodiments of the invention, the heating and stirring time is 6-12 h.
According to some embodiments of the invention, the heating and stirring time is 8-12 h.
According to some embodiments of the invention, the heating and stirring speed is 200 rpm-400 rpm.
In a third aspect of the present invention, there is provided an antimicrobial microbead formed from the antimicrobial material upon thermal decomposition.
The invention relates to a technical scheme of an antibacterial microbead, which has at least the following beneficial effects:
the antibacterial microbeads are formed by the antibacterial material of the invention after being heated and decomposed, and have all the beneficial effects of the antibacterial material, in particular:
the antibacterial microbeads disclosed by the invention comprise glass microbeads and nano silver particles attached to the surfaces of the glass microbeads, can be uniformly dispersed in a high polymer material, provide an excellent antibacterial effect for the high polymer material, do not need to be added in a large amount, reduce the cost and are beneficial to large-scale popularization and application.
The antibacterial microbeads are formed by the antibacterial material of the invention after being heated and decomposed in the preparation or forming process of the polymer material, are easy to prepare, can ensure that the polymer material has the characteristics of antibacterial property and light weight, and have wide application prospects in industries such as household appliances, automobiles and the like.
The fourth aspect of the invention provides a modified polymer material, and the preparation raw material comprises the antibacterial material.
The invention relates to a technical scheme of modified polymer materials, which has at least the following beneficial effects:
The modified polymer material has the beneficial effects that the antibacterial material is used as the preparation raw material, and particularly, the modified polymer material contains the antibacterial material, the surfaces of glass beads of the antibacterial material are provided with silver-amine complexes, the decomposition temperature of the silver-amine complexes can be distributed between 90 ℃ and 150 ℃ according to the difference of silver precursors and amine ligands, and the processing and forming temperature of the polymer material is well matched, so that the silver-amine complexes are heated and decomposed into nano silver particles in the processing and forming process of the polymer material, the nano silver particles are attached to the surfaces of the glass beads, the efficient antibacterial capability can be provided for the glass beads and the composite material prepared by taking the nano silver particles as the raw material, the efficient antibacterial effect can be exerted without a large amount of addition, the cost is reduced, and the large-scale popularization and application are facilitated.
The modified polymer material is easy to prepare, can enable the polymer material to have the characteristics of light weight and antibiosis, and has wide application prospect in industries such as household appliances, automobiles and the like.
According to some embodiments of the invention, the modified polymeric material comprises a modified plastic.
According to some embodiments of the invention, the modified polymeric material comprises a polymeric material matrix and antimicrobial microbeads dispersed in the polymeric material matrix, the antimicrobial microbeads being formed after the antimicrobial material is decomposed by heating.
According to some embodiments of the invention, the addition amount of the antibacterial material in the modified polymer material is 1-10 wt%.
According to some embodiments of the invention, the modified polymeric material may be extruded in a twin screw extruder to pellet and then injection molded by an injection molding machine.
The temperature of each zone of the twin-screw extruder can be 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 1 min-3 min.
In a fifth aspect, the present invention provides a household appliance, wherein the preparation raw material comprises the antibacterial material.
The invention relates to one of the technical schemes of household appliances, which has at least the following beneficial effects:
The household appliance has all the beneficial effects of the antibacterial material because the antibacterial material is used. Specifically, in the household appliance, the antibacterial microbeads are dispersed in the preparation raw materials, the antibacterial microbeads comprise a microbead matrix, and the nano silver particles are attached to the surface of the microbead matrix, so that the high-efficiency sterilization capability can be provided for the modified high-molecular material.
According to some embodiments of the invention, the household appliance includes a refrigerator, a washing machine, and an air conditioner.
Drawings
FIG. 1 is a schematic view of the thermal decomposition process of the antimicrobial material of the present invention.
Reference numerals:
1, glass beads;
silver amine complex;
3, nano silver particles.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the embodiments, but the present invention is not limited to these embodiments.
In some embodiments of the invention, the invention provides an antimicrobial material comprising glass beads having silver amine complexes attached to the surfaces of the glass beads.
Referring to fig. 1, it can be understood that, in the antibacterial material of the present invention, the silver amine complex 2 is attached to the surface of the glass bead 1, and when the antibacterial material is added into a polymer material, the silver amine complex 2 is decomposed into nano silver particles 3 by heating in the preparation process of the polymer material, and the nano silver particles 3 are attached to the surface of the glass bead 1, so that the antibacterial material has high-efficiency sterilization capability. When the antibacterial material is used as a raw material to prepare the modified polymer material, a large amount of antibacterial material is not required to be added, so that the efficient antibacterial effect can be exerted, the cost is reduced, and the large-scale popularization and application are facilitated.
