CN104356292A - Reaction type dispersing agent and preparation method for polyacrylamide water emulsion - Google Patents
Reaction type dispersing agent and preparation method for polyacrylamide water emulsion Download PDFInfo
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- CN104356292A CN104356292A CN201410564516.9A CN201410564516A CN104356292A CN 104356292 A CN104356292 A CN 104356292A CN 201410564516 A CN201410564516 A CN 201410564516A CN 104356292 A CN104356292 A CN 104356292A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 28
- 239000000839 emulsion Substances 0.000 title claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 title abstract 4
- 238000006757 chemical reactions by type Methods 0.000 title abstract 3
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 125000002091 cationic group Chemical group 0.000 claims abstract description 26
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 63
- 239000006185 dispersion Substances 0.000 claims description 61
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 230000004044 response Effects 0.000 claims description 37
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 28
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- -1 acrylyl Chemical group 0.000 claims description 21
- 238000010792 warming Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 239000012263 liquid product Substances 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 14
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 14
- 230000006837 decompression Effects 0.000 claims description 14
- 238000006392 deoxygenation reaction Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 239000001294 propane Substances 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 9
- 150000003863 ammonium salts Chemical class 0.000 claims description 8
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical compound C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004160 Ammonium persulphate Substances 0.000 claims description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 claims description 7
- 241000237502 Ostreidae Species 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 230000002349 favourable effect Effects 0.000 claims description 7
- 235000020636 oyster Nutrition 0.000 claims description 7
- NPSSWQJHYLDCNV-UHFFFAOYSA-N prop-2-enoic acid;hydrochloride Chemical compound Cl.OC(=O)C=C NPSSWQJHYLDCNV-UHFFFAOYSA-N 0.000 claims description 7
- 239000003507 refrigerant Substances 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012986 chain transfer agent Substances 0.000 claims description 6
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical compound [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 claims description 5
- ZGCZDEVLEULNLJ-UHFFFAOYSA-M benzyl-dimethyl-(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 ZGCZDEVLEULNLJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000004970 Chain extender Substances 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- UFAGAQUHRODLFO-UHFFFAOYSA-M [Cl-].CC=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 Chemical compound [Cl-].CC=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 UFAGAQUHRODLFO-UHFFFAOYSA-M 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 238000007334 copolymerization reaction Methods 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- MTPJEFOSTIKRSS-UHFFFAOYSA-N 3-(dimethylamino)propanenitrile Chemical compound CN(C)CCC#N MTPJEFOSTIKRSS-UHFFFAOYSA-N 0.000 claims description 2
- XRUKRHLZDVJJSX-UHFFFAOYSA-N 4-cyanopentanoic acid Chemical compound N#CC(C)CCC(O)=O XRUKRHLZDVJJSX-UHFFFAOYSA-N 0.000 claims description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 claims description 2
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 150000003851 azoles Chemical class 0.000 claims description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- 238000010538 cationic polymerization reaction Methods 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 229940093476 ethylene glycol Drugs 0.000 claims description 2
- 229940051250 hexylene glycol Drugs 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 claims description 2
- 150000002825 nitriles Chemical class 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 230000033116 oxidation-reduction process Effects 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 claims description 2
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 2
- 235000019252 potassium sulphite Nutrition 0.000 claims description 2
- IOZVKVQMRQRJFK-UHFFFAOYSA-N propane;quinoline Chemical compound CCC.N1=CC=CC2=CC=CC=C21 IOZVKVQMRQRJFK-UHFFFAOYSA-N 0.000 claims description 2
- 230000002829 reductive effect Effects 0.000 claims description 2
- VYGBQXDNOUHIBZ-UHFFFAOYSA-L sodium formaldehyde sulphoxylate Chemical compound [Na+].[Na+].O=C.[O-]S[O-] VYGBQXDNOUHIBZ-UHFFFAOYSA-L 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 2
- 229960001124 trientine Drugs 0.000 claims description 2
- 208000023445 Congenital pulmonary airway malformation Diseases 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 238000011056 performance test Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 5
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920003169 water-soluble polymer Polymers 0.000 description 3
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229920006322 acrylamide copolymer Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000004815 dispersion polymer Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QYUMESOEHIJKHV-UHFFFAOYSA-M prop-2-enamide;trimethyl(propyl)azanium;chloride Chemical compound [Cl-].NC(=O)C=C.CCC[N+](C)(C)C QYUMESOEHIJKHV-UHFFFAOYSA-M 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a reaction type dispersing agent and a preparation method for the polyacrylamide water emulsion. The method for preparing the water emulsion comprises the steps of preparing the reaction type dispersing agent; balancing the concentration of free radicals by multiple sections of composite initiating systems under the participation of a saline solution system and the dispersing agent, and performing water emulsion dispersing polymerization on acrylamide and cationic monomers. The water emulsion product can be quickly dissolved, has a high molecular weight, is high in flowability and high in stability and can be widely applied to the field of water treatment of all industries.
