CN107151289B - A kind of method of light initiation system preparation cationic polyacrylamide - Google Patents
A kind of method of light initiation system preparation cationic polyacrylamide Download PDFInfo
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 43
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000000977 initiatory effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 94
- 239000000178 monomer Substances 0.000 claims abstract description 83
- 239000003999 initiator Substances 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 19
- 239000006184 cosolvent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 washing purification Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 10
- 230000007717 exclusion Effects 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical group [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 8
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 8
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 235000019394 potassium persulphate Nutrition 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 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 description 2
- 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 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- FGRJGEWVJCCOJJ-UHFFFAOYSA-N 2,2-dimethylaziridine Chemical compound CC1(C)CN1 FGRJGEWVJCCOJJ-UHFFFAOYSA-N 0.000 claims 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 235000019270 ammonium chloride Nutrition 0.000 claims 1
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 150000003254 radicals Chemical class 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000003311 flocculating effect Effects 0.000 abstract description 6
- 239000012966 redox initiator Substances 0.000 abstract description 3
- 239000000084 colloidal system Substances 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- 208000023445 Congenital pulmonary airway malformation Diseases 0.000 description 31
- 238000004090 dissolution Methods 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 9
- 239000002253 acid Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 238000006683 Mannich reaction Methods 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical group [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- STYCVEYASXULRN-UHFFFAOYSA-N butanimidamide;hydrochloride Chemical compound [Cl-].CCCC(N)=[NH2+] STYCVEYASXULRN-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000010356 wave oscillation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/04—Azo-compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
Abstract
The present invention relates to a kind of methods of light initiation system preparation cationic polyacrylamide, this method is by sequentially adding deionized water in quartz reaction device, acrylamide monomer, cationic monomer and cosolvent are to being completely dissolved, adjust solution ph, azo initiator and redox initiator are sequentially added when being filled with High Purity Nitrogen to reaction unit, reaction unit sealing is placed on ultrasonoscope shaken well, it is placed on the turntable of uniform rotation, it is reacted using the control method of first low light intensity high light intensity again, through curing after generation polyacrylamide colloid, washing purification, final product is obtained after drying and grinding.This method is able to maintain certain density free radical in reaction system, guarantee the uniform sequential progress of chain growth, the polyacrylamide dissolubility prepared is good, flocculating property is good, and ultraviolet light initiation method has many advantages, such as low production energy consumption, high production efficiency, easy to operate easily controllable, the present invention has good market application prospect.
Description
Technical field
The present invention relates to a kind of synthetic method of aqueous solution high molecular polymer, and in particular to a kind of novel light-initiated body
The method of system's preparation cationic polyacrylamide.
Background technique
Cationic polyacrylamide (English name cationic polyacrylamide, be abbreviated as CPAM) is to grind at present
One of study carefully with most widely used organic polymer coargulator, this is because on CPAM strand with positive charge active group and
For linear polymeric polymer, it can be made by the effects of electrical neutralization, adsorption bridging water-borne glue body particle and suspended matter it is de- it is steady,
Flocculation is to achieve the purpose that sludge dewatering and sewage treatment.Currently, the preparation method of CPAM includes two kinds: polyacrylamide
Cation-modified method and copolymerization process.The cation-modified method of polyacrylamide mainly passes through methylol reaction or mannich reaction
It realizes, the CPAM product of this method preparation haves the shortcomings that storage time is short, cationic degree is low and cationic degree is not easy to control.
Copolymerization process is that acrylamide monomer and cationic monomer are caused combined polymerization under certain condition to obtain CPAM, and copolymerization process exists
The shortcomings that cation-modified method can be overcome to a certain extent, therefore it is more extensive to study application.