It can be further understood that the antibacterial material provided by the invention takes the glass beads as a matrix, is easy to prepare, can enable the polymer material to have the characteristics of light weight and antibacterial property when being used for modifying the polymer material, and has wide application prospects in industries such as household appliances, automobiles and the like.
It can also be appreciated that the antimicrobial material of the present invention has significantly lower use costs than the simple addition of nano silver particles.
It can be understood that the silver-amine complex is attached to the surface of the glass microsphere, and the decomposition temperature of the silver-amine complex can be distributed between 90 ℃ and 150 ℃ according to the difference of the silver precursor and the amine ligand which are the preparation raw materials of the silver-amine complex, so that the silver-amine complex better fits the processing forming temperature of most high polymer materials, and has wide application range.
In some embodiments of the invention, the glass beads have a particle size in the range of 10 μm to 80 μm.
In some embodiments of the present invention, the glass beads are hollow glass beads, which are advantageous for further achieving weight reduction.
In some embodiments of the invention, the antimicrobial material is prepared from raw materials including glass microspheres, silver precursors, amine ligands, silane coupling agents, and solvents.
The silver precursor is decomposed to form nano silver, which is attached to the surface of glass bead.
The amine ligand has the function of reducing the decomposition temperature of the silver precursor and controlling the growth rate and the grain diameter of the nano silver.
The silane coupling agent has the function of carrying out surface modification on the glass beads and increasing the compatibility of the glass beads and the polymer resin.
The solvent has the function of providing a reaction environment for the silver precursor, the amine ligand and the silane coupling agent, and is convenient for fully mixing and stirring the raw materials.
In some embodiments of the invention, the mass ratio of the glass beads in the preparation raw materials of the antibacterial material is 5-15 wt%.
In some embodiments of the invention, the molar ratio of amine groups in the silver precursor and the amine ligand is 1:1-5.
In some embodiments of the invention, the molar ratio of amine groups in the silver precursor and the amine ligand is 1:2-5.
In some embodiments of the invention, the molar ratio of amine groups in the silver precursor and the amine ligand is 1:2.
In some embodiments of the invention, the silver precursor comprises at least one of silver acetate, silver oxalate, silver citrate, and silver lactate.
Silver acetate is a complex compound with a practical structure of a dimer, wherein silver is in a linear coordination. Silver acetate is a light-sensitive white crystalline solid that can be used as a source of water-soluble silver ions. The CAS number for silver acetate is 563-63-3.
Silver oxalate can be decomposed into silver and carbon dioxide under geological conditions, and is a precursor for producing nano silver. CAS number 533-51-7.
The CAS number for silver citrate is 314040-92-1.
Silver lactate can be prepared by mixing an equimolar amount of silver nitrate solution with a sodium lactate solution, and can be used as disinfectant and preservative. CAS number 128-00-7.
In some embodiments of the invention, the silver precursor is silver oxalate.
In some embodiments of the invention, the mass ratio of the silver precursor in the preparation raw material of the antibacterial material is 20wt% to 50wt%.
In some embodiments of the invention, the amine ligand comprises at least one of 2-amino-2-methyl-1-propanol, diisobutylamine, propylenediamine, octylamine, sunflower amine, and 3-ethylpyridine. Specifically:
the CAS number for 2-amino-2-methyl-1-propanol is 124-68-5.
Diisobutylamine has a CAS number of 110-96-3.
The CAS number for propylene diamine is 78-90-0.
The CAS number for octylamine is 111-86-4.
The CAS number for sunflower amine is 2016-57-1.
3-Ethylpyridine has a CAS number of 536-78-7.
In some embodiments of the invention, the amine ligand is 2-amino-2-methyl-1-propanol.
In some embodiments of the present invention, the silane coupling agent includes at least one of 3-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane.
In some embodiments of the present invention, the silane coupling agent includes at least one of KH-550, KH-540, and KH-551.
In some embodiments of the invention, the mass ratio of the silane coupling agent in the preparation raw material of the antibacterial material is 5-10 wt%.
In some embodiments of the invention, the solvent comprises at least one of water, ethanol, ethylene glycol, glycerol, and t-butanol.
In some embodiments of the invention, the solvent is deionized water.
In some embodiments of the invention, the mass ratio of the solvent in the preparation raw material of the antibacterial material is 25wt% to 70wt%.
