CN101531745A - Preparation of plural gel water absorbent material composed of silk fibroin/acrylic acid/acrylamide - Google Patents
Preparation of plural gel water absorbent material composed of silk fibroin/acrylic acid/acrylamide Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 56
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 56
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 108010022355 Fibroins Proteins 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 20
- 239000002250 absorbent Substances 0.000 title claims description 11
- 230000002745 absorbent Effects 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title claims description 5
- 238000003756 stirring Methods 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
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- 238000009835 boiling Methods 0.000 claims description 3
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- 239000012460 protein solution Substances 0.000 claims 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 239000004160 Ammonium persulphate Substances 0.000 claims 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims 1
- 235000019395 ammonium persulphate Nutrition 0.000 claims 1
- 239000001110 calcium chloride Substances 0.000 claims 1
- 235000011148 calcium chloride Nutrition 0.000 claims 1
- 229910001628 calcium chloride Inorganic materials 0.000 claims 1
- 238000004140 cleaning Methods 0.000 claims 1
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- 238000010521 absorption reaction Methods 0.000 description 27
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 7
- 239000000017 hydrogel Substances 0.000 description 6
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- 239000002699 waste material Substances 0.000 description 4
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Abstract
本发明公开了一种制备丝素蛋白/丙烯酸/丙烯酰胺复合凝胶吸水材料的方法，在分析纯丙烯酸溶液中滴加NaOH溶液和丙烯酰胺固体物，搅拌后得到丙烯酸/丙烯酰胺单体的混合溶液；将丝素蛋白溶液水浴加热后加入引发剂过硫酸铵和丙烯酸/丙烯酰胺单体混合液，最后加入交联剂N，N’－二甲基双丙烯酰胺；加热搅拌成凝胶，静置后的凝胶取出，用去离子水水洗后，获得丝素蛋白/丙烯酸/丙烯酰胺复合凝胶吸水材料。本发明的材料既有亲水吸湿性，又具有生物降解性。The invention discloses a method for preparing a silk fibroin/acrylic acid/acrylamide composite gel water-absorbing material. NaOH solution and acrylamide solids are added dropwise to an analytically pure acrylic acid solution, and a mixture of acrylic acid/acrylamide monomers is obtained after stirring. solution; add the initiator ammonium persulfate and acrylic acid/acrylamide monomer mixture after heating the silk fibroin solution in a water bath, and finally add the crosslinking agent N, N'-dimethylbisacrylamide; heat and stir to form a gel, The post-placed gel is taken out and washed with deionized water to obtain the silk fibroin/acrylic acid/acrylamide composite gel water-absorbing material. The material of the invention has both hydrophilic and hygroscopic properties and biodegradability.
Description
技术领域 technical field
本发明涉及丝素蛋白的加工利用领域，特别涉及一种吸水保水用途的丝素蛋白/丙烯酸/丙烯酰胺复合凝胶吸水材料的制备方法。The invention relates to the field of processing and utilization of silk fibroin, in particular to a preparation method of a silk fibroin/acrylic acid/acrylamide composite gel water-absorbing material for water absorption and water retention.
背景技术 Background technique
丝素蛋白(Silk Fibroin：SF)是一种天然结构性蛋白，由结晶区和非结晶区组成，因其特殊的分子结构而具有亲水吸湿性、生物降解性、力学延伸性能等，是良好的吸水材料基材，可在废蚕茧丝中提取制备。Silk fibroin (Silk Fibroin: SF) is a natural structural protein composed of crystalline and non-crystalline regions. Because of its special molecular structure, it has hydrophilic and hygroscopic properties, biodegradability, and mechanical extension properties. The water-absorbing material base material can be prepared by extracting waste silkworm cocoons.
丙烯酸(acrylic acid：AA)是一种无色液体，可溶于水、乙醇和乙醚等。以树脂、合成橡胶乳液等应用于建筑、造纸、皮革、纺织、日用化工、水处理等领域。用丙烯酸生产的聚丙烯和丙烯酸共聚物，被用作分散剂、絮凝剂和增稠剂等，应用于高吸水树脂和助洗涤剂。Acrylic acid (acrylic acid: AA) is a colorless liquid, soluble in water, ethanol and ether, etc. It is used in construction, papermaking, leather, textile, daily chemical industry, water treatment and other fields with resin and synthetic rubber emulsion. Polypropylene and acrylic acid copolymers produced from acrylic acid are used as dispersants, flocculants and thickeners, etc., and are used in super absorbent resins and detergent builders.
