CN103613696A - Method for preparing super absorbent resin by using montmorillonite - Google Patents

Method for preparing super absorbent resin by using montmorillonite Download PDF

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Publication number
CN103613696A
CN103613696A CN201310579004.5A CN201310579004A CN103613696A CN 103613696 A CN103613696 A CN 103613696A CN 201310579004 A CN201310579004 A CN 201310579004A CN 103613696 A CN103613696 A CN 103613696A
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China
Prior art keywords
montmorillonite
absorbent resin
super absorbent
prepared
water
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CN201310579004.5A
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Inventor
洪锡全
杭渊
曹海斌
裴小苏
徐亮
潘伟
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YIXING DANSEN TECHNOLOGY CO LTD
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YIXING DANSEN TECHNOLOGY CO LTD
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Abstract

The invention discloses a method for preparing super absorbent resin by using montmorillonite. The method comprises the steps of preparing a neutralization solution and a montmorillonite turbid solution by using acrylic acid and montmorillonite as raw materials, adding a cross-linking agent and an initiating agent, and controlling temperature to realize a polymerization process; and drying and breaking to prepare the super absorbent resin. The super absorbent resin prepared by the method disclosed by the invention has the advantages of high water absorbing capacity, rapid water absorbing speed and high salt absorption multiplying power.

