CN101735386A - Method for preparing cationic polyacrylamide emulsion - Google Patents
Method for preparing cationic polyacrylamide emulsion Download PDFInfo
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- CN101735386A CN101735386A CN200910185927A CN200910185927A CN101735386A CN 101735386 A CN101735386 A CN 101735386A CN 200910185927 A CN200910185927 A CN 200910185927A CN 200910185927 A CN200910185927 A CN 200910185927A CN 101735386 A CN101735386 A CN 101735386A
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Abstract
The invention provides a method for preparing cationic polyacrylamide emulsion, comprising the following steps: taking the following components by weight percent: 20-60% of acrylamide, 20-40% of cationic monomer, 4-8% of organic acid, 1-2% of sodium chloride and 15-30% of desalted water, and evenly mixing to obtain aqueous phase; taking the following components by weight percent: 92-97% of solvent oil, 2.5-5% of Span80 and 0.5-3% of Tween61, and evenly mixing to obtain oil phase; mixing the aqueous phase and the oil phase according to the weight ratio of 0.8:1-1.5:1, fully emulsifying, and regulating the pH value to 4-6 to obtain dosing; and transferring the dosing to a reactor, adding chelant, chain transfer agent and initiator, introducing nitrogen and stirring for 10-30min, stopping introducing the nitrogen and sealing, performing polymerization for 4-8h in a segment temperature control manner, placing for 0.5-2h, discharging and sieving to obtain a stable emulsion product after temperature reduction. The method provided by the invention has stable and safe reaction, high conversion rate, low residual monomer content and simple process, and the obtained product has moderate and adjustable viscosity, good product dispersibility and rapid dissolving speed.
Description
Technical field
The present invention relates to a kind of preparation method of cationic polyacrylamide emulsion, belong to the synthetic field of water-soluble polymer.
Background technology
Along with the development of current industrial, the water-soluble polymers series product of active demand high solids content, high relative molecular weight, good stability, particularly the polyacrylamide compounds is still important research direction.The complex manufacturing of traditional poly-propionic acid amide power-product is tediously long, generally comprises unit operations such as polymerization, granulation, drying, pulverizing, the production cost height, and facility investment is big.Cationic polyacrylamide emulsion is because " breakdown of emulsion " phenomenon, its emulsifying technology complexity originally as positive polarity, take place so be subject to the influence of electron rich chain in radical polymerization process in function ingredients.Present many cationic polyacrylamide emulsions adopt organic solvents such as benzene, toluene as solvent oil, and bigger to the pollution of environment, security is low; And composite initiation system (redox+azo-initiator) initiated polymerization is adopted in the preparation of cationic polyacrylamide emulsion more at present.Its shortcoming is: long reaction time (normal about 18 hours), and the linking difficulty between the initiator is difficult to control reaction process; Oil phase and water collocation are unreasonable, and product stability is poor, easily layering and generation precipitation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cationic polyacrylamide emulsion, the initiator system of this method is simple, and the reaction times is short, and is easy and simple to handle.Product relative molecular weight height, cationic charge density by the preparation of this method is moderate, good stability, solid content height, and dissolution rate is fast.
The technical scheme that realizes the object of the invention is as follows:
A kind of preparation method of cationic polyacrylamide emulsion may further comprise the steps:
A, get acrylamide 20～60%, cationic monomer 20～40%, organic acid 4～8%, sodium-chlor 1～2%, de-salted water 15～30% uniform mixing by weight percentage, obtain water;
B, get solvent oil 92～97%, Span80 2.5～5%, Tween61 0.5～3% by weight percentage, mix, obtain oil phase;
C, oil phase and water were mixed by weight 0.8: 1～1.5: 1, make mixed water and oil phase fully emulsified, transfer pH value to 4～6, obtain to prepare burden with highly basic;
D, batching is transferred in the reactor, with a flat iron plate for making cakes mixture, chain-transfer agent, initiator join respectively in the reactor, and logical nitrogen stirs and stops nitrogen after 10～30 minutes and seal sectional temperature-controlled polyreaction 4～8 hours;
E, placement 0.5～2 hour are reduced to temperature below 50 ℃, and blowing sieves and obtains stable product emulsion.
Cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac (DAC) or methylacryoyloxyethyl trimethyl ammonium chloride (DMC); Organic acid is oxalic acid or methylene-succinic acid; Solvent oil is paraffin oil or low aromatic hydrocarbon oil.
Transferring the highly basic of pH value is sodium hydroxide or potassium hydroxide, and the preferred values of pH value is 5～6.
The a flat iron plate for making cakes mixture is a disodium ethylene diamine tetraacetate, chain-transfer agent is a sodium formiate, initiator is a Diisopropyl azodicarboxylate, and they are respectively with the mass ratio of total dosage in reactor: disodium ethylene diamine tetraacetate 10～100ppm, sodium formiate 20～200ppm, Diisopropyl azodicarboxylate 100～500ppm.
The temperature and time of each of sectional temperature-controlled polyreaction section is: 45～50 ℃ of first sections, temperature, 150～240 minutes time; 52～56 ℃ of second sections, temperature, 30～60 minutes time; 75～80 ℃ of the 3rd sections, temperature, 60～120 minutes time.
Low aromatic hydrocarbon oil is Exxsol D80 or Exxsol D110 or Exxsol D130 or Isoper M or HydrosealG232 or HydrosealG250 or HydrosealG400.
The present invention adopts the inverse emulsion polymerization technology, only needs a kind of initiator, one-step synthesis reaction can obtain final product, has simplified production technique greatly, has reduced investment and production cost.In addition, inverse emulsion polymerization can be produced the high molecular weight water-soluble product under high conversion and high rate of polymerization, the finished product are the product emulsion of good fluidity, have that apparent viscosity is low, good fluidity, characteristics such as instant, adapt to efficient need of industrial production.Product can be widely used in fields such as sewage disposal, papermaking, ore dressing.
Method reacting balance provided by the invention, safety, transformation efficiency height, residual monomer content is low, and production technique is simple, the low and three-waste free pollution problem of energy consumption; Products molecule structure by the present invention preparation is formed rationally, modest viscosity is adjustable, good product dispersibility, dissolution rate are fast, easy to use, and it is long to stablize the time of depositing.
Embodiment
Further specify the present invention below in conjunction with several embodiment.
Embodiment 1:
The preparation of a, water: in the beaker of 250ml, add acrylamide 63g, acrylyl oxy-ethyl-trimethyl salmiac (DAC) 50g, oxalic acid 9.5g, sodium-chlor 2.5g, de-salted water 50g uniform mixing;
B, oil phase preparation: in the beaker of 500ml, add the paraffin oil of 228g, the Span80 of 10.5g, the Tween61 of 1.75g mixes;
C, the water for preparing and oil phase added in 750 milliliters the emulsification still, the mixing speed of emulsification still is set at 10000rpm, and fully emulsified 30 minutes, and to regulate pH value with sodium hydroxide be 5.4-5.7, obtains batching;
D, the batching that makes is transferred in 750 milliliters of reactors that agitator, thermometer are housed, 20～30 ℃ of controlled temperature, mixing speed 200～300rpm, add disodium ethylene diamine tetraacetate 0.02g, sodium formiate 0.025g, Diisopropyl azodicarboxylate 0.08g respectively, logical nitrogen stirs and stops nitrogen after the deoxygenation in 30 minutes and seal and continue and stir, sectional temperature-controlled polyreaction: first section, be warmed up to 45 ℃ with water-bath, be incubated 180 minutes, second section, warming-in-water to 54 ℃, be incubated 40 minutes, the 3rd section, warming-in-water to 78 ℃ is incubated 120 minutes;
E, cool to blowing below 50 ℃, through obtaining product behind 20 mesh sieves.
The solid content that records product is 30%, and cationic ion degree is 35%, and viscosity is 3.6cps (test condition is a NDJ-1 type rotational viscosimeter, and 25 ℃ of temperature, UL rotor speed are 60rpm, under 1mol/L sodium chloride aqueous solution condition), and dissolution time is less than 2min.
