CN102127188A - Preparation method of polyacrylamide with ultrahigh molecular weight - Google Patents
Preparation method of polyacrylamide with ultrahigh molecular weight Download PDFInfo
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- CN102127188A CN102127188A CN2010100010467A CN201010001046A CN102127188A CN 102127188 A CN102127188 A CN 102127188A CN 2010100010467 A CN2010100010467 A CN 2010100010467A CN 201010001046 A CN201010001046 A CN 201010001046A CN 102127188 A CN102127188 A CN 102127188A
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Abstract
The invention discloses a preparation method of polyacrylamide with an ultrahigh molecular weight. The method comprises the following steps of: adding a mixed monomer aqueous solution of acrylamide and sodium acrylate, a chain growth agent, an aid and a composite initiator into a polymeric kettle; introducing high-purity nitrogen for performing adiabatic copolymerization; and granulating, drying and smashing to obtain an anionic acrylamide copolymer with an ultrahigh relative molecular mass. By adopting the method, no hydrolytic reagent is added in a polymerizing process, so that harmful gases such as carbon dioxide, ammonia gas and the like are not produced, and environmental pollution is avoided.
Description
[technical field]
The present invention relates to a kind of preparation method's of acrylamide copolymer, particularly a kind of super high molecular weight polyacrylamide preparation method.
[background technology]
At present, the high molecular weight anion-polyacrylamide mainly adopts two kinds of aqueous solution polymerization method preparations: a kind of is to add hydrolytic reagent in the acrylamide polymerization process, carry out " single stage method " of polymerization hydrolysis simultaneously, its advantage is that preparation technology is simple, the polymkeric substance hydrolysis is even, solvability good, but in preparation process, can produce obnoxious flavoures such as a large amount of carbonic acid gas, ammonia, contaminate environment, and be difficult for the preparation ultra high molecular weight anion-type polyacrylamide; Another kind is not add hydrolytic reagent in the polymerization of aqueous solution of acrylamide process, carry out just adding " two step method " that hydrolytic reagent is hydrolyzed after the polymerization, its advantage is to prepare high molecular anion type polycrylamide, but its polymerization technique complexity, hydrolysis is inhomogeneous, and also can produce obnoxious flavoures such as a large amount of carbonic acid gas, Ammonia and contaminate environment in preparation process.
[summary of the invention]
The objective of the invention is to: the deficiency of existing in order to overcome " single stage method ", " two step method ", a kind of preparation method of super high molecular weight polyacrylamide is provided, this preparation method need not add hydrolytic reagent, can not produce obnoxious flavour, free from environmental pollution, can prepare that solvability is good, the acrylamide copolymer of relative molecular mass superelevation.
The object of the present invention is achieved like this: it may further comprise the steps: add the acrylamide monomer aqueous solution, auxiliary agent, composite initiator in polymeric kettle, feed high pure nitrogen, drive oxygen and carry out adiabatic copolymerization, carry out granulation, oven dry, pulverizing then and obtain final product, its improvements are: add the sodium acrylate monomers aqueous solution that is used for hydrolysis in polymeric kettle, and add the chain propagation agent that improves relative molecular mass; The concentration of the mix monomer that the described acrylamide and the sodium acrylate monomers aqueous solution are formed is 10～40%, and the add-on of the sodium acrylate monomers aqueous solution is 10～60% of a mix monomer total amount; The add-on of chain propagation agent is 0.001～0.5% of a mix monomer total amount; Composite initiator is oxidation-reduction agent and azo-initiator, and the add-on of oxidation-reduction agent is 0.0005～0.3% of a mix monomer total amount, and the add-on of azo-initiator is 0.0002～0.1% of a mix monomer total amount; Auxiliary agent is complexing agent and solubilizing agent, and the add-on of complexing agent is 0～0.6% of a mix monomer total amount, and the add-on of solubilizing agent is 0.05～10% of a mix monomer total amount;
