CN105273131A - Preparation method of cationic polyacrylamide emulsion - Google Patents
Preparation method of cationic polyacrylamide emulsion Download PDFInfo
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- CN105273131A CN105273131A CN201510777962.2A CN201510777962A CN105273131A CN 105273131 A CN105273131 A CN 105273131A CN 201510777962 A CN201510777962 A CN 201510777962A CN 105273131 A CN105273131 A CN 105273131A
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Abstract
The invention relates to a preparation method of cationic polyacrylamide emulsion. The preparation method includes the following steps that polyethylene glycol, acrylamide, cationic monomer acrylamide (2-hydroxyl) propyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride and auxiliaries including beta-dimethylaminopropionitrile and urea are added to deionized water, stirred and dissolved, and evenly mixed; high-purity nitrogen is introduced for oxygen removal, initiator including ammonium persulfate, formaldehyde sodium sulfite and V-50 is added, and the polymer emulsion product is obtained after a stirring reaction. The preparation method has the advantages that novel cationic monomers are adopted, an aqueous two-phase dispersion copolymerization method is adopted, and the cationic polyacrylamide emulsion product which is low in production cost, low in viscosity, uniform in particle size distribution and high in stability is prepared.
Description
Technical field
The present invention relates to a kind of preparation method of cation polyacrylamide emulsion.
Background technology
Cationic polyacrylamide is the multipolymer be made up of a kind of positively charged ion unit and acrylamide non ionic unit, with the positive charge group that can ionize on its molecular chain, polycation and little negatively charged ion can be ionized in water, can adsorb with the suspended particles be scattered in solution and build bridge, have extremely strong throwing out.Cationic polyacrylamide is widely used in the field such as water treatment and metallurgy, papermaking, oil, chemical industry, weaving, ore dressing, as thickening material, flocculation agent, flow improver, has the effects such as gel, sedimentation, reinforcement.Cationic polyacrylamide is specially adapted to the processed of municipal effluent, municipal sludge, paper mill sludge and other industrial sludge.
With regard to current technology, still solid positively charged ion polyacrylamide product is produced in more employing homogeneous phase aqueous solution polymerization, but the superiority that double water-phase dispersion copolymerization method prepares cation polyacrylamide emulsion starts to obtain the attention of businessman, occurs the method synthetic emulsion product successively.Double water-phase dispersion copolymerization method, current product cut size distribution cannot control well, and the problems such as the stability of dispersion liquid is low, viscosity is high also do not solve well.Meanwhile, comonomer many employings MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or acrylyl oxy-ethyl-trimethyl salmiac, because purity Coriolis mass requires high, many dependence on import, price comparison is expensive, and during a large amount of production, cost is difficult to lower.Therefore, we prepare and select suitable inexpensive monomers, study acrylamide and two kinds of cationic monomer double water-phase method for ternary polymerization, the cation polyacrylamide emulsion product of development of new.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of preparation method of cation polyacrylamide emulsion.
The present invention solves the technical scheme that its technical problem adopts: a kind of preparation method of cation polyacrylamide emulsion, comprises the following steps:
(1) polyoxyethylene glycol, acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride, dimethyl diallyl ammonium chloride and auxiliary agent β-dimethylaminopropionitrile, urea is added in deionized water respectively, stirring and dissolving, mixes;
(2) be 3 ~ 5 by the pH value of solution system in dust technology regulating step (1);
(3) pass into the dissolved oxygen in high pure nitrogen expeling solution, add initiator ammonium persulfate, formaldehyde Sodium Thiosulfate and V-50, stirring reaction 3 ~ 4h at 40 DEG C, obtains polymer emulsion product.
Further, relative to the deionized water in system in step (1), by mass percentage, polyethyleneglycol content is 12 ~ 14%, acrylamide content is 12 ~ 14%, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride content is 2 ~ 3%, and dimethyl diallyl ammonium chloride content is 1.2 ~ 1.4%, and molecular weight polyethylene glycol is 20000.
Further, in step (1), β-dimethylaminopropionitrile accounts for 0.020 ~ 0.025% of monomer total mass, urea accounts for 5.5 ~ 6.5% of monomer total mass, and monomer total mass is the quality summation of acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride and dimethyl diallyl ammonium chloride three kinds of monomers.
Further, in step (2), dust technology volumetric concentration is 50%.
Further, in step (3), ammonium persulphate, formaldehyde Sodium Thiosulfate and V-50 all account for 0.35 ~ 0.40% of monomer total mass, and monomer total mass is the quality summation of acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride and dimethyl diallyl ammonium chloride three kinds of monomers.
