CN103087252B - Preparation method of high-absorption composite - Google Patents
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Abstract
本发明公开了一种高吸水性复合材料的制备方法，包括以下的步骤：1）将丙烯酰胺单体、高分子表面活性剂、水、埃洛石进行充分的混合，过滤，得到改性埃洛石；2）将丙烯酸制成质量浓度为50-60%的水溶液，加入吸附剂，混合均匀，过滤去除阻聚剂，滤液用氢氧化钠进行中和，得到丙烯酸中和液；3）室温下，在上步得到的丙烯酸中和液中加入丙烯酰胺单体、改性埃洛石、交联剂、引发剂，充分混合，在将混合物升温到70-85℃进行充分反应，得到凝胶，再将凝胶干燥、破碎、粉碎、过筛即可。与不加埃洛石所制备的高吸水性材料比较，本发明所制备的高吸水性复合材料不仅吸收速度、保水量和加压吸收量明显提高，可满足卫生材料要求，同时，干燥时间也明显缩短。The invention discloses a preparation method of a superabsorbent composite material, which comprises the following steps: 1) fully mixing acrylamide monomer, polymer surfactant, water and halloysite, and filtering to obtain modified angstrom Luoshi; 2) Make acrylic acid into an aqueous solution with a mass concentration of 50-60%, add an adsorbent, mix well, filter to remove the polymerization inhibitor, and neutralize the filtrate with sodium hydroxide to obtain acrylic acid neutralization solution; 3) Room temperature Next, add acrylamide monomer, modified halloysite, crosslinking agent, and initiator to the acrylic acid neutralization solution obtained in the previous step, mix thoroughly, and heat the mixture to 70-85°C for sufficient reaction to obtain a gel , and then the gel is dried, crushed, pulverized and sieved. Compared with the superabsorbent material prepared without halloysite, the superabsorbent composite material prepared by the present invention not only significantly improves the absorption speed, water retention capacity and pressure absorption capacity, but also can meet the requirements of hygienic materials. At the same time, the drying time is also shorter. Significantly shortened.
Description
技术领域 technical field
本发明涉及一种高吸水性复合材料的制备方法。 The invention relates to a preparation method of a superabsorbent composite material.
背景技术 Background technique
高吸水性材料主要是指高分子高吸水性树脂，是指具有亲水性但不溶于水的聚合物交联网络吸收自身重量数倍乃至数百倍上千倍的水形成的多相凝胶体系，广泛应用于妇女卫生巾、婴儿纸尿裤等卫生材料、抗旱保水、农林园艺、生物医用等领域，随着科技水平的日新月异和人们生活水平的不断提高，其应用领域正在不断扩大，逐渐渗透到工业生产和人们生活的各个领域。高吸水性材料按组成主要种类有聚丙烯酸及其共聚高吸水性材料、聚丙烯酰胺及其共聚高吸水性材料、纤维素或淀粉接枝高吸水性材料、聚乙烯醇高吸水性材料等，不同制备方法、不同组成的高吸水性材料在性能、应用领域等方面也有所差别。 Superabsorbent materials mainly refer to high-molecular superabsorbent resins, which refer to the multi-phase gel formed by the cross-linked network of polymers that are hydrophilic but insoluble in water absorb several times or even hundreds of times or thousands of times their own weight. system, widely used in women's sanitary napkins, baby diapers and other sanitary materials, drought resistance and water retention, agriculture, forestry and gardening, biomedical and other fields. All fields of industrial production and people's life. The main types of superabsorbent materials are polyacrylic acid and its copolymerized superabsorbent materials, polyacrylamide and its copolymerized superabsorbent materials, cellulose or starch grafted superabsorbent materials, polyvinyl alcohol superabsorbent materials, etc. Superabsorbent materials with different preparation methods and different compositions are also different in performance and application fields.
