CN102432721B - Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 - Google Patents
Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 Download PDFInfo
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- CN102432721B CN102432721B CN2011102713705A CN201110271370A CN102432721B CN 102432721 B CN102432721 B CN 102432721B CN 2011102713705 A CN2011102713705 A CN 2011102713705A CN 201110271370 A CN201110271370 A CN 201110271370A CN 102432721 B CN102432721 B CN 102432721B
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- molecular weight
- polyacrylamide
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- low molecular
- acrylamide
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003999 initiator Substances 0.000 claims abstract description 21
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 7
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims abstract description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 238000010992 reflux Methods 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 10
- 238000010189 synthetic method Methods 0.000 claims description 9
- 239000004160 Ammonium persulphate Substances 0.000 claims description 8
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims 2
- 239000000243 solution Substances 0.000 abstract description 25
- 239000007864 aqueous solution Substances 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 238000009941 weaving Methods 0.000 abstract description 2
- 150000002576 ketones Chemical class 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000007957 coemulsifier Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 5
- 238000012673 precipitation polymerization Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- -1 pottery Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CDULGHZNHURECF-UHFFFAOYSA-N 2,3-dimethylaniline 2,4-dimethylaniline 2,5-dimethylaniline 2,6-dimethylaniline 3,4-dimethylaniline 3,5-dimethylaniline Chemical group CC1=CC=C(N)C(C)=C1.CC1=CC=C(C)C(N)=C1.CC1=CC(C)=CC(N)=C1.CC1=CC=C(N)C=C1C.CC1=CC=CC(N)=C1C.CC1=CC=CC(C)=C1N CDULGHZNHURECF-UHFFFAOYSA-N 0.000 description 1
- 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 1
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000037048 polymerization activity Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- 230000001755 vocal effect Effects 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a method for synthesizing a polyacrylamide having low-molecular weight of 200000 to 450000, and belongs to the field of polymer synthesis. The method adopts an aqueous solution polymerization method, and utilizes C3-C4 ketone agents as a heat removal solvent and a chain transfer agent, ammonium persulfate as an initiator and ethylenediaminetetraacetic acid disodium salt as a stabilizing agent. The method comprises the following steps that a polymerization reaction is caused at a backflow temperature by continuous, respective and dropwise addition of an acrylamide solution and an initiator solution; and through adjustment on use amounts of the C3-C4 ketone agents and ammonium persulfate, the polyacrylamide having low-molecular weight of 200000 to 450000 is obtained. The polyacrylamide having low-molecular weight of 200000 to 450000 has good water solubility, and is suitable as a polymer co-emulsifier, a dispersant, an adhesive, a tackifier, a weaving auxiliary agent and the like.
Description
Technical field
The present invention relates to the synthetic method of macromolecular compound polyacrylamide, relate in particular to a kind of molecular weight and be (20～45) * 10
4The synthetic method of low molecular weight polyacrylamide belongs to the Polymer Synthesizing field.
Background technology
Lower molecular weight (molecular weight＜100 * 10
4) polyacrylamide is applied to fields such as building decoration, papermaking, weaving, printing and dyeing, refractory materials, pottery, chemical industry as tackiness agent, additive, dispersion agent, emulsifying agent, tackifier.Because the polymerization activity height of acrylamide monomer, reaction heat effect is big, and the laboratory is synthetic directly to prepare relatively difficulty of low molecular weight polyacrylamide with industrial production.