丙烯酰胺(Acrylamide：AM)是一种白色结晶固体，易溶于水、甲醇和乙醇等。主要用于树脂、黏合剂等的合成，应用于建筑、改良土壤、油漆、造纸及服装加工等。也用于经高温加工处理的淀粉食品及饮用水等日常生活中。Acrylamide (Acrylamide: AM) is a white crystalline solid, easily soluble in water, methanol and ethanol, etc. It is mainly used in the synthesis of resins, adhesives, etc., and is used in construction, soil improvement, paint, papermaking, and clothing processing. It is also used in daily life such as starch food and drinking water processed by high temperature.
国内外十分重视开发具有生物降解性能的高吸水材料。At home and abroad, great attention is paid to the development of superabsorbent materials with biodegradable properties.
目前，应用广泛的合成类高分子吸水材料虽然吸水倍率高，但不易降解，使用后易污染环境。而已开发的天然高分子类吸水材料有淀粉类、纤维素类、海藻酸类、聚乳酸类等，具有一定的生物降解性，但在材料来源、制备加工成本及使用后对土壤结构的影响等存在不足。蛋白质类吸水材料除明胶、羽毛等外，目前开发较少。丝素蛋白具有亲水性和生物降解性，原料来源广泛，提取制备方便，是一种很好的吸水材料基材。因此，以废蚕丝等为原料，利用蚕丝蛋白的凝胶特性和吸水性能，与有机高分子复合，研制一种吸水性能优良，具有可生物降解性能的新型高分子吸水材料。对于丰富吸水材料类型，拓展蚕丝蛋白用途，使丝素蛋白利用成为高吸水材料研究应用的一个发展方向有较重要意义和应用价值。At present, although the widely used synthetic polymer water-absorbing materials have a high water absorption rate, they are not easy to degrade, and they are easy to pollute the environment after use. The natural polymer water-absorbing materials that have been developed include starch, cellulose, alginic acid, polylactic acid, etc., which have certain biodegradability. It has a shortpart. Apart from gelatin and feathers, protein-based water-absorbing materials have been less developed at present. Silk fibroin is hydrophilic and biodegradable, has a wide range of raw material sources, and is easy to extract and prepare. It is a good substrate for water-absorbing materials. Therefore, using waste silk as raw materials, using the gel properties and water absorption properties of silk protein, and compounding with organic polymers, a new type of polymer water-absorbing material with excellent water absorption properties and biodegradable properties is developed. It is of great significance and application value to enrich the types of water-absorbent materials, expand the use of silk fibroin, and make the use of silk fibroin a development direction for the research and application of super-absorbent materials.
水凝胶态吸水材料是有别于固体吸水材料的形态以外，可即制即用、使用方便的优点，适用于即用性土壤保水和涂料等。Hydrogel state water-absorbing material is different from the form of solid water-absorbing material, it can be made and used immediately, and it is convenient to use. It is suitable for ready-to-use soil water retention and coatings.