Description
Technical field
The invention belongs to Polymer Synthesizing field, relate to the preparation method of a kind of response type dispersion agent and polyacrylamide emulsion.
Background technology
Polyacrylamide is called as " all trades auxiliary agent ", and cationic polyacrylamide (CPAM) is wherein then one of kind be most widely used.CPAM is the acrylamide copolymer of cation structural unit, molecular chain in water ionizable go out polycation and little negatively charged ion, adding of CPAM cationic increases polymkeric substance to electronegative colloid, the absorption viscosifying power of polymkeric substance and solid surface, stronger charge neutrality effect can be caused, enhance its absorption, bonding, decolouring, the effects such as precipitation and flocculation, be specially adapted to paper-making technique, foodstuffs industry, construction work, metallurgical engineering, ore dressing coal dust, oil recovery industry, sewage in the industry that the organic colloid such as aquatic products processing and fermentation content is higher and the process of waste water.
Double water-phase dispersion copolymerization method is a kind of novel method preparing water-soluble polymers, in the aqueous solution under utilizing this novel method the dissolving of one or more water-soluble monomers can be dispersed in dispersion agent existence, be polymerized under certain condition, form immiscible water-soluble polymer dispersion, be also aqueous polymer dispersion.
It is lower that water miscible liquid reaction system has viscosity, solid content is large, the water-soluble polymers that relative molecular mass is larger can be obtained, which overcome the shortcoming of traditional aqueous polymerization, organic solvent pollution problem is there is not in preparation and use procedure, and water miscible liquid product dissolves rapidly, directly can dilute use, therefore has broad application prospects and the value of environmental protection.
At present, the report of the preparation method of research water miscible liquid is few both at home and abroad, and product performance are perfect not enough.Subject matter concentrates in the dispersion stabilization difference of water miscible liquid product and the effective content of CPAM and the low these two aspects of molecular weight.In order to solve this two problems, technician has done a large amount of research work.Be that dispersion agent prepares CPAM water miscible liquid with tertiary butanol aqueous solution in patent CN201210097234.3, result shows the CPAM water miscible liquid poor stability prepared using the trimethyl carbinol as dispersion agent, and the shelf-time is not long.The CPAM molecular weight of preparation is on the low side, is no more than 3,500,000.In order to overcome the problems such as chain tra nsfer that small molecular alcohol causes as dispersion agent is strong, document (Liu Zaiman etc., " double-aqueous phase polymerization method synthesizing cationic polyacrylamide and flocculating property thereof ", applied chemistry, 2010,28 (8): 874 ~ 878) provide and a kind ofly substitute the dispersion agent of the trimethyl carbinol as reaction system using polyoxyethylene glycol, prepare the water miscible liquid that a kind of dispersion stabilization is good, but polyoxyethylene glycol consumption is very large in the method, make high expensive, and the viscosity of emulsion system is high, poor fluidity, the molecular weight of CPAM is low.The low molecular weight cationic polymkeric substance that what nearest Improvement was maximum is is obtained by cationic monomer homopolymerization, as dispersion agent, achieves good result.As provided in patent CN102321213B with the cationic monomers such as acrylyl oxy-ethyl-trimethyl salmiac homopolymerization and the dispersion agent obtained under the existence of molecular weight regulator.And prepared water miscible liquid product that is dispersed and the good higher molecular weight CPAM of mobility by homemade dispersion agent, but the stability of this water miscible liquid product is unknown, and the molecular weight control of dispersion agent and aqueous emulsion polymerization technique controlling difficulty high.
In current most water miscible liquid preparation technology, due to " gel effect " in polyacrylamide polymerization mechanism, autoacceleration process is there is in reaction process, the polymerization velocity of acrylamide copolymer is had and substantially exceeds the possible of the speed separated out from dispersion system, if it is improper to control, be easy to get gel product very much, causes and be polymerized unsuccessfully.
Summary of the invention
The object of the invention is to some shortcomings overcoming existing CPAM water miscible liquid product preparation process, provide that a kind of effective content is high, molecular weight is high, the preparation method of the CPAM water miscible liquid product of easy to operate easy control.
Another object of the present invention is to provide a kind of system viscosity to be less than 200mPaS, good fluidity, dissolution rate is fast, can at the not stratified high stable CPAM water miscible liquid product of 24 months long-term storage.
