CN103788268B - Hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide - Google Patents
Hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide Download PDFInfo
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Abstract
A kind of hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide, it is characterized in that, comprise the preparation of initiator, comprise the steps: 1) 5-10g azo two isobutyl imidazoline hydrochloride is dissolved in 80-100gN, in N-dimethyl-p-toluidine; 2) 5-10g azo two isobutyl imidazoline hydrochloride, 5-10g2,2-azo diisobutyl amidine disalt are dissolved in 80-120g Tetramethyl Ethylene Diamine; 3) by step 1), 2) solution mixing, add tensio-active agent 20g, 200g purified water and stir.The present invention changes conventional polymeric initiator system, adopts low temperature polymerization, static rear hydrolysis process, improves Molecular Weight for Polyacrylamide and reaches more than 3,000 ten thousand.
Description
Technical field
The invention provides a kind of method for making of polyacrylamide, specifically a kind of hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide.
Background technology
" functional materials " 35 volumes the 2nd phase in 2004 (Huang Liming, 5 admires) discloses " Synthesis of high molecular weight polyacrylamide by homopolymerization, " it is based on difunctionality redox system, coordinate other initiators to form NEW TYPE OF COMPOSITE initiator system, adopt the acrylamide triggered homopolymerization of homogeneous phase aqueous solution polymerization under cryogenic.Homopolymerization posthydrolysis operational path is adopted to prepare high molecular weight polyacrylamide again.The document also discloses that the concrete technology parameter of this route.
" synthesis of super high molecular weight polyacrylamide and suitability for industrialized production " (Zhejiang University Master's thesis author: Qin Xuefeng in 2005), its high spot reviews polymerizing condition, if the factors such as polymerization temperature, initiator solubility, ammoniacal liquor, urea, per unit volume concentration meter quality are on the impact of Molecular Weight for Polyacrylamide.The test recipe by optimization of orthogonal test, drawn best polymerization process condition, lab scale has synthesized the super high molecular weight polyacrylamide that molecular weight is greater than more than 2,500 ten thousand thus.
" research of super high molecular weight polyacrylamide " (Daqing Petroleum Institute Master's thesis author: Zhang Xuhong in 2002), it adopts homemade difunctionality superoxide, coordinate the acrylamide triggered aqueous solution homopolymerization of combined oxidation reduction system of reductive agent azo-compound composition, prepare super high molecular weight polyacrylamide.This paper also discloses concrete processing parameter, and it obtains being the partially hydrolyzed polyacrylamide that molecular weight is greater than 2,800 ten thousand.
" oil and gas chemical industry " the 34th volume the 5th phase in 2005 discloses " research of composite initiation system synthesis super-high relative molecular weight hydro-polyacrylamide " provide with Potassium Persulphate, sodium bisulfite be main initiator, AIBN and low temperature initiators F2 for co initiator, composition composite initiation system.The document also discloses that optimum process condition.
" University of Petroleum's journal " (natural science edition) the 6th phase in 2003 " high intrinsic viscosity partially hydrolyzed polyacrylamide Study on polymerization technology " disclose with ammonium persulphate vinylformic acid Of, formaldehyde and Sodium Thiosulfate composition redox initiator and azo (2-amidine propane) hydrochloride for composite initiation system.
" fine chemistry industry " the 20th volume the 5th phase " research of Polyacrylamide of Ultrahigh Viscosity Average Molecular Weight " in 2003 has inquired into the polymerization initiation system of acrylamide, establish one be enclosed within 5-10 DEG C of condition under, the low temperature composite initiation system be made up of Potassium Persulphate, ammoniacal liquor, urea, azo (2-amidine propane) hydrochloride and functional monomer MP, and add sodium formiate and polyoxyethylene 20 sorbitan monolaurate improves the water-soluble of polyacrylamide.
The optimum evocating agent that " application chemical industry " the 34th volume the 7th phase " research of synthesis of ultra-high molecular weight polyacrylamide by inverse emulsion polymerization " in 2005 is selected is Potassium Persulphate-V-Brite B.
Above-mentioned document is quoted at this as background technology of the present invention.
Summary of the invention
The invention provides a kind of method for making of super high molecular weight polyacrylamide, change conventional polymeric initiator system, adopt low temperature polymerization, static rear hydrolysis process, improve Molecular Weight for Polyacrylamide and reach more than 3,000 ten thousand.
