JP7422252B2 - High elasticity nylon and its manufacturing method - Google Patents

Description

The present invention relates to the technical field of nylon elastomer modification methods, and particularly to high modulus nylon and its manufacturing method.

Nylon elastomer (PEBAX) is a block polyamide elastomer product and belongs to engineering polymers. The product not only has a fairly wide hardness range and good impact resilience, but also its outstanding processing performance makes it an ideal material for component production.

Nylon elastomer also has excellent chemical resistance, heat resistance, and weather resistance, and is widely applied in fields such as exercise equipment, impact-resistant parts, and watch cases. However, conventional nylon elastomers have a low compression set rate and are difficult to recover to their original state after being compressed and deformed.

In the prior art, the conventional nylon elastomer has a low compression set rate and is difficult to recover to its original state after being compressed and deformed, which is a technical problem. provide a method. The specific technical solutions are as follows.

In a first aspect, an embodiment of the invention comprises:
obtaining nylon, polyborosiloxane, and polyethylene glycol, and drying the polyborosiloxane;
The nylon, the polyborosiloxane, and the polyethylene glycol are placed in a predetermined device and heated to mix uniformly to obtain a first mixed material;
Obtaining cyclopentane, and heating and kneading the cyclopentane and the mixed material in an internal mixer to obtain a second mixed material;
Forming the second mixed material into a sheet and placing the sheet in a granulator to granulate it to obtain particulate matter;
foaming the particulate material to obtain high modulus nylon;
The mass ratio of the nylon and the polyborosiloxane is 10 to 100:1, the mass of the polyethylene glycol is 10% of the mass of the polyborosiloxane, the heating temperature is 150 to 180°C, and the heating time is is 3 to 5 min, the mass of the cyclopentane is 5 to 10% of the mass of the first mixed material, the kneading temperature is 150 to 180 ° C., and the kneading time is 7 to 10 min. The present invention provides a method for producing high elastic nylon, in which the foaming temperature is 160-180°C, the foaming time is 5-7 min, and the foaming pressure is 140-160 kg/cm ² .

Optionally, the thickness of said sheet is 10mm.

Optionally, said predetermined device is an extruder.

Optionally, the extruder is a twin screw extruder or a single screw extruder.

In a second aspect, embodiments of the present invention provide high modulus nylon produced by the method for producing high modulus nylon.

The embodiment of the present invention includes the steps of obtaining nylon, polyborosiloxane, and polyethylene glycol, drying the polyborosiloxane, and heating and uniformly mixing the nylon, polyborosiloxane, and polyethylene glycol in a predetermined device. , a step of obtaining a first mixed material, a step of obtaining cyclopentane, and a step of heating and kneading the cyclopentane and the mixed material in an internal mixer to obtain a second mixed material; A method of producing high modulus nylon, comprising: forming a mixed material into a sheet, placing the sheet in a granulator to granulate it to obtain particulate matter, and foaming the particulate matter to obtain high modulus nylon. A manufacturing method is provided. By employing the high modulus nylon produced by the method provided by the embodiments of the present invention, boron in polyborosiloxane can form physical and chemical crosslinks through strong interaction with oxygen, and Compared to nylon elastomer, the permanent compression strain rate has been significantly improved.

In order to more clearly explain the technical solutions in the embodiments of the present invention or the prior art, the drawings necessary for explaining the embodiments or the prior art will be briefly introduced below.
1 is a flowchart of a method for manufacturing high modulus nylon provided by an embodiment of the present invention.

Hereinafter, technical solutions in embodiments of the present invention will be described with reference to the drawings in the embodiments of the present invention.

<Example 1>
Referring to FIG. 1, in a first aspect, an embodiment of the present invention provides a method of manufacturing high modulus nylon comprising the following steps.

Obtain nylon, polyborosiloxane, and polyethylene glycol, and dry the polyborosiloxane. The mass ratio of the nylon to the polyborosiloxane is 10 to 100:1, and the mass of the polyethylene glycol is 10% of the mass of the polyborosiloxane.