For reaching above technical purpose, the present invention realizes by the following technical solutions.
A preparation method for response type dispersion agent and polyacrylamide aqueous emulsion, is characterized in that: by the response type polymeric monomer shown in formula (1) as dispersion agent, formed by acrylamide and cationic monomer copolymerization,
formula (1).
In formula (1), m is the cationic polymerization degree of polymer segment in macromonomer; N is the polymerization degree of V-Pyrol RC in macromonomer; A is 2 ~ 3; A is H or CH
3, B is O or N element.
The molecular-weight average of polymeric monomer dispersion agent is 2 × 10
5~ 8 × 10
5.
Described cationic polyacrylamide water miscible liquid, its dissolution rate is less than 10min.Its molecular weight is more than 8,000,000.Its product system viscosity is less than 400 mPas.
The preparation method of described polymeric monomer dispersion agent is:
The N-V-Pyrol RC of the cationic monomer of 20 ~ 30 parts and 0 ~ 5 part adds in reactor by step 1), adds the dissolution with solvents of 30 ~ 100 parts; Nitrogen deoxygenation is passed into 15 ~ 30 minutes in reactor; The chain-transfer agent of 0.01 ~ 1 part and the initiator of 0.001 ~ 0.05 part is added in reactor; Stirring reaction 4 ~ 6 hours at 60 ~ 70 DEG C; Add sodium hydroxide solution adjust ph to 7 ~ 9, decompression pump most solvent, precipitate three times, centrifugation with 10 ~ 50 parts of precipitation agents, drying obtains white solid polymeric monomer precursor, its structural formula as the formula (2):
formula (2)
Step 2) in reactor, add the polymeric monomer precursor of aforementioned 10 ~ 20 parts and the tetrahydrofuran (THF) of 50 ~ 100 parts, be uniformly dissolved; 1 ~ 10 part of acrylate chloride is dissolved in 20 ~ 50 parts of tetrahydrofuran (THF)s, joins under stirring in above-mentioned solution, drip a certain amount of aqueous sodium carbonate simultaneously, control temperature of reaction at 0 ~ 4 DEG C with the jacket reactor of band refrigerant; React after 2 ~ 4 hours, be warming up to room temperature; Decompression pumps solvent, and precipitate three times in 10 ~ 50 parts of ether, obtain white solid response type dispersion agent after drying, its structural formula as the formula (1).
The preparation process 1 of described polymeric monomer dispersion agent) described in cationic monomer be selected from acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloxyethyldimethyl benzyl ammonium chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, 3-acrylamide propyl-trimethyl ammonium chloride, 3-(Methacrylamide propyl group) one or both in-trimethyl ammonium chloride; One in solvent selected from methanol, ethanol and acetonitrile, is preferably ethanol; Chain-transfer agent is sulfydryl b ammonium salt hydrochlorate; Described initiator is selected from 2, two (2-amidine propane) dihydrochloride, 2 of 2-azo, one or both in 2-azo two (2-amidine azoles quinoline propane) hydrochloride, azo two (2,5-dimethyl-6-carboxyl) own nitrile and Diisopropyl azodicarboxylate, preferred Diisopropyl azodicarboxylate; Described precipitation agent is selected from the one in ether and acetone, preferred ether.
Described cationic polyacrylamide water miscible liquid, preparation method is: by the acrylamide of 5 ~ 10 parts, the cationic monomer of 1 ~ 7 part, the above-mentioned response type dispersion agent of 0.1 ~ 2 part, the polyoxyethylene glycol (molecular weight 20000) of the ammonium sulfate of 20 ~ 35 parts and 0.1 ~ 4 part joins in reactor, add the chainextender of 0.001 ~ 0.05 part and the complexing agent of 0.001 ~ 0.01 part, add the deionized water of 40 ~ 60 parts, stirring and dissolving, pH is regulated to be 5 ~ 8 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 15 ~ 40min, be warming up to the oxidation-reduction initiator that 30 ~ 35 DEG C add the Oxidizing and Reducing Agents composition of 0.0001 ~ 0.01 part, regulate stirring velocity, after system becomes oyster white, add the azo initiator of 0.0001 ~ 0.01 part again.After being warming up to 50 ~ 55 DEG C of continuation reaction 4 ~ 6h, then add the ammonium sulfate of 2 ~ 5 parts, after cooling, namely obtain the stable CPAM water miscible liquid product of favorable dispersity.
