CN102603970B - Preparation method of cationic polyacrylamide - Google Patents
Preparation method of cationic polyacrylamide Download PDFInfo
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- CN102603970B CN102603970B CN201210010428.5A CN201210010428A CN102603970B CN 102603970 B CN102603970 B CN 102603970B CN 201210010428 A CN201210010428 A CN 201210010428A CN 102603970 B CN102603970 B CN 102603970B
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 41
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 67
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 239000000084 colloidal system Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000007670 refining Methods 0.000 claims description 9
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 7
- 239000004160 Ammonium persulphate Substances 0.000 claims description 5
- 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
- -1 acrylyl Chemical group 0.000 claims description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 5
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004159 Potassium persulphate Substances 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims 1
- 239000010802 sludge Substances 0.000 abstract description 15
- 239000003651 drinking water Substances 0.000 abstract description 9
- 235000020188 drinking water Nutrition 0.000 abstract description 9
- 238000006116 polymerization reaction Methods 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 7
- 239000010865 sewage Substances 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 208000005156 Dehydration Diseases 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 238000006392 deoxygenation reaction Methods 0.000 description 12
- 239000012752 auxiliary agent Substances 0.000 description 9
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 3
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- LBSPZZSGTIBOFG-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;dihydrochloride Chemical compound Cl.Cl.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 LBSPZZSGTIBOFG-UHFFFAOYSA-N 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 231100000570 acute poisoning Toxicity 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000012986 chain transfer agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 210000001331 nose Anatomy 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 231100000683 possible toxicity Toxicity 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Sludge (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a preparation method of cationic polyacrylamide. The cationic polyacrylamide is prepared by the following steps of: adding a certain amount of solubilizing agent and complexing agent into acrylamide (AM) and aqueous solution of two cationic monomers; regulating the pH value of a reaction system; then adding a certain amount of initiator; and performing the polymerization reaction under the ultraviolet light with a certain wavelength. The preparation method has the advantages that the polymerization reaction time is short; few types of auxiliaries are added; and the prepared product has high purity and is non-toxic and harmless. The cationic polyacrylamide obtained by the preparation method has multifunctionality, has the molecular weight of 1 million to 12 million, has ultralow concentration of a residual acrylamide monomer, is suitable for treatment of drinking water and sewage treatment and dehydration treatment of sludge and has excellent application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of aqueous solution high molecular polymer, be specifically related to a kind of preparation method of cationic polyacrylamide.
Background technology
At present, for sewage work's flocculation agent, mainly contain inorganic flocculating agent and the large class of organic polymer coargulator two.Polyacrylamide flocculant is a kind of important organic polymer coargulator, comprises cationic polyacrylamide (CPAM), anionic polyacrylamide (APAM), non-ionic polyacrylamide (NPAM) and zwitter-ion polyacrylamide; Wherein, cationic polyacrylamide (CPAM) is its high-end product, it has the advantages such as good turbidity removal, decoloration performance, existing preparation method's product is mostly because auxiliary agent is used too much, affect product purity and building-up reactions is insufficient, residual acrylamide monomer content is larger, and refining rear residual acrylamide monomer content is still greater than 0.05% and is not suitable for Drinking Water processing, is only suitable for industrial sewage, city domestic sewage processing and urban wastewater treatment firm sludge dewatering treatment.
