CN103275450B - Method for preparing super absorbent resin - Google Patents
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- CN103275450B CN103275450B CN201310212926.2A CN201310212926A CN103275450B CN 103275450 B CN103275450 B CN 103275450B CN 201310212926 A CN201310212926 A CN 201310212926A CN 103275450 B CN103275450 B CN 103275450B
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Abstract
The invention discloses a method for preparing a super absorbent resin. The method comprises the following steps: 1) dissolving a hydrophilic linear polymer in water, adding a monomer A, a crosslinking agent A and an initiator A, stirring for completely dissolving, thus obtaining a reaction solution A; 2) mixing acrylic acid and a sodium hydroxide solution, adding fumed silica, mixing, filtering for removing a polymerization inhibitor, thus obtaining a monomer solution B; 3) dissolving a crosslinking agent B and an initiator B in the monomer solution B to obtain a reaction solution B, and adding interpenetrating polymer network gel into the reaction solution B, so that the gel is fully swelled, heated and reacted, thus obtaining interpenetrating polymer network gel B, drying to constant weight, crushing, grinding and screening to obtain an initial super absorbent resin product; and 4) performing surface treatment on the initial super absorbent resin product by using a surface treatment solution, thus obtaining the final product. The product has high absorption speed, high water retaining capacity, high pressurized absorption amount and other performances and can be applied to sanitary towels and other hygienic products.
Description
Technical field
The present invention relates to a kind of preparation method of super absorbent resin.
Background technology
Super absorbent resin refers to water insoluble but can absorb the crosslinking polymer network of own wt decades of times and even thousands of times of moisture, be widely used in the fields such as the sanitary material such as sanitary napkin, baby paper diaper, drought-resistant water-preserving, agricultural gardening, bio-medical, along with making rapid progress of scientific and technological level and improving constantly of people's living standard, its Application Areas constantly expands, and penetrates into the every field of industrial production and people's life gradually.Super absorbent resin mainly contains cellulose family super absorbent resin, starch-grafted super absorbent resin, polyacrylic super absorbent resin, Polyacrylamide super absorbent resin, polyvinyl alcohol super absorbent resin etc. by composition, and difference forms, different preparation method obtains super absorbent resin respectively has relative merits in performance.
Consider the requirement with direct body contact and application performance, the super absorbent resin being applied to sanitary material requires higher in biocompatibility, absorption rate, pressurizing absorption amount, water-retaining capacity etc.Vinylformic acid and multipolymer super absorbent resin thereof are acknowledged as the development trend of sanitary material super absorbent resin, and at present, the super absorbent resin being applied to the sanitary material such as sanitary towel, baby paper diaper derives from acrylate copolymer mostly.The preparation method of acrylic acid series super absorbent resin mainly contains inverse suspension method and solution polymerization process, inverse suspension method directly obtains particle product, easily dry, product water absorbing properties is excellent, it is the target that super absorbent resin manufacturer is pursued always, but need with an organic solvent because this method exists, complex manufacturing, be difficult to realize the shortcomings such as continuous prodution and be difficult to popularize, Jin You minority manufacturer adopts the method.And solution polymerization process relatively easily realizes, it is the super absorbent resin production method that current most of manufacturer adopts, but solution polymerization process obtain product performance be difficult to compared with inverse suspension method product, the performances such as the absorption rate particularly required by sanitary material, pressurizing absorption amount, often need just can meet the demands through aftertreatment.In addition, due to acrylic acid strongly hydrophilic, the large technical barrier making drying become solution polymerization process to prepare polyacrylic super absorbent resin.
The present invention adopts the method for multistep interpenetrating polymer networks, by forming vinylformic acid (sodium), the low cross-linking network of acrylamide and at vinylformic acid, the wetting ability linear polymers such as polyvinylpyrrolidone are realized in the polymerization process respectively of acrylamide, low crosslinking degree polyacrylamide, network between low crosslinking degree polyacrylic acid (sodium) passes mutually, both the reduction of absorption rate because high-crosslinking-degree causes and water-retaining capacity had been avoided, it also avoid the problem of the pressurizing absorption quantity not sufficient caused because degree of crosslinking is too low, solve super absorbent resin absorption rate preferably, water-retaining capacity, contradiction between pressurizing absorption amount.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of super absorbent resin.