Description

Montmorillonite is prepared the method for super absorbent resin
Technical field
The present invention relates to a kind of preparation method of super absorbent resin, be specifically related to the method that montmorillonite is prepared super absorbent resin.
Background technology
Super absorbent resin is a kind of new functional macromolecule material with three-dimensional net structure, can absorb the hundreds of extremely deionized waters of thousands of times of own wt.For seeing in microtexture, its difference because of system presents diversity, the island type structure of starch graft acrylic acid, the acrylic acid honeycomb type structure of cellulose graft partial hydrolysis, its water-retaining capacity depends on the effect of repelling each other the ionic charge of polymer electrolyte in water the interaction of the stretching, extension causing and the prevention being caused by crosslinking structure and hydrogen bond expansion producing.
At present, in High hydrophilous resin, introducing inorganic component, to prepare inorganic/polymerization object height water suction compound resin be a kind of good developing direction, but due in the starting stage, relatively little to its research, prepared composite water absorbent resin is all relative on the low side aspect water regain, rate of water absorption and suction salt multiplying power.
Summary of the invention
The present invention is intended to overcome the deficiency that the problems referred to above exist, and provides that a kind of water regain is high, rate of water absorption is high, inhale the high composite high-water uptake resin of salt multiplying power.The technical scheme adopting is as follows:
Montmorillonite is prepared the method for super absorbent resin, it is characterized in that it is raw material that the method mainly be take vinylformic acid and montmorillonite, comprises following steps:
Figure 2013105790045100002DEST_PATH_IMAGE001
vinylformic acid is put into container cooling in ice-water bath, under agitation condition, slowly add aqueous sodium hydroxide solution neutralization, obtain neutralizer;
Figure 41043DEST_PATH_IMAGE002
get granularity≤220 object montmorillonite powder and pour in the container with agitator, add water and mix, after high speed dispersion 30min-50min, obtain polynite turbid solution;
Figure 2013105790045100002DEST_PATH_IMAGE003
neutralizer is imported in the four-hole boiling flask of upper opening with agitator, reflux exchanger, nitrogen conduit, constant pressure funnel and thermometer, and add described polynite turbid solution, pass into nitrogen 5min-15min, with four-hole boiling flask described in heating in water bath, and start agitator, under 40 ℃ of-50 ℃ of bath temperatures, stir 40min-80min, obtain mixed solution;
Figure 958183DEST_PATH_IMAGE004
continue to heat up, when bath temperature is 50 ℃-60 ℃, in described mixed solution, drip N, N '-methylene-bisacrylamide, stirs;
again with water bath, heat described container, and start to stir, when temperature rises to 55 ℃-75 ℃, add initiator, thermostatically heating 2-8h, stopped reaction is dried reaction mixture in 40 ℃ of-60 ℃ of baking ovens, and fragmentation, makes composite high-water uptake resin.
Described vinylformic acid degree of neutralization is 70%-90%.
Described aqueous sodium hydroxide solution concentration is 15%-25%, and introducing ratio is the 30%-50% of described Acrylic Acid Monomer quality.
Described polynite introduction volume is the 15%-30% of described Acrylic Acid Monomer quality.
Described initiator is K 2s 2o 8(NH 4) 2s 2o 8in a kind of.
Owing to adopting such scheme, technique effect of the present invention is: in polymerization process, by forming hydrogen bond between sodium polyacrylate and montmorillonite, one of the formation network that more effectively absorbs water that is also fully utilized of the side shoot beyond main polymer chain, promotes its water regain and rate of water absorption; And utilize the characteristic of inorganic hydrogel good salt tolerance, and anionic absorbent resin is coordinated with inorganic hydrogel thing and form gel complex body, promote it and inhale salt multiplying power.
Embodiment
Embodiment 1
100g vinylformic acid is added in 1000m Glass Containers cooling in ice-water bath, slowly add the aqueous sodium hydroxide solution 50g neutralization of mass concentration 15% under agitation condition, obtain neutralizer, vinylformic acid degree of neutralization is 70%; Get granularity 220 object montmorillonite powder 15g and pour in the container with agitator, add deionized water 85g and mix, after high speed dispersion 30min, obtain massfraction 15% polynite turbid solution; Neutralizer is imported in the container of upper opening with agitator, reflux exchanger, nitrogen conduit, constant pressure funnel and thermometer, and add polynite turbid solution, pass into nitrogen 5min, with container described in heating in water bath, and start stirring, high speed dispersion 40min under 40 ℃ of water-baths; To dripping mass concentration in described container, be 0.4% N, N '-methylene-bis acrylic acid amides solution 1.25g, stirs; Continue to heat up, when bath temperature is 55 ℃, drip (the NH of mass concentration 0.4% 4) 2s 2o 87.5g, and start to stir, thermostatically heating 8h, stopped reaction is dried reaction mixture in 40 ℃ of baking ovens, and fragmentation, makes composite high-water uptake resin.
Embodiment 2
100g vinylformic acid is added in 1000m Glass Containers cooling in ice-water bath, slowly add the aqueous sodium hydroxide solution 30g neutralization of mass concentration 25% under agitation condition, obtain neutralizer, vinylformic acid degree of neutralization is 80%; Get granularity 300 object montmorillonite powder 30g and pour in the container with agitator, add deionized water 70g and mix, after high speed dispersion 50min, obtain massfraction 30% polynite turbid solution; Neutralizer is imported in the container of upper opening with agitator, reflux exchanger, nitrogen conduit, constant pressure funnel and thermometer, and add described polynite turbid solution, pass into nitrogen 15min, with container described in heating in water bath, and start stirring, high speed dispersion 80min under 50 ℃ of water-baths; To dripping mass concentration in described container, be 0.4% N, N '-methylene-bis acrylic acid amides solution 1.25g, stirs; Continue to heat up, when temperature rises to 75 ℃, drip the K of mass concentration 0.4% 2s 2o 87.5g, thermostatically heating 2h, stopped reaction is dried reaction mixture in 60 ℃ of baking ovens, and fragmentation, makes composite high-water uptake resin.
Embodiment 3
100g vinylformic acid is added in 1000m Glass Containers cooling in ice-water bath, slowly add the aqueous sodium hydroxide solution 40g neutralization of mass concentration 20% under agitation condition, obtain neutralizer, vinylformic acid degree of neutralization is 90%; Get granularity 325 object montmorillonite powder 20g and pour in the container with agitator, add deionized water 80g and mix, after high speed dispersion 40min, obtain massfraction 20% polynite turbid solution; Neutralizer is imported in the container of upper opening with agitator, reflux exchanger, nitrogen conduit, constant pressure funnel and thermometer, and add polynite turbid solution, pass into nitrogen 10min, with container described in heating in water bath, and start stirring, high speed dispersion 60min under 45 ℃ of water-baths; To dripping mass concentration in described container, be 0.4% N, N '-methylene-bis acrylic acid amides solution 1.25g, stirs; Continue the described container of heating, when temperature rises to 60 ℃, drip the K of mass concentration 0.4% 2s 2o 87.5g, thermostatically heating 5h, stopped reaction is dried reaction mixture in 50 ℃ of baking ovens, and fragmentation, makes composite high-water uptake resin.
The composite high-water uptake resin property test structure that the inventive method prepares is as shown in table 1:
Table 1
Sample Inhale 0.9% salt solution multiplying power (g/g) Rate of water absorption (s) Water regain (GH 2O/g)
Embodiment 1 65.1 24.3 619.20
Embodiment 2 66.9 26.1 743.23
Embodiment 3 65.5 25.5 627.81