发明内容 Contents of the invention
针对现有技术中存在的不足之处，本发明的目的是提供一种制备丝素蛋白/丙烯酸/丙烯酰胺复合凝胶吸水材料的方法，包括以下步骤：For the deficiencies in the prior art, the object of the present invention is to provide a method for preparing silk fibroin/acrylic acid/acrylamide composite gel water-absorbing material, comprising the following steps:
(1)将一定质量分析纯丙烯酸溶液加入到烧杯中，在室温条件下，滴加一定质量的重量百分比浓度为10％的NaOH溶液，使丙烯酸的中和度达到70～80％；再加入一定质量分析纯丙烯酰胺固体物，使丙烯酰胺与丙烯酸的质量分数比为33％～51％。搅拌后得到丙烯酸/丙烯酰胺单体的混合溶液；(1) Add a certain mass of pure acrylic acid solution into a beaker, and at room temperature, drop a certain mass of NaOH solution with a concentration of 10% by weight to make the neutralization degree of acrylic acid reach 70-80%; The pure acrylamide solid is analyzed by mass, so that the mass fraction ratio of acrylamide to acrylic acid is 33%-51%. After stirring, a mixed solution of acrylic acid/acrylamide monomer is obtained;
(2)按丝素蛋白和丙烯酸/丙烯酰胺单体的质量分数比为25％～50％：将重量百分比浓度为8％丝素蛋白溶液加入反应器中，置于恒温磁力搅拌器上进行60～80℃水浴加热，然后加入过硫酸铵作为引发剂，再加入丙烯酸/丙烯酰胺单体混合液，最后加入N，N’-二甲基双丙烯酰胺作为交联剂；继续控制水浴温度60～80℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h；(2) The mass fraction ratio of silk fibroin and acrylic acid/acrylamide monomer is 25% to 50%: the silk fibroin solution with a concentration of 8% by weight is added to the reactor, placed on a constant temperature magnetic stirrer for 60 Heat in a water bath at ~80°C, then add ammonium persulfate as an initiator, then add acrylic acid/acrylamide monomer mixture, and finally add N,N'-dimethylbisacrylamide as a crosslinking agent; continue to control the temperature of the water bath to 60~ Stir while heating at 80°C, stop stirring when the reactant becomes gel and becomes viscous and difficult to stir, and then stand still, the reaction time of stirring and standing is 2 hours in total;
(3)将静置后的凝胶取出，用去离子水水洗后，获得丝素蛋白/丙烯酸/丙烯酰胺复合凝胶吸水材料。(3) Take out the gel after standing, wash it with deionized water, and obtain the silk fibroin/acrylic acid/acrylamide composite gel water-absorbing material.
步骤(1)所述的室温是20～30℃。The room temperature described in step (1) is 20-30°C.
步骤(1)所述的中和度是摩尔中和度。The degree of neutralization described in step (1) is a molar degree of neutralization.
步骤(2)中丝素蛋白溶液的制备方法：将清洁的桑蚕废茧丝，经Na2CO3沸水脱胶后，用重量百分比为50％的CaCl2溶液98℃溶解，过滤、透析、浓缩，获得丝素蛋白溶液。The preparation method of the silk fibroin solution in the step (2): after degumming the waste silkworm cocoons with Na 2 CO 3 boiling water, dissolve them with 50% by weight CaCl 2 solution at 98°C, filter, dialyze and concentrate , to obtain silk fibroin solution.
步骤(2)中引发剂过硫酸铵与丙烯酸/丙烯酰胺单体的质量分数比为1.8～2.5％。In the step (2), the mass fraction ratio of the initiator ammonium persulfate to the acrylic acid/acrylamide monomer is 1.8-2.5%.
步骤(2)中交联剂N，N’-二甲基双丙烯酰胺与丙烯酸/丙烯酰胺单体的质量分数比为0.15～0.3％。In the step (2), the mass fraction ratio of the crosslinking agent N,N'-dimethylbisacrylamide to the acrylic acid/acrylamide monomer is 0.15-0.3%.
本发明的优点：Advantages of the present invention:
1、将丝素蛋白(SF)与丙烯酸(AA)、丙烯酰胺(AM)复合制成吸水保水工程用吸水材料，一方面利用丝素蛋白的亲水吸湿性，拓展吸水材料的来源用途，另一方面由于丝素蛋白具有生物降解性，能够诱导所复合合成高分子的分解，减小环境污染。1. Combining silk fibroin (SF) with acrylic acid (AA) and acrylamide (AM) to make water-absorbing materials for water-absorbing and water-retaining projects. On the one hand, due to the biodegradability of silk fibroin, it can induce the decomposition of the compounded polymer and reduce environmental pollution.