应用于卫生材料的高吸水性材料由于其直接与人体接触，考虑到对人体皮肤以及器官的影响，在生物相容性、吸收速度、加压吸收量等方面具有较高的要求。目前应用于卫生材料的高吸水性材料主要为丙烯酸及其共聚物高吸水性材料，采用的制备方法主要由反相悬浮法和溶液聚合法，反相悬浮法由于存在需要使用有机溶剂、生产工艺复杂、难以实现连续化生产等缺点难以普及，目前大多采用溶液聚合法，但溶液聚合法所得到产品的性能难以与反相悬浮法产品相比，特别是卫生材料所要求的吸收速度、保水量和加压吸水量往往需要经过后处理才能满足要求。另外，溶液聚合法制备的聚丙烯酸树脂的干燥也是一大技术难题。 Due to its direct contact with the human body, the superabsorbent material used in hygienic materials has high requirements in terms of biocompatibility, absorption speed, and pressure absorption capacity, considering the impact on human skin and organs. At present, the superabsorbent materials used in hygienic materials are mainly acrylic acid and its copolymer superabsorbent materials. The preparation methods used are mainly reversed phase suspension method and solution polymerization method. The reversed phase suspension method requires the use of organic solvents and production processes due to the existence of Complicated, difficult to achieve continuous production and other shortcomings are difficult to popularize. At present, solution polymerization method is mostly used, but the performance of products obtained by solution polymerization method is difficult to compare with the products of reverse phase suspension method, especially the absorption speed and water retention required by hygienic materials. And pressurized water absorption often needs to be post-treated to meet the requirements. In addition, the drying of the polyacrylic acid resin prepared by the solution polymerization method is also a major technical problem.
发明内容 Contents of the invention
本发明的目的是提供一种高吸水性复合材料的制备方法。 The purpose of the present invention is to provide a method for preparing a superabsorbent composite material.
本发明所采取的技术方案是： The technical scheme that the present invention takes is:
一种高吸水性复合材料的制备方法，包括以下的步骤： A method for preparing a superabsorbent composite material, comprising the following steps:
1）将丙烯酰胺单体、高分子表面活性剂、水、埃洛石进行充分的混合，过滤，得到改性埃洛石； 1) Fully mix acrylamide monomer, polymer surfactant, water, and halloysite, and filter to obtain modified halloysite;
2）将丙烯酸单体制成质量浓度为50-60%的水溶液，加入丙烯酸单体质量1%的吸附剂，混合均匀，过滤去除阻聚剂，滤液用氢氧化钠进行中和，得到丙烯酸中和液； 2) Make acrylic acid monomer into an aqueous solution with a mass concentration of 50-60%, add an adsorbent with 1% mass of acrylic acid monomer, mix well, filter to remove the polymerization inhibitor, and neutralize the filtrate with sodium hydroxide to obtain acrylic acid and liquid;
3）室温下，在上步得到的丙烯酸中和液中加入丙烯酰胺单体、改性埃洛石、交联剂、引发剂，充分混合，在将混合物升温到70-85℃进行充分反应，得到凝胶，再将凝胶于120-140℃下干燥至恒重、破碎、粉碎、过筛即可； 3) At room temperature, add acrylamide monomer, modified halloysite, crosslinking agent, and initiator to the acrylic acid neutralization solution obtained in the previous step, mix well, and heat the mixture to 70-85°C for full reaction. Obtain the gel, then dry the gel at 120-140°C to constant weight, crush, pulverize, and sieve;
步骤1）中，丙烯酰胺单体的质量为埃洛石质量的5%-10%，高分子表面活性剂的质量为埃洛石质量的0.1%-0.5%，水的用量为埃洛石质量的500%-2000%； In step 1), the mass of the acrylamide monomer is 5%-10% of the mass of halloysite, the mass of the polymer surfactant is 0.1%-0.5% of the mass of halloysite, and the amount of water is the mass of halloysite 500%-2000%;
步骤2）中，氢氧化钠与丙烯酸单体的物质的量之比为0.6-0.8； In step 2), the ratio of sodium hydroxide to the amount of acrylic acid monomer is 0.6-0.8;
步骤3）中，丙烯酰胺单体的用量为步骤2）中丙烯酸单体质量的10%-30%，改性埃洛石的用量为步骤2）中丙烯酸单体质量的1~6%，交联剂的用量为步骤2）中丙烯酸单体质量的0.2%-1%，引发剂用量为步骤2）中丙烯酸单体质量的0.1%-0.5%。 In step 3), the amount of acrylamide monomer is 10%-30% of the mass of acrylic acid monomer in step 2), and the amount of modified halloysite is 1-6% of the mass of acrylic monomer in step 2). The dosage of the coupling agent is 0.2%-1% of the mass of the acrylic monomer in step 2), and the dosage of the initiator is 0.1%-0.5% of the mass of the acrylic monomer in the step 2).