The technical scheme that the present invention specifically adopts is: a kind of hydrolytic reagent spiral spray legal system, for the technique of super high molecular weight polyacrylamide, is characterized in that, comprises the preparation of initiator, comprise the steps:
1) 5-10g azo two isobutyl imidazoline hydrochloride is dissolved in 80-100gN, in N-dimethyl-p-toluidine;
2) 5-10g azo two isobutyl imidazoline hydrochloride, 5-10g2,2-azo diisobutyl amidine disalt are dissolved in 80-120g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mixing, add tensio-active agent 20g, 200g purified water and stir.
Described tensio-active agent is sorbitol anhydride oleate.
Described hydrolytic reagent spiral spray legal system, for the technique of super high molecular weight polyacrylamide, comprises first homopolymerization posthydrolysis technique, described hydrolysis process be homopolymerization static after, adopt spiral spray technique to be added in homopolymerization system by sodium hydroxide solution.
The Molecular Weight for Polyacrylamide that the present invention obtains is greater than 3,000 ten thousand, and degree of hydrolysis is 25-30%.
Advantage of the present invention is:
1) homopolymerization of the present invention static after be hydrolyzed again, can effectively stop because hydrolysis process in prior art brings polymeric solution impurity many, the growth of molecular chain during impact polymerization and the problem that causes molecular weight low;
2) multiple elements design initiator system of the present invention effectively can reduce the quantity of the free radical that the polymer initial stage produces, and carries out laddering free radical and causes growth, prevent molecular rupture and cause molecular weight low by the decomposition temperature of initiator different in initiator system.
Embodiment
Hydrolytic reagent spiral spray legal system, for a technique for super high molecular weight polyacrylamide, comprises first homopolymerization posthydrolysis technique, described hydrolysis process be homopolymerization static after, adopt spiral spray technique to be added in homopolymerization system by sodium hydroxide solution.
The preparation of initiator, comprises the steps:
1) 5g azo two isobutyl imidazoline hydrochloride is dissolved in 100gN, in N-dimethyl-p-toluidine;
2) 5g azo two isobutyl imidazoline hydrochloride, 5g2,2-azo diisobutyl amidine disalt are dissolved in 100g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mixing, add sorbitol anhydride oleate 20g, 200g purified water and stir.
Other and prior art are substantially identical.
Claims (2)
1. hydrolytic reagent spiral spray legal system is for a technique for super high molecular weight polyacrylamide, it is characterized in that, comprises the preparation of initiator, comprises the steps:
1) 5-10g azo two isobutyl imidazoline hydrochloride is dissolved in 80-100gN, in N-dimethyl-p-toluidine;
2) 5-10g azo two isobutyl imidazoline hydrochloride, 5-10g2,2-azo diisobutyl amidine disalt are dissolved in 80-120g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mixing, add tensio-active agent 20g, 200g purified water and stir;
Also comprise first homopolymerization posthydrolysis technique, described hydrolysis process be homopolymerization static after, adopt spiral spray technique to be added in homopolymerization system by sodium hydroxide solution.
2. hydrolytic reagent spiral spray legal system according to claim 1 is for the technique of super high molecular weight polyacrylamide, and it is characterized in that, described tensio-active agent is sorbitol anhydride oleate.
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| CN103788268B true CN103788268B (en) | 2016-03-16 |
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| CN101942052A (en) * | 2010-10-14 | 2011-01-12 | 郑州正力聚合物科技有限公司 | Method for producing anionic polyacrylamide |
| CN102731699A (en) * | 2011-04-01 | 2012-10-17 | 中国石油化工股份有限公司 | Preparation method of ultra high molecular weight anionic polyacrylamide |
| CN102863583A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Preparation method of ultra-high molecular weight temperature and salt resistant polyacrylamide |
| CN102887970A (en) * | 2011-07-18 | 2013-01-23 | 中国石油化工股份有限公司 | Solution polymerization method |
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Patent Citations (8)
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| US3022279A (en) * | 1959-05-06 | 1962-02-20 | Dow Chemical Co | Process for making hydrolyzed polyacrylamide |
| US4455411A (en) * | 1982-06-14 | 1984-06-19 | Nitto Kagaku Kogyo Kabushiki Kaisha | Process for preparing acrylamide polymers |
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| CN101942052A (en) * | 2010-10-14 | 2011-01-12 | 郑州正力聚合物科技有限公司 | Method for producing anionic polyacrylamide |
| CN102731699A (en) * | 2011-04-01 | 2012-10-17 | 中国石油化工股份有限公司 | Preparation method of ultra high molecular weight anionic polyacrylamide |
| CN102863583A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Preparation method of ultra-high molecular weight temperature and salt resistant polyacrylamide |
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