CN103819612A - Preparation method for modified cation retention and filter aid - Google Patents
Preparation method for modified cation retention and filter aid Download PDFInfo
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- CN103819612A CN103819612A CN201310708981.0A CN201310708981A CN103819612A CN 103819612 A CN103819612 A CN 103819612A CN 201310708981 A CN201310708981 A CN 201310708981A CN 103819612 A CN103819612 A CN 103819612A
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Abstract
The invention discloses a preparation method for a modified cation retention and filter aid, which comprises the following steps raw materials are mixed uniformly to obtain a homogeneous solution; a complexing agent and a defoaming agent are added sequentially; sufficient stirring is performed until the solution is clear; the pH value is adjusted via weak acid to obtain a homopolymerization solution; the homopolymerization solution is cooled and then pumped into a polymerization kettle; azodiisobutyronitrile is added; high-purity nitrogen is introduced; the solutions prepared by the raw materials are added sequentially; after the solutions are added fully, high-purity nitrogen is introduced continuously; then feeding is stopped; the temperature is controlled for polymerization reaction; aging reaction is performed for 4 h; a transparent elastic rubber block is obtained; the rubber block is taken out, cut, granulated, dried, smashed and sieved to obtain white powdery cation polyacrylamide According to the method, the obtained modified cation polyacrylamide can be widely applied to a paper technology, improve the dehydration property of pulp, increase retention rates of a fine fiber and a filler, and reduce consumption of the raw materials and environment pollution.
Description
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Technical field
The present invention relates to a kind of preparation method of modified cation retention filtration adjuvant, belong to the synthetic field of paper making water soluble macromolecular.
Background technology
Research of Cationic Polymeric Flocculant P (DAC-AM) is the multipolymer of cationic monomer acrylyl oxy-ethyl-trimethyl salmiac (DAC) and acrylamide (AM).It is a kind of linear polymer with cationic charge, have that electric density is high, the feature of good water solubility, at present, Papermaking Retention helps worry agent to be generally product emulsion, its Product transport inconvenience, the production cost that the storage time is shorter, the more high factor of price has increased paper, solid cationic polyacrylamide is prepared its method and is generally redox reaction system initiated polymerization technique on the other hand, this technique adds redox system initiated polymerization after cationic monomer and acrylamide are mixed in proportion, thereby makes cationic polyacrylamide.The cationic polyacrylamide product of this explained hereafter only can use as water treatment flocculant, due to its aspect solvability and in absorption paper pulp fiber fines and filler to keep aspect poor, therefore restricted in paper industry application.
Summary of the invention
The preparation method who the object of the present invention is to provide a kind of paper grade (stock) cationic retention aid flocculating aids, the product of being prepared by the method is uniformly dispersed, and steady quality is high to molecular weight, and dissolution rate is fast.
For achieving the above object, the preparation method of non-ionic polyacrylamide provided by the invention comprises the following steps:
(1) acrylyl oxy-ethyl-trimethyl salmiac solution 13.75-17.5%, the cm-chitosan 1-2%, the pure water 64.5-70.25% that are 80% by acrylamide 16-19%, concentration by weight percentage mix acquisition homogeneous phase solution, then add successively the complexing agent, the defoamer that are respectively 3-8ppm, 160-300ppm with homogeneous phase solution weight ratio, be stirred well to solution clarification, adjust pH value to 3.0～6.0 with weak acid, obtain the homopolymerization solution without solid insoluble;
(2) homopolymerization liquid is cooled to after 3-8 ℃, pump in polymeric kettle, add and account for homopolymerization solution quality than the Diisopropyl azodicarboxylate for 100-200ppm, pass into after high pure nitrogen 30min, add successively respectively by azo oxygenant, oxygenant, the concentration that reductive agent is mixed with is 5% solution, azo oxygenant, oxygenant, reductive agent, the mass ratio of assistant reducing agent and homopolymerization solution is respectively 50-65ppm, 20-35ppm, 10-15ppm, 6-10ppm, adding of every two kinds of solution is spaced apart 5 minutes, in each solution adition process, keep passing into high pure nitrogen, each solution stops filling nitrogen after continuing to pass into high pure nitrogen 5min after all adding, polymerization temperature is controlled at 5-8 ℃, after polyreaction 4-10 hour, be incubated again 60-90 ℃, aging reaction 4～6 hours, obtain transparent resilient blob of viscose,
(3) take out blob of viscose, cutting, granulation, dry, pulverize, screening, obtain white powder cationic polyacrylamide.