Solubility property is the crucial ginseng of a urgent problem to be solved and CPAM properties of product in the research application of CPAM
Number.In general CPAM strand crosslinking compared with indissoluble solution or can not then dissolve, and be easier to if CPAM strand linear degree is good
Dissolution.The form of CPAM strand and polymerization process are closely related, if polymerization process free radical quantity excessively if
The probability for occurring being crosslinked will greatly increase, and the quantity of free radical depends mainly on the additive amount of initiator, general initiator addition
The more more then free radicals generation quantity of amount are more, on the contrary then fewer；Initiation method also will affect the quantity of free radical generation, be drawn with heat
For hair, if initiation temperature is excessively high or heat transfer unevenly local temperature occur excessively high, free radical generates quantity can abruptly increase
The phenomenon that being easy to appear strand crosslinking.Therefore, it is the dissolubility for improving CPAM, the additive amount of initiator should be reduced, answered simultaneously
Guarantee that the initiation energy of initiation method generation is small and energy transmission is uniform.In addition to this, flocculating property, energy consumption in production process, life
Produce the critical aspects that efficiency etc. is also CPAM production technology.Although in recent years country's CPAM production technology achieve it is considerable into
Step, above-mentioned various aspects can access certain solution, but be often difficult to make overall plans.
For example, the patent " a kind of preparation method of cationic polyacrylamide " such as publication number 102603970A is to describe
A method of by ultraviolet light-initiated preparation CPAM, although the CPAM prepared is with high purity, nontoxic, and the reaction time
It is short, energy consumption of reaction is low, but there is no optimize CPAM solubility property.For another example patent " the instant capacity sun of publication number 101921365B
The preparation method of cationic polyacrylamide " describes a kind of method for preparing CPAM by heat initiation, what this method was prepared
CPAM dissolubility is good, can be used as organic flocculant, paper strengthening agent, retention agent etc. applied at city life and industry sewage
Reason and the fields such as papermaking, but there is also additive types that more, heat causes that energy consumption is high, reaction time long (production efficiency for this method
It is low) the disadvantages of.Currently, CPAM production technology still needs to further be promoted and improved.
Summary of the invention
In view of the problems of the existing technology, the object of the present invention is to provide a kind of novel light initiation system preparation sun from
The method of sub- polyacrylamide, this method addition auxiliary agent type is few, dosage is low, and CPAM solubility property is good, flocculating property is good, production
Low energy consumption, high production efficiency, easy to operate easily controllable.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of method of light initiation system preparation cationic polyacrylamide, the specific steps of which are as follows:
The first step sequentially adds a certain amount of deionized water, acrylamide monomer, cationic monomer and is helped in reaction unit
Solvent urea, it is agitated be uniformly dissolved after adjust solution ph to 3-9；It counts cationic monomer and acrylamide monomer is total single
Body, reaction system total monomer quality score are 15%-50%, and acrylamide monomer accounts for total monomer quality 20%-90%, cationic monomer
Account for total monomer quality 10%-80%；Cosolvent urea accounts for total monomer quality 0.4 ‰ -3.60 ‰.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
Addition accounts for the azo initiator of total monomer quality 0.06 ‰ -0.60 ‰, accounts for the oxygen of total monomer quality 0.03 ‰ -0.50 ‰ in solution
Change type initiator, the reduced form initiator for accounting for total monomer quality 0.06 ‰ -1.00 ‰, all initiators are to be configured to solution
After be added in reaction unit, after the air in reaction unit is excluded completely, reaction unit is sealed.Reaction is filled after sealing
Placement location vibrates 3-5min in ultrasonoscope.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, first
10min-60min is irradiated under low ultraviolet intensity, then improves light intensity and takes out after irradiating 10min ~ 60min, and it is small to stand curing 2
When, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.
Further, the material of the reaction unit is quartz, and quartzy light transmittance is high, improves making for ultraviolet light and initiator
With rate, therefore the additive amount of initiator can be reduced, reduce the crosslinking of strand in polymerization process, improve the dissolubility of CPAM,
The flocculating property that CPAM molecular weight can also be improved simultaneously, improve product.
Further, the cationic monomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride DMC, acrylyl oxy-ethyl
One of trimethyl ammonium chloride DAC or dimethyl diallyl ammonium chloride DMDAAC.
Further, the cosolvent urea adds in the form of a solution, and concentration range is 2.0 × 10-3 ~3.6×10-2g/
ml。
Further, the power of the ultrasonoscope is 480W, the frequency of generation ultrasound is 40kHz, passes through ultrasonic wave
Oscillation is so that each substance of reaction system, which is sufficiently mixed, uniformly avoids the occurrence of the excessively high phenomenon of partial region initiator concentration.
Third step be by sealing after reaction unit be placed on the turntable of uniform rotation, make the various pieces of reaction unit by
Light levels are consistent.The velocity of rotation of the turntable is 20-60s/r, makes various pieces light in reaction unit by turntable
It is consistent according to degree, reaction can even carry out, obtain the excellent CPAM of properties of product.
