CN103407205B - Konjac glucomannan fiber wet tissue and method for preparing same - Google Patents
Konjac glucomannan fiber wet tissue and method for preparing same Download PDFInfo
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- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 title claims abstract description 84
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
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- IIPCXIGUIPAGQB-OUKQBFOZSA-N (e)-4-dodecoxy-4-oxobut-2-enoic acid Chemical compound CCCCCCCCCCCCOC(=O)\C=C\C(O)=O IIPCXIGUIPAGQB-OUKQBFOZSA-N 0.000 claims description 8
- 229940099112 cornstarch Drugs 0.000 claims description 7
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- 229920001661 Chitosan Polymers 0.000 claims description 6
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 claims description 6
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Abstract
本发明涉及一种魔芋葡甘聚糖纤维湿纸巾及其制备方法。一种魔芋葡甘聚糖纤维湿纸巾的制备方法包括魔芋葡甘聚糖丙烯酸酯的制备、魔芋葡甘聚糖酯化改性、魔芋葡甘聚糖仿丝浆液的制备和魔芋葡甘聚糖纤维湿纸巾的制备。本发明的魔芋葡甘聚糖纤维湿纸巾,是以魔芋葡甘聚糖和玉米淀粉等天然纤维为主要原材料并辅以其他增塑剂制成的。魔芋葡甘聚糖是一种天然植物多糖,具有优良的持水性、吸水性、抗菌性并且拉伸强度大,柔韧性好,抗张强度、耐破度高;本发明的魔芋葡甘聚糖纤维湿纸巾与传统的合成纤维湿纸巾相比,由100%天然植物纤维制成,生产的湿纸巾产品具有高抗张强度、吸液量大、保液量高、使用手感细腻柔软、无菌卫生等特点,具有生产成本低,无环境污染,对人体没有伤害等优点,符合现代的消费理念和市场需求。The invention relates to a konjac glucomannan fiber wet tissue and a preparation method thereof. A preparation method of konjac glucomannan fiber wet tissue comprises preparation of konjac glucomannan acrylate, konjac glucomannan esterification modification, preparation of konjac glucomannan silk-like slurry and konjac glucomannan Preparation of fiber wet wipes. The konjac glucomannan fiber wet tissue of the present invention is made of natural fibers such as konjac glucomannan and corn starch as main raw materials and supplemented with other plasticizers. Konjac glucomannan is a kind of natural plant polysaccharide, which has excellent water holding capacity, water absorption, antibacterial property, high tensile strength, good flexibility, high tensile strength and burst resistance; the konjac glucomannan of the present invention Compared with traditional synthetic fiber wet wipes, fiber wet wipes are made of 100% natural plant fibers. The wet wipes produced have high tensile strength, large liquid absorption, high liquid retention, delicate and soft hand feeling, and are sterile Hygienic and other characteristics, with low production cost, no environmental pollution, no harm to the human body, etc., in line with modern consumption concepts and market demand.
Description
技术领域 technical field
本发明涉及一种纤维湿纸巾及其制备方法,具体涉及一种魔芋葡甘聚糖纤维湿纸巾及其制备方法。 The invention relates to a fiber wet tissue and a preparation method thereof, in particular to a konjac glucomannan fiber wet tissue and a preparation method thereof.
背景技术 Background technique
在我们日常生活环境中,细菌无处不在,但是由于工作和学习等各项社会活动,手需要不断的接触各种食物,由此我们会感染上大量的微生物和致病菌。所以我们必须养成经常洗手的习惯。但是,人们在日常生活中,特别是进行户外活动时,却不能及时洗手,这在一定程度上危害了人们的健康,于是湿纸巾的需求与日剧增。特别是近两年来, 湿纸巾的生产和市场发展非常迅速, 用途日趋多样化, 渐成卫生纸品市场的新宠。 In our daily life environment, bacteria are everywhere, but due to various social activities such as work and study, hands need to be in constant contact with various foods, so we will be infected with a large number of microorganisms and pathogenic bacteria. So we must develop the habit of washing our hands frequently. However, people cannot wash their hands in time in daily life, especially when performing outdoor activities, which endangers people's health to a certain extent, so the demand for wet paper towels is increasing day by day. Especially in the past two years, the production and market of wet wipes have developed very rapidly, and their uses have become increasingly diversified, gradually becoming the new darling of the toilet paper market.
