CN115490802A - Method for synthesizing acrylic acid type super absorbent resin - Google Patents
Method for synthesizing acrylic acid type super absorbent resin Download PDFInfo
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- CN115490802A CN115490802A CN202211181183.2A CN202211181183A CN115490802A CN 115490802 A CN115490802 A CN 115490802A CN 202211181183 A CN202211181183 A CN 202211181183A CN 115490802 A CN115490802 A CN 115490802A
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- CN
- China
- Prior art keywords
- acrylic acid
- absorbent resin
- super absorbent
- acid type
- type super
- 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.)
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 59
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229920005989 resin Polymers 0.000 title claims abstract description 54
- 239000011347 resin Substances 0.000 title claims abstract description 54
- 239000002250 absorbent Substances 0.000 title claims abstract description 48
- 230000002745 absorbent Effects 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 229920000247 superabsorbent polymer Polymers 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000012272 crop production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003898 horticulture Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004583 superabsorbent polymers (SAPs) Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
Abstract
The invention discloses a method for synthesizing acrylic acid type super absorbent resin, which comprises the following steps: mixing acrylic acid and sodium hydroxide solution for reaction, then adding a cross-linking agent, introducing nitrogen to prevent air from entering, and stirring and mixing uniformly; and raising the temperature to a certain degree, adding an initiator to react to form gel, taking out, and drying to obtain the acrylic acid type super absorbent resin. Compared with the resin synthesized by the traditional method, the acrylic acid type super absorbent resin synthesized by the invention has the advantages of greatly improved water absorption effect, simple process flow and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a method for synthesizing acrylic acid type super absorbent resin.
Background
The super absorbent resin is a cross-linked functional polymer, contains strong hydrophilic groups and is good at water absorption and water retention performance. In view of these characteristics, superabsorbent polymer has become one of important polymer materials in recent years, and is widely used in many fields such as agriculture, forestry, horticulture, oil exploration, medical health, mining, daily chemical industry, and the like.
Since the research and development work on the aspect of super absorbent resin was carried out in 1980 and the synthesis of polyacrylic acid super absorbent resin was started in 1982, the super absorbent resin is a novel material which is rapidly developed and has wide application prospect, and has wide attention and application in many fields such as agriculture and forestry crop production, urban landscaping and the like.
Superabsorbent polymers are rapidly developed and classified into various methods according to hydrophilicity, sample form, crosslinking method, raw material source, and the like, wherein superabsorbent resins are mainly classified into natural-based and synthetic-based ones according to raw material source. The natural system mainly includes starch system, cellulose system, etc., and the synthetic system includes polyacrylonitrile system, polyvinyl alcohol system, polyacrylamide system, polyoxyethylene system, copolymerization system, etc. The existing synthesis methods include reversed-phase suspension polymerization and radiation polymerization, and the two methods have complex reaction, higher cost and lower water absorption.
Therefore, the present inventors have developed a method for synthesizing an acrylic acid type super absorbent resin by an aqueous solution polymerization method to solve the above problems.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for synthesizing acrylic acid type super absorbent resin, which aims at overcoming the defects of the prior art. The method adopts nitrogen as protective gas, and oxygen is not involved in the reaction process; the N, N-methylene bisacrylamide is used as a cross-linking agent, the cross-linking degree of the product is ensured, the reaction process is simple, and the prepared acrylic acid type super absorbent resin has high water absorption.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for synthesizing an acrylic acid type super absorbent resin is characterized by comprising the following steps:
s1, measuring a certain amount of acrylic acid, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of normal-temperature water bath for neutralization reaction, stirring in the dropwise adding process, keeping the reading of the thermometer less than 40 ℃, and finishing the reaction to obtain a mixed solution;
s2, sequentially adding deionized water and a cross-linking agent into the mixed solution, introducing nitrogen, stirring for 15min until the mixture is uniformly mixed, then adding an initiator, and reacting for 3h at the temperature of 40-80 ℃ to obtain gel-like super absorbent resin; drying the gel-like super absorbent resin to obtain the acrylic acid type super absorbent resin.
Preferably, the neutralization degree of acrylic acid in the neutralization reaction in S1 is 50% to 80%.
Preferably, the amount of the cross-linking agent in S2 is 0.01g to 0.05g, and the cross-linking agent is N, N-methylene bisacrylamide.
Preferably, the initiator in S2 is used in an amount of 0.01g to 0.095g, and the initiator is potassium persulfate.
Preferably, the dosage of the deionized water in the S2 is 20ml to 30ml; the purity of the nitrogen gas was 99.999%.
Preferably, the drying temperature in S2 is 80 ℃, and the drying time is 8h.
Compared with the prior art, the invention has the following advantages:
the invention has higher water absorption performance than the prior synthesized resin, and has simple synthesis method and cost saving. The water absorption can reach 1000-2000 (g/g), and the water absorption of the previously synthesized resin is only 400-1000 (g/g); and the reaction time is shorter than before, thereby greatly improving the synthesis efficiency.
The technical solution of the present invention will be described in further detail by examples.
