CN103788268A - Process for preparing ultrahigh molecular weight polyacrylamide by hydrolytic agent spiral spray method - Google Patents
Process for preparing ultrahigh molecular weight polyacrylamide by hydrolytic agent spiral spray method Download PDFInfo
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- CN103788268A CN103788268A CN201310116945.5A CN201310116945A CN103788268A CN 103788268 A CN103788268 A CN 103788268A CN 201310116945 A CN201310116945 A CN 201310116945A CN 103788268 A CN103788268 A CN 103788268A
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Abstract
The invention provides a process for preparing ultrahigh molecular weight polyacrylamide by a hydrolytic agent spiral spray method. The process is characterized by comprising the preparation of an initiator. The process comprises the following steps: 1) dissolving 5 to 10g of ozo dihexylbutyl imidazoline hydrochloride to 80 to 100g of N, N-dimethyl-p-toluidine; 2) dissolving 5 to 10g of ozo dihexylbutyl imidazoline hydrochloride and 5 to 10g of 2, 2-2,2'-azobis(2-methylpropionamidine) dihydrochloride to 80 to 120g of tetramethylethylenediamine; and 3) mixing the solutions obtained in the step 1) and 2), adding 20g of surface active agent and 200g of purified water, and uniformly agitating to obtain ultrahigh molecular weight polyacrylamide. According to the process for preparing ultrahigh molecular weight polyacrylamide by the hydrolytic agent spiral spray method, the traditional polymerizing initiating system is changed, the process of polymerizing under a low temperature and hydrolyzing after standing is performed, and thus the molecular weight of polyacrylamide is increased to more than 30 million.
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 " the 2nd phase of 35 volumes in 2004 (Huang Liming, 5 admires) discloses " Synthesis of high molecular weight polyacrylamide by homopolymerization ", it is take difunctionality redox system as main, coordinate other initiator composition NEW TYPE OF COMPOSITE initiator systems, under cold condition, adopt the acrylamide triggered homopolymerization of homogeneous phase aqueous solution polymerization.Adopt again homopolymerization posthydrolysis operational path to prepare high molecular weight polyacrylamide.The document also discloses that the concrete technology parameter of this route.
" the synthetic and suitability for industrialized production of super high molecular weight polyacrylamide " (Master's thesis author: the Qin Xuefeng in 2005 of Zhejiang University), its high spot reviews polymerizing condition, as the impact of factor on Molecular Weight for Polyacrylamide such as polymerization temperature, initiator solubility, ammoniacal liquor, urea, per unit volume concentration meter quality.By optimization of orthogonal test test recipe, drawn best polymerization process condition, lab scale has synthesized molecular weight and has been greater than more than 2,500 ten thousand super high molecular weight polyacrylamides thus.
" research of super high molecular weight polyacrylamide " (Master's thesis author: the Zhang Xuhong in 2002 of Daqing Petroleum Institute), 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 is the partially hydrolyzed polyacrylamide that molecular weight is greater than 2,800 ten thousand.
" oil and gas chemical industry " the 34th the 5th phase of volume in 2005 discloses " research of the synthetic super-high relative molecular weight hydro-polyacrylamide of composite initiation system " and provides take Potassium Persulphate, sodium bisulfite as main initiator, AIBN and low temperature initiators F2 are as auxiliary 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 " discloses take the redox initiator of ammonium persulphate vinylformic acid diethylin ethyl ester, formaldehyde and Sodium Thiosulfate composition and azo (2-amidine propane) hydrochloride as composite initiation system.
" fine chemistry industry " the 20th the 5th phase of volume " research of Polyacrylamide of Ultrahigh Viscosity Average Molecular Weight " in 2003 has been inquired into the polymerization initiation system of acrylamide, having set up one is enclosed within 5-10 ℃ of condition, the low temperature composite initiation system being formed by 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 the 7th phase of volume " 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 concrete technical scheme adopting of the present invention is:
Hydrolytic reagent spiral spray legal system, for a technique for super high molecular weight polyacrylamide, is characterized in that, comprises the preparation of initiator, comprises the steps:
1) own 5-10g azo two Butamisole quinoline hydrochloride is dissolved in to 80-100gN, in N-dimethyl-p-toluidine;
2), by own 5-10g azo two Butamisole quinoline hydrochloride, 5-10g2,2-azo diisobutyl amidine disalt is dissolved in 80-120g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mix, add tensio-active agent 20g, 200g purified water to 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 that sodium hydroxide solution is added in homopolymerization system.
