CN102432721A - 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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- CN102432721A CN102432721A CN2011102713705A CN201110271370A CN102432721A CN 102432721 A CN102432721 A CN 102432721A CN 2011102713705 A CN2011102713705 A CN 2011102713705A CN 201110271370 A CN201110271370 A CN 201110271370A CN 102432721 A CN102432721 A CN 102432721A
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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 compound method of macromolecular compound SEPIGEL 305, relate in particular to a kind of molecular weight and be (20～45) * 10
4The compound method of low molecular weight polyacrylamide belongs to the Polymer Synthesizing field.
Background technology
Lower molecular weight (molecular weight<100 * 10
4) SEPIGEL 305 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 of acrylamide monomer is high, 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 SEPIGEL 305 " be solvent; With BPO-N; The N xylidine is a redox initiator, and 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 employing ethanol and acetone as solvent, with AIBN initiator; Mass ratio through adjustment 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
4SEPIGEL 305; " 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 " SEPIGEL 305 synthetic with use "; With Potassium Persulphate-nitrogen tripropyl amine is initiator system, and synthesizing molecular weight is 62 * 10
4SEPIGEL 305.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
4SEPIGEL 305; 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 goes on foot on above invention basis enterprising and improves, and has synthesized molecular weight and has 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 compound method of water-soluble good low molecular weight polyacrylamide.
In order to realize the object of the invention, technical scheme is following: 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 through the synthetic low molecular weight polyacrylamide of the consumption of regulating chain-transfer agent and initiator ammonium persulfate, concrete steps are following:
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 drum
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, from constant pressure funnel, drips remaining acrylamide soln and remaining ammonium persulfate initiator solution respectively continuously, in 1.5 hours, dropwises;
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 compound 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 following 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, from constant pressure funnel, drips remaining acrylamide monomer solution and remaining ammonium persulfate initiator solution respectively continuously, in 1.5 hours, dropwises;
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, from constant pressure funnel, drips remaining acrylamide monomer solution and remaining ammonium persulfate initiator solution respectively continuously, in 1.5 hours, dropwises;
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 compound 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 through the synthetic low molecular weight polyacrylamide of the consumption of regulating chain-transfer agent and initiator ammonium persulfate, concrete steps are following:
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 drum
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, from constant pressure funnel, drips remaining acrylamide soln and remaining ammonium persulfate initiator solution respectively continuously, in 1.5 hours, dropwises;
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.
2. molecular weight is the compound 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 acrylic amide in the step (1) is 15%.
3. molecular weight as claimed in claim 1 is the compound 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 compound 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435727A (en) * | 2013-09-06 | 2013-12-11 | 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 active Active
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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435727A (en) * | 2013-09-06 | 2013-12-11 | 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 |
| 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 |
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