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EP1838463B2 - Procede de calibrage d'une resine particulaire hydroabsorbante - Google Patents
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EP1838463B2 - Procede de calibrage d'une resine particulaire hydroabsorbante - Google Patents

Procede de calibrage d'une resine particulaire hydroabsorbante Download PDF

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Publication number
EP1838463B2
EP1838463B2 EP05821876.9A EP05821876A EP1838463B2 EP 1838463 B2 EP1838463 B2 EP 1838463B2 EP 05821876 A EP05821876 A EP 05821876A EP 1838463 B2 EP1838463 B2 EP 1838463B2
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EP
European Patent Office
Prior art keywords
process according
sieving apparatus
temperature
range
gas stream
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP05821876.9A
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German (de)
English (en)
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EP1838463B1 (fr
EP1838463A1 (fr
Inventor
Matthias Weismantel
Rüdiger Funk
Thomas Daniel
Uwe Stueven
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BASF SE
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BASF SE
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/46—Constructional details of screens in general; Cleaning or heating of screens
    • B07B1/56—Heated screens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/28—Moving screens not otherwise provided for, e.g. swinging, reciprocating, rocking, tilting or wobbling screens
    • B07B1/40—Resonant vibration screens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/46—Constructional details of screens in general; Cleaning or heating of screens