但是,已有的消毒湿纸巾大多以无纺布和传统造纸法造得的纸作为载体,以普通化学消毒剂浸泡而成,使用的安全性令人怀疑,整个工艺中还存在环境问题。 因此,随着人们环境保护意识的不断增强和对自身安全要求的不断提高及产品的不断更新改进,一种高持水率、高抗菌性的安全环保型湿纸巾亟待我们的研究和开发。 However, most of the existing disinfectant wet wipes use non-woven fabrics and paper made by traditional papermaking methods as carriers, and are soaked in common chemical disinfectants. The safety of use is doubtful, and there are environmental problems in the whole process. Therefore, with the continuous enhancement of people's awareness of environmental protection, the continuous improvement of their own safety requirements and the continuous update and improvement of products, a safe and environmentally friendly wet tissue with high water holding rate and high antibacterial property is urgently needed for our research and development.
申请号为97117967.0的发明专利“制造湿纸巾的方法”(申请日:1997.07.25),提供了使用时湿润强度提高了的湿纸巾。在湿纸巾的制造过程中,通过在水膨润性相对低的乃至水不溶性的羧甲基纤维素盐的片状物中浸渍含多价金属离子的液体,得到湿纸巾。该项发明虽然提高了湿纸巾的湿润度,但是其中的多价金属离子多是2价的铁、锌等碱性金属离子,对皮肤有较强的刺激性,长期使用不利于人体健康。本发明制造方法使用的原料,包括羧甲基纤维素或它的盐,多为合成纤维、尼龙、聚酯等合成纤维,使用后难以生物降解。 Application No. 97117967.0 for the invention patent "Method for Manufacturing Wet Paper Towels" (application date: 1997.07.25) provides wet paper towels with improved wet strength during use. In the manufacturing process of wet tissues, wet tissues are obtained by impregnating a liquid containing polyvalent metal ions in a sheet of carboxymethylcellulose salt having relatively low water swelling property or even water insoluble. Although this invention has improved the wetness of wet paper towels, the polyvalent metal ions therein are mostly basic metal ions such as divalent iron and zinc, which are highly irritating to the skin, and long-term use is not conducive to human health. The raw materials used in the production method of the present invention include carboxymethyl cellulose or its salts, mostly synthetic fibers such as synthetic fibers, nylon, polyester, etc., which are difficult to biodegrade after use.
申请号为200810101766.3的发明专利“一种高效杀菌湿纸巾”(申请日:2008.03.12),提供的一种杀菌纸巾,由纸巾浸泡杀菌剂制得。该消毒杀菌纸巾具备了良好的杀菌和消毒的功能,但是该湿纸巾是在原来湿纸巾基质的基础上浸泡杀菌剂制得,没有从根本上解决消毒纸巾的安全使用性问题。 The invention patent of application number 200810101766.3 "A high-efficiency sterilizing wet tissue" (application date: 2008.03.12) provides a bactericidal tissue, which is made by soaking the tissue in a bactericide. The sterilizing paper towel has a good function of sterilizing and disinfecting, but the wet paper towel is prepared by soaking a bactericide on the basis of the original wet paper towel base, which does not fundamentally solve the problem of safe use of the disinfecting paper towel.
发明内容 Contents of the invention
本发明的目的是提供一种魔芋葡甘聚糖纤维湿纸巾及其制备方法。利用魔芋葡甘聚糖和玉米淀粉等天然纤维为主要原材料,利用魔芋葡甘聚糖的高吸水性及膨润性,高持水性、高抗菌性并加入(甘油、乙醇)提高魔芋葡甘聚糖纤维湿纸巾的抗张强度、耐破度和伸长率、加入马来酸单月桂酯提高魔芋葡甘聚糖纤维湿纸巾的持水性,加入壳聚糖、丙烯酸,对魔芋葡甘聚糖酯化改性,提高魔芋葡甘聚糖纤维湿纸巾的抗菌能力,提供一种高持水率、高抗菌性的安全环保型湿纸巾及其制备方法。 The purpose of the present invention is to provide a kind of konjac glucomannan fiber wet tissue and its preparation method. Using natural fibers such as konjac glucomannan and corn starch as the main raw materials, using konjac glucomannan's high water absorption and swelling properties, high water holding capacity, high antibacterial properties and adding (glycerin, ethanol) to improve konjac glucomannan Tensile strength, bursting strength and elongation of fiber wet tissue, adding monolauryl maleate to improve the water holding capacity of konjac glucomannan fiber wet tissue, adding chitosan and acrylic acid to esterify konjac glucomannan Modification improves the antibacterial ability of the konjac glucomannan fiber wet tissue, and provides a safe and environment-friendly wet tissue with high water holding rate and high antibacterial property and a preparation method thereof.