2、本发明制备的丝素蛋白/丙烯酸/丙烯酰胺(SF/AA/AM)复合凝胶吸水材料，综合了三者的优良性能，优势互补，是一种新型可生物降解性吸水保水材料。2. The silk fibroin/acrylic acid/acrylamide (SF/AA/AM) composite gel water-absorbing material prepared by the present invention combines the excellent properties of the three and complements each other's advantages. It is a new type of biodegradable water-absorbing and water-retaining material.
3、丝素蛋白(SF)吸水量为0.3～50g/g，而本发明制备的SF/AA/AM复合凝胶吸水材料，吸水量为500～800g/g。3. The water absorption of silk fibroin (SF) is 0.3-50 g/g, while the SF/AA/AM composite gel water-absorption material prepared by the present invention has a water absorption of 500-800 g/g.
具体实施方式 Detailed ways
以下通过实施例进一步对本发明进行描述：The present invention is further described below by embodiment:
丝素蛋白溶液的制备：Preparation of silk fibroin solution:
将清洁的桑蚕废茧丝，经Na2CO3沸水脱胶后，用重量百分比浓度为50％CaCl2溶液98℃溶解，过滤、透析、浓缩，获得SF溶液，浓度为8％，备用。After degumming the cleaned waste silkworm cocoons with Na 2 CO 3 boiling water, dissolve them in a 50% CaCl 2 solution by weight at 98°C, filter, dialyze, and concentrate to obtain an SF solution with a concentration of 8% for later use.
实施例1：Example 1:
(1)称取2.65g分析纯AA溶液加入烧杯中，在20～30℃室温条件下，滴加1.03g 10％(w/w)NaOH溶液，使AA的中和度达到70％；再加入1.35g分析纯AM固体物，搅拌后得到单体(AA/AM)的混合溶液。(1) Weigh 2.65g of analytically pure AA solution into a beaker, and add 1.03g of 10% (w/w) NaOH solution dropwise at room temperature of 20-30°C to make the neutralization degree of AA reach 70%; then add 1.35 g of analytically pure AM solid was stirred to obtain a mixed solution of monomer (AA/AM).
(2)将2g SF加入25ml蒸馏水的反应器中，置于恒温磁力搅拌器上进行水浴加热(70℃)；然后加入0.072g过硫酸铵(简称APS)，再加入单体(AA/AM)混合液和0.006g N，N’-二甲基双丙烯酰胺(简称MBA)。(2) Add 2g of SF into a reactor containing 25ml of distilled water, place it on a constant temperature magnetic stirrer for heating in a water bath (70°C); then add 0.072g of ammonium persulfate (APS for short), and then add monomer (AA/AM) Mixed solution and 0.006g N, N'-dimethylbisacrylamide (abbreviated as MBA).
(3)控制水浴温度70℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h。(3) Control the temperature of the water bath to 70°C, and stir while heating. When the reactant becomes gel and becomes viscous and difficult to stir, stop stirring, and then stand still. The total reaction time of stirring and standing is 2 hours.
(4)将制得的凝胶取出，用去离子水水洗后，获得水凝胶状复合吸水材料。(4) The prepared gel was taken out and washed with deionized water to obtain a hydrogel-like composite water-absorbing material.
(5)将水凝胶状复合吸水材料，切粒后，放入7000ml去离子水中，静置浸泡12h，使充分吸水饱和。(5) Cut the hydrogel-like composite water-absorbing material into pellets, put it into 7000ml of deionized water, and let it soak for 12 hours to fully absorb water and saturate it.
(6)取出吸水膨胀凝胶材料，经2h搁挂无滴水止。然后称计水凝胶重量为5210g。(6) Take out the water-absorbing and swelling gel material, hang it for 2 hours without dripping water. Then weigh the hydrogel weight to be 5210g.
(7)再经100℃干燥后，称计干重量为6.77g。(7) After drying at 100°C, the measured dry weight is 6.77g.
(8)按以下公式计算吸水量：(8) Calculate the water absorption according to the following formula:
吸水量＝吸水凝胶重量-干重量/干重量Water absorption = weight of water-absorbing gel - dry weight/dry weight
复合吸水材料吸水量＝5210-6.77/6.77＝768.6g/gComposite absorbent material water absorption = 5210-6.77/6.77 = 768.6g/g
该实施例所研制的复合凝胶吸水材料的吸水量为768.6g/g。The water absorption capacity of the composite gel water-absorbing material developed in this example is 768.6 g/g.