Note that the above nylon, polyborosiloxane, and polyethylene glycol can all be purchased directly, and the examples of the present invention do not specifically limit the purity and content of each of the above components, but the effective content of each component. It is necessary to ensure that the amount satisfies the criteria that the mass ratio of nylon and polyborosiloxane is 10 to 100:1 and the mass of polyethylene glycol is 10% of the mass of polyborosiloxane. be.

The nylon, the polyborosiloxane, and the polyethylene glycol are placed in a predetermined device, heated, and mixed uniformly to obtain a first mixed material. The heating temperature is 150 to 180°C, and the heating time is 3 to 5 minutes.

The above-mentioned predetermined device may be any device capable of heating and lasting for a predetermined period of time, or may be a heating device. , the next step of manufacturing can be performed directly without cooling, and of course the next step may be performed after self-cooling.

While obtaining cyclopentane, the cyclopentane and the mixed material are placed in an internal mixer and heated and kneaded to obtain a second mixed material. The mass of the cyclopentane is 5 to 10% of the mass of the first mixed material, the kneading temperature is 150 to 180° C., and the kneading time is 7 to 10 min.

When the internal mixer operates, the two rotors rotate relative to each other, and the material from the loading port is sandwiched and brought into the roll gap, where it is pressed and sheared by the rotor, and after passing through the roll gap, it is dropped. It splits into two parts against the sharp edge of the door and returns again above the roll gap along the cap between the front and rear chamber walls and the rotor. During one revolution around the rotor, the material is constantly subjected to shear and frictional effects, which rapidly increases the temperature of the rubber compound, reduces its viscosity, increases the wettability of the rubber on the surface of the compound, and causes the gum to Enough contact with the surface of the formulation. The compound mass passes through the gap between the rotors, the rotor and the floating weight, the drop door, and the inner wall of the kneading chamber together with the rubber compound, is sheared and crushed, is surrounded by the tensile deformed rubber, and is in a crushed state. It is stable. At the same time, the ribs on the rotor move the rubber compound in the axial direction of the rotor to perform the stirring and mixing action, and the ingredients are mixed uniformly in the rubber compound. By repeatedly shearing and pulverizing the compounding agent in this way, the rubber compound is repeatedly deformed and recovered, and the continuous stirring by the rotor ribs ensures that the compounding agent is evenly dispersed in the rubber compound and has a constant The degree of dispersion is reached. The shearing action on the rubber compound during kneading with an internal mixer is much greater than that with an open mixer, and the rubber kneading temperature is higher, so the efficiency of rubber kneading with an internal mixer is significantly higher than that with an open mixer. Specifically, in this example, cyclopentane and the first mixture are added to the charging port of an internal mixer, and the second mixture is obtained after the above processing process is performed using the internal mixer.

The second mixed material is made into a sheet, and the sheet is put into a granulator and granulated to obtain particulate matter.

In addition, as a method of forming the second mixed material into a sheet, it may be pressed by a hydraulic machine, it may be crushed by a crushing column, or it may be manufactured by other devices or methods that can crush the object into a sheet. , the above-mentioned granulator is a forming machine that can manufacture materials into a specific shape. By adopting a special screw design, a different arrangement, and a high-torque design for the reduction case, we have achieved characteristics such as noiseless and stable operation. The screw and barrel undergo a special hardening process to withstand wear, have excellent kneading properties, and have the characteristics of high yield, and are vacuum-exhausted or with a general exhaust port design to prevent moisture and moisture during production. The exhaust gas could be discharged, making the material discharge more stable, making the rubber particles stronger, and ensuring the good quality of the products. Plasticization and molding of plastics is achieved by changing the physical properties of plastics during the process of high temperature melting, plasticization, and extrusion.

The particulate material is foamed to obtain high modulus nylon. The foaming temperature is 160-180°C, the foaming time is 5-7 min, and the foaming pressure is 140-160 kg/cm ² .

