CN1122052C - Synthesis of high-hydroscopicity resin - Google Patents
Synthesis of high-hydroscopicity resin Download PDFInfo
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- CN1122052C CN1122052C CN99126337A CN99126337A CN1122052C CN 1122052 C CN1122052 C CN 1122052C CN 99126337 A CN99126337 A CN 99126337A CN 99126337 A CN99126337 A CN 99126337A CN 1122052 C CN1122052 C CN 1122052C
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Abstract
The present invention belongs to a synthesizing method for high water absorption resin, which is characterized in that bentonite is added to an acrylic acid-starch graft copolymerization system, which enhances solid content and salt tolerance and reduces cost; a single component initiating agent is added for initiating, and potassium chloride is used for controlling the viscosity of the system, which solves the problem that water phase polymerization is difficult to be carried out by adding the bentonite to an acidic medium. The pH value of hydrogel of obtained products is not greater than 7. Thus, the high water absorption resin can be directly used for industries of agriculture, forests, etc., and the water absorption multiplying power of the high water absorption resin can meet requirements.
Description
The invention belongs to the synthetic method of High hydrophilous resin.
In recent years, High hydrophilous resin has obtained using widely in agricultural and industry such as forestry, and therefore, the water-absorbing resin kind of, forestry low-cost requirement agricultural for satisfying and synthetic method also constantly increase and improve.Chinese patent 89101086.6 discloses that to be entitled as " high-absorbent material synthetic method " this method be raw material with acrylamide and wilkinite, ammonium persulphate and S-WAT are initiator, NN ' methylene-bis acryloyl ammonium is a linking agent, 50～75 ℃ of outer heating 1～4 hour.This invention improves solid content owing to add the wilkinite copolymerization, reduces the ton cost significantly, improves the market competitiveness, beyond doubt a desirable technology.But, this product many unsatisfactory parts also occur in sector applications such as farming, woodss, because major ingredient acrylamide and wilkinite are alkalescence, the pH value of hydrogel is more than 8.5, is directly used in drought resisting or coating agent for seed base starting material, reduces seedling rate, be used for forestry and be stained with the root transplanting, easily produce and burn the root phenomenon, transfer pH value to acid although the agricultural user in use can add acid, this has drawn inconveniences such as technical, transportation, preservation.
The synthetic method that the purpose of this invention is to provide a kind of High hydrophilous resin.Synthetic to dose the wilkinite copolymerization in vinylformic acid-starch graft copolymer system, the goods hydrogel pH value that is obtained is not more than 7, and is directly available on industries such as farming, woods, cost is low, good salt tolerance, water absorbent rate can be satisfied the demand.
One of measure of the present invention is only to add oxidation component in the initiator, no longer add such as reduction components such as S-WATs, temperature rise in controlled polymerization speed and the polymerization, solve because of wilkinite at a large amount of metal ions of acidic medium stripping, cause the extremely low or polymerization of water absorbent rate to be difficult to finish; Another measure of the present invention is to add Repone K, produces salt effect, reduces wilkinite in acidic medium stripping metal ion quantity, and it is excessive to solve bentonite slurry and pasted starch viscosity in stirring simultaneously, the unworkable difficult problem of polymerization.
Synthesis step of the present invention is as follows: prepare six kinds of components respectively, component 1 is to add wilkinite in (weight percent, as follows) 1.60～3.10% aqueous sodium hydroxide solutions, is mixed with the soup compound that contains wilkinite 10.42～15.25%; Component 2 is mixed with starch-containing 29.11～37.60% starch salt brine solution for to stir into starch in 3.38～9.27% potassium chloride solutions; Component 3 is to make 13.50～18.10% aqueous sodium hydroxide solutions and 37.50～50% acrylic acid aqueous solution generation neutralization reactions, and the vinylformic acid that is neutralized accounts for and adds vinylformic acid 39.88～56.16%; Component 4 is a pure acrylic acid solution; Component 5 is 0.59～0.99% ammonium persulfate aqueous solution; Component 6 is NN '-methylene-bisacrylamide aqueous solution of 0.50～0.99%, under agitation each component is added reactor according to 1～6 order, component 1～6 accounts for total amount weight percent composition and is: 19.75～36.62%, 10～10.31%, 42.33～51.23%, 4.47～6.86%, 4.70～8.73%, 1.57～3.41%; The polymerization tank of packing into behind each component mixing, 40～70 ℃ of polymerizations 4～8 hours, obtain High hydrophilous resin through granulation, oven dry, pulverizing again, water absorbent rate is 461～802 times, it is neutral that hydrogel is, measure water absorbent rate with the nickel screen method, calculation formula is: weight before water absorbent rate=[suction back weight-blank weight]/suction; Check the hydrogel acid-basicity with the PH test paper.