In other embodiments of the present invention, a method of preparing an antimicrobial material is provided by mixing raw materials for preparing the antimicrobial material, heating and stirring the raw materials, and drying the raw materials to obtain the antimicrobial material.
It can be understood that the preparation method of the antibacterial material mixes the preparation raw materials of the antibacterial material, namely, the glass beads and the preparation raw materials of the silver-amine complex, wherein the preparation raw materials of the silver-amine complex specifically refer to silver precursors, amine ligands, silane coupling agents and solvents, and the preparation raw materials of the silver-amine complex react to form the silver-amine complex in the heating and stirring processes, and are attached to the surfaces of the glass beads, and then the solution is dried, so that the antibacterial material can be obtained.
In some embodiments of the invention, the method of making further comprises pre-treating the glass microspheres.
In some embodiments of the invention, the pretreatment method can be to ultrasonically clean the glass beads by sequentially using acetone, acetic acid aqueous solution and ethanol.
The pretreatment is used for removing impurities and grease on the surfaces of the glass beads, and is favorable for the adhesion of silver-amine complexes and the adhesion of nano silver particles.
In some embodiments of the present invention, the temperature of the heating and stirring is 60 ℃ to 90 ℃.
In some embodiments of the invention, the temperature of the heating and stirring is 80 ℃ to 90 ℃.
In some embodiments of the invention, the heating and stirring time is 6-12 hours.
In some embodiments of the invention, the heating and stirring time is 8-12 hours.
In some embodiments of the present invention, the speed of heating and stirring is 200rpm to 400rpm.
In still other embodiments of the present invention, an antimicrobial microbead is provided that is formed from the antimicrobial material of the present invention upon thermal decomposition.
It can be understood that the antibacterial microbead provided by the invention is formed by the antibacterial material provided by the invention after being heated and decomposed, and has all the beneficial effects of the antibacterial material, in particular:
In addition, the antibacterial microbeads comprise the glass microbeads and the nano silver particles attached to the surfaces of the glass microbeads, can be uniformly dispersed in a high polymer material, provide an excellent antibacterial effect for the high polymer material, do not need to be added in a large amount, reduce the cost and are beneficial to large-scale popularization and application.
Furthermore, the antibacterial microbeads are formed by the antibacterial material of the invention after being heated and decomposed in the preparation or molding process of the polymer material, are easy to prepare, can ensure that the polymer material has the characteristics of antibacterial property and light weight, and have wide application prospects in industries such as household appliances, automobiles and the like.
In still other embodiments of the present invention, a modified polymeric material is provided, the preparation feedstock comprising the antimicrobial material of the present invention.
It can be understood that the antibacterial material is used as the preparation raw material of the modified polymer material, so that the modified polymer material has the beneficial effects of the antibacterial material, in particular:
According to the modified polymer material, the antibacterial material is contained in the preparation raw material, the silver amine complex is arranged on the surfaces of the glass beads of the antibacterial material, the decomposition temperature of the silver amine complex can be distributed between 90 ℃ and 150 ℃ according to the difference of silver precursors and amine ligands, and the processing and forming temperature of the polymer material is well matched, so that the silver amine complex is heated and decomposed into nano silver particles in the processing and forming process of the polymer material, the nano silver particles are attached to the surfaces of the glass beads, the efficient sterilizing capability can be provided for the glass beads and the composite material prepared by taking the nano silver particles as the raw material, the efficient antibacterial effect can be exerted without adding a large amount, the cost is reduced, and the large-scale popularization and application are facilitated.
The modified polymer material is easy to prepare, can enable the polymer material to have the characteristics of light weight and antibiosis, and has wide application prospect in industries such as household appliances, automobiles and the like.
In some embodiments of the invention, the modified polymeric material comprises a modified plastic.
In some embodiments of the present invention, the modified polymeric material comprises a polymeric material matrix and antimicrobial microbeads dispersed in the polymeric material matrix, the antimicrobial microbeads being formed from the antimicrobial material of the present invention upon thermal decomposition.
In some embodiments of the invention, the addition amount of the antibacterial material in the modified polymer material is 1wt% to 10wt%.
In some embodiments of the invention, the modified polymeric material may be extruded in a twin screw extruder to pellet and then injection molded by an injection molding machine.
The temperature of each zone of the twin-screw extruder can be 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 1 min-3 min.
In still other embodiments of the present invention, there is provided a household appliance, the preparation raw material comprising the antibacterial material of the present invention.