本发明的魔芋葡甘聚糖纤维湿纸巾的制备方法,包括魔芋葡甘聚糖丙烯酸酯的制备、魔芋葡甘聚糖酯化改性、魔芋葡甘聚糖仿丝浆液的制备、魔芋葡甘聚糖纤维湿纸巾的制备,其特征在于: The preparation method of the konjac glucomannan fiber wet tissue of the present invention comprises preparation of konjac glucomannan acrylate, konjac glucomannan esterification modification, preparation of konjac glucomannan silk-like slurry, konjac glucomannan The preparation of polysaccharide fiber wet tissue is characterized in that:
(1)魔芋葡甘聚糖丙烯酸酯的制备: 取热水并保持45~50℃,边搅拌边加入魔芋葡甘聚糖、丙烯酸和体积浓度为98%的浓硫酸, 反应时间4h~4.5h;然后, 以500r/min的转速旋转并蒸发浓缩反应液,浓缩至含水率为0.1%~0.5%,加入体积浓度为60%的乙醇,沉淀,取沉淀物用体积浓度为95%的乙醇洗涤2~3次,过滤并将沉淀物在室温下风干后碾碎, 得到物质A,备用;所述丙烯酸和魔芋葡甘聚糖与水的质量比为1:100~200,丙烯酸与魔芋葡甘聚糖的质量比为3~3.82∶1,浓硫酸占丙烯酸体积的1%~2%; (1) Preparation of konjac glucomannan acrylate: Take hot water and keep it at 45-50°C, add konjac glucomannan, acrylic acid and concentrated sulfuric acid with a volume concentration of 98% while stirring, and the reaction time is 4h-4.5h Then, rotate at a speed of 500r/min and evaporate and concentrate the reaction solution until the water content is 0.1% to 0.5%, add ethanol with a volume concentration of 60%, precipitate, and take the precipitate and wash it with ethanol with a volume concentration of 95% 2 to 3 times, filter and air-dry the precipitate at room temperature, then crush to obtain substance A, for later use; the mass ratio of the acrylic acid and konjac glucomannan to water is 1:100-200, and the acrylic acid and konjac glucomannan The mass ratio of polysaccharide is 3-3.82:1, concentrated sulfuric acid accounts for 1%-2% of the volume of acrylic acid;
(2)魔芋葡甘聚糖酯化改性:按质量体积比(g/mL)为1∶200~300的比例将马来酸单月桂酯溶解于体积浓度为60%的乙醇中, 用体积浓度为20%的稀硫酸调pH值为3~5; 按马来酸单月桂酯和魔芋葡甘聚糖的质量比为1:10~20的比例加入魔芋葡甘聚糖, 搅拌均匀,在30~50℃温度下反应1~3h , 然后用体积浓度为60%的乙醇洗涤沉淀,过滤后将沉淀物在50℃下真空干燥, 得到物质B,碾碎备用; (2) Esterification modification of konjac glucomannan: Dissolve monolauryl maleate in ethanol with a volume concentration of 60% at a mass volume ratio (g/mL) of 1:200-300, and use volume The concentration is 20% dilute sulfuric acid to adjust the pH value to 3-5; add konjac glucomannan according to the mass ratio of monolauryl maleate and konjac glucomannan at a ratio of 1:10-20, stir evenly, and React at a temperature of 30-50°C for 1-3 hours, then wash the precipitate with ethanol with a volume concentration of 60%, filter and dry the precipitate in vacuum at 50°C to obtain substance B, which is crushed for later use;
(3)魔芋葡甘聚糖仿丝浆液的制备: (3) Preparation of konjac glucomannan imitation silk slurry:
(a)取玉米淀粉,按质量体积比(g/mL)为1∶100~300的比例加入无菌水,在65~90℃条件下溶胀12~14h,分散,得到物质C ; (a) Take cornstarch, add sterile water at a mass volume ratio (g/mL) of 1:100-300, swell at 65-90°C for 12-14 hours, and disperse to obtain substance C;
(b)按质量体积(g/mL)比为1∶100~300的比例,取壳聚糖加入pH 3~3.5的乙酸水溶液中,搅拌溶解后在65~90℃条件下溶胀12~14h,分散,得到物质D; (b) According to the ratio of mass to volume (g/mL) of 1:100-300, take chitosan and add it to acetic acid aqueous solution with pH 3-3.5, stir and dissolve, and swell at 65-90°C for 12-14 hours, Disperse to obtain substance D;
(c)将步骤(1)制得的物质A和步骤(2)制得的物质B按照质量比为1∶1~2的比例混合,得到AB混合物;将物质C和物质D按照体积比为2~3∶1的比例混合,得到CD混合液;将AB混合物加到CD混合液中,然后在超声波功率100~180W、25℃~90℃下分散15~20min,得到魔芋葡甘聚糖仿丝浆液; (c) Mix the substance A prepared in step (1) with the substance B prepared in step (2) according to the mass ratio of 1:1~2 to obtain the AB mixture; mix substance C and substance D according to the volume ratio Mix at a ratio of 2 to 3:1 to obtain a CD mixture; add the AB mixture to the CD mixture, and then disperse for 15 to 20 minutes at an ultrasonic power of 100 to 180 W at 25°C to 90°C to obtain konjac glucomannan imitation silk slurry;
(4) 魔芋葡甘聚糖纤维湿纸巾的制备:将步骤(3)的魔芋葡甘聚糖仿丝浆液经过纤维湿法纺丝全套设备处理,即得到纤维湿纸巾。所述纤维湿法纺丝全套设备处理 (4) Preparation of konjac glucomannan fiber wet wipes: the konjac glucomannan silk-like slurry in step (3) is processed through a complete set of fiber wet spinning equipment to obtain fiber wet wipes. The complete set of equipment for wet spinning of the fiber is processed
本发明的所用原料均为食品级。 The raw materials used in the present invention are all food grade.