Embodiment 2:
A, water preparation: add acrylamide 80g in the beaker of 500ml, methylacryoyloxyethyl trimethyl ammonium chloride (DMC) 80g, methylene-succinic acid 8.5g, sodium-chlor 2.1g, de-salted water 35g mix;
B, oil phase preparation: in the beaker of 500ml, add Span80, the Tween61 of 1.32g of Exxsol D110, the 8.75g of 210g, mix;
C, the water for preparing and oil phase added in 1000 milliliters the emulsification still, the mixing speed of emulsification still is 10000rpm, fully emulsified 30 minutes, and to regulate pH value with potassium hydroxide be 5.8-6, obtains batching;
D, the batching that makes is transferred in the reactor that agitator, thermometer are housed, 20～30 ℃ of controlled temperature, mixing speed 200-300rpm, add disodium ethylene diamine tetraacetate 0.025g respectively, sodium formiate 0.028g, Diisopropyl azodicarboxylate 0.15g, logical nitrogen stirs and stops nitrogen after the deoxygenation in 30 minutes and seal and continue and stir, sectional temperature-controlled polyreaction: first section, be warmed up to 47 ℃ with water-bath, be incubated 220 minutes, second section, warming-in-water to 56 ℃ is incubated 60 minutes, the 3rd section, warming-in-water to 80 ℃ is incubated 60 minutes;
E, cool to blowing below 50 ℃, through obtaining product behind 20 mesh sieves.
The solid content that records product is 40%, and ion degree is 41%, and viscosity is 3.9cps (test condition is a NDJ-1 type rotational viscosimeter, and 25 ℃ of temperature, UL rotor speed are 60rpm, under 1mol/L sodium chloride aqueous solution condition), and dissolution time is less than 5min.
Embodiment 3:
The preparation of a, water: in the beaker of 500ml, add acrylamide 84g, acrylyl oxy-ethyl-trimethyl salmiac (DAC) 56g, oxalic acid 9g, sodium-chlor 2g, de-salted water 30g mixes;
B, oil phase preparation: in the beaker of 500ml, add Span80, the Tween61 of 1.5g of HydrosealG250, the 7.875g of 192.5g, mix;
C, the water for preparing and oil phase added in 1000 milliliters the emulsification still, the mixing speed of emulsification still is 10000rpm, fully emulsified 30 minutes, and to regulate pH value with sodium hydroxide be 6, obtains batching;
D, the batching that makes is transferred in the reactor that agitator, thermometer are housed, 20～30 ℃ of controlled temperature, mixing speed 200-300rpm, add disodium ethylene diamine tetraacetate 0.022g respectively, sodium formiate 0.03g, Diisopropyl azodicarboxylate 0.1g, logical nitrogen stirs and stops nitrogen after the deoxygenation in 30 minutes and seal and continue and stir, and is warmed up to 45 ℃ with water-bath, keeps 150 minutes; Warming-in-water to 54 ℃ is incubated 50 minutes, and warming-in-water to 75 ℃ is incubated 120 minutes;
E, cool to blowing below 50 ℃, through obtaining product behind 20 mesh sieves.
The solid content that records product is 39%, and ion degree is 31.5%, and viscosity is 2.99cps (test condition is a NDJ-1 type rotational viscosimeter, and 25 ℃ of temperature, UL rotor speed are 60rpm, under 1mol/L sodium chloride aqueous solution condition), and dissolution time is less than 5min.
Claims (6)
1. the preparation method of a cationic polyacrylamide emulsion is characterized in that may further comprise the steps:
A, get acrylamide 20～60%, cationic monomer 20～40%, organic acid 4～8%, sodium-chlor 1～2%, de-salted water 15～30% uniform mixing by weight percentage, obtain water;
B, get solvent oil 92～97%, Span80 2.5～5%, Tween61 0.5～3% by weight percentage, mix, obtain oil phase;
C, oil phase and water were mixed by weight 0.8: 1～1.5: 1, make mixed water and oil phase fully emulsified, transfer pH value to 4～6, obtain to prepare burden with highly basic;
D, batching is transferred in the reactor, with a flat iron plate for making cakes mixture, chain-transfer agent, initiator join respectively in the reactor, and logical nitrogen stirs and stops nitrogen after 10～30 minutes and seal sectional temperature-controlled polyreaction 4～8 hours;
E, placement 0.5～2 hour are reduced to temperature below 50 ℃, and blowing sieves and obtains stable product emulsion.