Detailed Description
Example 1
The method for synthesizing the acrylic acid type super absorbent resin of the embodiment comprises the following steps:
s1, measuring acrylic acid into a four-necked bottle, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of a normal-temperature (25 ℃) water bath for neutralization reaction, wherein the neutralization degree of the acrylic acid is 50%, continuously stirring in the dropwise adding process, keeping the reading of the thermometer less than 40 ℃, and obtaining a mixed solution after the reaction is finished;
s2, sequentially adding 20ml of deionized water and 0.0126g of N, N-methylene bisacrylamide into the mixed solution, introducing nitrogen with the purity of 99.999% for protection, stirring for 15min until the mixture is uniformly mixed, then adding 0.01g of potassium persulfate, and reacting for 3h at the temperature of 60 ℃ to obtain the gel-like super absorbent resin; and (3) drying the gel-like super absorbent resin in an oven at the temperature of 80 ℃ for 8 hours to obtain the acrylic acid type super absorbent resin.
The water absorption of the acrylic acid type super absorbent resin prepared in this example was 2000g/g.
Comparative example 1
The method for synthesizing the acrylic acid type super absorbent resin of the present comparative example comprises the steps of:
s1, measuring acrylic acid in a four-necked bottle, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of a normal-temperature (21 ℃) water bath to perform a neutralization reaction, wherein the neutralization degree of the acrylic acid is 50%, continuously stirring in the dropwise adding process, and keeping the indication number of the thermometer less than 40 ℃ to obtain a mixed solution;
s2, sequentially adding 20ml of deionized water and 0.0126g of polyvinyl alcohol into the mixed solution, introducing nitrogen with the purity of 99.999% for protection, stirring for 15min until the mixture is uniformly mixed, then adding 0.01g of potassium persulfate, and reacting for 3h at the temperature of 60 ℃ to obtain the gelatinous super absorbent resin; and (3) drying the gel-like super absorbent resin in an oven at the temperature of 80 ℃ for 8 hours to obtain the acrylic acid type super absorbent resin.
The acrylic acid type super absorbent resin prepared in this comparative example was examined to have a water absorption of 650g/g.
It can be seen that when the crosslinking agent in comparative example 1 is polyvinyl alcohol, the water absorption of the obtained acrylic super absorbent resin is greatly reduced.
A large number of experiments show that when the dosage of the crosslinking agent (N, N-methylene-bisacrylamide) is too large, the crosslinking density is high, the network structure is reduced, and the water absorption performance is lowered; the proper amount of the cross-linking agent can form a larger network structure, and the larger the network is, the smaller the elastic contraction capacity of the network is, and the higher the water absorption capacity of the resin is; the molecular weight is reduced due to the excessive consumption of the initiator (potassium persulfate), the reaction speed is too fast and is difficult to control, and the reaction heat is difficult to remove in time, so that the rapid polymerization is easy to generate; the initiator dosage is too small, so that the reaction speed is relatively low; when polyvinyl alcohol is used as a crosslinking agent, the crosslinking density of the resin and the mechanical strength thereof can be increased, but the network structure formed becomes small and the water absorption property is lowered.
Example 2
The method for synthesizing the acrylic acid type super absorbent resin of the embodiment comprises the following steps:
s1, measuring acrylic acid into a four-necked bottle, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of a normal-temperature (24 ℃) water bath for neutralization reaction, wherein the neutralization degree of the acrylic acid is 80%, continuously stirring in the dropwise adding process, and keeping the reading of the thermometer to be less than 40 ℃ to obtain a mixed solution;
s2, sequentially adding 30ml of deionized water and 0.05gN, N-methylene-bisacrylamide into the mixed solution, introducing nitrogen with the purity of 99.999% for protection, stirring for 15min until the mixture is uniformly mixed, then adding 0.095g of potassium persulfate, and reacting for 3h at the temperature of 40 ℃ to obtain the gel-like super absorbent resin; and (3) drying the gel-like super absorbent resin in an oven at the temperature of 80 ℃ for 8 hours to obtain the acrylic acid type super absorbent resin.
The water absorption of the acrylic super absorbent resin prepared in this example was 1200g/g.
Example 3
The method for synthesizing the acrylic acid type super absorbent resin of the embodiment comprises the following steps:
s1, measuring acrylic acid in a four-necked bottle, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of normal-temperature (22 ℃) water bath for neutralization reaction, wherein the neutralization degree of the acrylic acid is 60%, continuously stirring in the dropwise adding process, and keeping the indication number of the thermometer less than 40 ℃ to obtain a mixed solution;
s2, sequentially adding 25ml of deionized water and 0.01gN, N-methylene bisacrylamide into the mixed solution, introducing nitrogen with the purity of 99.999% for protection, stirring for 15min until the mixture is uniformly mixed, then adding 0.06g of potassium persulfate, and reacting for 3h at the temperature of 80 ℃ to obtain the gel-like super absorbent resin; and (3) drying the gel-like super absorbent resin in an oven at the temperature of 80 ℃ for 8h to obtain the acrylic acid type super absorbent resin.
The water absorption of the acrylic acid type super absorbent resin prepared in this example was found to be 1700g/g.
