CN106317306B - A kind of preparation method of cationic polyacrylamide - Google Patents
A kind of preparation method of cationic polyacrylamide Download PDFInfo
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- CN106317306B CN106317306B CN201510349214.4A CN201510349214A CN106317306B CN 106317306 B CN106317306 B CN 106317306B CN 201510349214 A CN201510349214 A CN 201510349214A CN 106317306 B CN106317306 B CN 106317306B
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- 125000002091 cationic group Chemical group 0.000 title claims abstract description 47
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 28
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims abstract description 7
- 239000005457 ice water Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- -1 propylene amides Chemical class 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 claims description 5
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical group [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims 2
- 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 claims 1
- 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 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 239000012535 impurity Substances 0.000 abstract description 12
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 abstract description 11
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 abstract description 11
- 238000012546 transfer Methods 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 150000001412 amines Chemical class 0.000 abstract description 3
- 230000008676 import Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- 239000012966 redox initiator Substances 0.000 abstract description 3
- 229920006322 acrylamide copolymer Polymers 0.000 abstract description 2
- 238000006392 deoxygenation reaction Methods 0.000 abstract description 2
- 230000036284 oxygen consumption Effects 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 150000003926 acrylamides Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 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 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 2
- NRPSZPOPYCCBPK-UHFFFAOYSA-L S(=O)(=O)([O-])S(=O)[O-].[Na+].C(C)(C)(C)OO.[Na+] Chemical compound S(=O)(=O)([O-])S(=O)[O-].[Na+].C(C)(C)(C)OO.[Na+] NRPSZPOPYCCBPK-UHFFFAOYSA-L 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- KJESGYZFVCIMDE-UHFFFAOYSA-N 1-chloroethanol Chemical compound CC(O)Cl KJESGYZFVCIMDE-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 241001614291 Anoplistes Species 0.000 description 1
- 238000006683 Mannich reaction Methods 0.000 description 1
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical class COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 1
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 description 1
- SATQNYRZLIROHO-UHFFFAOYSA-N [NH4+].[Na].OS([O-])=O Chemical compound [NH4+].[Na].OS([O-])=O SATQNYRZLIROHO-UHFFFAOYSA-N 0.000 description 1
- FRTNIYVUDIHXPG-UHFFFAOYSA-N acetic acid;ethane-1,2-diamine Chemical class CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN FRTNIYVUDIHXPG-UHFFFAOYSA-N 0.000 description 1
- AJXBTRZGLDTSST-UHFFFAOYSA-N amino 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON AJXBTRZGLDTSST-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- YIOJGTBNHQAVBO-UHFFFAOYSA-N dimethyl-bis(prop-2-enyl)azanium Chemical compound C=CC[N+](C)(C)CC=C YIOJGTBNHQAVBO-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002171 ethylene diamines Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerization Catalysts (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention provides a kind of preparation methods of cationic polyacrylamide, the reproducibility of amine impurities in domestic cationic monomer is mainly utilized in this method, the a small amount of oxygen dissolved in system is as oxidant, it adds in and redox initiator initiation system prepolymerization is formed by auxiliary agent such as sodium hydrogensulfite of larger reactivity etc. together with oxygen, polymerization unit polymerization is transferred to by appropriate initiator is added after the monomelic impurities for having chain tra nsfer, inhibition in system and oxygen consumption completely.This method is low to the purity requirement of cationic monomer, without deoxygenation, and polymerize segment processing, and radiating control is convenient, has higher industrial production practical value.In addition, the method overcome the dependence of the low impurity cationic monomer to import, production cost is reduced, is particularly suitable for the preparation of highly cationic and/or the acrylamide copolymer of high molecular weight.
Description
Technical field
Preparation method more particularly to a kind of cationic polyacrylamide the present invention relates to a kind of acrylamido copolymer
Preparation method.
Background technology
Acrylamido copolymer is a kind of extremely important water-soluble polymer, is widely used in wastewater treatment, oil, spinning
Knit, papermaking, the industries such as mining.By ion characteristic, polyacrylamide can be divided into nonionic, anion, cation and amphoteric
Four types, the polyacrylamide of ionic can be prepared by common poly and modified.
Chinese patent or application CN104371054A, CN104262517A, CN102702401A, CN1257840A etc. are open
By hydrolyzing the either technical side of the method for modifying polyacrylamide anionic such as Mannich reactions or cationization
Case, above-mentioned technique resulting product reliable in quality and of low cost, but due to polyacrylamide, especially high-molecular-weight poly third
The solution viscosity of acrylamide is larger so that modified-reaction system concentration is relatively low, since common product is direct with aqueous solution
It uses, too low concentration limits its production capacity and sales range.Therefore, above-mentioned existing skill is used in large-scale industrial production
Art, there are drawbacks described above.
