CN100570055C - Preparation method of cationic polyacrylamide papermaking strengthening agent - Google Patents
Preparation method of cationic polyacrylamide papermaking strengthening agent Download PDFInfo
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- CN100570055C CN100570055C CNB2007100176776A CN200710017677A CN100570055C CN 100570055 C CN100570055 C CN 100570055C CN B2007100176776 A CNB2007100176776 A CN B2007100176776A CN 200710017677 A CN200710017677 A CN 200710017677A CN 100570055 C CN100570055 C CN 100570055C
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- 125000002091 cationic group Chemical group 0.000 title claims abstract description 23
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 13
- 238000005728 strengthening Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 9
- -1 polyoxyethylene Polymers 0.000 claims abstract description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 239000005977 Ethylene Substances 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 150000003141 primary amines Chemical class 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 11
- 239000007787 solid Substances 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229920001577 copolymer Polymers 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000002612 dispersion medium Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000005191 phase separation Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 4
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 4
- WKXGVFOESMDKRF-UHFFFAOYSA-L dipotassium;bromate;bromide Chemical compound [K+].[K+].[Br-].[O-]Br(=O)=O WKXGVFOESMDKRF-UHFFFAOYSA-L 0.000 description 3
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 2
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 description 2
- 238000012673 precipitation polymerization Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- GSQZCNGOIFGRPU-UHFFFAOYSA-M [Cl-].C(C=C)(=O)C(C1=CC=CC=C1)([N+](C)(C)C)CC Chemical compound [Cl-].C(C=C)(=O)C(C1=CC=CC=C1)([N+](C)(C)C)CC GSQZCNGOIFGRPU-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000012688 inverse emulsion polymerization Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
阳离子聚丙烯酰胺造纸增强剂的制备方法，首先将丙烯酰胺单体与聚氧化乙烯混合，然后加入水、阳离子单体和水溶性引发剂发生聚合反应即可。由于本发明使丙烯酰胺单体和阳离子单体共聚物溶解在聚氧化乙烯溶液中，通过聚合物与分散介质的相互作用，体系发生相分离，从而提高聚合物分子量和固含量，降低体系黏度，同时聚丙烯酰胺共聚物也拥有良好的溶解性，能够迅速溶解在水中，聚氧化乙烯同时对造纸纤维具有良好的分散作用，加入聚氧化乙烯可使生产纸张均匀度提高，和聚丙烯酰胺共聚物一起对纤维纸张的强度起到提高作用。The preparation method of the cationic polyacrylamide paper-making strengthening agent comprises firstly mixing the acrylamide monomer and polyethylene oxide, and then adding water, cationic monomer and water-soluble initiator to carry out polymerization reaction. Since the present invention dissolves the copolymer of acrylamide monomer and cationic monomer in the polyethylene oxide solution, the system undergoes phase separation through the interaction between the polymer and the dispersion medium, thereby increasing the molecular weight and solid content of the polymer and reducing the viscosity of the system. At the same time, polyacrylamide copolymer also has good solubility and can be quickly dissolved in water. Polyethylene oxide also has a good dispersion effect on paper-making fibers. Adding polyoxyethylene can improve the uniformity of paper production, and polyacrylamide copolymer Together, they can improve the strength of fiber paper.
Description
技术领域 technical field
本发明属于纸张增强剂的合成方法，具体涉及一种阳离子聚丙烯酰胺造纸增强剂的制备方法。The invention belongs to a synthesis method of a paper strengthening agent, in particular to a preparation method of a cationic polyacrylamide papermaking strengthening agent.
背景技术 Background technique
聚丙烯酰胺可采用自由基水溶液聚合、反相乳液聚合、沉淀聚合等方法制备，这类聚合物被广泛应用于水处理、造纸等要求产品黏度低可溶性好行业。Polyacrylamide can be prepared by free radical aqueous solution polymerization, inverse emulsion polymerization, precipitation polymerization and other methods. This kind of polymer is widely used in water treatment, papermaking and other industries that require low viscosity and good solubility.