In such scheme, complexing agent is ethylene diamine tetra methylene phosphonic acid five sodium or Sunmorl N 60S or sodium alginate; Defoamer is silicone oil.
In such scheme, oxygenant is Potassium Thiosulphate, and azo oxygenant is azoformamide, and reductive agent is sulfurous acid, and assistant reducing agent is ferrous sulfate.
In such scheme, acetic acid or oxalic acid or phosphoric acid are selected in the acid of adjust pH, and the optimum value of pH value is 3.5-5.5.
The feature that the present invention adopts equal polymerization to prepare cationic polyacrylamide technique is:
(1), due to after AM, DAC low-temperature mixed, by acid-conditioning solution pH value, to acidity, there is hardly amide group protonation reaction in acrylamide molecule in the time of polymerization.Imidization is crosslinked and side chain is little, easily the positively charged ion product of the superior solubility of system.
(2), because cm-chitosan has compared with strong cation group, after AM, DAC copolymerization, effectively increased molecular chain length, cation group, make it have stronger charge neutralization ability and molecular bridge ability.
(3), simple process, without in addition heat supply insulation, reactor is less, molecular weight width easy to control on the one hand, facility investment and production cost are low on the other hand, ion degree, the molecular weight of product are even.
(4) azo--redox initiation system is initiated polymerization at low temperatures, process is steadily slow, the narrow molecular weight distribution of product, molecular weight is up to 1000～1,300 ten thousand, apparent viscosity >=1200mpa.s, specific filtration resistance≤1.0, screen factor >=25, the molten thing < 0.05% of water portion, residual list≤0.05%.General cationic polyacrylamide molecular weight is 800～9,000,000, this molecular weight product is higher than usual production molecular weight 200～5,000,000, having captured cation acrylamide product helps and considers the charge neutralization ability of application aspect and the difficult problem that molecular bridge ability can not be taken into account simultaneously at Papermaking Retention, can reduce a ton paper pulp consumption, improve output.
Embodiment
Further illustrate the present invention below in conjunction with several embodiment.
Embodiment 1
(1) at 7m
3material-compound tank in, preparation 4m
3homogeneous phase solution, wherein contain 650kg acrylamide, 680kg acrylyl oxy-ethyl-trimethyl salmiac (concentration is 80%), 60kg cm-chitosan.Not enough 4m
3part water supply, after solution is mixed, adjust pH=4.0 with 52kg oxalic acid.Add complexing agent ethylene diamine tetra methylene phosphonic acid five sodium, the 580g defoamer silicone oil of 28g, fully mechanical stirring, to solution clarification, obtains the homopolymerization solution without solid insoluble again.
(2) by homopolymerization solution liquid circulation temperature lowering after 4.0-4.5 ℃, in the polymeric kettle pumping into, add 600g Diisopropyl azodicarboxylate, and pass into high pure nitrogen (purity 99.9%, flow 80 m
3/ h) 30min, add successively concentration to be 5% following solution: hypo solution, sodium thiosulfate content 220g, azoformamide solution, azoformamide content 100g, sodium sulfite solution, S-WAT content 50g, copperas solution, ferrous sulfate content 28g, every two kinds of solution add and are spaced apart 5 minutes, in each solution adition process, continue to pass into high pure nitrogen, after each solution adds, after continuing to pass into high pure nitrogen 5min, stop filling nitrogen, polymerization temperature is controlled at 5.6 ℃, polyreaction 4.3 hours, be incubated again 75 ℃, aging reaction 4 hours, obtain transparent resilient blob of viscose.
(3) take out blob of viscose, cutting, granulation, dry, pulverize, screening, obtain 20～80 orders, molecular weight 1,260 ten thousand, cationic degree 28.6%, solid content 89.8%, dissolution rate 30～40min, apparent viscosity 1390mpa.s, specific filtration resistance≤1.0, the white powder cationic polyacrylamide of residual monomer 0.047%.