所述的高分子表面活性剂为聚乙烯吡咯烷酮PVPK12、聚乙烯吡咯烷酮PVPK15、聚乙二醇PEG400、聚乙二醇PEG600中的一种。 The polymer surfactant is one of polyvinylpyrrolidone PVPK12, polyvinylpyrrolidone PVPK15, polyethylene glycol PEG400, polyethylene glycol PEG600.
所述的吸附剂为气相白炭黑或者活性炭。 The adsorbent is fumed white carbon black or activated carbon.
所述的交联剂为N，N，-亚甲基双丙烯酰胺、N，N，-二烯丙基酒石酸二酰胺、二丙烯酸乙二醇酯的一种。 The crosslinking agent is one of N,N,-methylenebisacrylamide, N,N,-diallyltartaric acid diamide, and ethylene glycol diacrylate.
所述的引发剂为过氧化苯甲酰、偶氮二异丁腈、过硫酸钾中的一种。 The initiator is one of benzoyl peroxide, azobisisobutyronitrile and potassium persulfate.
所述的埃洛石的白度大于90。 The whiteness of the halloysite is greater than 90.
本发明的有益效果是：本发明采用反应性单体丙烯酰胺与高分子表面活性剂对埃洛石进行表面包覆改性得到改性埃洛石，进而通过在丙烯酸、丙烯酰胺单体交联共聚的过程中实现改性埃洛石与聚合物的反应性复合，最终制备出高吸水性复合材料。 The beneficial effects of the present invention are: the present invention uses reactive monomer acrylamide and polymer surfactant to modify the surface of halloysite to obtain modified halloysite; In the process of copolymerization, the reactive composite of the modified halloysite and the polymer is realized, and finally a superabsorbent composite material is prepared.
与不加埃洛石所制备的高吸水性材料比较，所制备的高吸水性复合材料不仅吸收速度、保水量和加压吸收量明显提高，可满足卫生材料要求，同时，干燥时间也明显缩短。 Compared with the superabsorbent material prepared without halloysite, the prepared superabsorbent composite material not only significantly improves the absorption speed, water retention and pressure absorption, which can meet the requirements of hygienic materials, but also significantly shortens the drying time .
具体实施方式 Detailed ways
下面结合具体实施例对本发明做进一步的说明： The present invention will be further described below in conjunction with specific embodiment:
实施例1：Example 1:
（1）将丙烯酰胺单体、高分子表面活性剂溶解于蒸馏水中，搅拌均匀，然后加入高白埃洛石（白度大于90），在30℃下搅拌2小时，过滤，得到改性埃洛石。 (1) Dissolve acrylamide monomer and polymer surfactant in distilled water, stir evenly, then add high white halloysite (whiteness greater than 90), stir at 30°C for 2 hours, filter to obtain modified angstrom Luoshi.
其中，丙烯酰胺单体为埃洛石质量的6%，高分子表面活性剂为聚乙烯吡咯烷酮（PVPK15），用量为埃洛石质量的0.2%，蒸馏水用量为埃洛石质量的1000%。 Among them, the acrylamide monomer is 6% of the halloysite mass, the polymer surfactant is polyvinylpyrrolidone (PVPK15), the dosage is 0.2% of the halloysite mass, and the distilled water consumption is 1000% of the halloysite mass.