This method has solved and added the difficult problem that wilkinite is difficult to carry out aqueous polymerization in acidic medium, and it is neutral that hydrogel is, and the agricultural user can directly use; Compare with normally used vinylformic acid-starch grafting type high water absorption resin, owing to add wilkinite, improve solid content, cost is low, good salt tolerance.
Embodiment provided by the invention is as follows:
Embodiment 1:
The 3Kg wilkinite is stirred in 3.1% aqueous sodium hydroxide solution, make and contain wilkinite 10.42% component 1; Starch added obtain starch-containing 29.11% component 2 in 3.38% potassium chloride solution; With among 13.5% the aqueous sodium hydroxide solution 34.68Kg and 37.5% acrylic acid aqueous solution, the vinylformic acid that is neutralized accounts for and adds vinylformic acid 56.16%, obtains component 3; Get pure acrylic acid solution 10Kg and obtain component 4; Component 5 is 0.59% ammonium persulfate aqueous solution; Component 6 is 0.50%NN '-methylene-bisacrylamide solution; Under agitation each component is added reactor according to 1～6 order, component 1～6 accounts for total amount weight percent composition and is: 19.75%, 10%, 51.23%, 6.86%, 8.73%, 3.41%; The polymerization tank of packing into behind each component mixing, 40 ℃ of polymerizations 8 hours obtain High hydrophilous resin through granulation, oven dry, pulverizing, 802 times of its water absorbent rates.Check that with the PH test paper hydrogel is neutral.
Embodiment 2:
All the other stir into the 9Kg wilkinite in 1.6% sodium hydroxide solution with embodiment 1, make to contain wilkinite 15.25% component 1; Starch added obtain starch-containing 37.6% component 2 in 9.27% Klorvess Liquid; With among 18.1% the aqueous sodium hydroxide solution 25.88Kg and 50% acrylic acid aqueous solution, the vinylformic acid that is neutralized accounts for and adds vinylformic acid 39.88%, component 3; Get pure acrylic acid solution 7.2Kg and obtain component 4; Component 5 is 0.99% ammonium persulfate solution; Component 6 is 0.99%NN '-methylene-bisacrylamide solution; Component 1～6 accounts for the total amount weight percent and forms and to be: 36.62%, 10.31%, 42.33%, 4.47%, 4.7%, 1.57%, 70 ℃ of polymerization is 4 hours, 461 times of its water absorbent rates.Check that with the PH test paper hydrogel is neutral.
Embodiment 3:
All the other stir into the 5Kg wilkinite in 2.23% sodium hydroxide solution with embodiment 1, make to contain wilkinite 12.25% component 1; Starch added obtain starch-containing 29.22% component 2 in 5.66% Klorvess Liquid; With among 16.04% the aqueous sodium hydroxide solution 29.18Kg and 42.5% acrylic acid aqueous solution, the vinylformic acid that is neutralized accounts for and adds vinylformic acid 49.55%, component 3; Get pure acrylic acid solution 9Kg and obtain component 4; Component 5 is 0.70% ammonium persulfate solution; Component 6 is 0.55%NN '-methylene-bisacrylamide solution; Component 1～6 accounts for the total amount weight percent and forms and to be: 28.13%, 8.26%, 47.69%, 6.20%, 6.94%, 2.77%, 50 ℃ of polymerization is 6 hours, 714 times of its water absorbent rates.Check that with the PH test paper hydrogel is neutral.
Embodiment 4:
All the other stir into the 7Kg wilkinite in 1.91% sodium hydroxide solution with embodiment 1, make to contain wilkinite 14.34% component 1; Starch added obtain starch-containing 33.29% component 2 in 4.72% Klorvess Liquid; With among 14.77% the aqueous sodium hydroxide solution 31.68Kg and 44.19% acrylic acid aqueous solution, the vinylformic acid that is neutralized accounts for and adds vinylformic acid 44.36%, component 3; Get pure acrylic acid solution 8.5Kg and obtain component 4; Component 5 is 0.71% ammonium persulfate solution; Component 6 is 0.56%NN '-methylene-bisacrylamide solution; Component 1～6 accounts for the total amount weight percent and forms and to be: 29.83%, 10.1%, 45.65%, 5.2%, 6.16%, 3.07%, 60 ℃ of polymerization is 5 hours, 634 times of its water absorbent rates.Check that with the PH test paper hydrogel is neutral.