Further, second step and third step is compound using redox initiator-azo initiator, first low light
This novel light initiation system of the control method of Qiang Zaigao light intensity.The novel light initiation system mainly utilizes activation energy lower
Redox initiator is combined with the higher azo initiator of activation energy, and redox initiator generates freely under low light intensities
Base after the reaction the phase, can make azo initiator decomposition continue to generate free radicals, make free radical in reaction system by improving light intensity
A certain concentration is kept, carries out reaction more gentle, chain growth uniform sequential can carry out, and be less prone to strand crosslinking
Situation is easy to get the product that dissolubility is good, molecular weight is high.Wherein, azo initiator added by second step is that azo two is different
One of Butanimidamide, monohydrochloride V50 or azo dicyclohexyl formonitrile HCN hydrochloride VA-044, solution concentration range 9.6 × 10-4g/
ml-6.0×10-3g/ml.Oxidized form initiator includes one of potassium peroxydisulfate, ammonium persulfate, and solution concentration range 2.4 ×
10-4g/ml-2.8×10-3g/ml.Reduced form initiator includes one of sodium hydrogensulfite, sodium sulfite, solution concentration model
Enclose 7.2 × 10-4g/ml-5.6×10-3g/ml.Third step is using first low ultraviolet according to the controlling party of intensity highlight strength again
Method, wherein low ultraviolet intensity is 4-10mW/cm2, high ultraviolet light intensity is 12-18mW/cm2, ultraviolet light is adjustable by 1000W
The device for saving luminous intensity generates, and the ultraviolet light dominant wavelength of generation is 365nm.
Compared with prior art, the invention has the following beneficial effects:
1. novel light initiation system provided by the invention can control reaction process, make to keep a certain concentration in reaction system
Free radical can not only guarantee the uniform sequential progress of chain growth, make the good linearity, easy to dissolve of product, and enable to AM
Monomer and cationic monomer sufficiently participate in polymerization reaction, under the premise of guaranteeing monomer conversion improve product cationic degree and
Molecular weight improves product charge neutrality effect and adsorption bridging effect, achievees the purpose that the flocculating property for improving product.
2. the present invention controls polymerization process by the adjusting of ultraviolet light light intensity, excellent with ultraviolet light initiation method
Point, i.e., light-initiated specific heat initiation are more easily controlled, and the adjusting specific heat initiation of light intensity is more easily implemented and energy transmission speed is fast
And propagate uniformly, it is more advantageous to the progress of polymerization reaction, not only simple energy conservation, and preparation process is easy to control.Meanwhile also having
Have the advantages that reaction speed is fast, energy consumption of reaction is low.
3. novel light initiation system provided by the invention, quartz reaction device, supersonic oscillations and at the uniform velocity the methods of turntable,
Make each analog assistant (especially initiator) that can be fully utilized, therefore additive amount is extremely low, while saving production material
The generation of side reaction can effectively be avoided；And polymerization reaction is made to carry out uniformly, thoroughly, it can not only guarantee the molten of product
Performance is solved, and the flocculating property of product can be promoted.
4. raw material selected by the present invention are commercially available material, cheap, it is convenient to choose, and can directly buy, therefore,
Synthetic method production cost provided by the invention is low, is easily achieved the marketization.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
Inorganic acid is used as using HCl in following embodiment, NaOH can also be adopted as inorganic base adjusting pH value, when specific implementation
With other do not influence the inorganic acid of polymerization reaction in the prior art and inorganic base adjusts pH value.Prepare CPAM limiting viscosity and
Dissolution time refers to " technical conditions and test method of GB/T 31246-2014 water treatment agent cationic-type polyacrylamide "
It measures.