水溶液聚合工艺简单，聚合产率高，对环境污染少，是制备阳离子聚丙烯酰胺的首选方法。它可以通过调节引发体系、介质PH值、添加剂、温度等对聚合物反应过程和产物性能控制。水溶液聚合虽然有很多优点，但也存在很多缺点，难以制备高固含量的高分子量的聚合物。作为纸张增强剂通常要求分子量大于40～100万，以丙烯酰胺为例，通常当分子量超过50万，单体含量超过15％时，体系的黏度将达到50Pa·S反应散热非常困难，容易发生暴聚，而且聚合物水溶性很差。反相乳液、反相悬浮、沉淀聚合等虽能有效解决这些问题。但要大量用到有机溶剂，存在污染及生产成本等问题，而且产物的水溶性比较差，使用起来非常困难。现在市场上出售的阳离子纸张增强剂通常是10％左右的水溶液，固含量低，降解快，流动性差。The aqueous solution polymerization process is simple, the polymerization yield is high, and there is little environmental pollution. It is the preferred method for preparing cationic polyacrylamide. It can control the polymer reaction process and product properties by adjusting the initiation system, medium pH value, additives, temperature, etc. Although aqueous solution polymerization has many advantages, it also has many disadvantages, and it is difficult to prepare high molecular weight polymers with high solid content. As a paper strengthening agent, the molecular weight is usually required to be greater than 400,000 to 1 million. Taking acrylamide as an example, when the molecular weight exceeds 500,000 and the monomer content exceeds 15%, the viscosity of the system will reach 50Pa·S. poly, and the polymer is poorly soluble in water. Inverse emulsion, inverse suspension, precipitation polymerization, etc. can effectively solve these problems. However, a large amount of organic solvents are used, and there are problems such as pollution and production costs, and the water solubility of the product is relatively poor, so it is very difficult to use. The cationic paper strengthening agent sold in the market is usually about 10% aqueous solution, with low solid content, fast degradation and poor fluidity.
发明内容 Contents of the invention
本发明的目的在于克服上述现有技术的缺点，提供了一种能够提高聚合物分子量和固含量，降低体系黏度，同时拥有良好的溶解性，能够迅速溶解在水中的阳离子聚丙烯酰胺造纸增强剂的制备方法。The purpose of the present invention is to overcome the above-mentioned shortcomings of the prior art, and to provide a cationic polyacrylamide paper-making strengthening agent that can increase the molecular weight and solid content of the polymer, reduce the viscosity of the system, and has good solubility and can be quickly dissolved in water. method of preparation.
为达到上述目的，本发明采用的技术方案是：首先将丙烯酰胺单体与聚氧化乙烯按1∶0.5～1∶2的质量比混合，然后加入水使丙烯酰胺单体的含量为10％～25％，再加入丙烯酰胺单体质量10％～30％的阳离子单体和1.5％～10％的水溶性引发剂，在40℃～80℃聚合反应4～8小时即可；In order to achieve the above-mentioned purpose, the technical solution adopted in the present invention is: firstly mix the acrylamide monomer and polyethylene oxide at a mass ratio of 1:0.5 to 1:2, then add water to make the content of the acrylamide monomer be 10% to 10%. 25%, then add 10% to 30% cationic monomer and 1.5% to 10% water-soluble initiator by mass of acrylamide monomer, and polymerize at 40°C to 80°C for 4 to 8 hours;
所说的阳离子单体具有以下结构特征Said cationic monomer has the following structural features
其中R1为氢、甲基或乙基，R2、R3R4同时存在或其中的两个同时存在，R2、R3R4为碳数小于5的短链烃，R5为亚甲基、亚乙基或亚丙基；Wherein R 1 is hydrogen, methyl or ethyl, R 2 , R 3 R 4 or two of them exist at the same time, R 2 , R 3 R 4 are short-chain hydrocarbons with less than 5 carbons, R 5 is ethylene methyl, ethylene or propylene;
所说的水溶性引发剂为水溶性氧化剂或氧化还原体系引发剂：水溶性氧化剂为：过硫酸钾、过硫酸铵或过硫酸钠，氧化还原体系引发剂为：过硫酸盐和亚硫酸盐、过硫酸盐和伯胺或过硫酸盐和叔醇胺组成的氧化还原体系。Said water-soluble initiator is water-soluble oxidant or redox system initiator: water-soluble oxidant is: potassium persulfate, ammonium persulfate or sodium persulfate, and redox system initiator is: persulfate and sulfite, Redox system composed of persulfate and primary amine or persulfate and tertiary alcohol amine.
本发明的丙烯酰胺单体具有以下结构特征：The acrylamide monomer of the present invention has the following structural characteristics:
其中的R为氢、甲基或乙基。Wherein R is hydrogen, methyl or ethyl.
聚氧化乙烯的相对分子质量为10000～50000。The relative molecular mass of polyethylene oxide is 10,000-50,000.