In described cationic polyacrylamide water miscible liquid preparation process, cationic monomer be selected from acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloxyethyldimethyl benzyl ammonium chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, 2-acrylamido-2-trimethoxysilyl propyl methacrylate ammonium chloride one or both; Chainextender is selected from N, one or more in N-dimethylethanolamine, ethylene glycol, hexylene glycol, N, N-dimethyl-ethylenediamine, N, N-Tetramethyl Ethylene Diamine, triethylene tetramine, 1,3-dimethylamino propionitrile; Complexing agent is EDTA; Oxygenant be selected from ammonium persulphate, Sodium Persulfate, Potassium Persulphate, hydrogen peroxide and 2-methylethyl ketone peroxide one or more; Reductive agent be selected from ammonium sulphite, potassium sulfite, S-WAT, ammonium bisulfite, sodium bisulfite, Potassium hydrogen sulfite and sodium formaldehyde sulphoxylate one or more; Azo series initiators is 2,2 '-azo (2-amidine propane) dihydrochloride, 2,2 '-azo (2-tetrahydroglyoxaline propane) dihydrochloride and 4, one or more in 4 '-azo two (4-cyanopentanoic acid), be preferably 2,2 '-azo (2-amidine propane) dihydrochloride.
Relative to prior art, the present invention has following beneficial effect:
Present invention employs a kind of polymeric monomer dispersion agent that can participate in reacting, can guide and control the balanced of speed of separating out in polymerization process and polymerization velocity better, thus obtain the water miscible liquid of stably dispersing;
The present invention makes polymerization process at the uniform velocity controlled by sectional type polymerization technique, and this method can obtain the cationic polyacrylamide of high molecular, and molecular weight can reach more than 8,000,000 after testing;
In water miscible liquid product prepared by the present invention, inclusion is inorganic salt and polymer, overcomes the volatile small organic molecule that tradition uses, and polymerization turnover ratio is high, meets requirement that is green and point subeconomy synthesis, simultaneously very friendly with operating personnel to environment; Water miscible liquid product obtained by the present invention, out have outside the features such as traditional aqueous product dissolution rate is fast, good fluidity, more excellent part is that it has satisfactory stability, can long-term storage and layering, coacervation do not occur.
Embodiment
The present invention is described in detail below with reference to embodiment.
In following examples, the performance test of product adopts following methods to carry out:
1, polycation macromer molecular weight is measured by gel permeation chromatography (GPC);
2, solid content is measured according to the method specified in GB12005.2-89;
3, dissolution time is measured according to the method specified in GB12005.8-89;
4, measure according to the method specified in GB12005.1-89 and calculate the molecular weight of CPAM;
5, the apparent viscosity of emulsion system is with NDJ-5 type viscometer determining at 25 DEG C.
Embodiment 1
(1) synthesis of response type dispersion agent Disp-1
The N-V-Pyrol RC of the acrylyl oxy-ethyl-trimethyl salmiac of 150kg and 12kg is joined in two cubes of reactors, adds 550kg dissolve with ethanol; Nitrogen deoxygenation is passed into 20 minutes in reactor; The sulfydryl b ammonium salt hydrochlorate of 3.2kg and the Diisopropyl azodicarboxylate of 280g is added in reactor.Stirring reaction 4 hours at 70 DEG C.Add sodium hydroxide solution adjust ph to 7.0, decompression pumps most solvent, and with each 60kg ether sedimentation three times, centrifugation, drying obtains white solid polymeric monomer precursor;
In reactor, add above-mentioned polymeric monomer precursor and the 460kg tetrahydrofuran (THF) of aforementioned 100kg, be uniformly dissolved; 18.5kg acrylate chloride is dissolved in 80kg tetrahydrofuran (THF), joins in above-mentioned solution under stirring, drip the aqueous sodium carbonate of 50kg 30% simultaneously, control temperature of reaction at 3 DEG C with the jacket reactor of band refrigerant; React after 4 hours, be warming up to room temperature; Decompression pumps most of solvent, and precipitate three times in 60kg ether, obtain white solid response type dispersion agent Disp-1 after drying, molecule measuring test result is in table 1;
(2) preparation of CAPM water miscible liquid Hyem-1
By the acrylamide of 50kg, the acrylyl oxy-ethyl-trimethyl salmiac of 18kg, the above-mentioned response type dispersion agent Disp-1 of 2.5kg, the ammonium sulfate of 185kg and 3.6kg polyoxyethylene glycol (molecular weight 20000) join in reactor, add the N of 0.3kg, the EDTA of N-dimethylethanolamine and 0.2kg, add 190kg deionized water, stirring and dissolving, pH is regulated to be 6 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 30min, be warming up to 30 DEG C and add the ammonium persulphate of 2.25g and the ammonium bisulfite of 2.25g, polymkeric substance is stirred under 200rpm, after system becomes oyster white, add 2 of 5.12g again, 2 '-azo (2-amidine propane) dihydrochloride.After being warming up to 50 DEG C of continuation reaction 8h, then add the ammonium sulfate of 21kg, namely obtain the stable CPAM water miscible liquid product Hyem-1 of favorable dispersity after cooling, its performance test results is in table 2.