Embodiment 1:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 25.5ml, 7.2g acrylamide monomer (Zhan Zongdan in quartz reaction device
Weight 90%, total monomer account for reaction system gross mass 20%), DMC monomer 0.8g(account for total monomer quality 10%), cosolvent urea
2.0ml(solution concentration 8.0 × 10-3‰) g/ml accounts for total monomer quality 2.0, after being completely dissolved, adjusted with weak acid or weak base above-mentioned
Solution ph is to 3.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V-044(solution concentration 9.6 × 10 of 0.5ml is added in solution-4G/ml, account for total monomer quality 0.06 ‰), the persulfuric acid of 2.0ml
Potassium (solution concentration 2.0 × 10-3G/ml, account for total monomer quality 0.5 ‰), the sodium hydrogensulfite of 2.0ml (solution concentration 4.0 × 10-3‰) g/ml accounts for total monomer quality 1.0, after the air in reaction unit is excluded completely, reaction unit is sealed.It will after sealing
Reaction unit, which is placed in ultrasonoscope, vibrates 3min, power 480W, and the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 20s/r, is first 4.0mW/cm in ultraviolet ray intensity2Lower irradiation 10min, then ultraviolet ray intensity be 12mW/cm2According to
It is taken out after penetrating 60min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 10.8dL/g, dissolution time 118min.
Embodiment 2:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 15.0ml, 4.0g acrylamide monomer in reaction unit and (accounts for total monomer matter
Amount 20%, total monomer accounts for reaction system gross mass 50%), DMC monomer 16.0g(account for total monomer quality 80%), cosolvent urea
1.0ml(solution concentration 1.0 × 10-2‰) g/ml accounts for total monomer quality 0.5, after being completely dissolved, adjusted with weak acid or weak base above-mentioned
Solution ph is to 9.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V50(solution concentration 6.0 × 10 of 2.0ml is added in solution-3G/ml, account for total monomer quality 0.6 ‰), the Ammonium Persulfate 98.5 of 1.0ml
(solution concentration 6.0 × 10-4G/ml, account for total monomer quality 0.03 ‰), the sodium sulfite of 1.0ml (solution concentration 1.2 × 10-3g/
‰) ml accounts for total monomer quality 0.06, after the air in reaction unit is excluded completely, reaction unit is sealed.It will be anti-after sealing
It answers device to be placed in ultrasonoscope and vibrates 5min, power 480W, the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 40s/r, is first 10mW/cm in ultraviolet ray intensity2Lower irradiation 60min, then ultraviolet ray intensity be 18mW/cm2Irradiation
It is taken out after 10min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 6.3dL/g, dissolution time 58min.
Embodiment 3:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 30.0ml, 4.2g acrylamide monomer in reaction unit and (accounts for total monomer matter
Amount 70%, total monomer accounts for reaction system gross mass 15%), DMDAAC monomer 1.8g(account for total monomer quality 30%), cosolvent urea
1.0ml(solution concentration 2.4 × 10-3‰) g/ml accounts for total monomer quality 0.4, after being completely dissolved, adjusted with weak acid or weak base above-mentioned
Solution ph is to 6.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V50(solution concentration 1.2 × 10 of 1.0ml is added in solution-3G/ml, account for total monomer quality 0.2 ‰), the potassium peroxydisulfate of 1.0ml
(solution concentration 2.4 × 10-4G/ml, account for total monomer quality 0.04 ‰), the sodium hydrogensulfite of 1.0ml (solution concentration 7.2 × 10- 4‰) g/ml accounts for total monomer quality 0.12, after the air in reaction unit is excluded completely, reaction unit is sealed.After sealing
Reaction unit is placed in ultrasonoscope and vibrates 5min, power 480W, the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 60s/r, is first 8mW/cm in ultraviolet ray intensity2Lower irradiation 30min, then ultraviolet ray intensity be 12.5mW/cm2According to
It is taken out after penetrating 30min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 9.6dL/g, dissolution time 54min.
Embodiment 4:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 24.0ml, 7.2g acrylamide monomer in reaction unit and (accounts for total monomer matter
Amount 60%, total monomer accounts for reaction system gross mass 30%), DAC monomer 4.8g(account for total monomer quality 40%), cosolvent urea 1.0ml
(solution concentration 3.6 × 10-2‰) g/ml accounts for total monomer quality 3.0, after being completely dissolved, adjust above-mentioned solution with weak acid or weak base
PH value is to 5.0.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V50(solution concentration 2.4 × 10 of 1.0ml is added in solution-3G/ml, account for total monomer quality 0.2 ‰), the potassium peroxydisulfate of 1.0ml
(solution concentration 1.8 × 10-3G/ml, account for total monomer quality 0.15 ‰), the sodium hydrogensulfite of 1.0ml (solution concentration 3.6 × 10- 3‰) g/ml accounts for total monomer quality 0.30, after the air in reaction unit is excluded completely, reaction unit is sealed.After sealing
Reaction unit is placed in ultrasonoscope and vibrates 5min, power 480W, the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 30s/r, is first 8.5mW/cm in ultraviolet ray intensity2Lower irradiation 40min, then ultraviolet ray intensity be 13mW/cm2According to
It is taken out after penetrating 40min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 20.9dL/g, dissolution time 68min.