The device used for the above foaming is a molding machine or a digester, and the basic steps of foam molding are formation of bubble nuclei, growth or expansion of the bubble nuclei, and stabilization of the bubble nuclei. Under conditions of predetermined temperature and pressure, the solubility of the gas decreases and reaches a saturation state, and excess gas is exhausted to form bubbles, thereby achieving the formation of bubble nuclei. Specifically, in the present application, the foaming temperature is 160 to 180°C, the foaming time is 5 to 7 minutes, and the foaming pressure is 140 to 160 kg/cm ² .

Further, the thickness of the sheet is 10 mm.

Further, the predetermined device is an extruder.

Furthermore, the extruder is a twin-screw extruder or a single-screw extruder.

Note that the screw extruder can sufficiently plasticize and uniformly mix the materials using the pressure and shear force generated by the rotation of the screw, and then mold the materials through the die. Specifically, in the present application, nylon, polyborosiloxane, and polyethylene glycol in predetermined proportions are put into the charging port of an extruder, and the above three types of materials are uniformly mixed through processing by the extruder to form a first mixed material. A mixed material is obtained.

In a second aspect, embodiments of the present invention provide high modulus nylon produced by the above-described method for producing high modulus nylon.

The embodiment of the present invention includes the steps of obtaining nylon, polyborosiloxane, and polyethylene glycol, drying the polyborosiloxane, and heating and uniformly mixing the nylon, polyborosiloxane, and polyethylene glycol in a predetermined device. , a step of obtaining a first mixed material, a step of obtaining cyclopentane, and a step of heating and kneading the cyclopentane and the mixed material in an internal mixer to obtain a second mixed material; A method of producing high modulus nylon, comprising: forming a mixed material into a sheet, placing the sheet in a granulator to granulate it to obtain particulate matter, and foaming the particulate matter to obtain high modulus nylon. A manufacturing method is provided. The high modulus nylon produced by the method provided by the embodiments of the present invention has significantly improved permanent compression set compared to conventional nylon elastomers.

<Example 2>
Based on the above-mentioned Example 1, the embodiments of the present invention further explain the present invention through specific examples.

In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 150° C., the time was 5 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:5 and heated and kneaded. The training time was 10 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed at a foaming temperature of 160° C., a foaming time of 5 min, and a pressure of 160 kg/cm ² to obtain high modulus nylon.

<Example 3>
In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 180° C., the time was 3 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:10 and heated and kneaded. The training time was 7 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed at a foaming temperature of 180° C., a foaming time of 7 min, and a pressure of 140 kg/cm ² to obtain high elastic nylon.

<Example 4>
In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 150° C., the time was 5 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:5 and heated and kneaded. The training time was 7 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed at a foaming temperature of 170° C., a foaming time of 7 min, and a pressure of 140 kg/cm ² to obtain high modulus nylon.

<Example 5>
In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 180° C., the time was 3 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:10 and heated and kneaded. The training time was 8 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed at a foaming temperature of 180° C., a foaming time of 6 min, and a pressure of 140 kg/cm ² to obtain high elastic nylon.

<Example 6>
In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 150° C., the time was 5 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:5 and heated and kneaded. The training time was 7 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed at a foaming temperature of 170° C., a foaming time of 6 min, and a pressure of 150 kg/cm ² to obtain high modulus nylon.

<Example 7>
In step 1, nylon, polyborosiloxane (PBDMS) was dried and added to the extruder in a 10:1 mass ratio, and 10% of the total mass of polyethylene glycol-400 was added to the extruder, and the heating module of the extruder was The temperature was 150° C., the time was 5 min, and the various materials were mixed uniformly.

In step 2, the material obtained in step 1 and cyclopentane, which is a blowing agent, are put into an internal mixer at a mass ratio of 100:5 and heated and kneaded. The training time was 7 min.

In step 3, the material obtained in step 2 was formed into a 10 mm sheet.

In step 4, the sheet obtained in step 3 was fed into a granulator and granulated.

In step 5, the material obtained in step 4 was foamed, the foaming temperature was 180° C., the foaming time was 5 min, and the pressure was 150 kg/cm ² .