Embodiment 2
With embodiment 1, change 5 kilograms into unlike by the amount of N-V-Pyrol RC in step (1), the amount of sulfydryl b ammonium salt hydrochlorate changes 2.0kg into, and obtain corresponding product dispersion agent Disp-2, molecule measuring test result is in table 1; Response type dispersion agent Disp-1 in step (2) changes Disp-2 into, and obtain CPAM water miscible liquid product Hyem-2, its performance test results is in table 2.
Embodiment 3
(1) synthesis of response type dispersion agent Disp-3
The N-V-Pyrol RC of the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 140kg and 15kg is joined in two cubes of reactors, adds 550kg dissolve with ethanol; Nitrogen deoxygenation is passed into 20 minutes in reactor; The sulfydryl b ammonium salt hydrochlorate of 3.8kg and the Diisopropyl azodicarboxylate of 280g is added in reactor.Stirring reaction 4 hours at 70 DEG C.Add sodium hydroxide solution adjust ph to 7.0, decompression pumps most solvent, and with each 60kg ether sedimentation three times, centrifugation, drying obtains white solid polymeric monomer precursor;
In reactor, add above-mentioned polymeric monomer precursor and the 460kg tetrahydrofuran (THF) of aforementioned 100kg, be uniformly dissolved; 20.1kg acrylate chloride is dissolved in 80kg tetrahydrofuran (THF), joins in above-mentioned solution under stirring, drip the aqueous sodium carbonate of 55kg 30% simultaneously, control temperature of reaction at 3 DEG C with the jacket reactor of band refrigerant; React after 8 hours, be warming up to room temperature; Decompression pumps most of solvent, and precipitate three times in 60kg ether, obtain white solid response type dispersion agent Disp-3 after drying, molecule measuring test result is in table 1;
(2) preparation of CAPM water miscible liquid Hyem-3
By the acrylamide of 50kg, the acrylyl oxy-ethyl-trimethyl salmiac of 18kg, the above-mentioned response type dispersion agent Disp-3 of 2.2kg, the ammonium sulfate of 180kg and 3.5kg polyoxyethylene glycol (molecular weight 20000) join in reactor, add the N of 0.3kg, the EDTA of N-dimethylethanolamine and 0.2kg, add 190kg deionized water, stirring and dissolving, pH is regulated to be 6 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 30min, be warming up to 30 DEG C and add the ammonium persulphate of 2.10g and the ammonium bisulfite of 2.10g, polymkeric substance is stirred under 200rpm, after system becomes oyster white, add 2 of 5.10g again, 2 '-azo (2-amidine propane) dihydrochloride.After being warming up to 50 DEG C of continuation reaction 4h, then add the ammonium sulfate of 20kg, namely obtain the stable CPAM water miscible liquid product Hyem-3 of favorable dispersity after cooling, its performance test results is in table 2.
Embodiment 4
With embodiment 3, change 2 kilograms into unlike by the amount of N-V-Pyrol RC in step (1), the amount of sulfydryl b ammonium salt hydrochlorate changes 3.2kg into, and obtain corresponding product dispersion agent Disp-4, molecule measuring test result is in table 1; Response type dispersion agent Disp-3 in step (2) changes Disp-4 into, and obtain CPAM water miscible liquid product Hyem-4, its performance test results is in table 2.