由于本发明使丙烯酰胺单体和阳离子单体共聚物溶解在聚氧化乙烯溶液中，通过聚合物与分散介质的相互作用，体系发生相分离，从而提高聚合物分子量和固含量，降低体系黏度，同时聚丙烯酰胺共聚物也拥有良好的溶解性，能够迅速溶解在水中，聚氧化乙烯同时对造纸纤维具有良好的分散作用，加入聚氧化乙烯可使生产纸张均匀度提高，和聚丙烯酰胺共聚物一起对纤维纸张的强度起到提高作用。Since the present invention dissolves the copolymer of acrylamide monomer and cationic monomer in the polyethylene oxide solution, the system undergoes phase separation through the interaction between the polymer and the dispersion medium, thereby increasing the molecular weight and solid content of the polymer and reducing the viscosity of the system. At the same time, polyacrylamide copolymer also has good solubility and can be quickly dissolved in water. Polyethylene oxide also has a good dispersion effect on paper-making fibers. Adding polyoxyethylene can improve the uniformity of paper production, and polyacrylamide copolymer Together, they can improve the strength of fiber paper.
具体实施方式 Detailed ways
实施例1，首先将丙烯酰胺单体与相对分子质量为20000的聚氧化乙烯按1∶0.5的质量比混合，然后加入水使丙烯酰胺单体的含量为18％，再加入丙烯酰胺单体质量15％的阳离子单体甲基丙烯酸二甲胺乙酯和8％的过硫酸钾在80℃聚合反应4小时即可。Example 1, first mix the acrylamide monomer with polyethylene oxide with a relative molecular weight of 20000 at a mass ratio of 1:0.5, then add water to make the content of the acrylamide monomer 18%, then add the mass of the acrylamide monomer 15% cationic monomer dimethylaminoethyl methacrylate and 8% potassium persulfate are polymerized at 80° C. for 4 hours.
用溴酸钾溴化钾法对产品转化率进行测定，转化率超过98％，用转子粘度计对黏度进行测定，黏度为5Pa·s，远远小于一般的水溶液聚合。The conversion rate of the product was measured by the potassium bromate potassium bromide method, and the conversion rate exceeded 98%. The viscosity was measured by a rotor viscometer, and the viscosity was 5 Pa·s, which was far lower than that of ordinary aqueous solution polymerization.
同时对产品溶解性进行试验，在100g水中加入2g该聚合物乳液，轻轻搅拌，迅速溶解为透明溶液。而用同样量的阳离子丙烯酰胺则需要1小时以上的时间才能完全溶解。At the same time, the solubility of the product was tested, and 2 g of the polymer emulsion was added to 100 g of water, stirred gently, and quickly dissolved into a transparent solution. However, with the same amount of cationic acrylamide, it takes more than 1 hour to completely dissolve.
实施例2：首先将丙烯酰胺单体与相对分子质量为50000的聚氧化乙烯按1∶1.2的质量比混合，然后加入水使丙烯酰胺单体的含量为23％，再加入丙烯酰胺单体质量20％的阳离子单体二甲基二烯丙基氯化铵和5％的过硫酸钠在80℃聚合反应6小时即可。Example 2: First, the acrylamide monomer is mixed with polyethylene oxide with a relative molecular mass of 50,000 at a mass ratio of 1:1.2, then water is added to make the content of the acrylamide monomer 23%, and then the mass of the acrylamide monomer is added 20% cationic monomer dimethyl diallyl ammonium chloride and 5% sodium persulfate are polymerized at 80° C. for 6 hours.
用溴酸钾溴化钾法对产品转化率进行测定，转化率超过97％，用转子粘度计对黏度进行测定，黏度为5.8Pa·s。The conversion rate of the product was measured by the potassium bromate potassium bromide method, and the conversion rate exceeded 97%. The viscosity was measured by a rotor viscometer, and the viscosity was 5.8 Pa·s.
同时对产品溶解性进行试验，在100g水中加入2g该聚合物乳液，轻轻搅拌，迅速溶解为透明溶液。At the same time, the solubility of the product was tested, and 2 g of the polymer emulsion was added to 100 g of water, stirred gently, and quickly dissolved into a transparent solution.
实施例3，首先将丙烯酰胺单体与相对分子质量为10000的聚氧化乙烯按1∶1.7的质量比混合，然后加入水使丙烯酰胺单体的含量为10％，再加入丙烯酰胺单体质量30％的阳离子单体丙烯酰乙基三甲基苄基氯化铵和3％的过硫酸铵在70℃聚合反应7.5小时即可。Example 3, first mix the acrylamide monomer with the polyethylene oxide with a relative molecular weight of 10000 at a mass ratio of 1:1.7, then add water to make the content of the acrylamide monomer 10%, then add the mass of the acrylamide monomer 30% cationic monomer acryloyl ethyl trimethyl benzyl ammonium chloride and 3% ammonium persulfate are polymerized at 70° C. for 7.5 hours.