Adopt precipitation polymerization can synthesize low molecular weight polyacrylamide, but building-up process is used a large amount of organic solvents, has certain unsafe factor." Huabei Polytechnical College journal " (2000 the 21st the 4th phases of volume, 312～315 pages) to adopt acetone in " precipitation polymerization method synthesizes polyacrylamide " be solvent, with BPO-N, the N xylidine is a redox initiator, under 12-30% monomer mass percentage concentration, the synthetic Molecular Weight for Polyacrylamide is (60～90) * 10
4" Fujian Normal University's journal (natural science edition) " (2002 the 18th the 4th phases of volume, 61～63 pages) in " precipitation polymerization method prepares low molecular weight polyacrylamide ", reported that employing ethanol and acetone are as solvent, with AIBN is initiator, by adjusting the mass ratio of ethanol and acetone, synthesized low molecular weight polyacrylamide, be respectively 5% and at 30% o'clock at the monomer mass percentage concentration, the synthetic Molecular Weight for Polyacrylamide is minimum to be respectively 2 * 10
4With 9.3 * 10
4
The aqueous solution polymerization low molecular weight polyacrylamide also has a small amount of report." Anhui chemical industry " (1992 the 2nd phases, 17～19 pages) reported that at the monomer mass percentage concentration be at 20% o'clock in " preparation of low molecular weight polyacrylamide and application ", with the ammonium persulfate-sodium bisulfite is initiator system, synthesizes molecular weight and is (23～40) * 10
4Polyacrylamide; " Nantong Vocational College's journal " (15 the 2nd phases of volume of calendar year 2001,21～23 pages) reported that at the monomer mass percentage concentration be at 10% o'clock in " polyacrylamide synthetic with use ", with Potassium Persulphate-nitrogen tripropyl amine is initiator system, and synthesizing molecular weight is 62 * 10
4Polyacrylamide.The main inventor of present technique in ZL03126303.8, was chain-transfer agent and heat transferring solvent with the Virahol once, was 30% o'clock at the monomer mass percentage concentration, synthesized molecular weight (2～12) * 10
4Polyacrylamide; In ZL200810048457.5, be heat transferring solvent with ethanol, sodium formiate is a chain-transfer agent, under 40% monomer mass percentage concentration, the synthetic Molecular Weight for Polyacrylamide is (1～2.6) * 10
4, but can not synthetic molecular weight greater than 12 * 10
4Low molecular weight polyacrylamide.The present invention improved in an enterprising step of above invention basis, had synthesized molecular weight and had been (20～45) * 10
4Low molecular weight polyacrylamide.
Summary of the invention
The object of the present invention is to provide a kind of employing aqueous solution polymerization, molecular weight ranges is in (20～45) * 10
4 ,The synthetic method of water-soluble good low molecular weight polyacrylamide.
In order to realize the object of the invention, technical scheme is as follows: adopt water solution polymerization process, with C
3～C
4Ketone is heat transferring solvent and chain-transfer agent, and ammonium persulphate is an initiator, and disodium EDTA (EDTA) is a stablizer, and by the synthetic low molecular weight polyacrylamide of the consumption of regulating chain-transfer agent and initiator ammonium persulfate, concrete steps are as follows:
⑴ monomer preparation: the 100.0g mass percent concentration is 40% acrylamide solution, and adding water, to be mixed with mass percent concentration be 13.50%～16.5% acrylamide solution, and 0.2～0.6g ammonium persulphate is dissolved in the 10.0g water and is mixed with initiator solution;
⑵ add 5.0～20.0g C in reactor
3～C
4Ketones solvent, the above-mentioned acrylamide solution for preparing of 20.0g, 3.0g mass percent concentration are 3% the above-mentioned ammonium persulfate initiator solution for preparing of disodium EDTA solution, 1.2g, stir, and progressively are warming up to backflow;
⑶ keeping under stirring and the reflux state, drips remaining acrylamide soln and remaining ammonium persulfate initiator solution respectively from constant pressure funnel continuously, dropwised in 1.5 hours;
⑷ reflux and keep reaction 2 hours, steams C under the atmospheric pressure state
3～C
4Ketones solvent and water mixture, cooling obtains the low molecular weight polyacrylamide aqueous solution.
Measure the low molecular weight polyacrylamide that synthesizes according to GB17514-1998, its molecular weight is (20～45) * 10
4
Beneficial effect of the present invention is: this synthetic method adopts aqueous solution polymerization, and molecular weight is controlled easily, and is simple to operate, can synthesize the low molecular weight polyacrylamide of specified molecular weight section.Method synthetic low molecular weight polyacrylamide has good water-solubility thus, is applicable to polymeric retention aid emulsifying agent, dispersion agent, tackiness agent, tackifier, textile auxiliary agent etc.