It can be appreciated that the household appliance of the present invention has all the advantageous effects of the antibacterial material of the present invention due to the use of the antibacterial material of the present invention. Specifically, in the household appliance, the antibacterial microbeads are dispersed in the preparation raw materials, the antibacterial microbeads comprise a microbead matrix, and the nano silver particles are attached to the surface of the microbead matrix, so that the high-efficiency sterilization capability can be provided for the modified high-molecular material.
In some embodiments of the present invention, home appliances include refrigerators, washing machines, and air conditioners.
The technical solution of the present invention will be better understood by combining the following specific embodiments.
In the following examples and comparative examples, "parts" in the amounts of raw materials to be added, unless otherwise specified, refer to parts by mass.
Example 1
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
According to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Example 2
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
According to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 30 parts of silver organic source and 55 parts of ethanol are taken, stirred at a speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Example 3
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
According to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polystyrene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Example 4
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
According to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
10 parts of antibacterial glass beads, 85 parts of polypropylene and 5 parts of antioxidant 1010 are taken, extruded and granulated in a double-screw extruder, and then injection molded by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Example 5
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
And (3) taking silver oxalate and octylamine according to a molar ratio of 1:2, and stirring at room temperature to obtain the silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Example 6
The antibacterial material is prepared firstly, and comprises glass beads, and silver amine complexes are attached to the surfaces of the glass beads.
The specific preparation method comprises the following steps:
according to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, an antibacterial plastic was prepared in this example. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Comparative example 1
The comparative example first prepared an antibacterial material comprising glass beads with silver amine complexes attached to the surfaces.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
According to the molar ratio of 1:2, silver oxalate and 2-amino-2-methyl-1-propanol are taken and stirred at room temperature to obtain a silver organic source.
10 Parts of glass beads, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at a speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, this example prepared an antibacterial plastic containing nano silver. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
Comparative example 2
The comparative example first prepared an antibacterial material comprising glass beads with silver amine complexes attached to the surfaces.
The specific preparation method comprises the following steps:
Sequentially using acetone, 5% acetic acid aqueous solution and ethanol to ultrasonically clean the glass beads for 5min so as to remove impurities on the surfaces of the glass beads.
The silver organic source is silver oxalate.
10 Parts of glass beads, 5 parts of silane coupling agent KH550, 15 parts of silver organic source and 70 parts of ethanol are taken, stirred at the speed of 300rpm for 8 hours at 8 ℃, and then fully dried in an oven to obtain the antibacterial material.
The glass beads had a particle size of about 50. Mu.m.
Further, this example prepared an antibacterial plastic containing nano silver. The specific preparation method comprises the following steps:
Taking 5 parts of antibacterial material, 90 parts of polypropylene and 5 parts of antioxidant 1010, extruding and granulating in a double-screw extruder, and then performing injection molding by an injection molding machine.
The temperature of each zone of the twin-screw extruder is 180-210 ℃ in the first zone, 200-230 ℃ in the second zone, 200-220 ℃ in the third zone, 220-220 ℃ in the fourth zone and 190-220 ℃ in the fifth zone, and the residence time is 2min.
The antibacterial performance detection in the invention is carried out according to the standard QB/T2591-2003 antibacterial performance test method of antibacterial plastics. The antibacterial plastics prepared in examples and comparative examples were tested and the test results are shown in table 1.
TABLE 1
As can be seen from the results of table 1, after the glass beads were pretreated, the silver amine complex was more sufficiently adhered, and the number of nano silver adhered to the surfaces of the glass beads was more, and the antibacterial performance was better.
The glass beads of comparative example 1 were not surface-modified with the coupling agent, and the interfacial compatibility between the glass beads and the resin was poor, resulting in insufficient dispersion of the glass beads in the product and a decrease in antibacterial property.
In comparative example 2, it is difficult for the silver precursor alone to adhere to the glass beads and to be added to the resin with the glass beads, compared with the silver amine complex. Meanwhile, the decomposition of the silver precursor is uncontrolled, the nano silver particle size generated by the decomposition of the silver amine complex is smaller, and the antibacterial performance is reduced.
In still other embodiments of the present invention, the present invention provides a household appliance, the manufacturing raw materials comprising the antibacterial material of the present invention.
It can be understood that the antibacterial material is used for preparing raw materials of the household appliances such as refrigerators, washing machines and air conditioners, and has good antibacterial effect on the whole or special parts of the refrigerators, the washing machines and the air conditioners, can inhibit the growth of bacteria in the refrigerators and reduce the odor of the refrigerators, can inhibit the growth of bacteria and the adhesion of dirt in the washing machines, and has antibacterial effect on the air conditioners. The user's experience with the household appliances using the antibacterial material of the present invention can be further enhanced.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (17)
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