本发明还保护利用上述方法制备的魔芋葡甘聚糖纤维湿纸巾。 The present invention also protects the konjac glucomannan fiber wet tissue prepared by the above method.
本发明具有以下优点:本发明的魔芋葡甘聚糖纤维湿纸巾,是以魔芋葡甘聚糖和玉米淀粉等天然纤维为主要原材料并辅以其他增塑剂制成的。魔芋葡甘聚糖是一种天然植物多糖,具有优良的持水性、吸水性、抗菌性并且拉伸强度大,柔韧性好,抗张强度、耐破度高;本发明的玉米淀粉富含天然植物纤维,吸湿性强。本发明的魔芋葡甘聚糖纤维湿纸巾与传统的合成纤维湿纸巾相比,由100%天然植物纤维制成,生产的湿纸巾产品具有高抗张强度、吸液量大、保液量高、使用手感细腻柔软、无菌卫生等特点。该湿纸巾避免传统湿纸巾多次使用对皮肤造成的伤害,使用后可自然降解,回归自然,保护环境。本品适用于旅游、家庭、个人、酒店、宾馆、写字楼、医院、机场等娱乐、公共场所使用,以提高生活品质、提升服务档次。 The invention has the following advantages: the konjac glucomannan fiber wet tissue of the invention is made of natural fibers such as konjac glucomannan and corn starch as main raw materials and supplemented with other plasticizers. Konjac glucomannan is a kind of natural plant polysaccharide, which has excellent water holding capacity, water absorption, antibacterial property, high tensile strength, good flexibility, high tensile strength and burst resistance; the cornstarch of the present invention is rich in natural Plant fiber, strong hygroscopicity. Compared with the traditional synthetic fiber wet tissue, the konjac glucomannan fiber wet tissue of the present invention is made of 100% natural plant fiber, and the wet tissue product produced has high tensile strength, large liquid absorption capacity and high liquid retention capacity , The use of fine and soft feel, aseptic hygiene and other characteristics. The wet tissue avoids skin damage caused by repeated use of traditional wet tissue, and can be naturally degraded after use, returning to nature and protecting the environment. This product is suitable for use in entertainment and public places such as travel, family, personal, hotel, hotel, office building, hospital, airport, etc., to improve the quality of life and service level.
本发明的新型魔芋葡甘聚糖纤维湿纸巾的安全性和使用性能完全符合国家有关标准要求,本发明是以魔芋葡甘聚糖和玉米淀粉等天然纤维为主要原材料,辅以其他增塑剂(例如壳聚糖),本发明的壳聚糖是自然界中仅次于纤维素的第二大生物多糖,同时也是自然界中唯一大量存在的碱性多糖,具有很好的生物相容性,生物可降解性及抗菌、防腐等优良特性"。本发明利用魔芋葡甘聚糖与马来酸单月桂酯干法酯化改性,改性后的产品的粘度及持水性有显著的提高,且具有良好的生物降解性。本发明的魔芋葡甘聚糖丙烯酸酯有较强的抗菌效果,有良好的生物降解性,是一种安全环保的生物材料。本发明具有生产成本低,无环境污染,对人体没有伤害等优点,符合现代的消费理念和市场需求。 The safety and usability of the new konjac glucomannan fiber wet wipes of the present invention fully meet the requirements of relevant national standards. The present invention uses natural fibers such as konjac glucomannan and corn starch as main raw materials, supplemented by other plasticizers (such as chitosan), chitosan of the present invention is the second largest biological polysaccharide after cellulose in nature, and is also the only alkaline polysaccharide that exists in large quantities in nature, has good biocompatibility, biological Degradability and excellent properties such as antibacterial and antiseptic". The present invention utilizes konjac glucomannan and monolauryl maleate dry method esterification modification, the viscosity and water holding capacity of the modified product are significantly improved, and Has good biodegradability. Konjac glucomannan acrylate of the present invention has stronger antibacterial effect, has good biodegradability, is a kind of safe and environment-friendly biological material. The present invention has low production cost, no environmental pollution , no harm to the human body and other advantages, in line with modern consumption concepts and market demand.
