WO2021237379A1 - 阳离子聚丙烯酰胺絮凝剂的制备方法 - Google Patents
阳离子聚丙烯酰胺絮凝剂的制备方法 Download PDFInfo
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- WO2021237379A1 WO2021237379A1 PCT/CN2020/091947 CN2020091947W WO2021237379A1 WO 2021237379 A1 WO2021237379 A1 WO 2021237379A1 CN 2020091947 W CN2020091947 W CN 2020091947W WO 2021237379 A1 WO2021237379 A1 WO 2021237379A1
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- cationic polyacrylamide
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- 125000002091 cationic group Chemical group 0.000 title claims abstract description 13
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 235000010262 sodium metabisulphite Nutrition 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 abstract description 8
- 238000002791 soaking Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 7
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Definitions
- the invention relates to a preparation method of a cationic polyacrylamide flocculant.
- Oilfield operation wastewater contains pollutants such as oil, ammonia, sulfur, arsenic, and volatile phenols. It has the characteristics of complex pollution components, high concentration, large changes and difficult to dissolve.
- pollutants such as oil, ammonia, sulfur, arsenic, and volatile phenols. It has the characteristics of complex pollution components, high concentration, large changes and difficult to dissolve.
- the problems caused by wastewater from oilfield operations have become an important factor restricting the sustainable development of society and economy. Effective treatment of a large amount of oil field wastewater discharged to meet discharge standards and utilization requirements is an extremely important way to increase the utilization rate of water resources, and it is also a necessary measure to protect the ecological environment and human survival and promote social progress.
- cationic polyacrylamide Because cationic polyacrylamide has the advantages of high positive charge density, good water solubility, and easy control of relative molecular weight, it is currently widely used in oilfield wastewater treatment and other fields, but imported products are mostly used and the price is relatively high. Therefore, the research and development of oilfield wastewater flocculants with excellent performance is conducive to reducing treatment costs and improving treatment effects, and has good application prospects. Since acryloxyethyl trimethyl ammonium chloride (DAC) has one less hydrophobic -CH 3 branch than methacryloxy ethyl trimethyl ammonium chloride (DMC), it is a copolymer flocculant with AM It has better hydrophilicity and flexibility, which is conducive to the improvement of solubility and flocculation effect.
- DAC acryloxyethyl trimethyl ammonium chloride
- DMC methacryloxy ethyl trimethyl ammonium chloride
- acrylamide (AM) and acryloxyethyltrimethylammonium chloride (DAC) copolymer flocculants More research.
- domestic and foreign researchers mainly use a single initiator, which has more or less defects.
- inorganic initiators are prone to chain transfer, and organic initiators have high decomposition temperatures, resulting in low molecular weight and poor stability of the synthesized products.
- the purpose of the present invention is to provide a method for preparing cationic polyacrylamide flocculant.
- a preparation method of cationic polyacrylamide flocculant including the following steps: add 25-35 parts of DAC aqueous solution with a mass fraction of 80%, 10-20 parts of AM and 60- to a four-necked flask equipped with a stirrer and a thermometer.
- the water bath is heated to 56°C.
- the nitrogen gas is continued for 3 hours.
- the closed polymerization reaction is 9h.
- the white solid is dried in a vacuum drying oven at 55° C. for 6 hours.
- the prepared cationic polyacrylamide flocculant has a high removal rate of wastewater turbidity, and can be prepared on a large scale.
- a preparation method of cationic polyacrylamide flocculant including the following steps: add 30 parts of 80% DAC aqueous solution, 15 parts of AM and 65 parts of distilled water into a four-necked flask equipped with a stirrer and a thermometer, and mix them evenly , Blow in nitrogen to exhaust the air in the system, heat the water bath to 56°C, add 3 parts of initiator tert-butyl hydroperoxide and 2 parts of sodium metabisulfite, continue to flow nitrogen for 3h, close the polymerization reaction for 9h, take out the colloid, soak in acetone 26h, then soak in absolute ethanol for 26h, dry the white solid in a vacuum drying oven at 55°C for 6h, dry and pulverize to obtain; all raw materials are parts by weight.
