CN104693362A - Method for preparing cellulose graft copolymer super absorbent resin - Google Patents
Method for preparing cellulose graft copolymer super absorbent resin Download PDFInfo
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- CN104693362A CN104693362A CN201510056714.9A CN201510056714A CN104693362A CN 104693362 A CN104693362 A CN 104693362A CN 201510056714 A CN201510056714 A CN 201510056714A CN 104693362 A CN104693362 A CN 104693362A
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- Prior art keywords
- super absorbent
- absorbent resin
- preparation
- add
- graft copolymerization
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- 239000011347 resin Substances 0.000 title claims abstract description 27
- 229920005989 resin Polymers 0.000 title claims abstract description 27
- 239000002250 absorbent Substances 0.000 title claims abstract description 19
- 230000002745 absorbent Effects 0.000 title claims abstract description 19
- 229920002678 cellulose Polymers 0.000 title claims abstract description 16
- 239000001913 cellulose Substances 0.000 title claims abstract description 16
- 229920000578 graft polymer Polymers 0.000 title abstract 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 11
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical class [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 7
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L Potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000007334 copolymerization reaction Methods 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 229940105329 Carboxymethylcellulose Drugs 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 Dehydrated Alcohol Drugs 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N N,N'-Methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000010612 desalination reaction Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000012456 homogeneous solution Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 210000001736 Capillaries Anatomy 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 1
- 229920002521 Macromolecule Polymers 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Abstract
The invention discloses a method for preparing a cellulose graft copolymer super absorbent resin. The method comprises the following steps: (1) preparing the sodium carboxymethyl cellulose salt; (2) preparing the sodium carboxymethyl cellulose graft copolymer super absorbent resin: dissolving the sodium carboxymethyl cellulose by distilling water, introducing nitrogen to expel oxygen for 0.5h, in turn adding the monomer acrylic acid, acrylic amide, sodium p-styrenesulfonate and an initiator potassium peroxodisulfate which is 2% of the total mass of the monomer, heating to the temperature of 70 DEG C in a reaction kettle, reacting for 10 min, adding a cross-linking agent, performing thermostatic reaction for 2h, washing the product for many times by the absolute ethyl alcohol, drying to constant weight in a drying device at the temperature of 80 DEG C, and smashing by a pulverizer to obtain the sodium carboxymethyl cellulose graft copolymer super absorbent resin. Plenty of small and dense holes are arranged on the surface of the sodium carboxymethyl cellulose graft copolymer super absorbent resin, the capillary action can be well played, the water absorption and water retention capacity can be reinforced, and the water can be rapidly diffused to the inside of the resin granule so that the water absorption rate can be increased.
Description
Technical field
The invention belongs to the preparing technical field of water-retaining agent, particularly relate to a kind of preparation method of Graft Copolymerization of Cellulose super absorbent resin.
Background technology
High hydrophilous resin is through the appropriately crosslinked new functional macromolecule material with three-dimensional network-like structure, is usually also called " water-holding agent ", " high water absorbency polymer ", " super strength water absorbent " etc.Synthesized through polyreaction by lower-molecular substance or be made up through chemical reaction of macromolecular compound; that a kind of cross-linking density is low, water insoluble, the functional high molecule material of high-water expansion; its molecular chain has a lot of strongly hydrophilic group as carboxyl, amide group, ester group etc.; can specific absorption own wt many hundred times even moisture of several thousand times or decades of times more than own wt salt solution and in gel; and there is good water retention property, be now widely used in the fields such as industry, agricultural, food, health care, daily necessities and environment protection.
The raw material that the raw material preparing super absorbent resin use at present is mainly synthesized by petroleum refining and a small amount of cellulose materials, starch and derivative thereof.Although because the prices such as synthesis material is expensive, Mierocrystalline cellulose, starch are lower, Application and Development is less with production, and rate of water absorption is slower.
Summary of the invention
For the problems referred to above, the invention provides a kind of preparation method of Graft Copolymerization of Cellulose super absorbent resin.