（2）将丙烯酸溶解于蒸馏水中，制成质量浓度为60%的丙烯酸溶液，按丙烯酸单体质量的1%加入活性炭，在室温下搅拌0.5小时，过滤除去其中的阻聚剂。在余下滤液中加入氢氧化钠进行中和，得到丙烯酸中和液， (2) Dissolve acrylic acid in distilled water to make an acrylic acid solution with a mass concentration of 60%, add activated carbon according to 1% of the mass of acrylic acid monomer, stir at room temperature for 0.5 hours, and filter to remove the polymerization inhibitor. Sodium hydroxide is added in remaining filtrate and neutralized, obtains acrylic acid neutralized liquid,
其中，氢氧化钠与丙烯酸单体的物质的量之比为0.8； Wherein, the ratio of the amount of substance of sodium hydroxide and acrylic acid monomer is 0.8;
（3）在上述丙烯酸中和液中加入丙烯酰胺单体、改性埃洛石、交联剂、引发剂，现在常温下搅拌0.5小时得到反应液，然后将反应液转移到聚四氟乙烯反应盘中，在75℃下反应0.5小时得到凝胶，在120℃下干燥至恒重，经破碎、粉碎、过筛，得到粒径40~80目的高吸水性复合材料产品。 (3) Add acrylamide monomer, modified halloysite, cross-linking agent and initiator to the above-mentioned acrylic acid neutralization solution, and stir at room temperature for 0.5 hours to obtain a reaction solution, and then transfer the reaction solution to polytetrafluoroethylene for reaction In a tray, react at 75°C for 0.5 hours to obtain a gel, dry at 120°C to constant weight, crush, pulverize, and sieve to obtain a superabsorbent composite material product with a particle size of 40-80 mesh.
步骤（3）中，丙烯酰胺单体的用量为步骤（2）中丙烯酸单体质量的10%，改性埃洛石的用量为步骤（2）中丙烯酸单体质量的6%，交联剂为二丙烯酸乙二醇酯，用量为步骤（2）中丙烯酸单体质量的0.3%，引发剂为过氧化苯甲酰，用量为步骤（2）中丙烯酸单体质量的0.2%。 In step (3), the amount of acrylamide monomer is 10% of the mass of acrylic monomer in step (2), the amount of modified halloysite is 6% of the mass of acrylic monomer in step (2), and the crosslinking agent It is ethylene glycol diacrylate, and the dosage is 0.3% of the mass of the acrylic monomer in step (2), and the initiator is benzoyl peroxide, and the dosage is 0.2% of the mass of the acrylic monomer in the step (2).
比较实施例1：Comparative Example 1:
不加改性埃洛石，其余步骤同实施例1（即只需采用步骤（2）、（3），步骤（3）中不用改性埃洛石）。 Modified halloysite is not added, and the remaining steps are the same as in Example 1 (that is, only steps (2) and (3) are used, and no modified halloysite is used in step (3).
实施例2：Example 2:
（1）将丙烯酰胺单体、高分子表面活性剂溶解于蒸馏水中，搅拌均匀，然后加入高白埃洛石（白度大于90），在50℃下搅拌1小时，过滤，得到改性埃洛石。 (1) Dissolve acrylamide monomer and polymer surfactant in distilled water, stir evenly, then add high white halloysite (whiteness greater than 90), stir at 50°C for 1 hour, filter to obtain modified angstrom Luoshi.
其中，丙烯酰胺单体为埃洛石质量的10%，高分子表面活性剂为聚乙二醇（PEG600），用量为埃洛石质量的0.5%，蒸馏水用量为埃洛石质量的2000%。 Among them, the acrylamide monomer is 10% of the halloysite mass, the polymer surfactant is polyethylene glycol (PEG600), the dosage is 0.5% of the halloysite mass, and the distilled water consumption is 2000% of the halloysite mass.
