CN104448102A - Method for preparing super absorbent resin microspheres - Google Patents
Method for preparing super absorbent resin microspheres Download PDFInfo
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- CN104448102A CN104448102A CN201410694519.4A CN201410694519A CN104448102A CN 104448102 A CN104448102 A CN 104448102A CN 201410694519 A CN201410694519 A CN 201410694519A CN 104448102 A CN104448102 A CN 104448102A
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- absorbent resin
- super absorbent
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- lipoid microsphere
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Abstract
The invention relates to a method for preparing super absorbent resin microspheres, belongs to the technical field of high polymer materials, and solves the problems that a reversed phase suspension polymerization process for preparing super absorbent resin microspheres in the prior art is complex and is high in cost in the production process, the prepared microspheres are poor in molding and low in yield. The method adopts a reversed phase suspension technique and is simple in preparation process, the products can be used without further grinding, the after-processing process of products is simplified, the yield of products is improved, and the production cost of products is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of resin, more particularly, the present invention relates to a kind of preparation method of super absorbent resin lipoid microsphere, belong to technical field of polymer materials.
Background technology
High hydrophilous resin is development and Application face a kind of functional polymer very widely, the water of the heavy hundred times of its energy specific absorption own wt to thousands of times, the colorless transparent gel that a kind of height is swelling is become after water suction, even if also not easily expressed water is next for pressurized, there is excellent water retention property, therefore, as soil improvement agent, sanitary product material, industrial dewatering agent, preservation agent etc., the fields such as agricultural, forestry, gardening are widely used in.
It is CN103554331A that State Intellectual Property Office discloses a publication number in 2014.2.5, name is called " a kind of method that inverse suspension polymerization prepares polyacrylic acid high water absorptive resin microballoon ", which disclose a kind of method that inverse suspension polymerization prepares polyacrylic acid high water absorptive resin microballoon, the method take hexanaphthene as solvent, with comonomer, dispersion agent, linking agent and initiator are main reactant, employing inverse suspension polymerization forms, wherein said dispersion agent is selected from following two or three: sorbester p17, sorbester p18, span 40, hexadecanyl phosphate and octadecyl phosphoric acid ester.The inventive method significantly improves the stability of reaction system, and can realize step continuous production polyacrylic acid high water absorptive resin in enormous quantities microballoon, simple process, non-environmental-pollution, production cost are low, applied range, meet industrialized requirement completely.
The inverse suspension polymerization technique preparing super absorbent resin lipoid microsphere of above-mentioned patent is comparatively complicated, and production process cost is high, and obtained microballoon is shaping not good, and yield is not high.
Summary of the invention
The present invention is intended to the problem solving super absorbent resin preparation method of lipid microspheres in prior art, and provide a kind of preparation method of super absorbent resin lipoid microsphere, Simplified flowsheet, reduces costs, and improves product yield and quality.
In order to realize foregoing invention object, concrete technical scheme is as follows:
A preparation method for super absorbent resin lipoid microsphere, is characterized in that: comprise following processing step:
A, take hexanaphthene 500-1000ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 80-100g, acrylamide 20-40g, polyoxyethylene glycol 0.3-0.8g, ammonium persulphate 0.3-0.6g and sodium bicarbonate 0.3-0.6g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 30-50 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
In step, described stirring is stirred with the rotating speed of 200 revs/min in the present invention.
The present invention in step, described be positioned over heating in water-bath and refer to and be heated to 65 DEG C.
In step, described dispersion stabilizer is Ba Lafuluo in the present invention.
In step, the add-on of described dispersion stabilizer is the 0.3-0.5 of hexanaphthene in the present invention.
In stepb, described polyoxyethylene glycol is polyoxyethylene glycol PEG-400 in the present invention.
The present invention is in step C, and the speed of described stirring is 300 revs/min.
In step D, described insulation is all insulation 2-3 hour in the present invention.
The Advantageous Effects that the present invention brings:
The invention solves in prior art the inverse suspension polymerization technique preparing super absorbent resin lipoid microsphere comparatively complicated, and production process cost is high, obtained microballoon is shaping not good, the problem that yield is not high.The preparation of this super absorbent resin lipoid microsphere have employed reversed phase suspension technique, and preparation technology is simple, and product does not need to pulverize further and can use, and simplifies the post-treatment process of product, improves the yield of product, reduce the production cost of product.