The technical solution used in the present invention is:
A preparation method for super absorbent resin, the method comprises following each step:
1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, hydrophilic polymer mass content 1 ~ 3%, monomer A mass content is 5 ~ 10%, and linking agent A is 0.01 ~ 0.04% of monomer A quality, and initiator A is 0.2 ~ 0.5% of monomer A quality.Raised temperature to 80 ~ 90 DEG C, react 4 ~ 6 hours, are cooled to room temperature, obtain interpenetrating polymer networks gel A;
Wherein, wetting ability linear polymer is the one in polyvinylpyrrolidone, polyvinyl alcohol; Monomer A is acrylamide, and linking agent A is N, N ,-methylene-bisacrylamide, N, N ,-diallyl tartardiamide, N, N, the one in-vinyl bisacrylamide, and initiator A is Diisopropyl azodicarboxylate;
2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, add in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.7 ~ 0.85 with the ratio of acrylic acid amount of substance.Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B;
3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.02 ~ 0.05%, and initiator B consumption is add vinylformic acid quality 0.1 ~ 0.4%; Interpenetrating polymer networks gel A is added in reaction solution B, swelling 24 ~ 48 hours, then 75 ~ 85 DEG C are warming up to, react 2 ~ 3 hours, obtain interpenetrating polymer networks gel B, at 110 ~ 130 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product;
Wherein, the raw material propylene acid amides quality preparing gel A is 10 ~ 20% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is the one in ethylene glycol diacrylate, butanediol diacrylate, trimethylolpropane trimethacrylate;
4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed at 100 ~ 120 DEG C, obtain super absorbent resin product;
Above-mentioned surface treatment liquid is made up of component I and component I I, component I is the one in methyl alcohol, ethanol, Virahol, component I I is the one in ethylene glycol, propylene glycol, glycerol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 1 ~ 3% of super absorbent resin head product.
In step 1), described polyvinylpyrrolidone weight-average molecular weight is 40000 ~ 60000.
In step 1), polyvinyl alcohol alcoholysis degree 85 ~ 90%, mean polymerisation degree 1000 ~ 2000.
In step 3), described initiator B is the one in Potassium Persulphate, Sodium Persulfate.
In step 4), the treatment time is 1h.
The invention has the beneficial effects as follows: the present invention adopts the method for multistep interpenetrating polymer networks, by forming vinylformic acid (sodium), the low cross-linking network of acrylamide and at vinylformic acid, the wetting ability linear polymers such as polyvinylpyrrolidone are realized in the polymerization process respectively of acrylamide, low crosslinking degree polyacrylamide, network between low crosslinking degree polyacrylic acid (sodium) passes mutually, both the reduction of absorption rate because high-crosslinking-degree causes and water-retaining capacity had been avoided, it also avoid the problem of the pressurizing absorption quantity not sufficient caused because degree of crosslinking is too low, solve super absorbent resin absorption rate preferably, water-retaining capacity, contradiction between pressurizing absorption amount.Prepared super absorbent resin product has the performances such as good absorption rate, water-retaining capacity, pressurizing absorption amount, can be applicable to the sanitary products such as sanitary towel.
performance test methods of the present invention is as follows
Suck ionized water multiple (g/g): with reference to " People's Republic of China's agricultural industry criteria " (NY886-2004).
Absorbed dose (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Water-retaining capacity (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Pressurizing absorption amount (g/g): with reference to " National Standard of the People's Republic of China " (GB/T22905-2008).
Absorption rate (s): with reference to " National Standard of the People's Republic of China " (GB/T22875-2008).