Embodiment 5
(1) synthesis of response type dispersion agent Disp-5
The N-V-Pyrol RC of 140kg 3-acrylamide propyl-trimethyl ammonium chloride and 20kg is joined in two cubes of reactors, adds 580kg dissolve with ethanol; Nitrogen deoxygenation is passed into 20 minutes in reactor; The sulfydryl b ammonium salt hydrochlorate of 3.6kg and the Diisopropyl azodicarboxylate of 270g is added in reactor.Stirring reaction 4 hours at 70 DEG C.Add sodium hydroxide solution adjust ph to 7.0, decompression pumps most solvent, and with each 60kg ether sedimentation three times, centrifugation, drying obtains white solid polymeric monomer precursor;
In reactor, add above-mentioned polymeric monomer precursor and the 460kg tetrahydrofuran (THF) of aforementioned 100kg, be uniformly dissolved; 18.5kg acrylate chloride is dissolved in 80kg tetrahydrofuran (THF), joins in above-mentioned solution under stirring, drip the aqueous sodium carbonate of 52kg 30% simultaneously, control temperature of reaction at 3 DEG C with the jacket reactor of band refrigerant; React after 5 hours, be warming up to room temperature; Decompression pumps most of solvent, and precipitate three times in 60kg ether, obtain white solid response type dispersion agent Disp-5 after drying, molecule measuring test result is in table 1;
(2) preparation of CAPM water miscible liquid Hyem-3
By 50kg acrylamide, 18kg 3-acrylamide propyl-trimethyl ammonium chloride, 2.5kg above-mentioned response type dispersion agent Disp-5, 180kg ammonium sulfate and 3.3kg polyoxyethylene glycol (molecular weight 20000) join in reactor, add the N of 0.3kg, N-dimethylethanolamine and 0.2kg EDTA, add 190kg deionized water, stirring and dissolving, pH is regulated to be 6 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 30min, be warming up to 30 DEG C and add the ammonium persulphate of 2.20g and the ammonium bisulfite of 2.20g, polymkeric substance is stirred under 200rpm, after system becomes oyster white, add 2 of 5.10g again, 2 '-azo (2-amidine propane) dihydrochloride.After being warming up to 50 DEG C of continuation reaction 8h, then add the ammonium sulfate of 20kg, namely obtain the stable CPAM water miscible liquid product Hyem-5 of favorable dispersity after cooling, its performance test results is in table 2.
Embodiment 6
With embodiment 5, change 2 kilograms into unlike by the amount of N-V-Pyrol RC in step (1), the amount of sulfydryl b ammonium salt hydrochlorate changes 3.2kg into, and obtain corresponding product dispersion agent Disp-6, molecule measuring test result is in table 1; Response type dispersion agent Disp-5 in step (2) changes Disp-6 into, and obtain CPAM water miscible liquid product Hyem-6, its performance test results is in table 2.
Embodiment 7
(1) synthesis of response type dispersion agent Disp-7
The N-V-Pyrol RC of the 3-of 80kg acrylyl oxy-ethyl-trimethyl salmiac, 60kg acrylamide propyl-trimethyl ammonium chloride and 10kg is joined in two cubes of reactors, adds 580kg dissolve with ethanol; Nitrogen deoxygenation is passed into 20 minutes in reactor; The chain-transfer agent of 3.6kg and the Diisopropyl azodicarboxylate of 270g is added in reactor.Stirring reaction 4 hours at 70 DEG C.Add sodium hydroxide solution adjust ph to 7.0, decompression pumps most solvent, and with each 60kg ether sedimentation three times, centrifugation, drying obtains white solid polymeric monomer precursor;
In reactor, add above-mentioned polymeric monomer precursor and the 460kg tetrahydrofuran (THF) of aforementioned 100kg, be uniformly dissolved; 18.5kg acrylate chloride is dissolved in 80kg tetrahydrofuran (THF), joins in above-mentioned solution under stirring, drip the aqueous sodium carbonate of 52kg 30% simultaneously, control temperature of reaction at 3 DEG C with the jacket reactor of band refrigerant; React after 5 hours, be warming up to room temperature; Decompression pumps most of solvent, and precipitate three times in 60kg ether, obtain white solid response type dispersion agent Disp-7 after drying, molecule measuring test result is in table 1;
(2) preparation of CAPM water miscible liquid Hyem-7
By the acrylamide of 50kg, 3-acrylamide propyl-the trimethyl ammonium chloride of 18kg, the above-mentioned response type dispersion agent Disp-7 of 2.5kg, the ammonium sulfate of 180kg and 3.3kg polyoxyethylene glycol (molecular weight 20000) join in reactor, add the N of 0.3kg, the EDTA of N-dimethylethanolamine and 0.2kg, add 190kg deionized water, stirring and dissolving, pH is regulated to be 6 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 30min, be warming up to 30 DEG C and add the ammonium persulphate of 2.20g and the ammonium bisulfite of 2.20g, polymkeric substance is stirred under 200rpm, after system becomes oyster white, add 2 of 5.10g again, 2 '-azo (2-amidine propane) dihydrochloride.After being warming up to 50 DEG C of continuation reaction 8h, then add the ammonium sulfate of 20kg, namely obtain the stable CPAM water miscible liquid product Hyem-7 of favorable dispersity after cooling, its performance test results is in table 2.
