CN101649581A - Method for preparing amphoteric high molecular base AKD emulsion - Google Patents
Method for preparing amphoteric high molecular base AKD emulsion Download PDFInfo
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Abstract
The invention discloses a method for preparing amphoteric high molecular base AKD emulsion. The method comprises the following steps: under the function of a cosolvent and a molecular weight regulator, taking vinyl monomers, such as styrene, acrylate, acrylamide, a cation monomer, (methyl) acrylic acid and the like, as a copolymerization monomer and preparing amphoteric saponin-free benzene emulsion by a saponin-free emulsion polymerization method; taking the amphoteric saponin-free benzene emulsion as an amphoteric high molecular surfactant, emulsifying and dispersing a long-chain alkyl ketene multimer (AKD) with excellent hydrophobic property and preparing the AKD emulsion with favorable stability and sizing performance by shearing and dispersing. The invention does not use a small molecular emulsifying agent and cation starch in the preparation process and overcomes the defects of easy bubbling, poor stability, poor sizing effect and the like of the traditional AKD emulsion; the prepared amphoteric high molecular base AKD emulsion has anionic properties and cationic properties and is free from the interference of the anionic impurities of a papermaking wet part system, and the retention rate is greatly enhanced.
Description
Technical field
The invention belongs to chemical field, particularly a kind of preparation method of amphoteric high molecular base AKD emulsion.
Background technology
Along with the modernization of offset printing technology, the quality requirement of paper is improved day by day, the demand of neutral and alkali paper also increases gradually.Compare with acid applying glue, no matter neutral sizing is improving the paper whiteness, is improving printing adaptability, is reducing integrated cost, or market and user's favor degree, its advantage is obvious further.Through facts have proved, AKD has become domestic paper plant and has used ripe, the most fruitful neutral sizing agent.Between characteristics such as AKD high activity, facile hydrolysis, the preparation of its emulsion not only need solve its emulsification problem, also should solve its stability problem.Tradition AKD emulsion substantially with cationic starch and some micromolecule surfactants as emulsifying agent, all there are shortcomings such as many bubbles and poor stability in the AKD emulsion that makes thus, and the retention on fiber and all lower with the reactivity of fiber, thereby be prone to the phenomenon that sizing efficiency goes down, and the strength character of paper decreases after the applying glue.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation method with the good amphoteric high molecular base AKD emulsion of excellent stability, bond performance, filming performance and sizing efficiency is provided.
For achieving the above object, the technical solution used in the present invention is:
1) styrene, acrylic ester monomer, cationic monomer, acrylic monomer, acrylamide, molecular weight regulator are pressed (5-10): (5-10): (5-10): (2-5): (5-20): mass ratio (0.04-2) mixes and makes solution A, solution A and cosolvent are pressed (22-55): mass ratio (20-60) mixes and makes solution B, is warming up to 50-85 ℃; Oil-soluble initiator, cosolvent are pressed (0.2-2.5): (1-5) mix and make solution C, again C is added in 50-85 ℃ the B solution, wherein the mass ratio of solution C and solution B is 0.04-0.08: 1, continued insulation reaction 3-6 hour, regulate the pH value to 6-8, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 60-80 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is (0.2-0.6): 1: (3-5);
3) in AKD pre-emulsion E, add 60-80 ℃ hot water, behind the 20-30MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, the deionized water that adds-5～5 ℃ in AKD emulsion F makes the amphoteric high molecular base AKD emulsion that solid content is 15-20%.
Described acrylic ester monomer is a kind of of (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) butyl acrylate, (methyl) Hexyl 2-propenoate, (methyl) octadecyl acrylate, (methyl) acrylic acid n-octyl, (methyl) hydroxy-ethyl acrylate and (methyl) hydroxypropyl acrylate or wherein two to multiple mixing with arbitrary proportion.
Described cationic monomer is a kind of of methylacryoyloxyethyl trimethyl ammonium chloride, methylacryoyloxyethyl dimethyl benzyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, acrylyl oxy-ethyl dimethyl benzyl ammonium chloride, right-the vinyl benzyl trimethyl ammonium chloride, Dimethylaminoethyl Methacrylate benzyl chloride quaternary ammonium, diallyldimethylammonium chloride or dimethylaminoethyl methacrylate or wherein two to multiple mixing with arbitrary proportion.
Described acrylic monomer is the mixture of one or both arbitrary proportions of acrylic or methacrylic acid.