The preparation method of existing cationic polyacrylamide, is to take acrylamide as raw material, by the copolymerization with cationic monomer or modified-reaction, obtains.In the publication number patent " preparation method of high molecular weight instant cation polyacrylamide " that is CN101353392A, this patent is to be dissolved in deionized water with acrylamide and comonomer; Add certain additive, mixing of materials is evenly to thickness state, be poured in a plane and spread out and put on as laminar, pass into high pure nitrogen, then carry out UV-irradiation to spreading out and putting on for laminar material.The deficiency of the method is: 1, the reactive polymeric time long, preferably the time is 3～6 hours; 2, in reacting solution in additive except initiator, also add six kinds of auxiliary agents as sequestrant, chain propagation agent, chain-transfer agent, surfactant etc., and every kind of auxiliary agent also comprises one or more materials, the dosage summation of various auxiliary agents can be up to 1.95% of total monomer quality.Various auxiliary agents remain among synthetic product the most at last, are difficult for removing having a strong impact on product purity; 3, in auxiliary agent, also have part material toxicity larger, improper production and application, as chain propagation agent boric acid itself can be used as a kind of wound sterilizing agent, the oral acute poisoning that causes, main manifestations is gastrointestinal symptom, having nauseating, vomiting, stomachache, diarrhoea etc., is and to apply in water treatment as the raw material of water conditioner, can pollute have potential toxicity to water body; Chain regulator diethylenetriamine, its steam of triethylene diamine or mist are corrosive to nose, larynx and mucous membrane, and producers need wear a gas mask.
Summary of the invention
Technical problem to be solved by this invention is just to provide a kind of method of cationic polyacrylamide, and in the preparation process of the method, polymerization reaction time is short, adds that auxiliary agent kind is few, consumption is low, and the product purity of preparation is high, nontoxic.
Technical problem to be solved by this invention is to realize by such technical scheme, and it comprises the following steps:
The first step, takes 20%～80%, two kinds of cationic monomers 20%～80% of monomer acrylamide by monomer total mass per-cent; Add distilled water, and stir to dissolving completely, the monomer solution that the mass concentration that makes total monomer is 20%～50%;
Second step, in the monomer solution of above-mentioned preparation, add the urea with monomer total mass 0.05%～0.5%, add again the EDTA complex agent with monomer total mass 0.01%～0.2%, pH value 8～9 by weak base or weak acid regulation system, be filled with High Purity Nitrogen except oxygen, add fast the initiator with monomer total mass 0.1%～3%, this initiator comprises oxygenant Potassium Persulphate or ammonium persulphate and reductive agent S-WAT, oxygenant is 0.5～2 with the quality of reductive agent than scope, stir simultaneously, then be filled with High Purity Nitrogen except sealing after oxygen;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, under UV-irradiation, cause, irradiate after 10min～90min, standing slaking more than 1 hour, makes water white kation polyacrylamide colloid;
The 4th step, by described cationic polyacrylamide thickness colloid, through shredding granulation, dehydrated alcohol repeatedly wash refining, make cationic polyacrylamide white solid powder after drying, grinding.
The initiator that the present invention adopts can also be organic initiators or inorganic organic complex initiator.
Material therefor of the present invention is commercially available, cheap, can directly buy.
The initiator system of selecting due to the present invention is the shorter UV-light of wavelength, its energy is greater than the chemical bond energy of monomer, trigger monomer polymerization in a long time, after adding initiator, auxiliary agent, speed of reaction significantly promotes, and required initiator, auxiliary dosage are low, just can obtain that purity is high, the product of even molecular weight distribution.The present invention has advantages of following:
1, polymerization reaction time is short.What adopt due to the present invention is uv-light polymerization, and UV-light can be accelerated the fracture of chemical bond, by radical polymerization, so can greatly shorten the initiated polymerization time, minimum 10min of its initiated polymerization time.
2, synthetic required initiator, auxiliary agent kind is few, consumption is low, the residue in product is few, product purity is high; Adjuvant used nontoxic, product is used safety, is applicable to the processing of tap water.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
The first step, takes monomer acrylamide 7g, dimethyl diallyl ammonium chloride 2g, acrylyl oxy-ethyl-trimethyl salmiac 1g puts into wide-necked bottle, and adding distil water 23.3ml, stirs, the monomer solution that the mass concentration that makes total monomer is 30%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.02g urea as solubilizing agent (consumption be monomer total mass 0.2%), then add EDTA complex agent 0.004g(consumption be monomer total mass 0.04%), regulate pH=9; Pass into nitrogen deoxygenation, adding without organic initiators 0.144g(Potassium Persulphate and S-WAT mass ratio is 1:2), consumption is 1.44% of monomer total mass, stirs, then passes into nitrogen deoxygenation, airtight afterwards.