Embodiment 8
(1) synthesis of response type dispersion agent Disp-8
The N-V-Pyrol RC of the acrylyl oxy-ethyl-trimethyl salmiac of 140kg, 10kg acryloxyethyldimethyl benzyl ammonium chloride and 12kg is joined in two cubes of reactors, adds 550kg dissolve with ethanol; Nitrogen deoxygenation is passed into 20 minutes in reactor; The chain-transfer agent of 3.0kg and the Diisopropyl azodicarboxylate of 270g is added in reactor.Stirring reaction 4 hours at 70 DEG C.Add sodium hydroxide solution adjust ph to 7.0, decompression pumps most solvent, and with each 60kg ether sedimentation three times, centrifugation, drying obtains white solid polymeric monomer precursor;
In reactor, add above-mentioned polymeric monomer precursor and the 460kg tetrahydrofuran (THF) of aforementioned 100kg, be uniformly dissolved; 18.5kg acrylate chloride is dissolved in 80kg tetrahydrofuran (THF), joins in above-mentioned solution under stirring, drip the aqueous sodium carbonate of 50kg 30% simultaneously, control temperature of reaction at 3 DEG C with the jacket reactor of band refrigerant; React after 5 hours, be warming up to room temperature; Decompression pumps most of solvent, and precipitate three times in 60kg ether, obtain white solid response type dispersion agent Disp-8 after drying, molecule measuring test result is in table 1;
(2) preparation of CAPM water miscible liquid Hyem-8
By the acrylamide of 50kg, 3-acrylamide propyl-the trimethyl ammonium chloride of 18kg, the above-mentioned response type dispersion agent Disp-4 of 3.2 kg, the ammonium sulfate of 180kg and 3.0kg polyoxyethylene glycol (molecular weight 20000) join in reactor, add the N of 0.3kg, the EDTA of N-dimethylethanolamine and 0.2kg, add 190kg deionized water, stirring and dissolving, pH is regulated to be 6 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 30min, be warming up to 30 DEG C and add the ammonium persulphate of 2.10g and the ammonium bisulfite of 2.10g, polymkeric substance is stirred under 200rpm, after system becomes oyster white, add 2 of 5.10g again, 2 '-azo (2-amidine propane) dihydrochloride.After being warming up to 50 DEG C of continuation reaction 8h, then add the ammonium sulfate of 20kg, namely obtain the stable CPAM water miscible liquid product Hyem-8 of favorable dispersity after cooling, its performance test results is in table 2.
The molecule measuring test result of dispersion agent in each embodiment of table 1
The performance test results of CPAM water miscible liquid product in each embodiment of table 2
Claims (10)
1. a preparation method for response type dispersion agent and polyacrylamide aqueous emulsion, to is characterized in that by the response type polymeric monomer shown in formula (1), as dispersion agent, being formed by acrylamide and cationic monomer copolymerization,
formula (1).
2. the preparation method of a kind of response type dispersion agent according to claim 1 and polyacrylamide aqueous emulsion is characterized in that in formula (1), m is the cationic polymerization degree of polymer segment in macromonomer; N is the polymerization degree of V-Pyrol RC in macromonomer; A is 2 ~ 3; A is H or CH
3, B is O or N element.
3. the preparation method of a kind of response type dispersion agent according to claim 1 and polyacrylamide aqueous emulsion, is characterized in that the molecular-weight average of polymeric monomer dispersion agent is 2 × 10
5~ 8 × 10
5.
4., according to the preparation method of a kind of response type dispersion agent described in claim 1 and polyacrylamide aqueous emulsion, it is characterized in that described cationic polyacrylamide water miscible liquid, its dissolution rate is less than 10min.
5., according to the preparation method of a kind of response type dispersion agent described in claim 1 and polyacrylamide aqueous emulsion, it is characterized in that described cationic polyacrylamide water miscible liquid, its molecular weight is more than 8,000,000.
6., according to the preparation method of a kind of response type dispersion agent described in claim 1 and polyacrylamide aqueous emulsion, it is characterized in that described cationic polyacrylamide water miscible liquid, its product system viscosity is less than 400 mPas.