用溴酸钾溴化钾法对产品转化率进行测定，转化率超过98％，用转子粘度计对黏度进行测定，黏度为7Pa·s。The product conversion rate was measured by the potassium bromate potassium bromide method, and the conversion rate was over 98%. The viscosity was measured by a rotor viscometer, and the viscosity was 7Pa·s.
同时对产品溶解性进行试验，在100g水中加入2g该聚合物乳液，轻轻搅拌，迅速溶解为透明溶液。At the same time, the solubility of the product was tested, and 2 g of the polymer emulsion was added to 100 g of water, stirred gently, and quickly dissolved into a transparent solution.
实施例4，首先将丙烯酰胺单体与相对分子质量为30000的聚氧化乙烯按1∶2的质量比混合，然后加入水使丙烯酰胺单体的含量为15％，再加入丙烯酰胺单体质量30％的阳离子单体丙烯酸二甲胺乙酯，用3％的过硫酸钾和1.5％的伯胺在70℃聚合反应5小时即可。Example 4, first mix the acrylamide monomer with the polyethylene oxide with a relative molecular mass of 30000 at a mass ratio of 1:2, then add water to make the content of the acrylamide monomer 15%, and then add the mass of the acrylamide monomer 30% cationic monomer dimethylaminoethyl acrylate is polymerized with 3% potassium persulfate and 1.5% primary amine at 70° C. for 5 hours.
实施例5，首先将丙烯酰胺单体与相对分子质量为40000的聚氧化乙烯按1∶0.8的质量比混合，然后加入水使丙烯酰胺单体的含量为25％，再加入丙烯酰胺单体质量25％的阳离子单体甲基丙烯酸二甲胺乙酯，用4％的过硫酸铵和3％的叔醇胺在40℃聚合反应8小时即可。Example 5, first mix the acrylamide monomer with the polyethylene oxide with a relative molecular mass of 40000 at a mass ratio of 1:0.8, then add water to make the content of the acrylamide monomer 25%, and then add the mass of the acrylamide monomer 25% cationic monomer dimethylaminoethyl methacrylate is polymerized with 4% ammonium persulfate and 3% tertiary alcohol amine at 40° C. for 8 hours.
实施例6，首先将丙烯酰胺单体与相对分子质量为25000的聚氧化乙烯按1∶1.0的质量比混合，然后加入水使丙烯酰胺单体的含量为20％，再加入丙烯酰胺单体质量10％的阳离子单体丙烯酸二甲胺乙酯，用4％的过硫酸铵和5％的亚硫酸钠在55℃聚合反应6.5小时即可。Example 6, first mix the acrylamide monomer with polyethylene oxide with a relative molecular weight of 25000 at a mass ratio of 1:1.0, then add water to make the content of the acrylamide monomer 20%, and then add the mass of the acrylamide monomer 10% cationic monomer dimethylaminoethyl acrylate is polymerized with 4% ammonium persulfate and 5% sodium sulfite at 55°C for 6.5 hours.
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| CN105085896A (en) * | 2015-07-27 | 2015-11-25 | 天禾化学品（苏州）有限公司 | Preparation method for high-molecular surfactant |
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| WO2020000310A1 (en) * | 2018-06-28 | 2020-01-02 | 江苏富淼科技股份有限公司 | Crosslinking modified type water-soluble solid polyacrylamide and use thereof |
| CN109810240B (en) * | 2019-01-15 | 2021-06-15 | 陕西科技大学 | A kind of preparation method and application of piperidinamine-containing polyurethane fluorescent whitening emulsion |
| CN112553941A (en) * | 2020-11-09 | 2021-03-26 | 山东华泰纸业股份有限公司 | Production process of ink jet printing paper |
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2007
- 2007-04-13 CN CNB2007100176776A patent/CN100570055C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 新型阳离子聚丙烯酰胺微粒的研究---含PEO支链阳离子聚丙烯酰胺微粒的合成、助留性能及作用机理. 彭晓宏，佘娜，沈家瑞.精细与专用化学品，第21期. 2002 * |
| 阳离子有机高分子絮凝剂的研究进展及其应用. 胡瑞，周华，李田霞，陈存华.化工进展，第25卷第6期. 2006 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085896A (en) * | 2015-07-27 | 2015-11-25 | 天禾化学品（苏州）有限公司 | Preparation method for high-molecular surfactant |
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| Publication number | Publication date |
|---|---|
| CN101033592A (en) | 2007-09-12 |
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