Embodiment 2
(1) at 7m
3material-compound tank in, preparation 4m
3homogeneous phase solution, wherein contain 680kg acrylamide, 600kg acrylyl oxy-ethyl-trimethyl salmiac (concentration is 80%), 60kg carboxymethyl chitosan sugar soln.Not enough 4m
3part water supply, after solution is mixed, with 53kg oxalic acid acid for adjusting pH to 4.0.Add complexing agent ethylene diamine tetra methylene phosphonic acid five sodium, the 580g defoamer silicone oil of 28g, fully mechanical stirring, to solution clarification, obtains the homopolymerization solution without solid insoluble again.
(2) by homopolymerization solution liquid circulation temperature lowering after 4.0-4.5 ℃, in the polymeric kettle pumping into, add 600g Diisopropyl azodicarboxylate, and pass into high pure nitrogen (purity 99.9%, flow 80 m
3/ h) 30min, add successively concentration to be 5% following solution: hypo solution, sodium thiosulfate content 220g, azoformamide solution, azoformamide content 100g, sodium sulfite solution, S-WAT content 50g, copperas solution, ferrous sulfate content 28g, every two kinds of solution add and are spaced apart 5 minutes, in each solution adition process, continue to pass into high pure nitrogen, after each solution adds, after continuing to pass into high pure nitrogen 5min, stop filling nitrogen, polymerization temperature is controlled at 5.5 ℃, polyreaction 4.5 hours, be incubated again 80 ℃, aging reaction 4 hours, obtain transparent resilient blob of viscose.
(3) take out blob of viscose, cutting, granulation, dry, pulverize, screening, obtain 20～80 orders, molecular weight 1,210 ten thousand, cationic degree 24.3%, solid content 89.7%, dissolution rate 30～40min, apparent viscosity 1350mpa.s, specific filtration resistance≤1.0, the white powder cationic polyacrylamide of residual monomer 0.049%.
Embodiment 3
(1) at 7m
3material-compound tank in, preparation 4m
3homogeneous phase solution, wherein contain 750kg acrylamide, 620kg acrylyl oxy-ethyl-trimethyl salmiac (concentration is 80%), 65kg carboxymethyl chitosan sugar soln.Not enough 4m
3part water supply, after solution is mixed, with 60kg oxalic acid acid for adjusting pH to 3.8.Add complexing agent ethylene diamine tetra methylene phosphonic acid five sodium, the 580g defoamer silicone oil of 28g, fully mechanical stirring, to solution clarification, obtains the homopolymerization solution without solid insoluble again.
(2) by homopolymerization solution liquid circulation temperature lowering after 4.0-4.5 ℃, in the polymeric kettle pumping into, add 600g Diisopropyl azodicarboxylate, and pass into high pure nitrogen (purity 99.9%, flow 80 m
3/ h) 30min, add successively concentration to be 5% following solution: hypo solution, sodium thiosulfate content 220g, azoformamide solution, azoformamide content 100g, sodium sulfite solution, S-WAT content 50g, copperas solution, ferrous sulfate content 28g, every two kinds of solution add and are spaced apart 5 minutes, in each solution adition process, continue to pass into high pure nitrogen, after each solution adds, after continuing to pass into high pure nitrogen 5min, stop filling nitrogen, polymerization temperature is controlled at 5.9 ℃, polyreaction 3.8 hours, be incubated again 80 ℃, aging reaction 4 hours, obtain transparent resilient blob of viscose.
(3) take out blob of viscose, cutting, granulation, dry, pulverize, screening, obtain 20～80 orders, molecular weight 1,160 ten thousand, cationic degree 21.2%, solid content 90.8%, dissolution rate 30～40min, apparent viscosity 1270mpa.s, specific filtration resistance≤1.0, the white powder cationic polyacrylamide of residual monomer 0.041%.