Embodiment
Further illustrate content of the present invention below by way of specific embodiment, but be not limited to following embodiment.
embodiment 1:
(1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, hydrophilic polymer mass content 2%, monomer A mass content is 5%, and linking agent A is 0.01% of monomer A quality, and initiator A is 0.4% of monomer A quality.Raised temperature to 85 DEG C, reacts 5 hours, is cooled to room temperature, obtain interpenetrating polymer networks gel A.
Wherein, wetting ability linear polymer is polyvinylpyrrolidone, and its weight-average molecular weight is 45000; Monomer A is acrylamide, and linking agent A is N, N
,-methylene-bisacrylamide, initiator A is Diisopropyl azodicarboxylate.
(2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, add in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.75 with the ratio of acrylic acid amount of substance.Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B.
(3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.05%, and initiator B consumption is add vinylformic acid quality 0.2%.Interpenetrating polymer networks gel A is added in reaction solution B, swelling 24 hours, is then warming up to 85 DEG C, react 2 hours, obtain interpenetrating polymer networks gel B, at 120 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product.
Wherein, the raw material propylene acid amides quality preparing gel A is 10% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is ethylene glycol diacrylate, and initiator B is Potassium Persulphate.
(4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed 1 hour at 110 DEG C, obtain super absorbent resin product.
Above-mentioned surface treatment liquid is made up of component I and component I I, and component I is ethanol, and component I I is glycerol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 2% of super absorbent resin head product.
embodiment 2:
(1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, hydrophilic polymer mass content 1%, monomer A mass content is 6%, and linking agent A is 0.02% of monomer A quality, and initiator A is 0.3% of monomer A quality.Raised temperature to 90 DEG C, reacts 4 hours, is cooled to room temperature, obtain interpenetrating polymer networks gel A.
Wherein, wetting ability linear polymer is polyvinyl alcohol, its alcoholysis degree 87%, mean polymerisation degree 1200; Monomer A is acrylamide, and linking agent A is N, N
,-vinyl bisacrylamide, initiator A is Diisopropyl azodicarboxylate.
(2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, add in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.8 with the ratio of acrylic acid amount of substance.Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B.
(3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.02%, and initiator B consumption is add vinylformic acid quality 0.3%.Interpenetrating polymer networks gel A is added in reaction solution B, swelling 30 hours, is then warming up to 80 DEG C, react 2.5 hours, obtain interpenetrating polymer networks gel B, at 110 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product.
Wherein, the raw material propylene acid amides quality preparing gel A is 15% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is trimethylolpropane trimethacrylate, and initiator B is Sodium Persulfate.
(4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed 1 hour at 100 DEG C, obtain super absorbent resin product.
Above-mentioned surface treatment liquid is made up of component I and component I I, and component I is methyl alcohol, and component I I is propylene glycol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 1% of super absorbent resin head product.
embodiment 3:
(1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, hydrophilic polymer mass content 3%, monomer A mass content is 8%, and linking agent A is 0.03% of monomer A quality, and initiator A is 0.2% of monomer A quality.Raised temperature to 80 DEG C, reacts 6 hours, is cooled to room temperature, obtain interpenetrating polymer networks gel A.
Wherein, wetting ability linear polymer is polyvinylpyrrolidone, and weight-average molecular weight is 58000, and monomer A is acrylamide, and linking agent A is N, N
,-diallyl tartardiamide, initiator A is Diisopropyl azodicarboxylate.
(2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, add in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.85 with the ratio of acrylic acid amount of substance.Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B.
(3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.02%, and initiator B consumption is add vinylformic acid quality 0.4%.Interpenetrating polymer networks gel A is added in reaction solution B, swelling 48 hours, is then warming up to 75 DEG C, react 3 hours, obtain interpenetrating polymer networks gel B, at 130 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product.
Wherein, the raw material propylene acid amides quality preparing gel A is 20% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is butanediol diacrylate, and initiator B is Potassium Persulphate.
(4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed 1 hour at 120 DEG C, obtain super absorbent resin product.