Claims (1)
1. the synthetic method of a High hydrophilous resin is characterized in that preparing respectively six kinds of components, and component 1 is mixed with the soup compound that contains wilkinite 10.42～15.25 weight % for to add wilkinite in 1.60～3.10 weight % aqueous sodium hydroxide solutions; Component 2 is mixed with the aqueous solution of starch-containing 29.11～37.60 weight % for to stir into starch in 3.38～9.27 weight % potassium chloride solutions; Component 3 is to make 13.50～18.10 weight % aqueous sodium hydroxide solutions and 37.50～50 weight % acrylic acid aqueous solution generation neutralization reactions, and the vinylformic acid that is neutralized accounts for and adds vinylformic acid 39.88～56.16 weight %; Component 4 is a pure acrylic acid liquid; Component 5 is 0.59～0.99 weight % ammonium persulfate aqueous solution; Component 6 is NN '-methylene-bisacrylamide aqueous solution of 0.50～0.99 weight %, under agitation each component is added reactor according to 1～6 order, component 1～6 accounts for total amount weight percent composition: component 1 accounts for 19.75～36.62%, component 2 accounts for 10～10.31%, component 3 accounts for 42.33～51.23%, and component 4 accounts for 4.47～6.86%, and component 5 accounts for 4.70～8.73%, component 6 accounts for 1.57～3.41%, and each component percentage contains sum and should be 100%; Measure the polymerization tank of packing into behind each component mixing, 40～70 ℃ of polymerizations 4～8 hours obtain High hydrophilous resin through granulation, oven dry, pulverizing again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99126337A CN1122052C (en) | 1999-12-16 | 1999-12-16 | Synthesis of high-hydroscopicity resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99126337A CN1122052C (en) | 1999-12-16 | 1999-12-16 | Synthesis of high-hydroscopicity resin |
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| CN1299836A CN1299836A (en) | 2001-06-20 |
| CN1122052C true CN1122052C (en) | 2003-09-24 |
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| CN99126337A Expired - Fee Related CN1122052C (en) | 1999-12-16 | 1999-12-16 | Synthesis of high-hydroscopicity resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935379A (en) * | 2010-10-09 | 2011-01-05 | 内蒙古大学 | Method for synthesizing nitrogenous super absorbent resin from alkaline gelatinized potato starch through graft copolymerization |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987049B (en) | 2009-07-30 | 2014-10-01 | 上海微创医疗器械（集团）有限公司 | Method and device for loading medicine and/or polymers on medical appliance |
| CN102125474B (en) | 2010-01-19 | 2012-10-31 | 微创医疗器械(上海)有限公司 | Method and device for loading medicines and/or polymers on medical equipment |
| CN103588934A (en) * | 2013-11-20 | 2014-02-19 | 宜兴丹森科技有限公司 | Method for preparing salt tolerant super absorbent resin by bentonite |
| CN104788604B (en) * | 2014-01-22 | 2017-01-25 | 亿利资源集团有限公司 | Ecological moisture-retention water-storage composite material, and preparation method thereof |
| CN106010559A (en) * | 2016-05-31 | 2016-10-12 | 山东胜伟园林科技有限公司 | Bentonite-containing water retaining agent used for corn in saline and alkaline land, and preparation method thereof |
| CN111718554B (en) * | 2020-07-28 | 2021-04-27 | 中国科学院长春应用化学研究所 | Automobile suspension noise reduction damping liquid containing gel and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041601A (en) * | 1989-03-01 | 1990-04-25 | 荣庸 | High-absorbent material synthetic method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041601A (en) * | 1989-03-01 | 1990-04-25 | 荣庸 | High-absorbent material synthetic method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935379A (en) * | 2010-10-09 | 2011-01-05 | 内蒙古大学 | Method for synthesizing nitrogenous super absorbent resin from alkaline gelatinized potato starch through graft copolymerization |
| CN101935379B (en) * | 2010-10-09 | 2011-08-10 | 内蒙古大学 | Method for synthesizing nitrogenous super absorbent resin from alkaline gelatinized potato starch through graft copolymerization |
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| CN1299836A (en) | 2001-06-20 |
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