Among the preparation method of above-mentioned super high molecular weight polyacrylamide, the concentration of the described acrylamide monomer aqueous solution is 24%, and the concentration of the sodium acrylate monomers aqueous solution is 80%;
Among the preparation method of above-mentioned super high molecular weight polyacrylamide, described chain propagation agent is C
12～C
24The reaction product of fat amine or borate family compound;
Among the preparation method of above-mentioned super high molecular weight polyacrylamide, described oxygenant is Potassium Persulphate or Sodium Persulfate or ammonium persulphate; Reductive agent is S-WAT or sodium bisulfite or formaldehyde time sodium bisulfite or tetramethyl-second two ammoniums or β-dimethylaminopropionitrile or thanomin; Azo-initiator be Diisopropyl azodicarboxylate or 2,2 '-two (2-amidine propane) dihydrochlorides or 4,4 of azo '-two (4-cyanopentanoic acid) dihydrochlorides of azo;
Among the preparation method of above-mentioned super high molecular weight polyacrylamide, described complexing agent is ethylenediamine tetraacetic acid (EDTA) or disodium ethylene diamine tetraacetate or tetrasodium ethylenediamine tetraacetate; Solubilizing agent is urea or sodium formiate or Virahol;
Among the preparation method of above-mentioned super high molecular weight polyacrylamide, it is 3～25 ℃ that aqueous solution copolymerization closes kick off temperature, and polymerization time is 3～6h.
Compared to existing high molecular weight Preparation of Polyacrylamide method, beneficial effect of the present invention is: be hydrolyzed with sodium acrylate, all do not add hydrolytic reagent in polymerization process or after the polymerization, so can not produce obnoxious flavoures such as carbonic acid gas, ammonia, free from environmental pollution, the friendly production method of based environment; In polymerization formula, add an amount of chain propagation agent, can obtain ideal anionic acrylamide copolymer, its relative molecular mass is improved greatly; Adding solubilizing agent can improve the solvability of product.
[embodiment]
The invention will be further described below by embodiment.
Embodiment 1: the oxygenant in the present embodiment adopts ammonium persulphate, reductive agent adopts sodium bisulfite, azo-initiator employing 4,4 '-two (4-cyanopentanoic acid) dihydrochlorides (hereinafter to be referred as V-44) of azo, complexing agent adopts ethylenediamine tetraacetic acid (EDTA), and solubilizing agent adopts urea.The 477.6kg deionized water is put into polymeric kettle, adjust temperature to 5 ℃, to add concentration under the nitrogen successively be that 24% acrylamide monomer aqueous solution 1375kg, concentration are chain dose BC-18, urea 8.8kg, the ethylenediamine tetraacetic acid (EDTA) 0.02kg of 80% sodium acrylate monomers aqueous solution 137.5kg, 0.88kg feeding, and uses 10%NaCO
3It is 9 ± 0.5 that the aqueous solution is regulated pH value, the V-44, the 0.09kg ammonium persulphate that add 0.05kg sodium bisulfite, 0.08kg behind the logical nitrogen 30min of continuation successively, pass through about 20min again, material begins to be clamminess in the still, and begins to heat up, and stops logical nitrogen, carry out adiabatic polymerisation, temperature in the kettle reaches 82 ℃ behind the 4h, treats blowing behind the 30min, and granulation, oven dry, pulverizing obtain the anionic acrylamide copolymer of relative molecular mass 3,278 ten thousand.