Definitions

  • the present invention relates to a method for classifying a particulate water-absorbent resin by means of a sieving apparatus at a pressure reduced from the ambient pressure.
  • Water-absorbent resins typically have a centrifuge retention capacity of 15 to 60 g / g, preferably at least 20 g / g, preferably at least 25 g / g, more preferably at least 30 g / g, most preferably at least 35 g / g.
  • Centrifuge retention capacity is determined according to the EDANA (European Disposables and Nonwovens Association) recommended test method no. 441.2-02 "Centrifuge retention capacity".
  • the preparation of water-absorbing resins usually comprises the steps of polymerization, drying, comminution, classification, postcrosslinking and, if appropriate, renewed classification.
  • the object of the present invention was to find a simplified method for the classification of water-absorbing resins, which allows high screening performance and long equipment runtimes.
  • this object is achieved by classifying water-absorbing resins at reduced pressure relative to the ambient pressure, preferably at a pressure of at most 950 mbar, preferably at a pressure of at most 900 mbar, particularly preferably at a pressure of at most 800 mbar preferably at a pressure of at most 700 mbar, wherein the resin is overflown during the classifying with a gas, and wherein the gas flow in front of the screening device has a temperature of at least 40 ° C.
  • the pressure is usually at least 10 mbar, preferably at least 50 mbar, preferably at least 100 mbar, more preferably at least 200 mbar, most preferably at least 300 mbar.
  • Another aspect of the present invention is the screening device for carrying out the classification method according to the invention.
  • the screening devices which are suitable for the classification method according to the invention are not subject to any restrictions; plane sieve methods are preferred, tumble screening machines are very particularly preferred.
  • the screening device is typically shaken to aid classification. This is preferably done so that the material to be classified is spirally guided over the sieve.
  • This forced vibration typically has an amplitude of 0.7 to 40 mm, preferably 1.5 to 25 mm, and a frequency of 1 to 100 Hz, preferably of 5 to 10 Hz.
  • the water-absorbent resin is overflowed during the classifying with a gas stream, particularly preferably air.
  • the amount of gas is typically from 0.1 to 10 m 3 / h per m 2 screen area, preferably from 0.5 to 5 m 3 / h per m 2 screen area, particularly preferably from 1 to 3 m 3 / h per m 2 screen area, the gas volume being measured under standard conditions (25 ° C and 1 bar).
  • the gas stream is before entering the screening device to a temperature of at least 40 ° C, preferably to a temperature of at least 50 ° C, preferably to a temperature of at least 60 ° C, more preferably to a temperature of at least 65 ° C, all more preferably at a temperature of at least 70 ° C.
  • the temperature of the gas stream is usually less than 120 ° C, preferably less than 110 ° C, preferably less than 100 ° C, more preferably less than 90 ° C, most preferably less than 80 ° C.
  • the water content of the gas stream is typically not more than 5 g / kg, preferably not more than 4.5 g / kg, preferably not more than 4 g / kg, more preferably not more than 3.5 g / kg, most preferably not more than 3 g / kg.
  • a gas stream with a low water content can be generated, for example, by condensing a corresponding amount of water from the gas stream having a higher water content by cooling.
  • the screening device can still be heated and / or thermally insulated, such as in EP-A-0 855 232 described.
  • the screening device is operated at a temperature of 40 to 80 ° C.
  • Suitable monomers i) are, for example, ethylenically unsaturated carboxylic acids, such as acrylic acid, methacrylic acid, maleic acid, fumaric acid and itaconic acid, or derivatives thereof, such as acrylamide, methacrylamide, acrylic esters and methacrylic acid esters. Particularly preferred monomers are acrylic acid and methacrylic acid. Very particular preference is given to acrylic acid.
  • Preferred hydroquinone half ethers are hydroquinone monomethyl ether (MEHQ) and / or tocopherols.
  • Tocopherol is understood as meaning compounds of the following formula wherein R 1 is hydrogen or methyl, R 2 is hydrogen or methyl, R 3 is hydrogen or methyl and R 4 is hydrogen or an acid radical having 1 to 20 carbon atoms.
  • Preferred radicals for R 4 are acetyl, ascorbyl, succinyl, nicotinyl and other physiologically acceptable carboxylic acids.
  • the carboxylic acids may be mono-, di- or tricarboxylic acids.
  • R 4 is particularly preferably hydrogen or acetyl. Especially preferred is RRR-alpha-tocopherol.
  • the monomer solution preferably contains at most 130 ppm by weight, more preferably at most 70 ppm by weight, preferably at least 10 ppm by weight, more preferably at least 30 ppm by weight, particularly preferably around 50 ppm by weight, hydroquinone hemether, in each case on acrylic acid, wherein acrylic acid salts are mathematically taken into account as acrylic acid.
  • an acrylic acid having a corresponding content of hydroquinone half-ether may be used to prepare the monomer solution.
  • the water-absorbing polymers are crosslinked, ie the polymerization is carried out in the presence of compounds having at least two polymerisable groups which can be radically copolymerized into the polymer network.