Chinese patent or application CN101130938B, CN104558405A, CN102964518A etc. are disclosed suitable for most
Number scale enterprises industrial technical solution, main the employed copolymerization method of the above-mentioned prior art.However, the prior art
The quality requirement of used cationic monomer is higher in copolymerization method, and corresponding manufacturing requirements is higher, can only largely rely on
Import obtains, therefore expensive, and cost is higher.At present, it is big although some domestic enterprises can produce cationic monomer
The quality of portioned product still has certain gap with imported product, contains more impurity such as dimethylamine, two among homemade goods
Methylaminoethanol, methanol, chlorethanol, (methyl) acrylates and (methyl) esters of acrylic acid etc., there is many tools in these impurity
Have chain tra nsfer and inhibition, seriously affect the quality being smoothed out with product of polymerisation, production highly cationic and
During high molecular weight polyacrylamide, this phenomenon is particularly evident.
However, it is found by the inventors that under certain conditions, amine substance and oxygen in above-mentioned impurity can participate in oxidation
Reduction reaction initiated polymerization (referring to《Macromolecule is notified to》, 2011, page 5,39-50), therefore, it may be considered that it is suitable to find
Condition convert it into initiator, realize the effect turned bane into boon.
Invention content
In order to overcome above-mentioned problems of the prior art, a kind of cationic polyacrylamide is inventors herein proposed
Preparation method, the cationic monomer raw material used in this method can be containing more polymictic domestic cationic monomer, lead to
It crosses and adds a small amount of auxiliary agent, cause system prepolymerization with the objectionable impurities composition redox initiator in cationic monomer raw material,
Etc. in systems impurity add initiator after being exhausted and continue to complete polymerisation.
The present invention provides a kind of preparation methods of cationic polyacrylamide, which is characterized in that includes the following steps：
(1) 5~60 parts by weight cationic monomers are dissolved in 30~80 parts by weight of deionized water；
(2) 0.0015~0.05 parts by wt EDTA-disodium is added, is fully dissolved；
(3) 0.001~0.6 parts by weight auxiliary agent and 10~65 parts by weight propylene amides, stirring and dissolving are added in, and opens cycle
Ice water or ice-water bath cooling, carry out low temperature prepolymerization；
(4) to the end of prepolymerization, 0.003~0.6 parts by weight initiator is added in, after stirring evenly, transfers the material into appearance
Closed static polymerization is kept the temperature in device；
(5) polymerizate stripping and slicing is dried, then crushed, and redrying, finally smashing into product powder.
Preferably, in this method, the step (3) is：Add in 0.005-0.01 parts by weight auxiliary agent and 10~65 parts by weight
Acrylamide, stirring and dissolving, and cycle ice water or ice-water bath cooling are opened, carry out low temperature prepolymerization.
It is further preferred that in this method, the step (1) is：By 5~60 parts by weight cationic monomers and 1~20 weight
Amount part acrylic acid is dissolved in 30~80 parts by weight of deionized water, and be adjusted to neutrality system pH with soda bath.
It is further preferred that in this method, the container in the step (4) is template container.
It is further preferred that in this method, the cationic monomer is selected from quaternary ammonium type or tertiary amine-type cationic monomer.Its
In, the cationic monomer preferably is selected from following any one or more combination：Acryloyloxyethyl trimethyl ammonium chloride, methyl
Acrylyl oxy-ethyl-trimethyl salmiac, methylacryloxyethyldimethyl benzyl ammonium chloride, dimethyl diallyl chlorination
Ammonium.Wherein, the cationic monomer is much further preferably from acryloyloxyethyl trimethyl ammonium chloride.
It is further preferred that in this method, the auxiliary agent is sulphite or bisulfites.Wherein, the auxiliary agent
Preferably sodium hydrogensulfite.
It is further preferred that in this method, the initiator is water-soluble low temperature primosome series initiators.Wherein, institute
State initiator preferably be selected from it is following any：Potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-mercaptan, ammonium persulfate-bisulfite
Sodium, tert-butyl hydroperoxide-sodium pyrosulfite.
The present invention utilizes the reproducibility of amine impurities in domestic cationic monomer, and a small amount of oxygen dissolved in system is as oxygen
Agent adds in and forms redox initiator primosome together by auxiliary agent such as sodium hydrogensulfite of larger reactivity etc. with oxygen
It is prepolymerization, appropriate initiator will be added after the monomelic impurities for having chain tra nsfer, inhibition in system and oxygen consumption completely
It is transferred to polymerization unit polymerization.This method is low to the purity requirement of cationic monomer, without deoxygenation, and polymerize segment processing, dissipates
Thermal control is convenient, has higher industrial production practical value.In addition, the method overcome the low impurity cationic lists to import
The dependence of body, reduces production cost, is particularly suitable for the system of highly cationic and/or the acrylamide copolymer of high molecular weight
It is standby.