Embodiment 2: the oxygenant in the present embodiment adopts ammonium persulphate, and reductive agent adopts sodium bisulfite, and azo-initiator adopts V-44, and complexing agent adopts ethylenediamine tetraacetic acid (EDTA), and solubilizing agent adopts urea.With 476.3
The kg deionized water is put into polymeric kettle, adjust temperature to 5 ℃, to add concentration under the nitrogen successively be that 24% acrylamide monomer aqueous solution 1375kg, concentration are chain dose BC-18, urea 8.8kg, the ethylenediamine tetraacetic acid (EDTA) 0.02kg of 80% sodium acrylate monomers aqueous solution 137.5kg, 0.88kg feeding, and uses 10%NaCO
3It is 9 ± 0.5 that the aqueous solution is regulated pH value, add V-44, the 0.09kg ammonium persulphate of 0.05kg sodium bisulfite, 0.08kg behind the logical nitrogen 30min of continuation successively, pass through about 20min again, material begins to be clamminess in the still, and begin to heat up, stop logical nitrogen, carry out adiabatic polymerisation, temperature in the kettle reaches 84.5 ℃ behind the 3.5h, treat blowing behind the 30min, granulation, oven dry, pulverizing obtain the bad product of solvability, because of seriously crosslinked, can't measure relative molecular mass.
Embodiment 3: except that the add-on of BC-18 be the 0.44kg all the other with embodiment 1.The result obtains the multipolymer of relative molecular mass 1,232 ten thousand.
Embodiment 4: except that the add-on of V-44 be the 0.02kg all the other with embodiment 1.Behind the polymerization 10h, temperature in the kettle reaches 72 ℃ as a result, and the product relative molecular mass that obtains is 1,460 ten thousand.
Embodiment 5: except that the add-on of V-44 be the 0.2kg all the other with embodiment 1.Behind the polyase 13 h, temperature in the kettle reaches 84 ℃ as a result, and the product relative molecular mass that obtains is 1,328 ten thousand.
The foregoing description is preferred embodiment of the present invention only, is not to be used to limit scope of the present invention, when utilization, can simplify the foregoing description according to actual needs or the equivalence variation.
Claims (6)
1. the preparation method of a super high molecular weight polyacrylamide, in polymeric kettle, add the acrylamide monomer aqueous solution, auxiliary agent, composite initiator, feed high pure nitrogen, drive oxygen and carry out adiabatic copolymerization, carry out granulation, oven dry, pulverizing then and obtain final product, it is characterized in that: in polymeric kettle, add the sodium acrylate monomers aqueous solution that is used for hydrolysis, and add the chain propagation agent that improves relative molecular mass; The concentration of the mix monomer that the acrylamide and the sodium acrylate monomers aqueous solution are formed is 10～40%, and the add-on of the sodium acrylate monomers aqueous solution is 10～60% of a mix monomer total amount; The add-on of chain propagation agent is 0.001～0.5% of a mix monomer total amount; Composite initiator is oxidation-reduction agent and azo-initiator, and the add-on of oxidation-reduction agent is 0.0005～0.3% of a mix monomer total amount, and the add-on of azo-initiator is 0.0002～0.1% of a mix monomer total amount; Auxiliary agent is complexing agent and solubilizing agent, and the add-on of complexing agent is 0～0.6% of a mix monomer total amount, and the add-on of solubilizing agent is 0.05～10% of a mix monomer total amount.
2. the preparation method of super high molecular weight polyacrylamide according to claim 1, it is characterized in that: the concentration of the acrylamide monomer aqueous solution is 24%, the concentration of the sodium acrylate monomers aqueous solution is 80%.
3. the preparation method of super high molecular weight polyacrylamide according to claim 1 is characterized in that: chain propagation agent is the reaction product of C12～C24 fat amine or borate family compound.
4. the preparation method of super high molecular weight polyacrylamide according to claim 1, it is characterized in that: oxygenant is Potassium Persulphate or Sodium Persulfate or ammonium persulphate; Reductive agent is S-WAT or sodium bisulfite or formaldehyde time sodium bisulfite or tetramethyl-second two ammoniums or β-dimethylaminopropionitrile or thanomin; Azo-initiator be Diisopropyl azodicarboxylate or 2,2 '-two (2-amidine propane) dihydrochlorides or 4,4 of azo '-two (4-cyanopentanoic acid) dihydrochlorides of azo.