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 15 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.1870%, after dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 4747241, and cationic degree is 10.86%, the high purity product that residual acrylamide monomer content is 0.0153%.Be applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 2
The first step, takes monomer acrylamide 8g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 1g, dimethyl diallyl ammonium chloride 1g puts into wide-necked bottle, and adding distil water 10ml, stirs, the monomer solution that the mass concentration that makes total monomer is 50%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.05g urea as solubilizing agent (consumption be monomer total mass 0.5%), then add EDTA complex agent 0.02g(consumption be monomer total mass 0.2%), regulate pH=8; Pass into nitrogen deoxygenation, adding without organic initiators 0.015g(ammonium persulphate and S-WAT mass ratio is 2:1, consumption be monomer total mass 0.15%), stir, then pass into nitrogen deoxygenation, airtight afterwards;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 10 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.2262%, after dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 1280500, and cationic degree is 3.37%, and the high purity product that residual acrylamide monomer content is 0.0197% is applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 3
The first step, take monomer acrylamide 7g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 1.5g, dimethyl diallyl ammonium chloride 1.5g puts into wide-necked bottle, adding distil water 30ml, stirs, the monomer solution that the mass concentration that makes total monomer is 25%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.005g urea as solubilizing agent (consumption be monomer total mass 0.05%), then add EDTA complex agent 0.001g(consumption be monomer total mass 0.01%), regulate pH=6; Pass into nitrogen deoxygenation, add 0.12g organic initiators azo-bis-isobutyrate hydrochloride V50(consumption be monomer total mass 1.2%), stir, then pass into nitrogen deoxygenation, airtight afterwards;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 60 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.1221%; After dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 4051330, and cationic degree is 10.98%, and the high purity product that residual acrylamide monomer content is 0.0107% is applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 4
The first step, takes monomer acrylamide 2g, dimethyl diallyl ammonium chloride 4g, acrylyl oxy-ethyl-trimethyl salmiac 4g puts into wide-necked bottle, and adding distil water 30ml, stirs, the monomer solution that the mass concentration that makes total monomer is 25%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.024g urea as solubilizing agent (consumption be monomer total mass 0.24%), then add EDTA complex agent 0.02g(consumption be monomer total mass 0.2%), regulate pH=8; Pass into nitrogen deoxygenation, adding inorganic organic complex initiator 0.12g(Potassium Persulphate, S-WAT and v50 mass ratio is 1:1:8, consumption be monomer total mass 1.2%), stir, then pass into nitrogen deoxygenation, airtight afterwards;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 60 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.1416%, after dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 7051330, and cationic degree is 51.86%, and the high purity product that residual acrylamide monomer content is 0.0113% is applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 5
The first step, take monomer acrylamide 6g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 2g, acrylyl oxy-ethyl-trimethyl salmiac 2g puts into wide-necked bottle, adding distil water 40ml, stirs, the monomer solution that the mass concentration that makes total monomer is 20%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.005g urea as solubilizing agent (consumption be monomer total mass 0.05%), then add EDTA complex agent 0.001g(consumption be monomer total mass 0.01%), regulate pH=8; Pass into nitrogen deoxygenation, adding inorganic organic complex initiator 0.25g(ammonium persulphate, S-WAT and V-50 mass ratio is 2:2:1, consumption be monomer total mass 2.5%), stir, then pass into nitrogen deoxygenation, airtight afterwards;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 60 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.0866%, after dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 6378830, and cationic degree is 16.0%, and the high purity product that residual acrylamide monomer content is 0.0087% is applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 6
The first step, takes monomer acrylamide 4g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 3g, dimethyl diallyl ammonium chloride 3g puts into wide-necked bottle, and adding distil water 10ml, stirs, the monomer solution that the mass concentration that makes total monomer is 50%;
Second step, in the monomer solution of above-mentioned preparation, adds 0.05g urea as solubilizing agent (consumption be monomer total mass 0.5%), then add EDTA complex agent 0.001g(consumption be monomer total mass 0.01%), regulate pH=8; Pass into nitrogen deoxygenation, adding inorganic organic complex initiator 0.3g(ammonium persulphate, S-WAT and VA-044 mass ratio is 1:1:8, consumption be monomer total mass 3%), stir, then pass into nitrogen deoxygenation, airtight afterwards;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, and UV-irradiation, after 90 minutes, obtains water white kation polyacrylamide colloid; Residual acrylamide monomer content is 0.0582%, after dilution, can be directly used in sludge dewatering treatment.