7. the preparation method of a kind of response type dispersion agent according to claim 1 and polyacrylamide aqueous emulsion, is characterized in that the preparation method of polymeric monomer dispersion agent is:
The N-V-Pyrol RC of the cationic monomer of 20 ~ 30 parts and 0 ~ 5 part adds in reactor by step 1), adds the dissolution with solvents of 30 ~ 100 parts; Nitrogen deoxygenation is passed into 15 ~ 30 minutes in reactor; The chain-transfer agent of 0.01 ~ 1 part and the initiator of 0.001 ~ 0.05 part is added in reactor; Stirring reaction 4 ~ 6 hours at 60 ~ 70 DEG C; Add sodium hydroxide solution adjust ph to 7 ~ 9, decompression pump most solvent, precipitate three times, centrifugation with 10 ~ 50 parts of precipitation agents, drying obtains white solid polymeric monomer precursor, its structural formula as the formula (2):
formula (2)
Step 2) in reactor, add the polymeric monomer precursor of aforementioned 10 ~ 20 parts and the tetrahydrofuran (THF) of 50 ~ 100 parts, be uniformly dissolved; 1 ~ 10 part of acrylate chloride is dissolved in 20 ~ 50 parts of tetrahydrofuran (THF)s, joins under stirring in above-mentioned solution, drip a certain amount of aqueous sodium carbonate simultaneously, control temperature of reaction at 0 ~ 4 DEG C with the jacket reactor of band refrigerant; React after 2 ~ 4 hours, be warming up to room temperature; Decompression pumps solvent, and precipitate three times in 10 ~ 50 parts of ether, obtain white solid response type dispersion agent after drying, its structural formula as the formula (1).
8. a kind of response type dispersion agent according to claim 1 or 7 and the preparation method of polyacrylamide aqueous emulsion, is characterized in that: the preparation process 1 of polymeric monomer dispersion agent) described in cationic monomer be selected from acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloxyethyldimethyl benzyl ammonium chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, 3-acrylamide propyl-trimethyl ammonium chloride, 3-(Methacrylamide propyl group) one or both in-trimethyl ammonium chloride; One in solvent selected from methanol, ethanol and acetonitrile, is preferably ethanol; Chain-transfer agent is sulfydryl b ammonium salt hydrochlorate; Described initiator is selected from 2, two (2-amidine propane) dihydrochloride, 2 of 2-azo, one or both in 2-azo two (2-amidine azoles quinoline propane) hydrochloride, azo two (2,5-dimethyl-6-carboxyl) own nitrile and Diisopropyl azodicarboxylate, preferred Diisopropyl azodicarboxylate; Described precipitation agent is selected from the one in ether and acetone, preferred ether.
9. according to the preparation method of a kind of response type dispersion agent described in claim 1 and polyacrylamide aqueous emulsion, it is characterized in that described cationic polyacrylamide water miscible liquid, preparation method is: by the acrylamide of 5 ~ 10 parts, the cationic monomer of 1 ~ 7 part, the above-mentioned response type dispersion agent of 0.1 ~ 2 part, the polyoxyethylene glycol (molecular weight 20000) of the ammonium sulfate of 20 ~ 35 parts and 0.1 ~ 4 part joins in reactor, add the chainextender of 0.001 ~ 0.05 part and the complexing agent of 0.001 ~ 0.01 part, add the deionized water of 40 ~ 60 parts, stirring and dissolving, pH is regulated to be 5 ~ 8 with NaOH solution and dilute sulphuric acid, after logical nitrogen deoxygenation 15 ~ 40min, be warming up to the oxidation-reduction initiator that 30 ~ 35 DEG C add the Oxidizing and Reducing Agents composition of 0.0001 ~ 0.01 part, regulate stirring velocity, after system becomes oyster white, add the azo initiator of 0.0001 ~ 0.01 part again, after being warming up to 50 ~ 55 DEG C of continuation reaction 4 ~ 6h, add the ammonium sulfate of 2 ~ 5 parts again, namely the stable CPAM water miscible liquid product of favorable dispersity is obtained after cooling.
10. according to the preparation method of a kind of response type dispersion agent described in claim 1 or 9 and polyacrylamide aqueous emulsion, it is characterized in that in described cationic polyacrylamide water miscible liquid preparation process, cationic monomer be selected from acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloxyethyldimethyl benzyl ammonium chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, 2-acrylamido-2-trimethoxysilyl propyl methacrylate ammonium chloride one or both; Chainextender is selected from N, one or more in N-dimethylethanolamine, ethylene glycol, hexylene glycol, N, N-dimethyl-ethylenediamine, N, N-Tetramethyl Ethylene Diamine, triethylene tetramine, 1,3-dimethylamino propionitrile; Complexing agent is EDTA; Oxygenant be selected from ammonium persulphate, Sodium Persulfate, Potassium Persulphate, hydrogen peroxide and 2-methylethyl ketone peroxide one or more; Reductive agent be selected from ammonium sulphite, potassium sulfite, S-WAT, ammonium bisulfite, sodium bisulfite, Potassium hydrogen sulfite and sodium formaldehyde sulphoxylate one or more; Azo series initiators is 2,2 '-azo (2-amidine propane) dihydrochloride, 2,2 '-azo (2-tetrahydroglyoxaline propane) dihydrochloride and 4, one or more in 4 '-azo two (4-cyanopentanoic acid), be preferably 2,2 '-azo (2-amidine propane) dihydrochloride.
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