Described molecular weight regulator is lauryl mercaptan or isopropyl alcohol.
Described cosolvent is N, dinethylformamide, N,N-dimethylacetamide or N-Methyl pyrrolidone.
Described oil-soluble initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
Do not use micromolecule surfactant and cationic starch in the preparation process of the present invention, overcome the AKD emulsion at high temperature with the long term storage process in easily mouldy, rotten problem, solve emulsion and easily bubble, shortcomings such as stability and sizing efficiency difference; Prepared amphoteric high molecular base AKD emulsion has anionic property and cationic concurrently, makes the AKD emulsion not disturbed by the anionic impurity of paper making wet part system, and retention rate significantly improves, and has greatly shortened the maturation period of AKD simultaneously; And have good synergy with filler and oxidized starch, can significantly improve the water proofing property and the physical strength of paper.
The specific embodiment
Embodiment 1:
1) with styrene, methyl methacrylate, methylacryoyloxyethyl trimethyl ammonium chloride, acrylic acid, acrylamide, lauryl mercaptan by 10: 5: 8: 2.5: 8: 0.5 mass ratio mixes and makes solution A, with solution A and N, dinethylformamide mixes by 22: 20 mass ratio and makes solution B, is warming up to 85 ℃; With azodiisobutyronitrile and N, dinethylformamide mixed by 0.5: 2 and makes solution C, again in the B solution with 85 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.04: 1, continued insulation reaction 3 hours, regulate pH value to 6, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 80 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.2: 1: 5;
3) in AKD pre-emulsion E, add 80 ℃ hot water, behind the 20MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding-5 ℃ deionized water in AKD emulsion F, to make solid content be 15% amphoteric high molecular base AKD emulsion.
Embodiment 2:
1) with styrene, methyl acrylate, methylacryoyloxyethyl dimethyl benzyl ammonium chloride, methacrylic acid, acrylamide, isopropyl alcohol by 8: 10: 5: 4.5: 12: 1.3 mass ratio mixes and makes solution A, with solution A and N, the N-dimethylacetylamide mixes by 40: 50 mass ratio and makes solution B, is warming up to 60 ℃; With 2,2'-Azobis(2,4-dimethylvaleronitrile) and N, the N-dimethylacetylamide mixed by 1.8: 5 and makes solution C, again in the B solution with 60 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.06: 1, continued insulation reaction 5 hours, regulate pH value to 8, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 60 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.6: 1: 3;
3) in AKD pre-emulsion E, add 60 ℃ hot water, behind the 30MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding 0 ℃ deionized water in AKD emulsion F, to make solid content be 18% amphoteric high molecular base AKD emulsion.
Embodiment 3:
1) with styrene, ethyl methacrylate, acrylyl oxy-ethyl-trimethyl salmiac, acrylic acid, acrylamide, lauryl mercaptan by 5: 7: 10: 3: 20: 0.8 mass ratio mixes and makes solution A, solution A and N-Methyl pyrrolidone mixed by 30: 40 mass ratio make solution B, be warming up to 75 ℃; Dibenzoyl peroxide and N-Methyl pyrrolidone mixed by 2.5: 3 make solution C, again in the B solution with 75 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.08: 1, continued insulation reaction 4 hours, regulate pH value to 7, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 70 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.3: 1: 4;
3) in AKD pre-emulsion E, add 70 ℃ hot water, behind the 25MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding 3 ℃ deionized water in AKD emulsion F, to make solid content be 16% amphoteric high molecular base AKD emulsion.
Embodiment 4:
1) with styrene, butyl acrylate, acrylyl oxy-ethyl dimethyl benzyl ammonium chloride, methacrylic acid, acrylamide, isopropyl alcohol by 7: 8: 9: 4.2: 10: 1 mass ratio mixes and makes solution A, with solution A and N, dinethylformamide mixes by 55: 60 mass ratio and makes solution B, is warming up to 50 ℃; With dibenzoyl peroxide and N, dinethylformamide mixed by 1: 1 and makes solution C, again in the B solution with 50 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.05: 1, continued insulation reaction 6 hours, regulate pH value to 7, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 65 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.5: 1: 3.5;
3) in AKD pre-emulsion E, add 65 ℃ hot water, behind the 23MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding-2 ℃ deionized water in AKD emulsion F, to make solid content be 20% amphoteric high molecular base AKD emulsion.