实施例2：Example 2:
(1)称取2.65g AA溶液加入烧杯中，在20～30℃室温条件下，滴加1.177g10％(w/w)NaOH溶液，使AA的中和度达到80％；再加入1.35g AM固体物，搅拌后得到单体(AA/AM)的混合溶液。(1) Weigh 2.65g of AA solution into a beaker, and add 1.177g of 10% (w/w) NaOH solution dropwise at room temperature of 20-30°C to make the neutralization degree of AA reach 80%; then add 1.35g of AM Solid matter, after stirring, a mixed solution of monomer (AA/AM) was obtained.
(2)将2g SF加入25ml蒸馏水的反应器中，置于恒温磁力搅拌器上进行水浴加热(80℃)；然后加入0.1g过硫酸铵(简称APS)，再加入单体(AA/AM)混合液和0.012g N，N’-二甲基双丙烯酰胺(简称MBA)。(2) Add 2g of SF into a reactor containing 25ml of distilled water, place it on a constant temperature magnetic stirrer for water bath heating (80°C); then add 0.1g of ammonium persulfate (APS for short), and then add monomer (AA/AM) Mixed solution and 0.012g N, N'-dimethylbisacrylamide (abbreviated as MBA).
(3)控制水浴温度80℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h。(3) Control the temperature of the water bath to 80°C, and stir while heating. When the reactant becomes gel and becomes viscous and difficult to stir, stop stirring, and then stand still. The total reaction time of stirring and standing is 2 hours.
(4)将制得的凝胶取出，用去离子水水洗后，获得水凝胶状复合吸水材料。(4) The prepared gel was taken out and washed with deionized water to obtain a hydrogel-like composite water-absorbing material.
(5)将水凝胶状复合吸水材料，切粒后，放入7000ml去离子水中，静置浸泡12h，使充分吸水饱和。(5) Cut the hydrogel-like composite water-absorbing material into pellets, put it into 7000ml of deionized water, and let it soak for 12 hours to fully absorb water and saturate it.
(6)取出吸水膨胀凝胶材料，经2h搁挂无滴水止。称计水凝胶重量为3520g。(6) Take out the water-absorbing and swelling gel material, hang it for 2 hours without dripping water. The weighed hydrogel weighed 3520g.
(7)再经100℃干燥后，获得干重量为6.95g。(7) After drying at 100° C., the obtained dry weight is 6.95 g.
(8)按以下公式计算吸水量：(8) Calculate the water absorption according to the following formula:
吸水量＝吸水凝胶重量-干重量/干重量Water absorption = weight of water-absorbing gel - dry weight/dry weight
复合吸水材料吸水量＝3520-6.95/6.95＝505.5g/gComposite absorbent material water absorption = 3520-6.95/6.95 = 505.5g/g
该实施例所研制的复合凝胶吸水材料的吸水量为505.5g/g。The water absorption capacity of the composite gel water-absorbing material developed in this example is 505.5 g/g.
实施例3：Example 3:
(1)称取2.65g AA溶液加入烧杯中，在20～30℃室温条件下，滴加1.03g10％(w/w)NaOH溶液，使AA的中和度达到70％；再加入1.35g AM固体物，搅拌后得到单体(AA/AM)的混合溶液。(1) Weigh 2.65g of AA solution into a beaker, and add 1.03g of 10% (w/w) NaOH solution dropwise at room temperature of 20-30°C to make the neutralization degree of AA reach 70%; then add 1.35g of AM Solid matter, after stirring, a mixed solution of monomer (AA/AM) was obtained.
(2)将2g SF加入25ml蒸馏水的反应器中，置于恒温磁力搅拌器上进行水浴加热(70℃)；然后加入0.08g过硫酸铵(简称APS)，再加入单体(AA/AM)混合液和0.008g N，N’-二甲基双丙烯酰胺(简称MBA)。(2) Add 2g of SF into a reactor containing 25ml of distilled water, place it on a constant temperature magnetic stirrer for water bath heating (70°C); then add 0.08g of ammonium persulfate (APS for short), and then add monomer (AA/AM) Mixed solution and 0.008g N, N'-dimethylbisacrylamide (abbreviated as MBA).