The technical solution used in the present invention:
A preparation method for Graft Copolymerization of Cellulose super absorbent resin, its step is,
(1) sodium carboxymethyl-cellulose preparation: be 3.4:1:35.4 with mass ratio by carboxymethyl cellulose, sodium hydroxide and water, being hybridly prepared into homogeneous solution adds in reactor, add the epoxy chloropropane accounting for gross weight 2.6%, after being warming up to 40 DEG C of reaction 20h, with methanol solution dehydration, the desalination of 90%, obtain white particles shape Xylo-Mucine;
(2) Xylo-Mucine graft copolymerization High hydrophilous resin preparation: Xylo-Mucine distilled water is dissolved, pass into nitrogen flooding oxygen 0.5h, add successively monomeric acrylic, acrylamide, sodium p styrene sulfonate and for monomer total mass 2% initiator potassium persulfate, reactor is warming up to 70 DEG C and carries out reaction 10min, add linking agent, after isothermal reaction 2h, by dehydrated alcohol repeatedly washed product, constant weight is dried in the drying plant of 80 DEG C, pulverize with pulverizer, obtain Xylo-Mucine graft copolymerization High hydrophilous resin.
The preparation method of described Graft Copolymerization of Cellulose super absorbent resin, in its step (2), the ratio of monomeric acrylic, acrylamide, sodium p styrene sulfonate add-on is 2:2:1.
The preparation method of described Graft Copolymerization of Cellulose super absorbent resin, in its step (2), the add-on of Xylo-Mucine is 9% of monomer total mass.
The preparation method of described Graft Copolymerization of Cellulose super absorbent resin, linking agent used in its step (2) is N,N methylene bis acrylamide, and add-on is 1% of monomer total mass.
Beneficial effect of the present invention: there is hole small and dense in a large number on Carboxymethyl Cellulose Graft Acrylic Acid Copolymer surface of the present invention, better can play capillary action, strengthen water suction and water retention capacity, and water rapid diffusion can be made to enter resin particle inside thus improve rate of water absorption.
Embodiment
A preparation method for Graft Copolymerization of Cellulose super absorbent resin, its step is,
(1) sodium carboxymethyl-cellulose preparation: be 3.4:1:35.4 with mass ratio by carboxymethyl cellulose, sodium hydroxide and water, being hybridly prepared into homogeneous solution adds in reactor, add the epoxy chloropropane accounting for gross weight 2.6%, after being warming up to 40 DEG C of reaction 20h, with methanol solution dehydration, the desalination of 90%, obtain white particles shape Xylo-Mucine;
(2) Xylo-Mucine graft copolymerization High hydrophilous resin preparation: 18g Xylo-Mucine distilled water is dissolved, pass into nitrogen flooding oxygen 0.5h, add monomeric acrylic 80g, acrylamide 80g, sodium p styrene sulfonate 40g and 4g initiator potassium persulfate successively, reactor is warming up to 70 DEG C and carries out reaction 10min, add N, N-methylene-bisacrylamide 2g, after isothermal reaction 2h, by dehydrated alcohol repeatedly washed product, constant weight is dried in the drying plant of 80 DEG C, pulverize with pulverizer, obtain Xylo-Mucine graft copolymerization High hydrophilous resin.
Claims (4)
1. a preparation method for Graft Copolymerization of Cellulose super absorbent resin, is characterized in that, its preparation process is,
(1) sodium carboxymethyl-cellulose preparation: be 3.4:1:35.4 with mass ratio by carboxymethyl cellulose, sodium hydroxide and water, being hybridly prepared into homogeneous solution adds in reactor, add the epoxy chloropropane accounting for gross weight 2.6%, after being warming up to 40 DEG C of reaction 20h, with methanol solution dehydration, the desalination of 90%, obtain white particles shape Xylo-Mucine;
(2) Xylo-Mucine graft copolymerization High hydrophilous resin preparation: Xylo-Mucine distilled water is dissolved, pass into nitrogen flooding oxygen 0.5h, add successively monomeric acrylic, acrylamide, sodium p styrene sulfonate and for monomer total mass 2% initiator potassium persulfate, reactor is warming up to 70 DEG C and carries out reaction 10min, add linking agent, after isothermal reaction 2h, by dehydrated alcohol repeatedly washed product, constant weight is dried in the drying plant of 80 DEG C, pulverize with pulverizer, obtain Xylo-Mucine graft copolymerization High hydrophilous resin.