<Test example>
A compression set test was performed on Examples 2 and 3 and the control example, and the test method was to compress and deform by 10% in an environment at a temperature of 70 ° C, and after processing for 24 hours, calculate the compression set rate CS. , CS is calculated as follows.
CS=(h0-h2)/(h0-h1)
In the formula, h0 is the height of the sample before compression/mm, h1 is the height of compression deformation/mm, and h2 is the height of the sample after recovery/mm.

The manufacturing method of the control example is as follows.

In step 1, nylon, polyethylene glycol-400, and cyclopentane were put into an internal mixer at a mass ratio of 100:10:5, heated and kneaded, and the heating temperature was 150°C and the kneading time was It was 10 minutes.

In step 2, the material obtained in step 1 was formed into a 10 mm sheet.

In step 3, the sheet obtained in step 2 was fed into a granulator and granulated.

In step 4, the material obtained in step 3 was foamed, with a foaming temperature of 160° C., a foaming time of 5 min, and a pressure of 160 kg/cm ² .

The test results are as follows.

As can be seen from the test results, the compression set ratio CS of Examples 2 and 3 was improved by 16.7% and 25%, respectively, compared to the control example, and the permanent compression of nylon elastomer was improved by the method of this patent. This shows that the distortion rate can be clearly improved.

Note that in this specification, related terms such as first and second are used only to distinguish one entity or operation from another entity or operation, and are used to distinguish between any of these entities or operations. They do not necessarily require or imply that any actual relationship or order exists. Also, the terms "comprises," "includes," or any other variations thereof are intended to cover non-exclusive inclusion, whereby a process, method, article, or apparatus that includes a set of elements is , including those elements, but may also include other elements not explicitly recited or may further include elements inherent in such process, method, article or apparatus. Unless further limited, an element qualified by the phrase "comprising a" does not exclude the presence of additional identical elements in a process, method, article, or apparatus that includes said element. .

Each of the embodiments herein will be described in a related manner, the same or similar parts of each embodiment may be referred to with each other, and the differences between each embodiment and other embodiments will be described. This was explained as an important point. In particular, although the system embodiments have been briefly described because they are substantially similar to the method embodiments, relevant portions may refer to portions of the description of the method embodiments.

The above are only preferred embodiments of the present invention, and do not limit the protection scope of the present invention. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention shall all fall within the protection scope of the present invention.

Claims (5)

obtaining nylon, polyborosiloxane, and polyethylene glycol, and drying the polyborosiloxane;
The nylon, the polyborosiloxane, and the polyethylene glycol are placed in a predetermined device and heated to mix uniformly to obtain a first mixed material;
Obtaining cyclopentane, and heating and kneading the cyclopentane and the mixed material in an internal mixer to obtain a second mixed material;
Forming the second mixed material into a sheet and placing the sheet in a granulator to granulate it to obtain particulate matter;
foaming the particulate material to obtain high modulus nylon;
The mass ratio of the nylon and the polyborosiloxane is 10 to 100:1, the mass of the polyethylene glycol is 10% of the mass of the polyborosiloxane, the heating temperature is 150 to 180°C, and the heating time is is 3 to 5 min, the mass of the cyclopentane is 5 to 10% of the mass of the first mixed material, the kneading temperature is 150 to 180 ° C., and the kneading time is 7 to 10 min. A method for producing high elastic nylon, characterized in that the foaming temperature is 160 to 180°C, the foaming time is 5 to 7 minutes, and the foaming pressure is 140 to 160 kg/cm ² . 2. The method of manufacturing high elastic nylon according to claim 1, wherein the sheet has a thickness of 10 mm. The method for producing high modulus nylon according to claim 1, wherein the predetermined device is an extruder. 4. The method for producing high modulus nylon according to claim 3, wherein the extruder is a twin-screw extruder or a single-screw extruder. High modulus nylon produced by the method for producing high modulus nylon according to any one of claims 1 to 4.