The 4th step, by described kation polyacrylamide colloid, through shredding granulation, refining, make cationic polyacrylamide white solid powder after drying, grinding; Recording molecular weight is 11200730, and cationic degree is 29.85%, and the high purity product that residual acrylamide monomer content is 0.0068% is applicable to drinking water treatment and sludge dewatering treatment.
Embodiment 7
Identical with embodiment 3, but add 0.25g organic initiators azo di-isopropyl imidazoline salt hydrochlorate VA-044(consumption be monomer total mass 2.5%), obtaining molecular weight is 6378830, cationic degree is 11.85%, residual acrylamide monomer content is 0.0087% high purity product, is applicable to drinking water treatment and sludge dewatering treatment.
In above-described embodiment, the indoor environment temperature that polyreaction is used is 5 ℃～45 ℃ room temps, and above-mentioned UV-light is produced by high voltage mercury lamp, and its ultraviolet wavelength is at 220nm～2000nm, predominant wavelength 365nm.
Claims (2)
1. a preparation method for cationic polyacrylamide, is characterized in that, comprises the following steps:
The first step, takes 20%～80%, two kinds of cationic monomers 20%～80% of monomer acrylamide by monomer total mass per-cent; Add distilled water, and stir to dissolving completely, the monomer solution that the mass concentration that makes total monomer is 20%～50%;
Second step, in the monomer solution of above-mentioned preparation, add the urea with monomer total mass 0.05%～0.5%, add again the EDTA complex agent with monomer total mass 0.01%～0.2%, pH value 8～9 by weak base or weak acid regulation system, be filled with High Purity Nitrogen except oxygen, add fast the initiator with monomer total mass 0.1%～3%, this initiator comprises oxygenant Potassium Persulphate or ammonium persulphate and reductive agent S-WAT, oxygenant is 0.5～2 with the quality of reductive agent than scope, stir simultaneously, then be filled with High Purity Nitrogen except sealing after oxygen;
The 3rd step, under indoor environment temperature, puts into the mixture of above-mentioned preparation in UV-light reaction unit, under UV-irradiation, cause, irradiate after 10min～90min, standing slaking more than 1 hour, makes water white kation polyacrylamide colloid;
The 4th step, by described cationic polyacrylamide thickness colloid, through shredding granulation, dehydrated alcohol repeatedly wash refining, make cationic polyacrylamide white solid powder after drying, grinding.
2. the preparation method of cationic polyacrylamide according to claim 1, it is characterized in that adopting terpolymer, two kinds of described cationic monomers are optional two kinds in MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC), acrylyl oxy-ethyl-trimethyl salmiac (DAC), dimethyl diallyl ammonium chloride (DMDAAC).
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| KR20140016557A (en) * | 2012-07-30 | 2014-02-10 | (주)엘지하우시스 | Photopolymerization resin composition and photopolymerization resin including the same |
| CN103059219B (en) * | 2013-01-28 | 2015-06-24 | 重庆大学 | Preparation method for hydrophobic-association cationic polyacrylamide |
| CN103819692A (en) * | 2014-02-28 | 2014-05-28 | 重庆大学 | Simplified processing method of polyacrylamide by template copolymerization |
| CN103833117B (en) * | 2014-03-07 | 2015-07-15 | 重庆大学 | Organic-inorganic composite coagulant for processing printing and dyeing wastewater and preparation method thereof |
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