The invention has the beneficial effects as follows: adopt novel cation monomer, by double water-phase dispersion copolymerization method, prepare the cation polyacrylamide emulsion product that production cost is low, viscosity is low, even particle size distribution, stability are high.
Embodiment
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) prepare the polyglycol solution 150ml of 13%, stir;
(2) in above-mentioned solution, add acrylamide 20g, cationic monomer acrylamido (2-hydroxyl) the hydroxypropyltrimonium chloride solution 5ml of 50%, the dimethyl diallyl ammonium chloride solution 3ml of 60%, and β-dimethylaminopropionitrile 6mg, urea 1g, stirring and dissolving, mixes;
(3) be 3 by the nitric acid regulator solution pH value of 50%, proceed in reactor;
(4) pass into high pure nitrogen 20 minutes, add the ammonium persulfate solution 4ml of initiator 2%, 2% the V-50 solution 4ml of formaldehyde Sodium Thiosulfate solution 4ml and 2%;
(5) heating in water bath to 40 DEG C, stirring reaction 3.5h, obtains product emulsion.
Embodiment 2
(1) prepare the polyglycol solution 150ml of 14%, stir;
(2) in above-mentioned solution, add acrylamide 22g, cationic monomer acrylamido (2-hydroxyl) the hydroxypropyltrimonium chloride solution 8ml of 50%, the dimethyl diallyl ammonium chloride solution 5ml of 60%, and β-dimethylaminopropionitrile 7mg, urea 1g, stirring and dissolving, mixes;
(3) be 5 by the dust technology regulator solution pH value of 50%, proceed in reactor;
(4) pass into high pure nitrogen 20 minutes, add the ammonium persulfate solution 5ml of initiator 2%, 2% the V-50 solution 5ml of formaldehyde Sodium Thiosulfate solution 5ml and 2%;
(5) heating in water bath to 40 DEG C, stirring reaction 3h, obtains product emulsion.
Embodiment 3
(1) prepare the polyglycol solution 150ml of 12%, stir;
(2) in above-mentioned solution, add acrylamide 18g, cationic monomer acrylamido (2-hydroxyl) the hydroxypropyltrimonium chloride solution 4ml of 50%, the dimethyl diallyl ammonium chloride solution 4ml of 60%, and β-dimethylaminopropionitrile 8mg, urea 1g, stirring and dissolving, mixes;
(3) be 4 by the dust technology regulator solution pH value of 50%, proceed in reactor;
(4) pass into high pure nitrogen 20 minutes, add the ammonium persulfate solution 4.5ml of initiator 2%, 2% the V-50 solution 4.5ml of formaldehyde Sodium Thiosulfate solution 4.5ml and 2%;
(5) heating in water bath to 40 DEG C, stirring reaction 4h, obtains product emulsion.
This technique adopts double-aqueous phase system polymerization, and building-up process does not have three waste discharge, and Heating temperature is not high, and finished product does not need heating, drying, energy-conserving and environment-protective.
Cationic monomer diallyldimethylammonChloride Chloride structure properties is good, form that multipolymer has that positive charge density is high, good water solubility, high effect nontoxic, the advantage such as cheap, but its activity is low, not easily forms high-molecular weight polymer and affects flocculating property.Add cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride, its reactive behavior is high, is easy to polymerization, containing hydroxyl in structure, can improve the flocculating property of product.
Adopt more efficiently ammonium persulphate, formaldehyde Sodium Thiosulfate and V-50 redox-azo-compound composite initiation system, by the auxiliary agent added, prepare that solvability is good, the novel cation polyacrylamide amine product of good emulsion stability, flocculating property excellence.
This synthetic method cost reduces, and compare with the cationic monomer of routine, product per ton reduces costs about 1000 yuan.Stability of emulsion improves, and stability is greater than half a year, and level of residual monomers is less than 1%, and flocculating property is better than similar product emulsion and solid cationic polyacrylamide product.To in 0.1% bentonite simulated wastewater process, show good flocculating effect when cationic polyacrylamide addition is 4mg/L, turbidity is less than 20NTU.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (5)
1. a preparation method for cation polyacrylamide emulsion, is characterized in that: comprise the following steps:
(1) polyoxyethylene glycol, acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride, dimethyl diallyl ammonium chloride and auxiliary agent β-dimethylaminopropionitrile, urea is added in deionized water respectively, stirring and dissolving, mixes;
(2) be 3 ~ 5 by the pH value of solution system in dust technology regulating step (1);
(3) pass into the dissolved oxygen in high pure nitrogen expeling solution, add initiator ammonium persulfate, formaldehyde Sodium Thiosulfate and V-50, stirring reaction 3 ~ 4h at 40 DEG C, obtains polymer emulsion product.