Embodiment 5:
1) with styrene, octadecyl methacrylate, right-the vinyl benzyl trimethyl ammonium chloride, acrylic acid, acrylamide, lauryl mercaptan by 9: 6: 7: 3.5: 5: 0.04 mass ratio mixes and makes solution A, with solution A and N, the N-dimethylacetylamide mixes by 50: 55 mass ratio and makes solution B, is warming up to 70 ℃; With 2,2'-Azobis(2,4-dimethylvaleronitrile) and N, the N-dimethylacetylamide mixed by 0.2: 4 and makes solution C, again in the B solution with 70 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.07: 1, continued insulation reaction 3.5 hours, regulate pH value to 8, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 75 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.4: 1: 4.5;
3) in AKD pre-emulsion E, add 75 ℃ hot water, behind the 27MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding 5 ℃ deionized water in AKD emulsion F, to make solid content be 17% amphoteric high molecular base AKD emulsion.
Embodiment 6:
1) with styrene, octadecyl methacrylate, acrylic acid n-octyl, Dimethylaminoethyl Methacrylate benzyl chloride quaternary ammonium, diallyldimethylammonium chloride, acrylic acid, methacrylic acid, acrylamide, isopropyl alcohol by 6: 3: 5: 3: 3: 1: 1: 18: 1.5 mass ratio mixed and makes solution A, solution A and N-Methyl pyrrolidone mixed by 25: 30 mass ratio make solution B, be warming up to 55 ℃; Azodiisobutyronitrile and N-Methyl pyrrolidone mixed by 1.5: 2.5 make solution C, again in the B solution with 55 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.06: 1, continued insulation reaction 4.5 hours, regulate pH value to 6, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 63 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.6: 1: 3.8;
3) in AKD pre-emulsion E, add 63 ℃ hot water, behind the 29MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding 1 ℃ deionized water in AKD emulsion F, to make solid content be 19% amphoteric high molecular base AKD emulsion.
Embodiment 7:
1) with styrene, hydroxy-ethyl acrylate, hydroxy propyl methacrylate, diallyldimethylammonium chloride, dimethylaminoethyl methacrylate, acrylic acid, methacrylic acid, acrylamide, lauryl mercaptan by 10: 2: 3: 4: 6: 3: 2: 14: 2 mass ratio mixed and makes solution A, with solution A and N, dinethylformamide mixes by 35: 45 mass ratio and makes solution B, is warming up to 80 ℃; With azodiisobutyronitrile and N, dinethylformamide mixed by 2.3: 3.5 and makes solution C, again in the B solution with 80 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.04: 1, continued insulation reaction 5.5 hours, regulate pH value to 8, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 68 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.4: 1: 4.2;
3) in AKD pre-emulsion E, add 68 ℃ hot water, behind the 21MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding-1 ℃ deionized water in AKD emulsion F, to make solid content be 18% amphoteric high molecular base AKD emulsion.
Embodiment 8:
1) with styrene, methyl acrylate, butyl methacrylate, octadecyl acrylate, methylacryoyloxyethyl trimethyl ammonium chloride, methylacryoyloxyethyl dimethyl benzyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, acrylic acid, acrylamide, isopropyl alcohol by 5: 3: 3: 4: 1: 2: 2: 4: 7: 1.7 mass ratio mixed and makes solution A, solution A and N-Methyl pyrrolidone mixed by 45: 35 mass ratio make solution B, be warming up to 65 ℃; Dibenzoyl peroxide and N-Methyl pyrrolidone mixed by 2: 1.5 make solution C, again in the B solution with 65 ℃ of C addings, wherein the mass ratio of solution C and solution B is 0.08: 1, continued insulation reaction 3 hours, regulate pH value to 6, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 77 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, and make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is 0.2: 1: 4.7;
3) in AKD pre-emulsion E, add 77 ℃ hot water, behind the 24MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, adding 4 ℃ deionized water in AKD emulsion F, to make solid content be 15% amphoteric high molecular base AKD emulsion.