  • Suitable crosslinkers ii) are, for example, ethylene glycol dimethacrylate, diethylene glycol diacrylate, allyl methacrylate, trimethylolpropane triacrylate, triallylamine, tetraallyloxyethane, as in EP-A-0 530 438 described, di- and triacrylates, as in EP-A-0 547 847 . EP-A-0 559 476 . EP-A-0 632 068 . WO-A-93/21237 .
  • WO-A-03/104299 WO-A-03/104300 .
  • WO-A-03/104301 and in the German patent application with the file number 10331450.4 described, mixed acrylates containing in addition to acrylate groups further ethylenically unsaturated groups, as in the German patent applications with the file reference 10331456.3 and 10355401.7 or crosslinker mixtures, such as in DE-A-195 43 368 .
  • DE-A-196 46 484 WO 90/15830 and WO-A-02/32962 described.
  • Suitable crosslinkers ii) are, in particular, N, N'-methylenebisacrylamide and N, N'-methylenebismethacrylamide, esters of unsaturated monocarboxylic or polycarboxylic acids of polyols, such as diacrylate or triacrylate, for example butanediol or ethylene glycol diacrylate or methacrylate, and trimethylolpropane triacrylate and allyl compounds, such as allyl (meth) acrylate, triallyl cyanurate, maleic acid diallyl esters, polyallyl esters, tetraallyloxyethane, triallylamine, tetraallylethylenediamine, allyl esters of phosphoric acid and vinylphosphonic acid derivatives, as described, for example, in US Pat EP-A-0 343 427 are described.
  • crosslinkers ii) are pentaerythritol di-, pentaerythritol tri- and pentaerythritol tetraallyl ethers, polyethylene glycol diallyl ether, ethylene glycol diallyl ether, glycerol and glycerol triallyl ethers, polyallyl ethers based on sorbitol, and ethoxylated variants thereof.
  • Useful in the process according to the invention are di (meth) acrylates of polyethylene glycols, wherein the polyethylene glycol used has a molecular weight between 300 and 1000.
  • crosslinkers ii) are di- and triacrylates of 3 to 20 times ethoxylated glycerol, 3 to 20 times ethoxylated trimethylolpropane, 3 to 20 times ethoxylated trimethylolethane, especially di- and triacrylates of 2 to 6-fold ethoxylated glycerol or trimethylolpropane, 3-fold propoxylated glycerin or trimethylolpropane, as well as the 3-times mixed ethoxylated or propoxylated glycerol or trimethylolpropane, the 15-fold ethoxylated glycerol or trimethylolpropane, and at least 40-times ethoxylated glycerol, trimethylolethane or trimethylolpropane.
  • Very particularly preferred crosslinkers ii) are the polyethoxylated and / or propoxylated glycerols esterified with acrylic acid or methacrylic acid to form di- or triacrylates, as described, for example, in the earlier German application with file reference DE 10319462.2 are described.
  • Particularly advantageous are di- and / or triacrylates of 3- to 10-fold ethoxylated glycerol.
  • Most preferred are the triacrylates of 3 to 5 times ethoxylated and / or propoxylated glycerin.
  • acrylamide, methacrylamide, crotonic acid amide, dimethylaminoethyl methacrylate, dimethylaminoethyl acrylate, dimethylaminopropyl acrylate, diethylaminopropyl acrylate, dimethylaminobutyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, dimethylaminoneopentyl acrylate, and dimethylaminoneopentyl methacrylate are exemplified by ethylenically unsaturated monomers iii) copolymerizable with monomers i).
  • water-soluble polymers iv) it is possible to use polyvinyl alcohol, polyvinylpyrrolidone, starch, starch derivatives, polyglycols or polyacrylic acids, preferably polyvinyl alcohol and starch.
  • the reaction is preferably carried out in a kneader, such as in WO-A-01/38402 described, or on a belt reactor, such as in EP-A-0 955 086 described, performed.
  • the acid groups of the hydrogels obtained are usually partially neutralized, preferably from 25 to 95 mol%, preferably from 27 to 80 mol%, particularly preferably from 27 to 30 mol% or from 40 to 75 mol%, using the usual neutralizing agents may, preferably alkali metal hydroxides, alkali metal oxides, alkali metal carbonates or alkali metal hydrogencarbonates and mixtures thereof. Instead of alkali metal salts and ammonium salts can be used. Sodium and potassium are particularly preferred as alkali metals, but most preferred are sodium hydroxide, sodium carbonate or sodium bicarbonate and mixtures thereof.
  • the neutralization is achieved by mixing the neutralizing agent as an aqueous solution, as a melt, or preferably as a solid.
  • sodium hydroxide with a water content well below 50 wt .-% may be present as a waxy mass with a melting point above 23 ° C. In this case, a dosage as general cargo or melt at elevated temperature is possible.
  • the neutralization can be carried out after the polymerization at the hydrogel stage. However, it is also possible to neutralize up to 40 mol%, preferably 10 to 30 mol%, particularly preferably 15 to 25 mol%, of the acid groups before the polymerization by adding a part of the neutralizing agent already to the monomer solution and the desired final degree of neutralization only after the polymerization is adjusted at the level of the hydrogel.
  • the monomer solution can be neutralized by mixing in the neutralizing agent.
  • the hydrogel can be mechanically comminuted, for example by means of a meat grinder, wherein the neutralizing agent can be sprayed, sprinkled or poured over and then thoroughly mixed. For this purpose, the gel mass obtained can be further gewolfft for homogenization. Neutralization of the monomer solution directly to the final degree of neutralization is preferred.