Example 4
The method for synthesizing the acrylic acid type super absorbent resin of the embodiment comprises the following steps:
s1, measuring acrylic acid into a four-necked bottle, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of a water bath at normal temperature (21 ℃) to perform a neutralization reaction, wherein the neutralization degree of the acrylic acid is 70%, continuously stirring in the dropwise adding process, and keeping the reading of the thermometer to be less than 40 ℃ to obtain a mixed solution;
s2, adding 27ml of deionized water and 0.03gN, N-methylene-bisacrylamide into the mixed solution in sequence, introducing nitrogen with the purity of 99.999% for protection, stirring for 15min until the mixture is uniformly mixed, adding 0.07g of potassium persulfate, and reacting for 3h at the temperature of 70 ℃ to obtain the gel-like super absorbent resin; and (3) drying the gel-like super absorbent resin in an oven at the temperature of 80 ℃ for 8h to obtain the acrylic acid type super absorbent resin.
The water absorption of the acrylic acid type super absorbent resin prepared in this example was 1500g/g.
The above examples are preferred embodiments of the present invention and are not intended to limit the present invention in any way. Any simple modifications, alterations and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (6)
1. A method for synthesizing an acrylic acid type super absorbent resin is characterized by comprising the following steps:
s1, measuring a certain amount of acrylic acid, inserting a thermometer into the acrylic acid, dropwise adding a sodium hydroxide solution with the mass fraction of 40% into the acrylic acid under the condition of normal-temperature water bath for neutralization reaction, stirring in the dropwise adding process, keeping the reading of the thermometer less than 40 ℃, and finishing the reaction to obtain a mixed solution;
s2, sequentially adding deionized water and a cross-linking agent into the mixed solution, introducing nitrogen, stirring for 15min until the mixture is uniformly mixed, then adding an initiator, and reacting for 3h at the temperature of 40-80 ℃ to obtain gel-like super absorbent resin; drying the gel-like super absorbent resin to obtain the acrylic acid type super absorbent resin.
2. The method according to claim 1, wherein the neutralization degree of acrylic acid in the neutralization reaction in S1 is 50% to 80%.
3. The method of claim 1, wherein the amount of the cross-linking agent used in S2 is 0.01g to 0.05g, and the cross-linking agent is N, N-methylenebisacrylamide.
4. The method of claim 1, wherein the amount of the initiator used in S2 is 0.01g to 0.095g, and the initiator is potassium persulfate.
5. The method for synthesizing acrylic acid type super absorbent resin according to claim 1, wherein the amount of the deionized water used in S2 is 20ml to 30ml; the purity of the nitrogen gas was 99.999%.
6. The method according to claim 1, wherein the drying temperature in S2 is 80 ℃ and the drying time is 8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211181183.2A CN115490802A (en) | 2022-09-27 | 2022-09-27 | Method for synthesizing acrylic acid type super absorbent resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211181183.2A CN115490802A (en) | 2022-09-27 | 2022-09-27 | Method for synthesizing acrylic acid type super absorbent resin |
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| CN115490802A true CN115490802A (en) | 2022-12-20 |
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| CN202211181183.2A Pending CN115490802A (en) | 2022-09-27 | 2022-09-27 | Method for synthesizing acrylic acid type super absorbent resin |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214616A (en) * | 2013-04-16 | 2013-07-24 | 华南理工大学 | Preparation method of porous-super-absorbent resin |
| CN103342779A (en) * | 2013-05-23 | 2013-10-09 | 内蒙古大学 | Novel technology of preparing super absorbent resin by using carboxymethyl potato starch ether sodium |
| CN105622826A (en) * | 2014-11-06 | 2016-06-01 | 陈玉梅 | Novel synthesis technology of sodium polyacrylate super absorbent resin |
| CN110092862A (en) * | 2019-05-27 | 2019-08-06 | 廊坊师范学院 | A kind of preparation method of acrylic type water-absorbing resin |
| US20200115508A1 (en) * | 2017-12-08 | 2020-04-16 | Lg Chem, Ltd. | Preparation Method of Super Absorbent Polymer |
-
2022
- 2022-09-27 CN CN202211181183.2A patent/CN115490802A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214616A (en) * | 2013-04-16 | 2013-07-24 | 华南理工大学 | Preparation method of porous-super-absorbent resin |
| CN103342779A (en) * | 2013-05-23 | 2013-10-09 | 内蒙古大学 | Novel technology of preparing super absorbent resin by using carboxymethyl potato starch ether sodium |
| CN105622826A (en) * | 2014-11-06 | 2016-06-01 | 陈玉梅 | Novel synthesis technology of sodium polyacrylate super absorbent resin |
| US20200115508A1 (en) * | 2017-12-08 | 2020-04-16 | Lg Chem, Ltd. | Preparation Method of Super Absorbent Polymer |
| CN110092862A (en) * | 2019-05-27 | 2019-08-06 | 廊坊师范学院 | A kind of preparation method of acrylic type water-absorbing resin |
Non-Patent Citations (2)
| Title |
|---|
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Application publication date: 20221220 |