Claims (7)
1, the preparation method of amphoteric high molecular base AKD emulsion is characterized in that:
1) styrene, acrylic ester monomer, cationic monomer, acrylic monomer, acrylamide, molecular weight regulator are pressed (5-10): (5-10): (5-10): (2-5): (5-20): mass ratio (0.04-2) mixes and makes solution A, solution A and cosolvent are pressed (22-55): mass ratio (20-60) mixes and makes solution B, is warming up to 50-85 ℃; Oil-soluble initiator, cosolvent are pressed (0.2-2.5): (1-5) mix and make solution C, again C is added in 50-85 ℃ the B solution, wherein the mass ratio of solution C and solution B is 0.04-0.08: 1, continued insulation reaction 3-6 hour, regulate the pH value to 6-8, add deionized water regulation system solid content to 20%, both got the Amphiphatic high polymer surfactant D;
2) keep the temperature of Amphiphatic high polymer surfactant D, AKD and each system of deionized water at 60-80 ℃; After treating the AKD fusion, AKD and deionized water with Amphiphatic high polymer surfactant D, fusion under stirring condition mix, make AKD pre-emulsion E, wherein Amphiphatic high polymer surfactant D: AKD: the mass ratio of deionized water is (0.2-0.6): 1: (3-5);
3) in AKD pre-emulsion E, add 60-80 ℃ hot water, behind the 20-30MPa homogeneous, make solid content and be 30% AKD emulsion F;
4) under stirring condition, the deionized water that adds-5～5 ℃ in AKD emulsion F makes the amphoteric high molecular base AKD emulsion that solid content is 15-20%.
2, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described acrylic ester monomer is a kind of of (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) butyl acrylate, (methyl) Hexyl 2-propenoate, (methyl) octadecyl acrylate, (methyl) acrylic acid n-octyl, (methyl) hydroxy-ethyl acrylate and (methyl) hydroxypropyl acrylate or wherein two to multiple mixing with arbitrary proportion.
3, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described cationic monomer is a kind of of methylacryoyloxyethyl trimethyl ammonium chloride, methylacryoyloxyethyl dimethyl benzyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, acrylyl oxy-ethyl dimethyl benzyl ammonium chloride, right-the vinyl benzyl trimethyl ammonium chloride, Dimethylaminoethyl Methacrylate benzyl chloride quaternary ammonium, diallyldimethylammonium chloride or dimethylaminoethyl methacrylate or wherein two to multiple mixing with arbitrary proportion.
4, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described acrylic monomer is the mixture of one or both arbitrary proportions of acrylic or methacrylic acid.
5, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described molecular weight regulator is lauryl mercaptan or isopropyl alcohol.
6, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described cosolvent is N, dinethylformamide, N,N-dimethylacetamide or N-Methyl pyrrolidone.
7, the preparation method of amphoteric high molecular base AKD emulsion according to claim 1 is characterized in that: described oil-soluble initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
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| CN102635024B (en) * | 2012-05-04 | 2014-01-29 | 陕西科技大学 | Preparation method for non-soap cationic polymer AKD (alkyl ketene dimer) neutral/alkali sizing agent |
| CN102627745B (en) * | 2012-05-04 | 2014-01-29 | 陕西科技大学 | Preparation method for alkyl ketene dimmer (AKD) neutral/alkali sizing agent with high reactivity |
| CN102660904B (en) * | 2012-05-04 | 2014-01-29 | 陕西科技大学 | Preparation method for amphiprotic potato starch microcrystalline wax/AKD (Alkyl Ketene dimer) neutral/alkaline sizing agent |
| CN102660903B (en) * | 2012-05-04 | 2014-07-02 | 陕西科技大学 | Preparation method for soap-free polymer anionic alkyl ketene dimer (AKD) neutral/alkaline sizing agent |
| CN106381760A (en) * | 2016-09-16 | 2017-02-08 | 武汉市知富企业管理咨询有限公司 | Modified AKD (alkyl ketene dimer) neutral sizing agent production technique and application thereof in internal sizing |
| CN106543358A (en) * | 2016-11-03 | 2017-03-29 | 青岛科技大学 | A kind of anion liquid AKD neutral sizing agents and preparation method thereof |
| CN106543358B (en) * | 2016-11-03 | 2019-07-05 | 青岛科技大学 | A kind of anion liquid AKD neutral sizing agent and preparation method thereof |
| JP2019099991A (en) * | 2017-11-30 | 2019-06-24 | 東邦化学工業株式会社 | Ketene dimer based emulsion sizing agent and method for producing paper |
| JP7154705B2 (en) | 2017-11-30 | 2022-10-18 | 東邦化学工業株式会社 | Ketene dimer emulsion sizing agent and paper manufacturing method |
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