（2）将丙烯酸溶解于蒸馏水中，制成质量浓度为50%的丙烯酸溶液，按丙烯酸单体质量的1%加入气相白炭黑，在室温下搅拌0.5小时，过滤除去其中的阻聚剂。在余下清液中加入氢氧化钠进行中和，得到丙烯酸中和液， (2) Dissolve acrylic acid in distilled water to make an acrylic acid solution with a mass concentration of 50%, add gas-phase silica according to 1% of the mass of acrylic acid monomer, stir at room temperature for 0.5 hours, and filter to remove the polymerization inhibitor. Add sodium hydroxide to the remaining clear liquid for neutralization to obtain acrylic acid neutralized liquid,
其中，氢氧化钠与丙烯酸单体的物质的量之比为0.7； Wherein, the ratio of the amount of substance of sodium hydroxide and acrylic acid monomer is 0.7;
（3）在上述丙烯酸中和液中加入丙烯酰胺单体、改性埃洛石、交联剂、引发剂，现在常温下搅拌0.5小时得到反应液，然后将反应液转移到聚四氟乙烯反应盘中，在80℃下反应0.5小时得到凝胶，在130℃下干燥至恒重，经破碎、粉碎、过筛，得到粒径40~80目的高吸水性复合材料产品。 (3) Add acrylamide monomer, modified halloysite, cross-linking agent and initiator to the above-mentioned acrylic acid neutralization solution, and stir at room temperature for 0.5 hours to obtain a reaction solution, and then transfer the reaction solution to polytetrafluoroethylene for reaction In a tray, react at 80°C for 0.5 hours to obtain a gel, dry at 130°C to constant weight, crush, pulverize, and sieve to obtain a superabsorbent composite material product with a particle size of 40-80 mesh.
步骤（3）中，丙烯酰胺单体的用量为步骤（2）中丙烯酸单体质量的20%，改性埃洛石的用量为步骤（2）中丙烯酸单体质量的2%，交联剂为N，N，-亚甲基双丙烯酰胺，用量为步骤（2）中丙烯酸单体质量的0.5%，引发剂为偶氮二异丁腈，用量为步骤（2）中丙烯酸单体质量的0.3%。 In step (3), the amount of acrylamide monomer is 20% of the mass of acrylic monomer in step (2), the amount of modified halloysite is 2% of the mass of acrylic monomer in step (2), and the crosslinking agent N,N , -methylenebisacrylamide, the amount is 0.5% of the mass of acrylic acid monomer in step (2), the initiator is azobisisobutyronitrile, and the amount is 0.5% of the mass of acrylic acid monomer in step (2) 0.3%.
比较实施例2：Comparative Example 2:
不加改性埃洛石，其余步骤同实施例2（即只需采用步骤（2）、（3），步骤（3）中不用改性埃洛石）。 Modified halloysite is not added, and the remaining steps are the same as in Example 2 (that is, only steps (2) and (3) are used, and no modified halloysite is used in step (3).
实施例3：Example 3:
（1）将丙烯酰胺单体、高分子表面活性剂溶解于蒸馏水中，搅拌均匀，然后加入管状的优质高白埃洛石（白度大于90），在40℃下搅拌1.5小时，过滤，得到改性埃洛石。 (1) Dissolve acrylamide monomer and polymer surfactant in distilled water, stir evenly, then add tubular high-quality high-white halloysite (whiteness greater than 90), stir at 40°C for 1.5 hours, and filter to obtain Modified Halloysite.
其中，丙烯酰胺单体为埃洛石质量的8%，高分子表面活性剂为聚乙烯吡咯烷酮（PVPK12），用量为埃洛石质量的0.3%，蒸馏水用量为埃洛石质量的1500%。 Among them, the acrylamide monomer is 8% of the halloysite mass, the polymer surfactant is polyvinylpyrrolidone (PVPK12), the dosage is 0.3% of the halloysite mass, and the distilled water consumption is 1500% of the halloysite mass.
（2）将丙烯酸溶解于蒸馏水中，制成质量浓度为55%的丙烯酸溶液，按丙烯酸单体质量的1%加入活性炭，在室温下搅拌0.5小时，过滤除去其中的阻聚剂。在余下清液中加入氢氧化钠进行中和，得到丙烯酸中和液， (2) Dissolve acrylic acid in distilled water to make an acrylic acid solution with a mass concentration of 55%, add activated carbon according to 1% of the mass of acrylic acid monomer, stir at room temperature for 0.5 hours, and filter to remove the polymerization inhibitor. Add sodium hydroxide to the remaining clear liquid for neutralization to obtain acrylic acid neutralized liquid,
其中，氢氧化钠与丙烯酸单体的物质的量之比为0.6； Wherein, the ratio of the amount of substance of sodium hydroxide and acrylic acid monomer is 0.6;
（3）在上述丙烯酸中和液中加入丙烯酰胺单体、改性埃洛石、交联剂、引发剂，现在常温下搅拌0.5小时得到反应液，然后将反应液转移到聚四氟乙烯反应盘中，在70℃下反应0.5小时得到凝胶，在140℃下干燥至恒重，经破碎、粉碎、过筛，得到粒径40~80目的高吸水性复合材料产品。 (3) Add acrylamide monomer, modified halloysite, cross-linking agent and initiator to the above-mentioned acrylic acid neutralization solution, and stir at room temperature for 0.5 hours to obtain a reaction solution, and then transfer the reaction solution to polytetrafluoroethylene for reaction In a tray, react at 70°C for 0.5 hours to obtain a gel, dry at 140°C to constant weight, crush, pulverize, and sieve to obtain a superabsorbent composite material product with a particle size of 40-80 mesh.