Claims (4)
1. a preparation method for modified cation retention filtration adjuvant, is characterized in that comprising the following steps:
(1) acrylyl oxy-ethyl-trimethyl salmiac (DAC) the solution 13.75-17.5%, cm-chitosan 1-2%, the pure water 64.5-70.25% that are 80% by acrylamide (AM) 16-19%, concentration by weight percentage mix acquisition homogeneous phase solution, then add successively the complexing agent, the defoamer that are respectively 3-8ppm, 160-300ppm with homogeneous phase solution weight ratio, be stirred well to solution clarification, adjust pH value to 3.0～6.0 with weak acid, obtain the homopolymerization solution without solid insoluble;
(2) homopolymerization liquid is cooled to after 3-8 ℃, pump in polymeric kettle, add and account for homopolymerization solution quality than the Diisopropyl azodicarboxylate for 100-200ppm, pass into after high pure nitrogen 30min, add successively respectively by azo oxygenant, oxygenant, the concentration that reductive agent is mixed with is 5% solution, azo oxygenant, oxygenant, reductive agent, the mass ratio of assistant reducing agent and homopolymerization solution is respectively 50-65ppm, 20-35ppm, 10-15ppm, 6-10ppm, adding of every two kinds of solution is spaced apart 5 minutes, in each solution adition process, keep passing into high pure nitrogen, each solution stops filling nitrogen after continuing to pass into high pure nitrogen 5min after all adding, polymerization temperature is controlled at 5-8 ℃, after polyreaction 4-10 hour, be incubated again 60-90 ℃, aging reaction 4～6 hours, obtain transparent resilient blob of viscose,
(3) take out blob of viscose, cutting, granulation, dry, pulverize, screening, obtain white powder cationic polyacrylamide.
2. a kind of preparation method of modified cation retention filtration adjuvant according to claim 1, is characterized in that: complexing agent is disodium ethylene diamine tetraacetate or Sunmorl N 60S or sodium alginate; Defoamer is silicone oil.
3. a kind of preparation method of modified cation retention filtration adjuvant according to claim 1, is characterized in that: azo oxygenant is that azoformamide, oxygenant are Potassium Thiosulphate, and reductive agent is potassium sulfite, and assistant reducing agent is ferrous sulfate.
4. a kind of preparation method of modified cation retention filtration adjuvant according to claim 1, is characterized in that: acetic acid or oxalic acid or phosphoric acid are selected in the acid of adjust pH, and the optimum value of pH value is 3.5-5.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254811A (en) * | 2015-11-10 | 2016-01-20 | 陕西科技大学 | Carboxymethyl chitosan quaternary ammonium salt and preparation method thereof |
| CN105484100A (en) * | 2015-11-18 | 2016-04-13 | 江门市高力依科技实业有限公司 | Preparation method for retention and drainage aid for fiber fines |
| CN107556432A (en) * | 2017-10-11 | 2018-01-09 | 青岛科技大学 | A kind of method added molecular weight regulator and prepare paper grade (stock) cationic retention aid filter aid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880356A (en) * | 2010-07-12 | 2010-11-10 | 南京大学 | Preparation method of grafting amphoteric chitosan flocculant |
| CN102690389A (en) * | 2012-05-25 | 2012-09-26 | 安徽巨成精细化工有限公司 | Preparation method for high molecular weight cationic polyacrylamide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880356A (en) * | 2010-07-12 | 2010-11-10 | 南京大学 | Preparation method of grafting amphoteric chitosan flocculant |
| CN102690389A (en) * | 2012-05-25 | 2012-09-26 | 安徽巨成精细化工有限公司 | Preparation method for high molecular weight cationic polyacrylamide |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254811A (en) * | 2015-11-10 | 2016-01-20 | 陕西科技大学 | Carboxymethyl chitosan quaternary ammonium salt and preparation method thereof |
| CN105484100A (en) * | 2015-11-18 | 2016-04-13 | 江门市高力依科技实业有限公司 | Preparation method for retention and drainage aid for fiber fines |
| CN105484100B (en) * | 2015-11-18 | 2017-12-26 | 江门市高力依科技实业有限公司 | A kind of preparation method of fiber fines retention and drainage aid agent |
| CN107556432A (en) * | 2017-10-11 | 2018-01-09 | 青岛科技大学 | A kind of method added molecular weight regulator and prepare paper grade (stock) cationic retention aid filter aid |
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