(3)控制水浴温度70℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h。(3) Control the temperature of the water bath to 70°C, and stir while heating. When the reactant becomes gel and becomes viscous and difficult to stir, stop stirring, and then stand still. The total reaction time of stirring and standing is 2 hours.
(4)将制得的凝胶取出，用去离子水水洗后，获得水凝胶状复合吸水材料。(4) The prepared gel was taken out and washed with deionized water to obtain a hydrogel-like composite water-absorbing material.
(5)将水凝胶状复合吸水材料，切粒后，放入7000ml去离子水中，静置浸泡12h，使充分吸水饱和。(5) Cut the hydrogel-like composite water-absorbing material into pellets, put it into 7000ml of deionized water, and let it soak for 12 hours to fully absorb water and saturate it.
(6)取出吸水膨胀凝胶材料，经2h搁挂无滴水止。称计水凝胶重量为4500g。(6) Take out the water-absorbing and swelling gel material, hang it for 2 hours without dripping water. The weight of the hydrogel was weighed to be 4500g.
(7)再经100℃干燥后，称计干重量为6.85g。(7) After drying at 100°C, the measured dry weight is 6.85g.
(8)按以下公式计算吸水量：(8) Calculate the water absorption according to the following formula:
吸水量＝吸水凝胶重量-干重量/干重量Water absorption = weight of water-absorbing gel - dry weight/dry weight
复合吸水材料吸水量＝4500-6.85/6.85＝655.4g/gComposite absorbent material water absorption = 4500-6.85/6.85 = 655.4g/g
该实施例所研制的复合凝胶吸水材料的吸水量为655.4g/g。The water absorption capacity of the composite gel water-absorbing material developed in this example is 655.4 g/g.
实施例4：Example 4:
(1)称取2.65g AA溶液加入烧杯中，在20～30℃室温条件下，滴加1.03g 10％(w/w)NaOH溶液，使AA的中和度达到70％；再加入1.35g AM固体物，搅拌后得到单体(AA/AM)的混合溶液。(1) Weigh 2.65g of AA solution into a beaker, and add 1.03g of 10% (w/w) NaOH solution dropwise at room temperature of 20-30°C to make the neutralization degree of AA reach 70%; then add 1.35g AM solid, after stirring, a mixed solution of monomer (AA/AM) was obtained.
(2)将1g SF加入25ml蒸馏水的反应器中，置于恒温磁力搅拌器上进行水浴加热(60℃)；然后加入0.072g过硫酸铵(简称APS)，再加入单体(AA/AM)混合液和0.0072g N，N’-二甲基双丙烯酰胺(简称MBA)。(2) Add 1g of SF to a reactor containing 25ml of distilled water, place it on a constant temperature magnetic stirrer for heating in a water bath (60°C); then add 0.072g of ammonium persulfate (APS for short), and then add monomer (AA/AM) Mixed solution and 0.0072g N, N'-dimethylbisacrylamide (abbreviated as MBA).
(3)控制水浴温度60℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h。(3) Control the temperature of the water bath to 60°C, and stir while heating. When the reactant becomes gel and becomes viscous and difficult to stir, stop stirring, and then stand still. The total reaction time of stirring and standing is 2 hours.
(4)将制得的凝胶取出，用去离子水水洗后，获得水凝胶状复合吸水材料。(4) The prepared gel was taken out and washed with deionized water to obtain a hydrogel-like composite water-absorbing material.
(5)将水凝胶状复合吸水材料，切粒后，放入7000ml去离子水中，静置浸泡12h，使充分吸水饱和。(5) Cut the hydrogel-like composite water-absorbing material into pellets, put it into 7000ml of deionized water, and let it soak for 12 hours to fully absorb water and saturate it.
(6)取出吸水膨胀凝胶材料，经2h搁挂无滴水止。称计水凝胶重量为3600g。(6) Take out the water-absorbing and swelling gel material, hang it for 2 hours without dripping water. The weight of the hydrogel was weighed to be 3600g.