Embodiment 5:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 28ml, 6.4g acrylamide monomer in reaction unit and (accounts for total monomer quality
80%, total monomer accounts for reaction system gross mass 20%), DMDAAC monomer 1.6g(account for total monomer quality 20%), cosolvent urea
1.0ml(solution concentration 2.9 × 10-2‰) g/ml accounts for total monomer quality 3.6, after being completely dissolved, adjusted with weak acid or weak base above-mentioned
Solution ph is to 5.5.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V50(solution concentration 2.4 × 10 of 1.0ml is added in solution-3G/ml, account for total monomer quality 0.3 ‰), the potassium peroxydisulfate of 1.0ml
(solution concentration 4.8 × 10-4G/ml, account for total monomer quality 0.06 ‰), the sodium hydrogensulfite of 1.0ml (solution concentration 1.4 × 10- 3‰) g/ml accounts for total monomer quality 0.18, after the air in reaction unit is excluded completely, reaction unit is sealed.After sealing
Reaction unit is placed in ultrasonoscope and vibrates 5min, power 480W, the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 50s/r, is first 7.5mW/cm in ultraviolet ray intensity2Lower irradiation 40min, then ultraviolet ray intensity be 13mW/cm2According to
It is taken out after penetrating 50min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 19.6dL/g, dissolution time 61min.
Embodiment 6:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step sequentially adds deionized water 22ml, 10.5g acrylamide monomer in reaction unit and (accounts for total monomer matter
Amount 75%, total monomer accounts for reaction system gross mass 35%), DMC monomer 3.5g(account for total monomer quality 25%), cosolvent urea 1.0ml
(solution concentration 2.5 × 10-2‰) g/ml accounts for total monomer quality 1.8, after being completely dissolved, adjust above-mentioned solution with weak acid or weak base
PH value is to 6.
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V-044(solution concentration 5.6 × 10 of 1.0ml is added in solution-3G/ml, account for total monomer quality 0.4 ‰), the persulfuric acid of 1.0ml
Potassium (solution concentration 2.8 × 10-3G/ml, account for total monomer quality 0.2 ‰), the sodium hydrogensulfite of 1.0ml (solution concentration 5.6 × 10-3‰) g/ml accounts for total monomer quality 0.4, after the air in reaction unit is excluded completely, reaction unit is sealed.It will after sealing
Reaction unit, which is placed in ultrasonoscope, vibrates 5min, power 480W, and the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 20s/r, is first 9.0mW/cm in ultraviolet ray intensity2Lower irradiation 20min, then ultraviolet ray intensity be 14.0mW/cm2
It is taken out after irradiation 15min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 17.6dL/g, dissolution time 71min.
Embodiment 7:
A kind of method that light initiation system prepares CPAM flocculant, the specific steps are as follows:
The first step, in reaction unit successively deionized water 21ml, 6.0g acrylamide monomer (account for total monomer quality 50%,
Total monomer accounts for reaction system gross mass 30%), DAC monomer 6.0g(account for total monomer quality 50%), cosolvent urea 1.0ml(solution
Concentration 3.6 × 10-2‰) g/ml accounts for total monomer quality 3.0, after being completely dissolved, with weak acid or weak base adjust above-mentioned solution ph to
5.5。
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, is stated upwards in turn on one side
The V50(solution concentration 2.4 × 10 of 2.0ml is added in solution-3G/ml, account for total monomer quality 0.4 ‰), the potassium peroxydisulfate of 2.0ml
(solution concentration 1.8 × 10-3G/ml, account for total monomer quality 0.30 ‰), the sodium hydrogensulfite of 2.0ml (solution concentration 3.6 × 10- 3‰) g/ml accounts for total monomer quality 0.60, after the air in reaction unit is excluded completely, reaction unit is sealed.After sealing
Reaction unit is placed in ultrasonoscope and vibrates 5min, power 480W, the frequency of ultrasonic wave is 40kHz.