- a preparation method of cationic polyacrylamide flocculant includes the following steps: add 25 parts of 80% DAC aqueous solution, 10 parts of AM and 60 parts of distilled water into a four-necked flask equipped with a stirrer and a thermometer, and mix them evenly , Blow in nitrogen to exhaust the air in the system, heat the water bath to 54°C, add 2 parts of initiator tert-butyl hydroperoxide and 1 part of sodium metabisulfite, continue to flow nitrogen for 2h, seal the polymerization reaction for 8h, take out the colloid, soak in acetone After 25h, soak in absolute ethanol for 25h, dry the white solid in a vacuum drying oven at 50°C for 5h, dry and pulverize, and get it; all raw materials are parts by weight.
- a preparation method of cationic polyacrylamide flocculant including the following steps: add 35 parts of 80% DAC aqueous solution, 20 parts of AM and 70 parts of distilled water into a four-necked flask equipped with a stirrer and a thermometer, and mix them evenly , Blow in nitrogen gas to exhaust the air in the system, heat in a water bath to raise the temperature to 58°C, add 4 parts of initiator tert-butyl hydroperoxide and 3 parts of sodium metabisulfite, continue to bubbling with nitrogen for 4 hours, and after 10 hours of airtight polymerization, take out the colloid and soak in acetone 27h, then soak in absolute ethanol for 27h, dry the white solid in a vacuum drying oven at 60°C for 7h, dry and pulverize to obtain; each raw material is part by weight.
- the prepared cationic polyacrylamide flocculant has a high removal rate of wastewater turbidity, and can be prepared on a large scale.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
一种阳离子聚丙烯酰胺絮凝剂的制备方法，步骤如下：在装有搅拌器、温度计的四口烧瓶中加入质量分数为80％的DAC水溶液、AM和蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至54-58℃，加入引发剂叔丁基过氧化氢和焦亚硫酸钠，继续通氮气2-4h，密闭聚合反应8-10h后取出胶体，用丙酮浸泡25-27h，再用无水乙醇浸泡25-27h，将白色固体于50-60℃真空干燥箱中干燥5-7h，烘干粉碎，即得。该方法简便、快捷、易操作，制备的阳离子聚丙烯酰胺絮凝剂对废水浊度去除率高，可大规模制备。
Description
本发明涉及一种阳离子聚丙烯酰胺絮凝剂的制备方法。
近年来，随着油田开采力度越来越大，各种作业废水的排放量急剧增加。油田作业废水含有油、氨、硫、砷和挥发酚等污染物，具有污染成份复杂、浓度高、变化大且难以溶解等特点。油田作业废水所产生的问题已成为制约社会经济可持续发展的重要因素。对于大量排放的油田废水进行有效处理，达到排放标准和利用要求，是增加水资源利用率的极为重要的途径，也是保护生态环境与人类生存、促进社会进步的必要措施。由于阳离子聚丙烯酰胺具有正电荷密度高、水溶性好、相对分子质量易控制等优点，目前在油田废水处理等领域得到广泛应用，但多采用进口产品，价格较高。因此研究和开发性能优异的油田废水絮凝剂，有利于降低处理成本和提高处理效果，具有良好的应用前景。由于丙烯酰氧乙基三甲基氯化铵(DAC)比甲基丙烯酰氧乙基三甲基氯化铵(DMC)少一个疏水的-CH