Claims (5)

1. montmorillonite is prepared the method for super absorbent resin, it is characterized in that it is raw material that the method mainly be take vinylformic acid and montmorillonite, comprises following steps:
Figure 2013105790045100001DEST_PATH_IMAGE002
vinylformic acid is put into container cooling in ice-water bath, under agitation condition, slowly add aqueous sodium hydroxide solution neutralization, obtain neutralizer;
Figure 2013105790045100001DEST_PATH_IMAGE004
get granularity≤220 object montmorillonite powder and pour in the container with agitator, add water and mix, after high speed dispersion 30min-50min, obtain polynite turbid solution;
Figure DEST_PATH_IMAGE006
neutralizer is imported in the four-hole boiling flask of upper opening with agitator, reflux exchanger, nitrogen conduit, constant pressure funnel and thermometer, and add described polynite turbid solution, pass into nitrogen 5min-15min, with four-hole boiling flask described in heating in water bath, and start agitator, under 40 ℃ of-50 ℃ of bath temperatures, stir 40min-80min, obtain mixed solution;
Figure DEST_PATH_IMAGE008
continue to heat up, when bath temperature is 50 ℃-60 ℃, in described mixed solution, drip N, N '-methylene-bisacrylamide, stirs;
again with water bath, heat described container, and start to stir, when temperature rises to 55 ℃-75 ℃, add initiator, thermostatically heating 2-8h, stopped reaction is dried reaction mixture in 40 ℃ of-60 ℃ of baking ovens, and fragmentation, makes composite high-water uptake resin.
2. montmorillonite according to claim 1 is prepared the method for super absorbent resin, it is characterized in that described vinylformic acid degree of neutralization is 70%-90%.
3. montmorillonite according to claim 1 is prepared the method for super absorbent resin, it is characterized in that described aqueous sodium hydroxide solution concentration is 15%-25%, and introducing ratio is the 30%-50% of described Acrylic Acid Monomer quality.
4. montmorillonite according to claim 1 is prepared the method for super absorbent resin, it is characterized in that described polynite introduction volume is the 15%-30% of described Acrylic Acid Monomer quality.
5. montmorillonite according to claim 1 is prepared the method for super absorbent resin, it is characterized in that described initiator is K 2s 2o 8(NH 4) 2s 2o 8in a kind of.
CN201310579004.5A 2013-11-19 2013-11-19 Method for preparing super absorbent resin by using montmorillonite Pending CN103613696A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110577433A (en) * 2019-06-28 2019-12-17 同济大学 Preparation method of kitchen waste-based composite gel slow-release fertilizer
CN116162214A (en) * 2023-04-26 2023-05-26 中国地质大学(北京) Grouting material and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101270173A (en) * 2007-11-27 2008-09-24 中国科学院长春应用化学研究所 High-gel strength, salt resistant amphoteric ion type nano-composite hydrogel and preparing method
CN101712785A (en) * 2008-10-06 2010-05-26 常琛 Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof
CN101787101A (en) * 2010-01-25 2010-07-28 陕西科技大学 Preparation method of nanometer resin with high hygroscopy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101270173A (en) * 2007-11-27 2008-09-24 中国科学院长春应用化学研究所 High-gel strength, salt resistant amphoteric ion type nano-composite hydrogel and preparing method
CN101712785A (en) * 2008-10-06 2010-05-26 常琛 Novel super absorbent resin/inorganic nanoparticle composite material, preparation method thereof and usage thereof
CN101787101A (en) * 2010-01-25 2010-07-28 陕西科技大学 Preparation method of nanometer resin with high hygroscopy

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110577433A (en) * 2019-06-28 2019-12-17 同济大学 Preparation method of kitchen waste-based composite gel slow-release fertilizer
CN116162214A (en) * 2023-04-26 2023-05-26 中国地质大学(北京) Grouting material and application thereof

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Application publication date: 20140305