  • the neutralized hydrogel is then dried with a belt or drum dryer until the residual moisture content is preferably below 15 wt .-%, in particular below 10 wt .-%, wherein the water content according to the recommended by the EDANA (European Disposables and Nonwovens Association) Test Method no 430.2-02 "Moisture content" is determined.
  • a fluidized bed dryer or a heated ploughshare mixer can be used for drying.
  • it is advantageous in the drying of this gel to ensure rapid removal of the evaporating water.
  • the dryer temperature must be optimized, the air supply and removal must be controlled, and it is in any case to ensure adequate ventilation.
  • the drying is naturally simpler and the product is the whiter, if the solids content of the gel is as high as possible.
  • the solids content of the gel before drying is therefore preferably between 30 and 80% by weight.
  • Particularly advantageous is the ventilation of the dryer with nitrogen or other non-oxidizing inert gas.
  • nitrogen or other non-oxidizing inert gas it is also possible simply to lower only the partial pressure of the oxygen during the drying in order to prevent oxidative yellowing processes.
  • sufficient ventilation and removal of the water vapor also leads to an acceptable product.
  • Advantageous in terms of color and product quality is usually the shortest possible drying time.
  • the dried hydrogel is thereafter ground and classified, wherein for grinding usually one- or multi-stage roller mills, preferably two- or three-stage roller mills, pin mills, hammer mills or vibratory mills can be used.
  • water-absorbent polymer particles are generally postcrosslinked. This postcrosslinking can be carried out in aqueous gel phase.
  • ground and sieved polymer particles base polymer
  • crosslinkers suitable for this purpose are compounds which contain at least two groups which can form covalent bonds with the carboxylate groups of the hydrophilic polymer or which can crosslink at least two carboxyl groups or other functional groups of at least two different polymer chains of the base polymer.
  • Suitable postcrosslinkers v) are compounds which contain at least two groups which can form covalent bonds with the carboxylate groups of the polymers.
  • Suitable compounds are, for example, alkoxysilyl compounds, polyaziridines, polyamines, polyamidoamines, di- or polyglycidyl compounds, as in EP-A-0 083 022 .
  • EP-A-543,303 and EP-A-937 736 described polyhydric alcohols, as in DE-C-33 14 019 .
  • mixed functionality such as glycidol, 3-ethyl-3-oxetanemethanol (trimethylolpropane oxetane), as in EP-A-1 199 327 described, aminoethanol, diethanolamine, triethanolamine or compounds which form a further functionality after the first reaction, such as ethylene oxide, propylene oxide, isobutylene oxide, aziridine, azetidine or oxetane.
  • the post-crosslinking is usually carried out so that a solution of the postcrosslinker is sprayed onto the hydrogel or the dry base polymer particles. Subsequent to the spraying, it is thermally dried, whereby the postcrosslinking reaction can take place both before and during the drying.
  • the spraying of a solution of the crosslinker is preferably carried out in mixers with agitated mixing tools, such as screw mixers, paddle mixers, disk mixers, plowshare mixers and paddle mixers.
  • agitated mixing tools such as screw mixers, paddle mixers, disk mixers, plowshare mixers and paddle mixers.
  • Vertical mixers are particularly preferred, plowshare mixers and paddle mixers are very particularly preferred.
  • Suitable mixers are, for example, Lödige® mixers, Bepex® mixers, Nauta® mixers, Processall® mixers and Schugi® mixers.
  • the thermal drying is preferably carried out in contact dryers, more preferably paddle dryers, very particularly preferably disk dryers.
  • Suitable dryers include Bepex® dryers and, Nara® dryers.
  • fluidized bed dryers can also be used.
  • the drying can take place in the mixer itself, by heating the jacket or blowing hot air. Also suitable is a downstream dryer, such as a hopper dryer, a rotary kiln or a heatable screw. However, it is also possible, for example, to use an azeotropic distillation as the drying process.
  • Preferred drying temperatures are in the range 50 to 250 ° C, preferably at 50 to 200 ° C, and particularly preferably at 50 to 150 ° C.
  • the preferred residence time at this temperature in the reaction mixer or dryer is less than 30 minutes, more preferably less than 10 minutes.
  • the classification method according to the invention is preferably carried out after the drying of the base polymer, before the post-crosslinking and / or after the post-crosslinking.
  • the water content of the water-absorbing resin after drying of the base polymer or before post-crosslinking is typically from 2 to 10% by weight and after post-crosslinking typically below 1% by weight, preferably below 0.1% by weight.
  • the temperature of the heating mantle was adjusted to the reaction temperature in the reactor by means of control.
  • the crumbly gel finally obtained was then dried at 160 ° C for 3 hours in a convection oven. It was then ground and sieved to 250 to 850 microns.
  • the water content was 2.7% by weight.
  • the ground base polymer was added to the sieve at the indicated temperature.
  • the sieve could be operated at reduced pressure.
  • the screen was covered with preheated air with defined water vapor content. The amount of air was 2 m 3 / h per m 2 screen area.