Reaction unit after sealing in second step is placed on the turntable of uniform rotation by third step under room temperature environment, is turned
Disk rotating speed is 60s/r, is first 10mW/cm in ultraviolet ray intensity2Lower irradiation 30min, then ultraviolet ray intensity be 16mW/cm2Irradiation
It is taken out after 30min, stands curing 2 hours, glue cationic polyacrylamide is made；
Gluey polyacrylamide obtained is refined by acetone and ethanol wash, is dried in a vacuum drying oven by the 4th step
Grinding is after dry to get cationic polyacrylamide powder.Measuring its limiting viscosity is 8.2dL/g, dissolution time 42min.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (8)
1. a kind of method of light initiation system preparation cationic polyacrylamide, which is characterized in that specific step is as follows:
The first step sequentially adds deionized water, acrylamide monomer, cationic monomer and cosolvent urea in reaction unit,
It is agitated be uniformly dissolved after adjust solution ph to 3-9；It counts cationic monomer and acrylamide monomer is total monomer, reaction system
Middle total monomer quality score is 15%-50%, and acrylamide monomer accounts for total monomer quality 20%-90%, and cationic monomer accounts for total monomer
Quality 10%-80%；Cosolvent urea accounts for total monomer quality 0.4 ‰ -3.60 ‰；The cosolvent urea adds in the form of a solution,
Concentration range is 2.0 × 10-3 g/ml-3.6×10-2g/ml；
Second step, the air being filled on one side in high pure nitrogen exclusion reaction unit to reaction unit, states solution upwards in turn on one side
Middle addition accounts for the azo initiator of total monomer quality 0.06 ‰ -0.60 ‰, accounts for the oxidized form of total monomer quality 0.03 ‰ -0.50 ‰
Initiator, the reduced form initiator for accounting for total monomer quality 0.06 ‰ -1.00 ‰, all initiators are added after being configured to solution
It is added in reaction unit, after the air in reaction unit is excluded completely, reaction unit is sealed, puts reaction unit after sealing
It sets and vibrates 3-5min in ultrasonoscope；
Third step, under room temperature environment, the reaction unit after second step is vibrated is placed on the turntable of uniform rotation, using main wave
The ultraviolet light of a length of 365nm, first in 4-10mW/cm210min-60min is irradiated under ultraviolet ray intensity, then improves light intensity to 12-
18mW/cm2It is taken out after irradiation 10min ~ 60min, stands curing 2 hours, glue cationic polyacrylamide is made；
4th step is refined gluey polyacrylamide obtained by acetone and ethanol wash, after drying in a vacuum drying oven
Grinding is to get cationic polyacrylamide powder.
2. preparation method according to claim 1, it is characterised in that: the reaction unit is quartz material.
3. preparation method according to claim 1, it is characterised in that: the cationic monomer is methylacryoyloxyethyl
One in trimethyl ammonium chloride DMC, acrylyl oxy-ethyl-trimethyl salmiac DAC or dimethyl diallyl ammonium chloride DMDAAC
Kind.
4. preparation method according to claim 1, it is characterised in that: in the second step, the power of ultrasonoscope is
480W, the frequency for generating ultrasound are 40kHz.
5. preparation method according to claim 1, it is characterised in that: the velocity of rotation of the turntable is 20-60s/r.
6. preparation method according to claim 1, it is characterised in that: the azo initiator is two NSC 18620 hydrochloric acid of azo
Salt or azo dicyclohexyl formonitrile HCN hydrochloride, the concentration range for the solution that the azo initiator is prepared are 9.6 × 10-4g/
ml-6.0×10-3g/ml。
7. preparation method according to claim 1, it is characterised in that: the oxidized form initiator is potassium peroxydisulfate, over cure
Sour ammonium, the concentration range for the solution that the oxidized form initiator is prepared are 2.4 × 10-4g/ml-2.8×10-3g/ml。
8. preparation method according to claim 1, it is characterised in that: the reduced form initiator is sodium hydrogensulfite, Asia
Sodium sulphate, the concentration range for the solution that the reduced form initiator is prepared are 7.2 × 10-4g/ml-5.6×10-3g/ml。
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