CN1081200C - Method for manufacturing water-absorption material by use of supercritical fluid technology - Google Patents
Method for manufacturing water-absorption material by use of supercritical fluid technology Download PDFInfo
- Publication number
- CN1081200C CN1081200C CN98113171A CN98113171A CN1081200C CN 1081200 C CN1081200 C CN 1081200C CN 98113171 A CN98113171 A CN 98113171A CN 98113171 A CN98113171 A CN 98113171A CN 1081200 C CN1081200 C CN 1081200C
- Authority
- CN
- China
- Prior art keywords
- absorption material
- polyacrylic acid
- water absorption
- fluid technology
- sodium polyacrylate
- 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.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 238000005516 engineering process Methods 0.000 title claims abstract description 6
- 239000012530 fluid Substances 0.000 title claims abstract description 5
- 239000000463 material Substances 0.000 title abstract description 6
- 238000010521 absorption reaction Methods 0.000 title abstract 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 9
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 7
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011358 absorbing material Substances 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000004132 cross linking Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to a method for preparing a water absorption material, namely crosslinked sodium polyacrylate which is widely used as a super water absorption material. In the traditional preparation method, a dewatering and drying step consumes a large number of energy sources, and the product cost is increased. Therefore, the present invention provides the method for obtaining crosslinked polyacrylic acid in a high-pressure kettle by using a supercritical CO2 fluid technology, the polyacrylic acid treated by the method has no need to be heated and dewatered, the production cost of the water absorption material is greatly reduced, and the whiteness of the water absorption material is increased.
Description
The present invention relates to the manufacture method of water-absorbing material-crosslinking sodium polyacrylate.
Crosslinking sodium polyacrylate is a kind of super-strong water-absorbing material that development in recent years is got up, and has been widely used in sanitary materials such as soil moisturizing agent, chinampa, diaper, and field such as water-proof building material.Present traditional production method, be that vinylformic acid is neutralized to degree of neutralization 70-90% with NaOH, add water again and be made into the sodium acrylate aqueous solution, add linking agent and initiator heated polymerizable, obtain jelly dry again super-strong water-absorbing material (Zou Xinxi work " super-strong water-absorbing material "), traditional processing technology, the baking step that dewaters expends a large amount of energy, and product cost is risen.
For addressing this problem, a kind of method with supercritical fluid technology manufacturing water-absorbing material is provided, need not heating and dewater, can directly obtain the super-strong water-absorbing material of solid state.
Method implementation process provided by the invention is: vinylformic acid, polymerization starter, linking agent are added in the autoclave, the crosslinked polyacrylic acid that obtains of elder generation, and then obtain sodium polyacrylate with sodium hydroxide neutralization, its core is that the linking agent that adds is a glycerine, and charge into temperature 60-70 ℃, pressure 13-16MPa supercritical carbon dioxide, react and made the polyacrylic acid powder in 6-8 hour, this powder is dropped into the solution that sodium hydroxide and ethanol are made into, be neutralized to pH=10, remove by filter ethanol then, the air-dry crosslinking sodium polyacrylate super-strong water-absorbing material that promptly gets.Polymerization starter and dosage of crosslinking agent are the 0.2-1.0% of monomer weight, and the vinylformic acid volumetric concentration is 10-30%.
Method of the present invention can be saved the very big baking step of power consumption, and product cost is reduced greatly, and whiteness improves, for the suitability for industrialized production of product is laid a good foundation.
Add vinylformic acid 20ml in the example 1:100ml autoclave, sealing and nitrogen blowing were driven away oxygen in 10 minutes.Intensification also charges into CO
2Make to reach 65 ℃, 15MPa, stirring reaction 7 hours divides to add Diisopropyl azodicarboxylate (AIBN) 0.1 gram for three times, DAM 0.1 gram therebetween.Last cooling decompression drops into the white powder that obtains in the 500ml ethanol with 11.8 gram NaOH, reaches pH=10 after 5 hours, removes by filter ethanol, and hot blast drying promptly obtains super-strong water-absorbing material-crosslinking sodium polyacrylate, and water absorbent rate is 400 times.
Add vinylformic acid 20ml in the example 2:100ml autoclave, glycerine 0.1 gram, sealing and nitrogen blowing were driven away oxygen in 10 minutes.Intensification also charges into CO
2Make to reach 65 ℃, 15MPa, stirring reaction 7 hours divides to add Diisopropyl azodicarboxylate (AIBN) 0.1 gram for three times therebetween.Last cooling decompression toasts half an hour at 110 ℃ earlier with the white powder that obtains, and drops in the 500ml ethanol with 11.8 gram NaOH again, reach pH=10 after 5 hours, remove by filter ethanol, hot blast drying, promptly obtain super-strong water-absorbing material-crosslinking sodium polyacrylate, water absorbent rate is 200 times.
Claims (4)
1. method of making water-absorbing material with supercritical fluid technology, this method is that vinylformic acid, polymerization starter, linking agent are added in the autoclave, the first crosslinked polyacrylic acid that obtains, and then neutralize sodium polyacrylate, it is characterized in that adding glycerine and make linking agent, charge into temperature 60-70 ℃, pressure 13-16MPa supercritical carbon dioxide reacted 6-8 hour, made the polyacrylic acid powder earlier, with the alcoholic solution neutralization of sodium hydroxide, get sodium polyacrylate again.
2. according to the method described in the claim 1, it is characterized in that polymerization starter and dosage of crosslinking agent are the 0.2-1.0% of monomer weight.
3. according to the method described in the claim 1, it is characterized in that the vinylformic acid volume by volume concentration is 10-30%.
4. according to the method described in the claim 1, it is characterized in that using in the ethanolic soln of sodium hydroxide and polyacrylic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98113171A CN1081200C (en) | 1998-04-13 | 1998-04-13 | Method for manufacturing water-absorption material by use of supercritical fluid technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98113171A CN1081200C (en) | 1998-04-13 | 1998-04-13 | Method for manufacturing water-absorption material by use of supercritical fluid technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1211585A CN1211585A (en) | 1999-03-24 |
| CN1081200C true CN1081200C (en) | 2002-03-20 |
Family
ID=5222933
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98113171A Expired - Fee Related CN1081200C (en) | 1998-04-13 | 1998-04-13 | Method for manufacturing water-absorption material by use of supercritical fluid technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1081200C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314751B (en) * | 2018-01-18 | 2020-06-19 | 嘉兴学院 | Method for synthesizing diacetone acrylamide and sodium acrylate copolymer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4954562A (en) * | 1986-04-21 | 1990-09-04 | American Colloid Company | Water absorbent resins |
| WO1994015971A1 (en) * | 1993-01-18 | 1994-07-21 | Sanyo Chemical Industries, Ltd. | Process for producing water-absorbent resin |
-
1998
- 1998-04-13 CN CN98113171A patent/CN1081200C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4954562A (en) * | 1986-04-21 | 1990-09-04 | American Colloid Company | Water absorbent resins |
| WO1994015971A1 (en) * | 1993-01-18 | 1994-07-21 | Sanyo Chemical Industries, Ltd. | Process for producing water-absorbent resin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1211585A (en) | 1999-03-24 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20020320 Termination date: 20120413 |