Above-mentioned surface treatment liquid is made up of component I and component I I, and component I is Virahol, and component I I is ethylene glycol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 2% of super absorbent resin head product.
embodiment 4:
(1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, hydrophilic polymer mass content 2%, monomer A mass content is 10%, and linking agent A is 0.01% of monomer A quality, and initiator A is 0.2% of monomer A quality.Raised temperature to 85 DEG C, reacts 5 hours, is cooled to room temperature, obtain interpenetrating polymer networks gel A.
Wherein, wetting ability linear polymer is polyvinyl alcohol, alcoholysis degree 89%, mean polymerisation degree 1700; Monomer A is acrylamide, and linking agent A is N, N
,-methylene-bisacrylamide, initiator A is Diisopropyl azodicarboxylate.
(2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, add in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.7 with the ratio of acrylic acid amount of substance.Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B.
(3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.03%, and initiator B consumption is add vinylformic acid quality 0.3%.Interpenetrating polymer networks gel A is added in reaction solution B, swelling 40 hours, is then warming up to 80 DEG C, react 2.5 hours, obtain interpenetrating polymer networks gel B, at 120 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product.
Wherein, the raw material propylene acid amides quality preparing gel A is 13% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is butanediol diacrylate, and initiator B is Potassium Persulphate.
(4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed 1 hour at 110 DEG C, obtain super absorbent resin product.
Above-mentioned surface treatment liquid is made up of component I and component I I, and component I is methyl alcohol, and component I I is ethylene glycol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 3% of super absorbent resin head product.
The performance test results of above-described embodiment is as table 1:
table 1 embodiment effect
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Suck ionized water multiple, g/g | 426 | 435 | 414 | 42.8 |
| Absorbed dose, g/g | 61.2 | 65.3 | 61.8 | 63.4 |
| Water-retaining capacity, g/g | 48.7 | 51.6 | 50.6 | 47.9 |
| Pressurizing absorption amount, g/g | 35.6 | 34.1 | 32.2 | 31.7 |
| Absorption rate, second | 145 | 142 | 150 | 148 |
implementation result is analyzed:
The present invention adopts the method for multistep interpenetrating polymer networks, by forming vinylformic acid (sodium), the low cross-linking network of acrylamide and at vinylformic acid, the wetting ability linear polymers such as polyvinylpyrrolidone are realized in the polymerization process respectively of acrylamide, low crosslinking degree polyacrylamide, network between low crosslinking degree polyacrylic acid (sodium) passes mutually, both the reduction of absorption rate because high-crosslinking-degree causes and water-retaining capacity had been avoided, it also avoid the problem of the pressurizing absorption quantity not sufficient caused because degree of crosslinking is too low, solve super absorbent resin absorption rate preferably, water-retaining capacity, contradiction between pressurizing absorption amount.As can be seen from Table 1, prepared super absorbent resin product has the performances such as good absorption rate, water-retaining capacity, pressurizing absorption amount, can be applicable to the sanitary products such as sanitary towel.