Embodiment
For the present invention will be described better, it is as follows to enumerate embodiment:
Embodiment 1
⑴ monomer preparation: the 100.0g mass percent concentration is 40% acrylamide solution, adding water 150.0g, to be mixed with mass percent concentration be 16% acrylamide solution 250.0g, and the 0.35g ammonium persulphate is dissolved in the 10.0g water and is mixed with ammonium persulfate initiator solution;
⑵ add 20.0g acetone, the above-mentioned acrylamide monomer solution for preparing of 20g, 3.0g mass percent concentration in the 500ml flask be 3% the above-mentioned ammonium persulfate initiator solution for preparing of EDTA solution, 1.2g, stir, progressively be warming up to backflow, kept reflux temperature 10 minutes;
⑶ keeping under stirring and the reflux state, drips remaining acrylamide monomer solution and remaining ammonium persulfate initiator solution respectively from constant pressure funnel continuously, dropwised in 1.5 hours;
⑷ reflux and keep reaction 2 hours, steams acetone and water mixture 20.0g under the atmospheric pressure state, and cooling obtains the low molecular weight polyacrylamide aqueous solution.
Measuring its molecular weight by GB17514-1998 is 21.5 * 10
4
Embodiment 2
With embodiment 1, changing the acetone consumption in the step (2) is 15.0g, and step (4) steams acetone and water mixture 15g, obtains the low molecular weight polyacrylamide aqueous solution, and measuring its molecular weight by GB17514-1998 is 28.9 * 10
4
Embodiment 3
With embodiment 1, changing the acetone consumption in the step (2) is 10.0g, and step (4) steams acetone and water mixture 10g, obtains the low molecular weight polyacrylamide aqueous solution, and measuring its molecular weight by GB17514-1998 is 30.0 * 10
4
Embodiment 4
With embodiment 1, changing the acetone consumption in the step (2) is 6.0g, and step (4) steams acetone and water mixture 6.0g, obtains the low molecular weight polyacrylamide aqueous solution, and measuring its molecular weight by GB17514-1998 is 38.5 * 10
4
Embodiment 5
⑴ monomer preparation: the 100.0g mass percent concentration is 40% acrylamide solution, adding water 150.0g, to be mixed with mass percent concentration be 16% acrylamide solution 250.0g, and the 0.25g ammonium persulphate is dissolved in the 10.0g water and is mixed with ammonium persulfate initiator solution;
⑵ add 10.0g acetone, the above-mentioned acrylamide monomer solution for preparing of 20g, 3.0g mass percent concentration in the 500ml flask be 3% the above-mentioned ammonium persulfate initiator solution for preparing of EDTA solution, 1.2g, stir, progressively be warming up to backflow, kept reflux temperature 10 minutes;
⑶ keeping under stirring and the reflux state, drips remaining acrylamide monomer solution and remaining ammonium persulfate initiator solution respectively from constant pressure funnel continuously, dropwised in 1.5 hours;
⑷ reflux and keep reaction 2 hours, steams acetone and water mixture 10.0g under the atmospheric pressure state, and cooling obtains the low molecular weight polyacrylamide aqueous solution.