Landscapes

  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Combined Means For Separation Of Solids (AREA)
  • Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)

Claims (14)

  1. Procédé pour la classification d'une résine particulaire absorbant l'eau au moyen d'un dispositif de tamisage, caractérisé en ce que le dispositif de tamisage est exploité à une pression diminuée par rapport à la pression environnante et la résine est submergée par un gaz pendant la classification, le flux de gaz étant chauffé à une température d'au moins 40°C avant l'entrée dans le dispositif de tamisage.
  2. Procédé selon la revendication 1, caractérisé en ce que le dispositif de tamisage est exploité à une pression d'au plus 950 mbars.
  3. Procédé selon la revendication 2, caractérisé en ce que le dispositif de tamisage est exploité à une pression de 300 à 700 mbars.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que la quantité de gaz est de 0,1 à 10 m3/h par m2 de surface de tamisage.
  5. Procédé selon la revendication 4, caractérisé en ce que le flux de gaz est de l'air.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que le flux de gaz présente une température de 40 à 120°C.
  7. Procédé selon l'une quelconque des revendications 4 à 6, caractérisé en ce que la teneur en eau du flux de gaz est inférieure à 5 g/kg.
  8. Procédé selon l'une quelconque des revendications 4 à 7, caractérisé en ce que le flux volumique de gaz est de 1 à 10 m3/h par m2 de surface de tamisage, le volume de gaz étant mesuré à une température de 25°C et une pression de 1 bar.
  9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce que le dispositif de tamisage est au moins partiellement isolé thermiquement.
  10. Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que la température du dispositif de tamisage est de 40 à 80°C.
  11. Procédé selon l'une quelconque des revendications 1 à 10, caractérisé en ce que le dispositif de tamisage vibre.
  12. Procédé selon la revendication 11, caractérisé en ce que la fréquence de vibration est de 1 à 100 Hz.
  13. Procédé selon l'une quelconque des revendications 1 à 12, caractérisé en ce que la résine particulaire absorbant l'eau est obtenue par polymérisation d'une solution contenant de l'acide acrylique et/ou méthacrylique.
  14. Procédé selon la revendication 13, caractérisé en ce que l'acide acrylique et/ou méthacrylique est neutralisé à raison d'au moins 40%.
EP05821876.9A 2005-01-13 2005-12-31 Procede de calibrage d'une resine particulaire hydroabsorbante Expired - Lifetime EP1838463B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005001789A DE102005001789A1 (de) 2005-01-13 2005-01-13 Verfahren zum Klassieren eines teilchenförmigen wasserabsorbierenden Harzes
PCT/EP2005/014163 WO2006074816A1 (fr) 2005-01-13 2005-12-31 Procede de calibrage d'une resine particulaire hydroabsorbante

Publications (3)

Publication Number Publication Date
EP1838463A1 EP1838463A1 (fr) 2007-10-03
EP1838463B1 EP1838463B1 (fr) 2011-06-22
EP1838463B2 true EP1838463B2 (fr) 2019-08-14

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EP05821876.9A Expired - Lifetime EP1838463B2 (fr) 2005-01-13 2005-12-31 Procede de calibrage d'une resine particulaire hydroabsorbante

Country Status (8)

Country Link
US (1) US8104621B2 (fr)
EP (1) EP1838463B2 (fr)
JP (1) JP2008526498A (fr)
CN (1) CN101102854B (fr)
AT (1) ATE513627T1 (fr)
DE (1) DE102005001789A1 (fr)
TW (1) TW200631676A (fr)
WO (1) WO2006074816A1 (fr)

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US10537874B2 (en) 2015-04-02 2020-01-21 Nippon Shokubai Co., Ltd. Method for producing particulate water-absorbing agent
EP3464427B1 (fr) 2016-05-31 2021-01-06 Basf Se Procédé de fabrication de superabsorbants
EP3661662B1 (fr) * 2017-07-31 2024-09-11 Basf Se Procédé de production de particules de polymère superabsorbant

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JPH06126252A (ja) † 1992-10-16 1994-05-10 Ube Ind Ltd フライアッシュの品質改善方法
EP0780424A1 (fr) † 1995-07-07 1997-06-25 Nippon Shokubai Co., Ltd. Poudre absorbant l'eau et son procede de fabrication
JPH11179187A (ja) † 1997-12-24 1999-07-06 Terunaito:Kk 分散機構付き粉体供給機並びにそれを用いた高分子水溶液の調製方法及び廃水または高含水泥土の処理方法
WO2000010619A1 (fr) † 1998-08-18 2000-03-02 Stockhausen Gmbh & Co. Kg Polymeres superabsorbants dotes de caracteristiques anti-agglomeration
EP1178059A2 (fr) † 2000-08-03 2002-02-06 Nippon Shokubai Co., Ltd. Résine absorbant de l'eau, hydropolymère, procédé de sa préparation et son usage:
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EP1462473A1 (fr) † 2003-03-14 2004-09-29 Nippon Shokubai Co., Ltd. Procédé pour la réticulation de la surface d'une poudre de résine absorbantl'eau

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EP1838463B1 (fr) 2011-06-22
JP2008526498A (ja) 2008-07-24
CN101102854A (zh) 2008-01-09
US20080202987A1 (en) 2008-08-28
WO2006074816A1 (fr) 2006-07-20
EP1838463A1 (fr) 2007-10-03
CN101102854B (zh) 2013-04-17
TW200631676A (en) 2006-09-16
US8104621B2 (en) 2012-01-31
DE102005001789A1 (de) 2006-07-27
ATE513627T1 (de) 2011-07-15

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