3支链，其与AM的共聚物絮凝剂具有更好的亲水性和柔顺性，有利于溶解性和絮凝效果的提高，因此国内外关于丙烯酰胺(AM)和丙烯酰氧乙基三甲基氯化铵(DAC)共聚物絮凝剂的研究较多。但是国内外研究者主要采用的是单一的引发剂，或多或少存在一些缺陷，例如无机引发剂易发生链转移，有机引发剂分解温度高，使合成的产物分子质量低、稳定性差。
发明内容
本发明的目的在于提供一种阳离子聚丙烯酰胺絮凝剂的制备方法。
本发明通过下面技术方案实现：
一种阳离子聚丙烯酰胺絮凝剂的制备方法，包括如下步骤：在装有搅拌器、温度计的四口烧瓶中加入25-35份质量分数为80％的DAC水溶液、10-20份AM和60-70份蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至54-58℃，加入2-4份引发剂叔丁基过氧化氢和1-3份焦亚硫酸钠，继续通氮气2-4h，密闭聚合反应8-10h后取出胶体，用丙酮浸泡25-27h，再用无水乙醇浸泡25-27h，将白色固体于50-60℃真空干燥箱中干燥5-7h，烘干粉碎，即得；各原料均为重量份。
优选地，所述的制备方法中，水浴加热升温至56℃。
优选地，所述的制备方法中，继续通氮气3h。
优选地，所述的制备方法中，密闭聚合反应9h。
优选地，所述的制备方法中，用丙酮浸泡26h，再用无水乙醇浸泡26h。
优选地，所述的制备方法中，将白色固体于55℃真空干燥箱中干燥6h。
本发明技术效果：
该方法简便、快捷、易操作，制备的阳离子聚丙烯酰胺絮凝剂对废水浊度去除率高，可大规模制备。
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种阳离子聚丙烯酰胺絮凝剂的制备方法，包括如下步骤：在装有搅拌器、温度计的四口烧瓶中加入30份质量分数为80％的DAC水溶液、15份AM和65份蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至56℃，加入3份引发剂叔丁基过氧化氢和2份焦亚硫酸钠，继续通氮气3h，密闭聚合反应9h后取出胶体，用丙酮浸泡26h，再用无水乙醇浸泡26h，将白色固体于55℃真空干燥箱中干燥6h，烘干粉碎，即得；各原料均为重量份。
实施例2
一种阳离子聚丙烯酰胺絮凝剂的制备方法，包括如下步骤：在装有搅拌器、温度计的四口烧瓶中加入25份质量分数为80％的DAC水溶液、10份AM和60份蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至54℃，加入2份引发剂叔丁基过氧化氢和1份焦亚硫酸钠，继续通氮气2h，密闭聚合反应8h后取出胶体，用丙酮浸泡25h，再用无水乙醇浸泡25h，将白色固体于50℃真空干燥箱中干燥5h，烘干粉碎，即得；各原料均为重量份。
实施例3
一种阳离子聚丙烯酰胺絮凝剂的制备方法，包括如下步骤：在装有搅拌器、温度计的四口烧瓶中加入35份质量分数为80％的DAC水溶液、20份AM和70份蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至58℃，加入4份引发剂叔丁基过氧化氢和3份焦亚硫酸钠，继续通氮气4h，密闭聚合反应10h后取出胶体，用丙酮浸泡27h，再用无水乙醇浸泡27h，将白色固体于60℃真空干燥箱中干燥7h，烘干粉碎，即得；各原料均为重量份。
该方法简便、快捷、易操作，制备的阳离子聚丙烯酰胺絮凝剂对废水浊度去除率高，可大规模制备。
Claims (6)
- 一种阳离子聚丙烯酰胺絮凝剂的制备方法，其特征在于包括如下步骤：在装有搅拌器、温度计的四口烧瓶中加入25-35份质量分数为80％的DAC水溶液、10-20份AM和60-70份蒸馏水，混合均匀，通入氮气排出体系内的空气，水浴加热升温至54-58℃，加入2-4份引发剂叔丁基过氧化氢和1-3份焦亚硫酸钠，继续通氮气2-4h，密闭聚合反应8-10h后取出胶体，用丙酮浸泡25-27h，再用无水乙醇浸泡25-27h，将白色固体于50-60℃真空干燥箱中干燥5-7h，烘干粉碎，即得；各原料均为重量份。
- 根据权利要求1所述的制备方法，其特征在于：水浴加热升温至56℃。
- 根据权利要求1所述的制备方法，其特征在于：继续通氮气3h。
- 根据权利要求1所述的制备方法，其特征在于：密闭聚合反应9h。
- 根据权利要求1所述的制备方法，其特征在于：用丙酮浸泡26h，再用无水乙醇浸泡26h。
- 根据权利要求1所述的制备方法，其特征在于：将白色固体于55℃真空干燥箱中干燥6h。
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| CN114751499A (zh) * | 2022-06-16 | 2022-07-15 | 山东艾维斯特精细化工有限公司 | 处理染料废水用复合絮凝剂及其制备方法和应用 |
| CN114805688A (zh) * | 2022-05-25 | 2022-07-29 | 重庆交通大学 | 一种改性絮凝剂及其制备方法和应用 |
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