步骤（3）中，丙烯酰胺单体的用量为步骤（2）中丙烯酸单体质量的30%，改性埃洛石的量为步骤（2）中丙烯酸单体质量的4%，交联剂为N，N，-二烯丙基酒石酸二酰胺，用量为步骤（2）中丙烯酸单体质量的0.8%，引发剂为过硫酸钾，用量为步骤（2）中丙烯酸单体质量的0.5%。 In step (3), the amount of acrylamide monomer is 30% of the mass of acrylic monomer in step (2), the amount of modified halloysite is 4% of the mass of acrylic monomer in step (2), and the crosslinking agent N,N , -diallyltartaric acid diamide, the dosage is 0.8% of the mass of the acrylic monomer in step (2), the initiator is potassium persulfate, and the dosage is 0.5% of the mass of the acrylic monomer in the step (2) .
比较实施例3：Comparative Example 3:
不加改性埃洛石，其余步骤同实施例3（即只需采用步骤（2）、（3），步骤（3）中不用改性埃洛石）。 Modified halloysite is not added, and the remaining steps are the same as in Example 3 (that is, only steps (2) and (3) are used, and no modified halloysite is used in step (3).
上述实施例与比较实施例的性能测试结果如表1： The performance test result of above-mentioned embodiment and comparative embodiment is as table 1:
表1：实施例与比较实施例的效果Table 1: Effects of Examples and Comparative Examples
说明：illustrate:
本发明的性能测试方法如下：Performance testing method of the present invention is as follows:
吸去离子水倍数（g/g）：参照《中华人民共和国农业行业标准》（NY886-2004）。 Absorption of deionized water multiples (g/g): Refer to "Agricultural Industry Standards of the People's Republic of China" (NY886-2004).
吸收量（g/g）：参照《中华人民共和国国家标准》（GB/T22905-2008）。 Absorption (g/g): refer to "National Standard of the People's Republic of China" (GB/T22905-2008).
保水量（g/g）：参照《中华人民共和国国家标准》（GB/T22905-2008）。 Water retention (g/g): refer to "National Standard of the People's Republic of China" (GB/T22905-2008).
加压吸收量（g/g）：参照《中华人民共和国国家标准》（GB/T22905-2008）。 Absorption under pressure (g/g): refer to "National Standard of the People's Republic of China" (GB/T22905-2008).
吸收速度（s）：参照《中华人民共和国国家标准》（GB/T22875-2008）。 Absorption speed (s): refer to "National Standard of the People's Republic of China" (GB/T22875-2008).
效果分析：Effectiveness analysis:
从上述实施例的结果可以看出，与不加埃洛石所制备的聚丙烯酸系高吸水性材料比较，本发明方法所制备的高吸水性复合材料吸去离子水倍数有所降低，但对于卫生材料的使用无明显影响。虽然吸收量有所降低，但保水量、吸收速度和加压吸收量明显提高，可满足卫生材料要求，同时，干燥时间明显缩短，可提高生产效率、降低生产成本。 As can be seen from the results of the above examples, compared with the polyacrylic acid superabsorbent material prepared without halloysite, the deionized water absorption ratio of the superabsorbent composite material prepared by the method of the present invention is reduced, but for The use of hygienic materials had no significant effect. Although the absorption is reduced, the water retention, absorption speed and pressure absorption are significantly improved, which can meet the requirements of hygienic materials. At the same time, the drying time is significantly shortened, which can improve production efficiency and reduce production costs.
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