Measuring its molecular weight by GB17514-1998 is 41.4 * 10
4
Embodiment 6
With embodiment 5, changing the ammonium persulphate consumption in the step (1) is 0.45g, obtains low molecular weight polyacrylamide, and measuring its molecular weight by GB17514-1998 is 22.2 * 10
4
Embodiment 7
With embodiment 5, changing the ammonium persulphate consumption in the step (1) is 0.51g, obtains low molecular weight polyacrylamide, and measuring its molecular weight by GB17514-1998 is 21.0 * 10
4
Claims (4)
1. a molecular weight is the synthetic method of 20～450,000 low molecular weight polyacrylamide, it is characterized in that: adopt water solution polymerization process, with C
3～C
4Ketone is heat transferring solvent and chain-transfer agent, and ammonium persulphate is an initiator, and disodium EDTA is a stablizer, and by the synthetic low molecular weight polyacrylamide of the consumption of regulating chain-transfer agent and initiator ammonium persulfate, concrete steps are as follows:
⑴ monomer preparation: the 100.0g mass percent concentration is 40% acrylamide solution, and adding water, to be mixed with mass percent concentration be 13.50%～16.5% acrylamide solution, and 0.2～0.6g ammonium persulphate is dissolved in the 10.0g water and is mixed with initiator solution;
⑵ add 5.0～20.0g C in reactor
3～C
4Ketones solvent, the above-mentioned acrylamide solution for preparing of 20.0g, 3.0g mass percent concentration are 3% the above-mentioned ammonium persulfate initiator solution for preparing of disodium EDTA solution, 1.2g, stir, and progressively are warming up to backflow;
⑶ keeping under stirring and the reflux state, drips remaining acrylamide soln and remaining ammonium persulfate initiator solution respectively from constant pressure funnel continuously, dropwised in 1.5 hours;
⑷ reflux and keep reaction 2 hours, steams C under the atmospheric pressure state
3～C
4Ketones solvent and water mixture, cooling obtains low molecular weight polyacrylamide.
2. molecular weight is the synthetic method of 20～450,000 low molecular weight polyacrylamide according to claim 1, and it is characterized in that: the mass percent concentration of the acrylamide in the step (1) is 15%.
3. molecular weight as claimed in claim 1 is the synthetic method of 20～450,000 low molecular weight polyacrylamide, it is characterized in that the C in the step (2)
3～C
4Ketones solvent is acetone or butanone.
4. molecular weight as claimed in claim 1 is the synthetic method of 20～450,000 low molecular weight polyacrylamide, it is characterized in that the reflux temperature in the step (3) is 82～92 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102713705A CN102432721B (en) | 2011-09-14 | 2011-09-14 | Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102713705A CN102432721B (en) | 2011-09-14 | 2011-09-14 | Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 |
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| CN102432721A CN102432721A (en) | 2012-05-02 |
| CN102432721B true CN102432721B (en) | 2013-07-31 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435727B (en) * | 2013-09-06 | 2015-07-01 | 河南省科学院高新技术研究中心 | Preparation method of low molecular weight (LMW) polyacrylamide with molecular weight of 0.4-1 million |
| CN105111343A (en) * | 2015-09-23 | 2015-12-02 | 山东聚鑫化工有限公司 | Preparation method of salt-resistant low molecular weight polyacrylamide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0048094A1 (en) * | 1980-09-08 | 1982-03-24 | Rohm And Haas Company | Method of producing acrylamide homopolymers and copolymers useful as flow modifiers in aqueous multiphase systems and compositions containing them |
| US5932671A (en) * | 1997-06-04 | 1999-08-03 | Phillips Petroleum Company | Polymerization process |
| CN1580086A (en) * | 2003-08-12 | 2005-02-16 | 河南省科学院质量检验与分析测试研究中心 | Method for preparing low molecular weight polyacrylamide |
| CN1887923A (en) * | 2006-07-26 | 2007-01-03 | 河南省科学院质量检验与分析测试研究中心 | Prepn of low molecular weight polyacrylamide |
-
2011
- 2011-09-14 CN CN2011102713705A patent/CN102432721B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0048094A1 (en) * | 1980-09-08 | 1982-03-24 | Rohm And Haas Company | Method of producing acrylamide homopolymers and copolymers useful as flow modifiers in aqueous multiphase systems and compositions containing them |
| US5932671A (en) * | 1997-06-04 | 1999-08-03 | Phillips Petroleum Company | Polymerization process |
| CN1580086A (en) * | 2003-08-12 | 2005-02-16 | 河南省科学院质量检验与分析测试研究中心 | Method for preparing low molecular weight polyacrylamide |
| CN1887923A (en) * | 2006-07-26 | 2007-01-03 | 河南省科学院质量检验与分析测试研究中心 | Prepn of low molecular weight polyacrylamide |
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