5. the preparation method of super high molecular weight polyacrylamide according to claim 1, it is characterized in that: complexing agent is ethylenediamine tetraacetic acid (EDTA) or disodium ethylene diamine tetraacetate or tetrasodium ethylenediamine tetraacetate; Solubilizing agent is urea or sodium formiate or Virahol.
6. the preparation method of super high molecular weight polyacrylamide according to claim 1, it is characterized in that: it is 3～25 ℃ that aqueous solution copolymerization closes kick off temperature, polymerization time is 3～6h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633335A (en) * | 2012-04-20 | 2012-08-15 | 河北大学 | Sewage treatment method |
| CN102649828A (en) * | 2012-05-25 | 2012-08-29 | 安徽巨成精细化工有限公司 | Preparation method of ultrahigh-hydrolysis-degree polyacrylamide |
| CN102675509A (en) * | 2012-05-25 | 2012-09-19 | 安徽巨成精细化工有限公司 | Preparation method of nonionic polyacrylamide (NPAM) |
| CN102690389A (en) * | 2012-05-25 | 2012-09-26 | 安徽巨成精细化工有限公司 | Preparation method for high molecular weight cationic polyacrylamide |
| CN103539947A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Graft-modified ultrahigh-molecular-weight polyacrylamide and preparation method thereof |
| CN105566566A (en) * | 2015-12-29 | 2016-05-11 | 赵吉滨 | Polynary composite water-soluble high molecular polymer and preparation method thereof |
| CN108659164A (en) * | 2018-04-28 | 2018-10-16 | 东营市诺尔化工有限责任公司 | A kind of ultra-high molecular weight cationic polyacrylamide and its preparation method and application |
| CN110294820A (en) * | 2018-03-21 | 2019-10-01 | 上海四奥化工有限公司 | A kind of preparation method of super high molecular weight polyacrylamide |
-
2010
- 2010-01-19 CN CN2010100010467A patent/CN102127188A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633335A (en) * | 2012-04-20 | 2012-08-15 | 河北大学 | Sewage treatment method |
| CN102649828A (en) * | 2012-05-25 | 2012-08-29 | 安徽巨成精细化工有限公司 | Preparation method of ultrahigh-hydrolysis-degree polyacrylamide |
| CN102675509A (en) * | 2012-05-25 | 2012-09-19 | 安徽巨成精细化工有限公司 | Preparation method of nonionic polyacrylamide (NPAM) |
| CN102690389A (en) * | 2012-05-25 | 2012-09-26 | 安徽巨成精细化工有限公司 | Preparation method for high molecular weight cationic polyacrylamide |
| CN102690389B (en) * | 2012-05-25 | 2014-01-29 | 安徽巨成精细化工有限公司 | Preparation method for high molecular weight cationic polyacrylamide |
| CN103539947A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Graft-modified ultrahigh-molecular-weight polyacrylamide and preparation method thereof |
| CN103539947B (en) * | 2012-07-12 | 2016-06-08 | 中国石油化工股份有限公司 | Graft modification super high molecular weight polyacrylamide and preparation method thereof |
| CN105566566A (en) * | 2015-12-29 | 2016-05-11 | 赵吉滨 | Polynary composite water-soluble high molecular polymer and preparation method thereof |
| CN110294820A (en) * | 2018-03-21 | 2019-10-01 | 上海四奥化工有限公司 | A kind of preparation method of super high molecular weight polyacrylamide |
| CN110294820B (en) * | 2018-03-21 | 2022-06-24 | 上海四奥化工有限公司 | Preparation method of polyacrylamide with ultrahigh molecular weight |
| CN108659164A (en) * | 2018-04-28 | 2018-10-16 | 东营市诺尔化工有限责任公司 | A kind of ultra-high molecular weight cationic polyacrylamide and its preparation method and application |
| CN108659164B (en) * | 2018-04-28 | 2021-03-23 | 东营市诺尔化工有限责任公司 | Ultrahigh molecular weight cationic polyacrylamide, and preparation method and application thereof |
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Application publication date: 20110720 |