Embodiment
embodiment 1
A preparation method for super absorbent resin lipoid microsphere, comprises following processing step:
A, take hexanaphthene 500ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 80g, acrylamide 20g, polyoxyethylene glycol 0.3g, ammonium persulphate 0.3g and sodium bicarbonate 0.3g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 30 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
embodiment 2
A preparation method for super absorbent resin lipoid microsphere, comprises following processing step:
A, take hexanaphthene 1000ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 100g, acrylamide 40g, polyoxyethylene glycol 0.8g, ammonium persulphate 0.6g and sodium bicarbonate 0.6g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 50 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
embodiment 3
A preparation method for super absorbent resin lipoid microsphere, comprises following processing step:
A, take hexanaphthene 750ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 90g, acrylamide 30g, polyoxyethylene glycol 0.55g, ammonium persulphate 0.45g and sodium bicarbonate 0.45g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 40 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
embodiment 4
A preparation method for super absorbent resin lipoid microsphere, comprises following processing step:
A, take hexanaphthene 600ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 82g, acrylamide 21g, polyoxyethylene glycol 0.75g, ammonium persulphate 0.5g and sodium bicarbonate 0.52g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 33 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
embodiment 5
On the basis of embodiment 1-4, preferred:
In step, described stirring is stirred with the rotating speed of 200 revs/min.
In step, be describedly positioned over heating in water-bath and refer to and be heated to 65 DEG C.
In step, described dispersion stabilizer is Ba Lafuluo.
In step, the add-on of described dispersion stabilizer is 0.3 of hexanaphthene.
In stepb, described polyoxyethylene glycol is polyoxyethylene glycol PEG-400.
In step C, the speed of described stirring is 300 revs/min.
In step D, described insulation is all insulation 2 hours.
embodiment 6
On the basis of embodiment 1-4, preferred:
In step, described stirring is stirred with the rotating speed of 200 revs/min.
In step, be describedly positioned over heating in water-bath and refer to and be heated to 65 DEG C.
In step, described dispersion stabilizer is Ba Lafuluo.
In step, the add-on of described dispersion stabilizer is 0.5 of hexanaphthene.
In stepb, described polyoxyethylene glycol is polyoxyethylene glycol PEG-400.
In step C, the speed of described stirring is 300 revs/min.
In step D, described insulation is all insulation 3 hours.
embodiment 7
On the basis of embodiment 1-4, preferred:
In step, described stirring is stirred with the rotating speed of 200 revs/min.
In step, be describedly positioned over heating in water-bath and refer to and be heated to 65 DEG C.
In step, described dispersion stabilizer is Ba Lafuluo.
In step, the add-on of described dispersion stabilizer is 0.4 of hexanaphthene.
In stepb, described polyoxyethylene glycol is polyoxyethylene glycol PEG-400.
In step C, the speed of described stirring is 300 revs/min.
In step D, described insulation is all insulation 2.5 hours.
embodiment 8
On the basis of embodiment 1-4, preferred:
In step, described stirring is stirred with the rotating speed of 200 revs/min.
In step, be describedly positioned over heating in water-bath and refer to and be heated to 65 DEG C.
In step, described dispersion stabilizer is Ba Lafuluo.
In step, the add-on of described dispersion stabilizer is 0.45 of hexanaphthene.
In stepb, described polyoxyethylene glycol is polyoxyethylene glycol PEG-400.
In step C, the speed of described stirring is 300 revs/min.
In step D, described insulation is all insulation 2.75 hours.
Claims (8)
1. a preparation method for super absorbent resin lipoid microsphere, is characterized in that: comprise following processing step:
A, take hexanaphthene 500-1000ml and put into reaction vessel, start to stir, then reaction vessel is positioned in water-bath and heats, add dispersion agent stablizer, obtain oil-based system;
B, take methacrylic acid 80-100g, acrylamide 20-40g, polyoxyethylene glycol 0.3-0.8g, ammonium persulphate 0.3-0.6g and sodium bicarbonate 0.3-0.6g and mix, obtain aqueous phase system, then dropped into the reaction vessel of steps A, and be warming up to 75 DEG C;
C, start stirring, make aqueous phase form uniform pearl body and be dispersed in oil phase;
After D, pearl body-shaping, temperature is risen to 80 DEG C, insulation; Be warming up to 85 DEG C, insulation; Be warming up to 90 DEG C, insulation; Be cooled to 30-50 DEG C, filter and obtain spheroid, adopt ethanol to carry out drip washing to spheroid, namely dry, sealing obtains super absorbent resin lipoid microsphere.
2. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in step, and described stirring is stirred with the rotating speed of 200 revs/min.
3. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in step, described be positioned over heating in water-bath and refer to and be heated to 65 DEG C.
4. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in step, and described dispersion stabilizer is Ba Lafuluo.
5. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1 or 4, is characterized in that: in step, and the add-on of described dispersion stabilizer is the 0.3-0.5 of hexanaphthene.
6. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in stepb, and described polyoxyethylene glycol is polyoxyethylene glycol PEG-400.
7. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in step C, and the speed of described stirring is 300 revs/min.
8. the preparation method of a kind of super absorbent resin lipoid microsphere according to claim 1, is characterized in that: in step D, and described insulation is all insulation 2-3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410694519.4A CN104448102A (en) | 2014-11-27 | 2014-11-27 | Method for preparing super absorbent resin microspheres |
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| CN201410694519.4A CN104448102A (en) | 2014-11-27 | 2014-11-27 | Method for preparing super absorbent resin microspheres |
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| CN104448102A true CN104448102A (en) | 2015-03-25 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788620A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Preparation method for super water-absorbent resin |
| CN106000248A (en) * | 2016-05-30 | 2016-10-12 | 常熟理工学院 | Preparation method of controllable-expansion superwater absorbent resin microcapsules |
| CN106747897A (en) * | 2016-11-10 | 2017-05-31 | 钟燕红 | A kind of water supports the preparation method of ball |
| CN106916260A (en) * | 2017-03-29 | 2017-07-04 | 中山大学惠州研究院 | A kind of preparation method of hud typed porous high water absorption microballoon |
| CN115746483A (en) * | 2022-12-08 | 2023-03-07 | 广州市侗富贵化工原材料有限公司 | Porous water-absorbing resin, preparation method thereof, hygienic product, water-retaining agent and waterproof coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587289A (en) * | 2004-07-09 | 2005-03-02 | 浙江大学 | Process for preparing high water absorption resin |
| JP2012041419A (en) * | 2010-08-18 | 2012-03-01 | Sumitomo Seika Chem Co Ltd | Method for producing water-absorbing resin |
| CN103864980A (en) * | 2014-02-24 | 2014-06-18 | 杭州电子科技大学 | Method for preparing agricultural super absorbent resin for ternary copolymerization |
-
2014
- 2014-11-27 CN CN201410694519.4A patent/CN104448102A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587289A (en) * | 2004-07-09 | 2005-03-02 | 浙江大学 | Process for preparing high water absorption resin |
| JP2012041419A (en) * | 2010-08-18 | 2012-03-01 | Sumitomo Seika Chem Co Ltd | Method for producing water-absorbing resin |
| CN103864980A (en) * | 2014-02-24 | 2014-06-18 | 杭州电子科技大学 | Method for preparing agricultural super absorbent resin for ternary copolymerization |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788620A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Preparation method for super water-absorbent resin |
| CN106000248A (en) * | 2016-05-30 | 2016-10-12 | 常熟理工学院 | Preparation method of controllable-expansion superwater absorbent resin microcapsules |
| CN106000248B (en) * | 2016-05-30 | 2018-07-13 | 常熟理工学院 | A kind of preparation method of controllable expansion super moisture absorbing resin microcapsules |
| CN106747897A (en) * | 2016-11-10 | 2017-05-31 | 钟燕红 | A kind of water supports the preparation method of ball |
| CN106916260A (en) * | 2017-03-29 | 2017-07-04 | 中山大学惠州研究院 | A kind of preparation method of hud typed porous high water absorption microballoon |
| CN106916260B (en) * | 2017-03-29 | 2019-04-16 | 中山大学惠州研究院 | A kind of preparation method of hud typed porous high water absorption microballoon |
| CN115746483A (en) * | 2022-12-08 | 2023-03-07 | 广州市侗富贵化工原材料有限公司 | Porous water-absorbing resin, preparation method thereof, hygienic product, water-retaining agent and waterproof coating |
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Application publication date: 20150325 |
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