2. the preparation method of a kind of cation polyacrylamide emulsion according to claim 1, it is characterized in that: relative to the deionized water in system in described step (1), by mass percentage, polyethyleneglycol content is 12 ~ 14%, acrylamide content is 12 ~ 14%, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride content is 2 ~ 3%, dimethyl diallyl ammonium chloride content is 1.2 ~ 1.4%, and molecular weight polyethylene glycol is 20000.
3. the preparation method of a kind of cation polyacrylamide emulsion according to claim 1, it is characterized in that: in described step (1), β-dimethylaminopropionitrile accounts for 0.020 ~ 0.025% of monomer total mass, urea accounts for 5.5 ~ 6.5% of monomer total mass, and monomer total mass is the quality summation of acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride and dimethyl diallyl ammonium chloride three kinds of monomers.
4. the preparation method of a kind of cation polyacrylamide emulsion according to claim 1, is characterized in that: in described step (2), dust technology volumetric concentration is 50%.
5. the preparation method of a kind of cation polyacrylamide emulsion according to claim 1, it is characterized in that: in described step (3), ammonium persulphate, formaldehyde Sodium Thiosulfate and V-50 all account for 0.35 ~ 0.40% of monomer total mass, and monomer total mass is the quality summation of acrylamide, cationic monomer acrylamido (2-hydroxyl) hydroxypropyltrimonium chloride and dimethyl diallyl ammonium chloride three kinds of monomers.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773441A (en) * | 2021-08-09 | 2021-12-10 | 佳化化学科技发展（上海）有限公司 | Anti-flocculant and preparation method and application thereof |
| CN114426675A (en) * | 2021-12-17 | 2022-05-03 | 湖北康创科技有限公司 | Hyperbranched cationic polymer emulsion and application thereof in sludge dewatering |
| CN115651121A (en) * | 2022-11-15 | 2023-01-31 | 东营宝莫环境工程有限公司 | Production method of cationic polyacrylamide of ultralow molecular weight solid powder |
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| CN101514240A (en) * | 2008-12-30 | 2009-08-26 | 上海东升新材料有限公司 | Anionic polyacrylamide and preparation method thereof |
| CN101648740A (en) * | 2009-06-29 | 2010-02-17 | 上海东升新材料有限公司 | Cationic flocculant and preparation method thereof |
| CN102627725A (en) * | 2012-04-05 | 2012-08-08 | 西北师范大学 | Synthetic method for cationic polyacrylamide emulsion |
| CN103524672A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Method for preparing cationic flocculant |
-
2015
- 2015-11-13 CN CN201510777962.2A patent/CN105273131A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514240A (en) * | 2008-12-30 | 2009-08-26 | 上海东升新材料有限公司 | Anionic polyacrylamide and preparation method thereof |
| CN101648740A (en) * | 2009-06-29 | 2010-02-17 | 上海东升新材料有限公司 | Cationic flocculant and preparation method thereof |
| CN102627725A (en) * | 2012-04-05 | 2012-08-08 | 西北师范大学 | Synthetic method for cationic polyacrylamide emulsion |
| CN103524672A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Method for preparing cationic flocculant |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773441A (en) * | 2021-08-09 | 2021-12-10 | 佳化化学科技发展（上海）有限公司 | Anti-flocculant and preparation method and application thereof |
| CN114426675A (en) * | 2021-12-17 | 2022-05-03 | 湖北康创科技有限公司 | Hyperbranched cationic polymer emulsion and application thereof in sludge dewatering |
| CN114426675B (en) * | 2021-12-17 | 2023-04-07 | 湖北康创科技有限公司 | Hyperbranched cationic polymer emulsion and application thereof in sludge dewatering |
| CN115651121A (en) * | 2022-11-15 | 2023-01-31 | 东营宝莫环境工程有限公司 | Production method of cationic polyacrylamide of ultralow molecular weight solid powder |
| CN115651121B (en) * | 2022-11-15 | 2023-09-19 | 东营宝莫环境工程有限公司 | Production method of ultra-low molecular weight solid powder cationic polyacrylamide |
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