2. the preparation method of Graft Copolymerization of Cellulose super absorbent resin according to claim 1, is characterized in that, in step (2), the ratio of monomeric acrylic, acrylamide, sodium p styrene sulfonate add-on is 2:2:1.
3. the preparation method of Graft Copolymerization of Cellulose super absorbent resin according to claim 1, is characterized in that, in step (2), the add-on of Xylo-Mucine is 9% of monomer total mass.
4. the preparation method of Graft Copolymerization of Cellulose super absorbent resin according to claim 1, is characterized in that, linking agent used in step (2) is N,N methylene bis acrylamide, and add-on is 1% of monomer total mass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510056714.9A CN104693362A (en) | 2015-02-03 | 2015-02-03 | Method for preparing cellulose graft copolymer super absorbent resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510056714.9A CN104693362A (en) | 2015-02-03 | 2015-02-03 | Method for preparing cellulose graft copolymer super absorbent resin |
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| Publication Number | Publication Date |
|---|---|
| CN104693362A true CN104693362A (en) | 2015-06-10 |
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| CN201510056714.9A Pending CN104693362A (en) | 2015-02-03 | 2015-02-03 | Method for preparing cellulose graft copolymer super absorbent resin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957390A (en) * | 2016-01-12 | 2017-07-18 | 鲁东大学 | A kind of method that inorganic matter crosslinking prepares natural macromolecule modification polyacrylic acid high water absorptive resin |
| CN107938341A (en) * | 2017-12-04 | 2018-04-20 | 宜宾惠美纤维新材料股份有限公司 | A kind of preparation method of deodorization fiber cellulose fiber |
| CN109021170A (en) * | 2017-06-09 | 2018-12-18 | 天津科技大学 | A kind of preparation method of salt-resistance Nano/micron filament fibers element gel |
| CN110404516A (en) * | 2019-08-14 | 2019-11-05 | 徐州工程学院 | A kind of adsorption of metal ions hydrogel and its preparation method and application |
| CN112126305A (en) * | 2020-09-15 | 2020-12-25 | 中山市富日印刷材料有限公司 | Preparation method of environment-friendly printing plate protective adhesive |
| CN114276045A (en) * | 2021-12-29 | 2022-04-05 | 砼牛（上海）智能科技有限公司 | Multi-effect concrete water reducing agent |
-
2015
- 2015-02-03 CN CN201510056714.9A patent/CN104693362A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957390A (en) * | 2016-01-12 | 2017-07-18 | 鲁东大学 | A kind of method that inorganic matter crosslinking prepares natural macromolecule modification polyacrylic acid high water absorptive resin |
| CN109021170A (en) * | 2017-06-09 | 2018-12-18 | 天津科技大学 | A kind of preparation method of salt-resistance Nano/micron filament fibers element gel |
| CN107938341A (en) * | 2017-12-04 | 2018-04-20 | 宜宾惠美纤维新材料股份有限公司 | A kind of preparation method of deodorization fiber cellulose fiber |
| CN107938341B (en) * | 2017-12-04 | 2020-01-10 | 宜宾惠美纤维新材料股份有限公司 | Preparation method of deodorizing cellulose fiber |
| CN110404516A (en) * | 2019-08-14 | 2019-11-05 | 徐州工程学院 | A kind of adsorption of metal ions hydrogel and its preparation method and application |
| CN112126305A (en) * | 2020-09-15 | 2020-12-25 | 中山市富日印刷材料有限公司 | Preparation method of environment-friendly printing plate protective adhesive |
| CN114276045A (en) * | 2021-12-29 | 2022-04-05 | 砼牛（上海）智能科技有限公司 | Multi-effect concrete water reducing agent |
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Legal Events
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150610 |