CN101372524B - Process for producing cation polyacrylamide - Google Patents
Process for producing cation polyacrylamide Download PDFInfo
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- CN101372524B CN101372524B CN2008100462950A CN200810046295A CN101372524B CN 101372524 B CN101372524 B CN 101372524B CN 2008100462950 A CN2008100462950 A CN 2008100462950A CN 200810046295 A CN200810046295 A CN 200810046295A CN 101372524 B CN101372524 B CN 101372524B
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- cationic polyacrylamide
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- potassium persulphate
- urea
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Abstract
The invention provides a technique for producing cationic polyacrylamide, and comprises the raw materials by mass percent: 10.0 to 25.0% of acrylamide, 5.0 to 10.0% of acryloxyethyl trimethylammonium chloride, 0.02-0.04% of redox, 0.03-0.015% of azo compound, 0.5 to 5.0 of urea, 0.02 to 0.15% of fatty acid salt, and 65.5-84% of deionized water; the raw materials are put into a reactor and added with the redox to have induced polymerization reaction under nitrogen protection at the room temperature, and then added with the azo compound to have secondary induced polymerization reaction; finally, the products of the invention are obtained after granulation and dryness. The technique is stable, slow in induction, even in reaction, mild and ordered, and easy in the control of operation process; the obtained products are rapid in dissolution rate, little in usage, large in water yield, big and dense in floccules, and not easy in fragmentation. The technique is mainly used for various environment-friendly fields such as sewage disposal, sludge dewatering, etc.
Description
Technical field
The present invention relates to a kind of production technique of polymkeric substance, particularly relate to a kind of production technique of cationic polyacrylamide.
Background technology
Cationic polyacrylamide has efficiency flocculating agent to be widely used in the environmental protection field as sewage disposal and sludge dewatering.In producing the process of cationic polyacrylamide because the difference of production technique, cause electric charge intensity and electric density and distribution etc. in the molecular weight, molecular order, molecule of product cationic polyacrylamide all can produce, thereby directly influence flocculation sediment effect, dewatering and effect than big difference.The synthesizing cationic polyacrylamide mainly adopts copolyreaction at present.Chinese patent CN1824682A discloses a kind of preparation method of extra high molecular cation polyacrylamide, comonomer acrylamide (AM) that adopts and acryloxy ethyl-trimethyl salmiac (DAC) need refining, purification process, need use the N-BUTYL ACETATE extracting as DAC, AM needs ion exchange resin treatment, adopt 99.999% high pure nitrogen deoxygenation during polymerization, used initiator is persulphate, sulphite and water-soluble organic diazo salt, also need add various additives in addition, as sequestrant, chain-transfer agent, chain propagation agent, chain regulator etc.Used reactor need with adiabatic and in be coated with the silicon rubber anti-stick coating.This method all increases production cost and facility investment expense, owing to add various additives, production control is complicated, thereby influences the stability of product performance.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming, provide a kind of processing condition lower, smooth production process, easy to control, products obtained therefrom superior performance and stable, the production technique of the cationic polyacrylamide that relative cost is lower.
Used starting material are by mass percentage in the production technique of cationic polyacrylamide of the present invention:
Acrylamide 10.0～25.0,
Acrylyl oxy-ethyl-trimethyl salmiac 5.0～10.0,
Redox agent 0.02～0.4,
Azo-compound 0.03～0.15,
Urea 0.5～5.0,
Soap 0.02～0.15.
Deionized water 65.5～84.0.
Its operation steps is; in reactor, add deionized water; feed nitrogen to oxygen saturation≤5%; add acrylamide (AM) successively; acrylyl oxy-ethyl-trimethyl salmiac (DAC); urea and soap; regulate pH value to 6.0～7.0; by going into nitrogen and keeping oxygen saturation≤5%; add redox agent; form first section initiator system; copolyreaction is 45 ± 2 minutes under the nitrogen protection condition, at this moment, generates the lower molecular weight interpolymer of molecular weight 1000～10000; afterwards; add azo-compound and form second section initiator system, continue reaction after 50～70 minutes, reaction system becomes thick; can put into polymerization tank; under 70 ℃ of temperature, reacted again 4～5 hours, last, get the copolymer colloid of molecular weight 5,000,000～1,000 ten thousand; be cooled to room temperature; granulation, the dry cationic polyacrylamide that gets under 60～70 ℃ of temperature.Wherein, redox agent is Potassium Persulphate and fat tertiary amine, and its cooperation ratio is 1:1 by mass parts.Azo-compound is a Diisopropyl azodicarboxylate, 2, a kind of in the two amidine propanes of 2-azo two (2-amidine propane), azo.Soap is a kind of in sodium formiate, sodium acetate, Sodium Propionate and the Sodium propanecarboxylate.Fat tertiary amine is a kind of in Trimethylamine 99, triethylamine, trolamine and the dimethyl octylame.The general sodium hydroxide solution that adopts 10% (weight) of pH regulator agent in the reaction.Add urea and soap and can improve its solubility property.