(7)再经100℃干燥后，获得干重量为6.63g。(7) After drying at 100°C, a dry weight of 6.63 g was obtained.
(8)按以下公式计算吸水量：(8) Calculate the water absorption according to the following formula:
吸水量＝吸水凝胶重量-干重量/干重量Water absorption = weight of water-absorbing gel - dry weight/dry weight
复合吸水材料吸水量＝3600-6.63/6.63＝542g/gComposite absorbent material water absorption = 3600-6.63/6.63 = 542g/g
该实施例所研制的复合凝胶吸水材料的吸水量为542g/g。The water absorption capacity of the composite gel water-absorbing material developed in this example is 542 g/g.
实施例5：Example 5:
(1)称取3g AA溶液加入烧杯中，在20～30℃室温条件下，滴加1.03g10％(w/w)NaOH溶液，使AA的中和度达到70％；再加入1g AM固体物，搅拌后得到单体(AA/AM)的混合溶液。(1) Weigh 3g of AA solution into a beaker, add 1.03g of 10% (w/w) NaOH solution dropwise at room temperature of 20-30°C to make the neutralization degree of AA reach 70%; then add 1g of AM solid , A mixed solution of monomer (AA/AM) was obtained after stirring.
(2)将2g SF加入25ml蒸馏水的反应器中，置于恒温磁力搅拌器上进行水浴加热(80℃)；然后加入0.09g过硫酸铵(简称APS)，再加入单体(AA/AM)混合液和0.006g N，N’-二甲基双丙烯酰胺(简称MBA)。(2) Add 2g of SF into a reactor containing 25ml of distilled water, place it on a constant temperature magnetic stirrer for water bath heating (80°C); then add 0.09g of ammonium persulfate (APS for short), and then add monomer (AA/AM) Mixed solution and 0.006g N, N'-dimethylbisacrylamide (abbreviated as MBA).
(3)控制水浴温度80℃，边加热边搅拌，当反应物成凝胶，变得粘稠至搅拌困难时停止搅拌，然后静置，搅拌与静置反应时间共2h。(3) Control the temperature of the water bath to 80°C, and stir while heating. When the reactant becomes gel and becomes viscous and difficult to stir, stop stirring, and then stand still. The total reaction time of stirring and standing is 2 hours.
(4)将制得的凝胶取出，用去离子水水洗后，获得水凝胶状复合吸水材料。(4) The prepared gel was taken out and washed with deionized water to obtain a hydrogel-like composite water-absorbing material.
(5)将水凝胶状复合吸水材料，切粒后，放入7000ml去离子水中，静置浸泡12h，使充分吸水饱和。(5) Cut the hydrogel-like composite water-absorbing material into pellets, put it into 7000ml of deionized water, and let it soak for 12 hours to fully absorb water and saturate it.
(6)取出吸水膨胀凝胶材料，经2h搁挂无滴水止。称计水凝胶重量为4350g。(6) Take out the water-absorbing and swelling gel material, hang it for 2 hours without dripping water. The weight of the hydrogel was weighed to be 4350g.
(7)再经100℃干燥后，获得干重量为5.8g。(7) After drying at 100°C, a dry weight of 5.8 g was obtained.
(8)按以下公式计算吸水量：(8) Calculate the water absorption according to the following formula:
吸水量＝吸水凝胶重量-干重量/干重量Water absorption = weight of water-absorbing gel - dry weight/dry weight
复合吸水材料吸水量＝4350-5.8/5.8＝749g/gComposite absorbent material water absorption = 4350-5.8/5.8 = 749g/g
该实施例所研制的复合凝胶吸水材料的吸水量为749g/g。The water absorption of the composite gel water-absorbing material developed in this embodiment is 749g/g.
最后，还需要注意的是，以上列举的仅是本发明的具体实施例子。显然，本发明不限于以上实施例子，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。Finally, it should also be noted that the above examples are only specific implementation examples of the present invention. Apparently, the present invention is not limited to the above examples, and many variations are possible. All deformations that can be directly derived or associated by those skilled in the art from the content disclosed in the present invention should be considered as the protection scope of the present invention.
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