2. the preparation method of cationic polyacrylamide emulsion according to claim 1, it is characterized in that: cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac (DAC) or methylacryoyloxyethyl trimethyl ammonium chloride (DMC); Organic acid is oxalic acid or methylene-succinic acid; Solvent oil is paraffin oil or low aromatic hydrocarbon oil.
3. the preparation method of cationic polyacrylamide emulsion according to claim 1 is characterized in that: transferring the highly basic of pH value is sodium hydroxide or potassium hydroxide, and the preferred values of pH value is 5～6.
4. the preparation method of cationic polyacrylamide emulsion according to claim 1, it is characterized in that: a flat iron plate for making cakes mixture is a disodium ethylene diamine tetraacetate, chain-transfer agent is a sodium formiate, initiator is a Diisopropyl azodicarboxylate, and they are respectively with the mass ratio of total dosage in reactor: disodium ethylene diamine tetraacetate 10～100ppm, sodium formiate 20～200ppm, Diisopropyl azodicarboxylate 100～500ppm.
5. the preparation method of cationic polyacrylamide emulsion according to claim 1 is characterized in that, the temperature and time of each of sectional temperature-controlled polyreaction section is: 45～50 ℃ of first sections, temperature, 150～240 minutes time; 52～56 ℃ of second sections, temperature, 30～60 minutes time; 75～80 ℃ of the 3rd sections, temperature, 60～120 minutes time.
6. the preparation method of cationic polyacrylamide emulsion according to claim 2, it is characterized in that: low aromatic hydrocarbon oil is Exxsol D80 or Exxsol D110 or Exxsol D130 or Isoper M or HydrosealG232 or HydrosealG250 or HydrosealG400.
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| CN200910185927A CN101735386A (en) | 2009-12-13 | 2009-12-13 | Method for preparing cationic polyacrylamide emulsion |
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| CN200910185927A CN101735386A (en) | 2009-12-13 | 2009-12-13 | Method for preparing cationic polyacrylamide emulsion |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242480A (en) * | 2013-04-15 | 2013-08-14 | 北京恒聚化工集团有限责任公司 | Preparation method of cationic polyacrylamide emulsion and emulsion prepared by same |
| CN108034021A (en) * | 2018-01-15 | 2018-05-15 | 安徽龙谷商贸有限公司 | A kind of method that inverse emulsion polymerization prepares cationic polyacrylamide microgranule |
| CN108350346A (en) * | 2015-08-26 | 2018-07-31 | 索尔维美国有限公司 | Diluted cationic friction reducers |
| CN114478905A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for improving conversion rate of cationic monomer and preparation method of polymer microsphere emulsion |
-
2009
- 2009-12-13 CN CN200910185927A patent/CN101735386A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242480A (en) * | 2013-04-15 | 2013-08-14 | 北京恒聚化工集团有限责任公司 | Preparation method of cationic polyacrylamide emulsion and emulsion prepared by same |
| CN103242480B (en) * | 2013-04-15 | 2015-06-24 | 北京恒聚化工集团有限责任公司 | Preparation method of cationic polyacrylamide emulsion and emulsion prepared by same |
| CN108350346A (en) * | 2015-08-26 | 2018-07-31 | 索尔维美国有限公司 | Diluted cationic friction reducers |
| CN108034021A (en) * | 2018-01-15 | 2018-05-15 | 安徽龙谷商贸有限公司 | A kind of method that inverse emulsion polymerization prepares cationic polyacrylamide microgranule |
| CN114478905A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for improving conversion rate of cationic monomer and preparation method of polymer microsphere emulsion |
| CN114478905B (en) * | 2020-10-23 | 2023-10-31 | 中国石油化工股份有限公司 | Method for improving conversion rate of cationic monomer and preparation method of polymer microsphere emulsion |
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Open date: 20100616 |