The advantage of the production technique of cationic polyacrylamide of the present invention was to adopt two steps to cause, can guarantee to react mild, even, gentle, reaction is easy to control, production process is very stable, the existence of fat tertiary amine can reduce in the reaction system requirement to material purity greatly, thereby reduces production costs and the facility investment expense.The inventive method products obtained therefrom dissolution rate is fast, consumption is little, aquifer yield is big, floc sedimentation is big and closely knit, be difficult for fragmentation, have extremely strong turbidity removal, remove look, deodorizing and eliminate the ability of some harmful bacterium, and the function that reduces COD, BOD and SS arranged, especially remarkable to high pollution, high depth aqueous systems effect.Be mainly used in the sewage and the wastewater treatment of industries such as public works sewage disposal, chemical industry, sugaring, printing and dyeing, papermaking, steel-making, and sludge dewatering, etc. the environmental protection field.
Embodiment
Embodiment 1:
Each starting material starting material is by mass percentage:
Acrylamide 10.0
Acrylyl oxy-ethyl-trimethyl salmiac 5.05
Redox agent (Potassium Persulphate: Trimethylamine 99=1: 1) 0.4
Diisopropyl azodicarboxylate 0.03
Urea 0.5
Sodium formiate 0.02
Deionized water 84.0
Its operation steps is; in reactor, add deionized water; feed nitrogen to oxygen saturation≤5%; add acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, urea and sodium formiate successively; regulate pH value to 6.0; by going into nitrogen and keeping oxygen saturation≤5%; add redox agent; reaction is 43 minutes under the nitrogen protection condition, adds Diisopropyl azodicarboxylate afterwards, continues reaction after 60 minutes; under 60 ℃ of temperature, reacted again 4 hours; get copolymer colloid, be cooled to room temperature, granulation, the dry cationic polyacrylamide that gets under 60～70 ℃ of temperature.Its performance index are as shown in table 1, and result of use is shown in table 2, table 3, table 4.
Embodiment 2:
Each starting material starting material is by mass percentage:
Acrylamide 25.0
Acrylyl oxy-ethyl-trimethyl salmiac 6.98
Redox agent (Potassium Persulphate: dimethyl octylame=1: 1) 0.02
The two amidine propanes 0.15 of azo
Urea 2.2
Sodium Propionate 0.15
Deionized water 65.5
Its operation steps is; in reactor, add deionized water; feed nitrogen to oxygen saturation≤5%; add acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, urea and Sodium Propionate successively; regulate pH value to 6.5; by going into nitrogen and keeping oxygen saturation≤5%; add redox agent; reaction is 45 minutes under the condition of nitrogen protection, adds the two amidine propanes of azo afterwards, continues reaction after 50 minutes; reacted again 4.5 hours in 50 ℃ of temperature; get copolymer colloid, be cooled to room temperature, granulation, the dry cationic polyacrylamide that gets under 60～70 ℃ of temperature.Its performance index are as shown in table 1, and result of use is shown in table 2, table 3, table 4.
Embodiment 3:
Each starting material starting material is by mass percentage:
Acrylamide 14.5
Acrylyl oxy-ethyl-trimethyl salmiac 10.0
Redox agent (Potassium Persulphate: trolamine=1: 1) 0.3
2,2 azos two (2-amidine propane) 0.1
Urea 5.0
Sodium propanecarboxylate 0.1
Deionized water 70.0
Its operation steps is; in reactor, add deionized water; feed nitrogen to oxygen saturation≤5%; add acrylamide successively; the acryloxy ethyl-trimethyl salmiac; urea and Sodium propanecarboxylate; regulate pH value to 7; by going into nitrogen and keeping oxygen saturation≤5%; add redox agent; reaction is 47 minutes under the condition of nitrogen protection, adds 2 afterwards; 2 azos two (2-amidine propane) continued reaction after 60 minutes; reacted again 5 hours in 40 ℃ of temperature; get copolymer colloid, be cooled to room temperature; granulation, the dry cationic polyacrylamide that gets under 60～70 ℃ of temperature.Its performance index are as shown in table 1, and result of use is shown in table 2, table 3, table 4.