Claims (5)
1. a preparation method for super absorbent resin, is characterized in that, the method comprises following each step:
1) wetting ability linear polymer is dissolved in deionized water, make abundant dissolving, then monomer A, linking agent A, initiator A is added, stirring makes to dissolve completely, obtains reaction solution A, wherein, wetting ability linear polymer mass content 1 ~ 3%, monomer A mass content is 5 ~ 10%, and linking agent A is 0.01 ~ 0.04% of monomer A quality, and initiator A is 0.2 ~ 0.5% of monomer A quality; Raised temperature to 80 ~ 90 DEG C, react 4 ~ 6 hours, are cooled to room temperature, obtain interpenetrating polymer networks gel A;
Wherein, wetting ability linear polymer is the one in polyvinylpyrrolidone, polyvinyl alcohol; Monomer A is acrylamide, and linking agent A is N, N ,-methylene-bisacrylamide, N, N ,-diallyl tartardiamide, N, N, the one in-vinyl bisacrylamide, and initiator A is Diisopropyl azodicarboxylate;
2) be dissolved in deionized water by sodium hydroxide, obtain the alkaline solution of sodium hydroxide mass content 60%, join in alkaline solution under stirring by vinylformic acid, obtain the acrylic acid solution of part neutralization, sodium hydroxide is 0.7 ~ 0.85 with the ratio of acrylic acid amount of substance; Add gas-phase silica by 1% of vinylformic acid quality, at room temperature stir 0.5 hour, cross the stopper filtered wherein, obtain monomer solution B;
3) crosslinking agent B, initiator B are dissolved in monomer solution B and obtain reaction solution B, crosslinking agent B consumption is add vinylformic acid quality 0.02 ~ 0.05%, and initiator B consumption is add vinylformic acid quality 0.1 ~ 0.4%; Interpenetrating polymer networks gel A is added in reaction solution B, swelling 24 ~ 48 hours, then 75 ~ 85 DEG C are warming up to, react 2 ~ 3 hours, obtain interpenetrating polymer networks gel B, at 110 ~ 130 DEG C, be dried to constant weight, through broken, pulverize, sieve, obtain particle diameter 40 ~ 80 object super absorbent resin head product;
Wherein, the raw material propylene acid amides quality preparing gel A is 10 ~ 20% of the raw material propylene acid quality of preparation feedback liquid B, and crosslinking agent B is the one in ethylene glycol diacrylate, butanediol diacrylate, trimethylolpropane trimethacrylate;
4) the super absorbent resin head product surface treatment liquid obtained in (3) is processed at 100 ~ 120 DEG C, obtain super absorbent resin product;
Above-mentioned surface treatment liquid is made up of component I and component I I, component I is the one in methyl alcohol, ethanol, Virahol, component I I is the one in ethylene glycol, propylene glycol, glycerol, and component I and component I I mass ratio are 1:1, and surface treatment liquid consumption is 1 ~ 3% of super absorbent resin head product.
2. the preparation method of a kind of super absorbent resin according to claim 1, is characterized in that: in step 1), and described polyvinylpyrrolidone weight-average molecular weight is 40000 ~ 60000.
3. the preparation method of a kind of super absorbent resin according to claim 1, is characterized in that: in step 1), polyvinyl alcohol alcoholysis degree 85 ~ 90%, mean polymerisation degree 1000 ~ 2000.
4. the preparation method of a kind of super absorbent resin according to claim 1, is characterized in that: in step 3), and described initiator B is the one in Potassium Persulphate, Sodium Persulfate.
5. the preparation method of a kind of super absorbent resin according to claim 1, is characterized in that: in step 4), and the treatment time is 1h.
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| CN106633111B (en) * | 2017-01-11 | 2018-12-25 | 福州大学 | A kind of preparation method of high strength poly vinyl alcohol base double-network hydrogel |
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| CN108559108B (en) * | 2018-04-20 | 2021-07-13 | 延安大学 | Preparation method of three-dimensional interpenetrating network hydrogel with pH response |
| CN109810215B (en) * | 2018-12-28 | 2019-11-08 | 珠海得米新材料有限公司 | A kind of preparation method of double cross connection super absorbent resin |
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| CN112210042B (en) * | 2020-11-11 | 2023-06-09 | 西北师范大学 | Preparation method of white carbon black-biological glue composite water-absorbing material |
| CN112552468B (en) * | 2020-12-10 | 2022-12-06 | 山东诺尔生物科技有限公司 | Super absorbent resin and preparation method thereof |
| CN116043606B (en) * | 2023-03-29 | 2023-07-04 | 智微合聚先进材料科技(苏州)有限责任公司 | High-wet-strength multi-layer tissue composite moisture-absorbing material and preparation method thereof |
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| CN1172124A (en) * | 1996-07-25 | 1998-02-04 | 化学工业部北京化工研究院 | Wate-absorption resin and preparing method thereof |
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