Specific embodiment
The present invention is further elaborated With reference to embodiment, but the present invention is not limited to following embodiment party
Formula.
A kind of preparation method of cationic polyacrylamide, which is characterized in that include the following steps：
(1) 5~60 parts by weight cationic monomers are dissolved in 30~80 parts by weight of deionized water；
(2) 0.0015~0.05 parts by wt EDTA-disodium is added, is fully dissolved；
(3) 0.001~0.6 parts by weight auxiliary agent and 10~65 parts by weight propylene amides, stirring and dissolving are added in, and opens cycle
Ice water or ice-water bath cooling, carry out low temperature prepolymerization；
(4) to the end of prepolymerization, 0.003~0.6 parts by weight initiator is added in, after stirring evenly, transfers the material into appearance
Closed static polymerization is kept the temperature in device；
(5) polymerizate stripping and slicing is dried, then crushed, and redrying, finally smashing into product powder.
In a preferred embodiment, in this method, the step (3) is：Add in 0.005-0.01 parts by weight auxiliary agent and
10~65 parts by weight propylene amides, stirring and dissolving, and cycle ice water or ice-water bath cooling are opened, carry out low temperature prepolymerization.
In a further preferred embodiment, in this method, the step (1) is：By 5~60 parts by weight cation
Monomer and 1~20 parts by weight of acrylic acid are dissolved in 30~80 parts by weight of deionized water, and with soda bath by system pH adjust to
It is neutral.
In a further preferred embodiment, in this method, the container in the step (4) holds for template
Device.
In an embodiment still more preferably, in this method, the cationic monomer is selected from quaternary ammonium type or tertiary amine
Type cationic monomer.Wherein, the cationic monomer preferably is selected from following any one or more combination：Acryloyl-oxyethyl three
Ammonio methacrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, diformazan
Base diallyl ammonium chloride.Wherein, the cationic monomer is much further preferably from acryloyloxyethyl trimethyl ammonium chloride.
In an embodiment still more preferably, in this method, the auxiliary agent is sulphite or bisulfites.
Wherein, the auxiliary agent is preferably sodium hydrogensulfite.
In an embodiment still more preferably, in this method, the initiator is that water-soluble low temperature causes system
Initiator.Wherein, the initiator preferably is selected from following any：Potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-mercaptan, over cure
Sour ammonium-sodium hydrogensulfite, tert-butyl hydroperoxide-sodium pyrosulfite.
Embodiment 1
By the domestic acrylyl oxy-ethyl-trimethyl salmiacs of 250g (being converted into 100%), 100g acrylic acid, 0.8g ethylenediamines
Tetraacethyl disodium is dissolved in 1.5kg deionized waters, starts stirring, and adds in 0.5g sodium hydrogensulfites and 650g acrylamides, and
System is placed in stirring cooling reaction half an hour in ice-water bath, system viscosity becomes larger, and can pull out long filament.It is separately added into 1g Asias
Niter cake and 2g ammonium persulfates, and transfer the material into the static polymerization 10 hours of 30 DEG C or so of template vessel insulation.By gel
Shape product takes out, 70 DEG C of vacuum drying after stripping and slicing, up to product after redrying after siccative crushes.Products therefrom is easy to dissolve,
It is 10,700,000 through intrinsic viscosity conversion molecular weight.
Embodiment 2
By the domestic MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides of 400g (being converted into 100%), 0.8g ethylenediamine tetra-acetic acids
Disodium is dissolved in 1.5kg deionized waters, starts stirring, and adds in 0.5g sodium hydrogensulfites and 600g acrylamides, and by system
It is placed in ice-water bath and is stirred to react half an hour, system viscosity becomes larger, and can pull out long filament.Be separately added into 1g sodium hydrogensulfites and
2g ammonium persulfates, and transfer the material into the static polymerization 10 hours of 30 DEG C or so of template vessel insulation.Gel-like product is taken out,
70 DEG C of vacuum drying after stripping and slicing, up to product after redrying after siccative crushes.Products therefrom is easy to dissolve, is rolled over through intrinsic viscosity
It is 9,200,000 to calculate molecular weight.