Table 1: product performance detected result of the present invention
| Embodiment 1 | Embodiment 2 | Stockhausen (Germany) | |
| Dissolution time (min) | 45 | 50 | 50 |
| Aquifer yield (ml/100ml) | 70 | 70 | 70 |
| Consumption (ppm) | 11 | 11 | 15 |
| Flocculating effect | Floc sedimentation is big and closely knit | Floc sedimentation is big and closely knit | Floc sedimentation is more broken |
Table 2: product of the present invention reaches sludge dewatering effect in the same old way
| Polyacrylamide | Consumption (ppm) | Water rate (%) | Water outlet transmittance (%) | Phenomenon |
| Produce in Jiangsu | 15 | 70 | 83.9 | Mud is little group, and sedimentation is slow, and it is muddy to deviate from water. |
| Japan produces | 15 | 72 | 89.2 | Mud is middle group, and sedimentation is fast, deviates from clarification of water. |
| Example 1,2,3 mean values of the present invention | 15 | 78 | 91.3 | Mud is middle group, and sedimentation is fast, deviates from clarification of water. |
Table 3: product of the present invention and to Processing Paper Wastewater effect in the same old way
Table 4: product of the present invention and to treatment of dyeing and printing effect in the same old way
Claims (3)
1. the production technique of a cationic polyacrylamide is characterized in that used starting material are by mass percentage:
Acrylamide 10.0～25.0,
Acrylyl oxy-ethyl-trimethyl salmiac 5.0～10.0,
Redox agent 0.02～0.4,
Azo-compound 0.03～0.15,
Urea 0.5～5.0.
Soap 0.02～0.15,
Deionized water 65.5～84.0;
Its operation steps is; in reactor, add deionized water; feed nitrogen to oxygen saturation≤5%; add acrylamide successively; acrylyl oxy-ethyl-trimethyl salmiac; urea and soap; regulate pH value to 6.0～7.0; feed nitrogen and keep oxygen saturation≤5%; add redox agent; under the condition of nitrogen protection, reacted 45 ± 2 minutes; add azo-compound afterwards, continue reaction after 50～70 minutes, under 70 ℃ of temperature, reacted again 4～5 hours; get copolymer colloid; cooling; granulation, the dry cationic polyacrylamide that gets under 60～70 ℃ of temperature, wherein; redox agent is Potassium Persulphate and Trimethylamine 99; Potassium Persulphate and triethylamine; a kind of mixture in Potassium Persulphate and trolamine and Potassium Persulphate and the dimethyl octylame, its cooperation ratio is 1: 1 by mass parts.
2. the production technique of cationic polyacrylamide as claimed in claim 1 is characterized in that azo-compound is a Diisopropyl azodicarboxylate, 2, a kind of in the two amidine propanes of 2-azo two (2-amidine propane), azo.
3. the production technique of cationic polyacrylamide as claimed in claim 1 is characterized in that soap is a kind of in sodium formiate, sodium acetate, Sodium Propionate and the Sodium propanecarboxylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100462950A CN101372524B (en) | 2008-10-17 | 2008-10-17 | Process for producing cation polyacrylamide |
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| CN2008100462950A CN101372524B (en) | 2008-10-17 | 2008-10-17 | Process for producing cation polyacrylamide |
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| CN101372524A CN101372524A (en) | 2009-02-25 |
| CN101372524B true CN101372524B (en) | 2011-05-04 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921365B (en) * | 2010-09-09 | 2015-04-22 | 广东省工程技术研究所 | Preparation method for instant cationic polyacrylamide |
| CA2880415A1 (en) * | 2012-04-13 | 2013-10-17 | Basf Se | New cationic polymers |
| CN103772559A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Initiator composition used for preparing oil displacing agent of polymer used in tertiary oil recovery |
| CN106349427A (en) * | 2016-08-29 | 2017-01-25 | 浙江大川新材料股份有限公司 | AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method |
| CN107033846B (en) * | 2017-04-14 | 2019-07-23 | 四川通丰科技有限公司 | A kind of haze inhibitor and preparation method thereof |
| CN107298735B (en) * | 2017-07-21 | 2019-09-27 | 广州安达净水材料有限公司 | A kind of liquid flocculant and preparation method thereof |
| CN108912267B (en) * | 2018-06-11 | 2020-09-29 | 宁夏神耀科技有限责任公司 | Preparation method of cationic polyacrylamide flocculant for coal gasification black water treatment |
| CN113262748A (en) * | 2021-06-23 | 2021-08-17 | 河南正佳能源环保股份有限公司 | Polymerization kettle for producing polyacrylamide |
| CN114349901A (en) * | 2021-12-15 | 2022-04-15 | 常州市振邦化工制造有限公司 | Preparation method of flocculant |
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