The Molecular Weight for Polyacrylamide that the present invention makes 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 is hydrolyzed after static again, can effectively stop because hydrolysis process in prior art brings polymeric solution impurity more the growth of molecular chain while affecting polymerization and cause the problem that molecular weight is low;
2) polynary composite initiation system of the present invention can effectively reduce the quantity of free radical that the polymer initial stage produces, and carries out laddering free radical cause and increase by the decomposition temperature of different initiators in initiator system, prevents molecular rupture and causes molecular weight low.
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 that sodium hydroxide solution is added in homopolymerization system.
The preparation of initiator, comprises the steps:
1) own 5g azo two Butamisole quinoline hydrochloride is dissolved in to 100gN, in N-dimethyl-p-toluidine;
2), by own 5g azo two Butamisole quinoline hydrochloride, 5g2,2-azo diisobutyl amidine disalt is dissolved in 100g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mix, add sorbitol anhydride oleate 20g, 200g purified water to stir.
Other and prior art are basic identical.
Claims (3)
1. hydrolytic reagent spiral spray legal system, for a technique for super high molecular weight polyacrylamide, is characterized in that, comprises the preparation of initiator, comprises the steps:
1) own 5-10g azo two Butamisole quinoline hydrochloride is dissolved in to 80-100gN, in N-dimethyl-p-toluidine;
2), by own 5-10g azo two Butamisole quinoline hydrochloride, 5-10g2,2-azo diisobutyl amidine disalt is dissolved in 80-120g Tetramethyl Ethylene Diamine;
3) by step 1), 2) solution mix, add tensio-active agent 20g, 200g purified water to stir.
2. hydrolytic reagent spiral spray legal system according to claim 1, for the technique of super high molecular weight polyacrylamide, is characterized in that, described tensio-active agent is sorbitol anhydride oleate.
3. hydrolytic reagent spiral spray legal system according to claim 1 is for the technique of super high molecular weight polyacrylamide, it is characterized in that, comprise first homopolymerization posthydrolysis technique, described hydrolysis process be homopolymerization static after, adopt spiral spray technique that sodium hydroxide solution is added in homopolymerization system.
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| CN201310116945.5A CN103788268B (en) | 2013-04-07 | 2013-04-07 | Hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide |
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| CN201310116945.5A CN103788268B (en) | 2013-04-07 | 2013-04-07 | Hydrolytic reagent spiral spray legal system is for the technique of super high molecular weight polyacrylamide |
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| CN103788268A true CN103788268A (en) | 2014-05-14 |
| CN103788268B CN103788268B (en) | 2016-03-16 |
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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 |
| CN1865298A (en) * | 2005-05-20 | 2006-11-22 | 中国石油天然气股份有限公司 | Trisegment composite initiator for synthesizing super high molecular weight polyacrylamide |
| CN101157741A (en) * | 2007-09-28 | 2008-04-09 | 东营顺通化工（集团）有限公司 | Synthesis technology of high molecular weight temperature-tolerant anti-salt polyacrylamide |
| 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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2013
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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 |
| CN1865298A (en) * | 2005-05-20 | 2006-11-22 | 中国石油天然气股份有限公司 | Trisegment composite initiator for synthesizing super high molecular weight polyacrylamide |
| CN101157741A (en) * | 2007-09-28 | 2008-04-09 | 东营顺通化工（集团）有限公司 | Synthesis technology of high molecular weight temperature-tolerant anti-salt polyacrylamide |
| 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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Effective date of registration: 20200415 Address after: 256400 4f, block A6, Chuangzhi Valley, Huantai County, Zibo City, Shandong Province Patentee after: Zibo Ruijie New Technology Development Co., Ltd. Address before: Tangshan Huantai County town of Shandong city of Zibo province Xu Dian Cun 256400 Patentee before: SHANDONG TONGLI CHEMICAL Co.,Ltd. |
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