Embodiment 3
The domestic dimethyl diallyl ammonium chlorides of 300g (being converted into 100%), 0.8g disodium ethylene diamine tetraacetates are dissolved in
In 1kg deionized waters, stirring is started, and adds in 0.5g sodium hydrogensulfites and 700g acrylamides, and system is placed in ice-water bath
In be stirred to react half an hour, system viscosity becomes larger, and can pull out long filament.It is separately added into 1g sodium hydrogensulfites and 2g persulfuric acid
Ammonium, and transfer the material into the static polymerization 10 hours of 30 DEG C or so of template vessel insulation.Gel-like product is taken out, 70 after stripping and slicing
DEG C vacuum drying, siccative crush after after redrying up to product.Products therefrom is easy to dissolve, and molecular weight is converted through intrinsic viscosity
It is 3,200,000.
Comparative example 1
By the domestic MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides of 400g (being converted into 100%), 600g acrylamides, 0.8g
Disodium ethylene diamine tetraacetate is dissolved in 1kg deionized waters, starts stirring, is separately added into 1.5g sodium hydrogensulfites and 2g persulfuric acid
Ammonium, and the static polymerization 10 hours of 30 DEG C or so of template vessel insulation is transferred the material into, the micro- Huang of system, viscosity very little fails to gather
Synthetic product.
Comparative example 2
By the domestic MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides of 400g (being converted into 100%), 600g acrylamides, 0.8g
Disodium ethylene diamine tetraacetate is dissolved in 1kg deionized waters, starts stirring, is separately added into 3g sodium hydrogensulfites and 4g ammonium persulfates,
And the static polymerization 10 hours of 30 DEG C or so of template vessel insulation is transferred the material into, gel-like product is taken out, 70 DEG C after stripping and slicing
Vacuum drying, up to product after redrying after siccative crushes.Heat release is violent in the course of the polymerization process, and products therefrom is molten for material
Solve it is relatively difficult, through intrinsic viscosity conversion molecular weight be 6,400,000.
By above-described embodiment and comparative example application examples it is found that method therefor of the present invention is very enough to overcome impurity in system well
Influence to polymerization, enables polymerization to be smoothed out, and the molecular weight of product of acquisition is higher, and dissolubility is good.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (9)
1. a kind of preparation method of cationic polyacrylamide, which is characterized in that include the following steps：
(1) 5~60 parts by weight cationic monomers are dissolved in 30~80 parts by weight of deionized water；
(2) 0.0015~0.05 parts by wt EDTA-disodium is added, is fully dissolved；
(3) 0.001~0.6 parts by weight auxiliary agent and 10~65 parts by weight propylene amides, stirring and dissolving are added in, and opens cycle ice water
Or ice-water bath cooling, carry out low temperature prepolymerization；
(4) to the end of prepolymerization, 0.003~0.6 parts by weight initiator is added in, after stirring evenly, is transferred the material into container
Keep the temperature closed static polymerization；
(5) polymerizate stripping and slicing is dried, then crushed, and redrying, finally smashing into product powder；
The step (3) is：Addition 0.005-0.01 parts by weight auxiliary agent and 10~65 parts by weight propylene amides, stirring and dissolving, and
Cycle ice water or ice-water bath cooling are opened, carries out low temperature prepolymerization；
The auxiliary agent is sulphite or bisulfites.
2. the preparation method of cationic polyacrylamide according to claim 1, which is characterized in that the step (1) is：
5~60 parts by weight cationic monomers and 1~20 parts by weight of acrylic acid are dissolved in 30~80 parts by weight of deionized water, and use caustic soda
System pH is adjusted to neutrality by solution.
3. the preparation method of cationic polyacrylamide according to claim 1, which is characterized in that in the step (4)
The container be template container.
4. the preparation method of cationic polyacrylamide according to any one of claim 1-3, which is characterized in that described
Cationic monomer is selected from quaternary ammonium type or tertiary amine-type cationic monomer.
5. the preparation method of cationic polyacrylamide according to claim 4, which is characterized in that the cationic monomer
Selected from following any one or more combination：Acryloyloxyethyl trimethyl ammonium chloride, methylacryoyloxyethyl trimethyl
Ammonium chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, dimethyl diallyl ammonium chloride.
6. the preparation method of cationic polyacrylamide according to claim 5, which is characterized in that the cationic monomer
For acryloyloxyethyl trimethyl ammonium chloride.
7. the preparation method of cationic polyacrylamide according to claim 1, which is characterized in that the auxiliary agent is sulfurous
Sour hydrogen sodium.
8. the preparation method of cationic polyacrylamide according to any one of claim 1-3, which is characterized in that described
Initiator is water-soluble low temperature primosome series initiators.
9. the preparation method of cationic polyacrylamide according to claim 8, which is characterized in that the initiator is selected from
It is any below：Potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-mercaptan, ammonium persulfate-sodium bisulfite, tert-butyl hydroperoxide
Hydrogen-sodium pyrosulfite.
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