将本发明的魔芋葡甘聚糖纤维湿纸巾与普通湿纸巾作如下性能测试: The konjac glucomannan fiber wet tissue of the present invention and common wet tissue are tested as follows:
(1)保水性:分别取本发明的魔芋葡甘聚糖纤维湿纸巾与普通湿纸巾各3块,置于同等温度环境即50℃高温下;再各取3块,置于同等温度环境即常温15℃下,计算每种湿纸巾在不同温度下完全失水时所需的平均时间。 (1) Water retention: Take 3 pieces of the konjac glucomannan fiber wet tissue of the present invention and ordinary wet tissue respectively, and place them in the same temperature environment, that is, at a high temperature of 50°C; then take 3 pieces each, and place them in the same temperature environment. At room temperature of 15°C, calculate the average time required for each type of wet tissue to completely lose water at different temperatures.
(2)抗菌性:试验普通湿纸巾、魔芋葡甘聚糖纤维湿纸巾对几个人的右手上的自然菌群进行杀菌消毒,擦手2min,并分别观察了杀菌平均效果。 (2) Antibacterial property: test ordinary wet wipes and konjac glucomannan fiber wet wipes to sterilize and disinfect the natural flora on the right hands of several people, wipe hands for 2 minutes, and observe the average sterilization effect respectively.
(3)可生物降解性:分别把普通湿纸巾、魔芋葡甘聚糖纤维湿纸巾各3块掩埋在同一土壤中,一个月后对湿纸巾降解情况进行观察。 (3) Biodegradability: Bury three ordinary wet wipes and three konjac glucomannan fiber wet wipes in the same soil, and observe the degradation of the wet wipes after one month.
本发明的魔芋葡甘聚糖纤维湿纸巾与普通湿纸巾的性能对比的结果如表1所示。 Table 1 shows the performance comparison results between the konjac glucomannan fiber wet tissue of the present invention and ordinary wet tissue.
表1本发明的湿纸巾和普通湿纸巾的性能对比 Table 1 The performance comparison of wet paper towels of the present invention and ordinary wet paper towels
经过以上对比测试,用本发明的魔芋葡甘聚糖纤维湿纸巾保水能力很强,抗菌性好,几乎可以完全生物降解,各项性能优异于普通湿纸巾,具有极好的发展前景。 Through the above comparative tests, the konjac glucomannan fiber wet tissue of the present invention has strong water retention capacity, good antibacterial property, almost complete biodegradability, and various performances are superior to ordinary wet tissue, and has excellent development prospects.
具体实施例specific embodiment
下面结合实施例对本发明做进一步的阐述。 Below in conjunction with embodiment the present invention is further elaborated.
实施例1:一种魔芋葡甘聚糖纤维湿纸巾的制备方法 Embodiment 1: A kind of preparation method of konjac glucomannan fiber wet tissue
一种魔芋葡甘聚糖纤维湿纸巾的制备方法,包括以下步骤: A preparation method of konjac glucomannan fiber wet tissue, comprising the following steps:
(1)魔芋葡甘聚糖丙烯酸酯的制备: 取热水并保持45~50℃,边搅拌边加入魔芋葡甘聚糖、丙烯酸和体积浓度为98%的浓硫酸, 反应时间4h;然后,以500r/min的转速旋转并蒸发浓缩反应液,浓缩至含水率为0.5%,加入体积浓度为60%的乙醇,沉淀,取沉淀物用体积浓度为95%的乙醇洗涤3次,过滤并将沉淀物在室温下风干后碾碎, 得到物质A,备用;所述丙烯酸和魔芋葡甘聚糖与水的质量比为1:150,丙烯酸与魔芋葡甘聚糖的质量比为3.5∶1,浓硫酸占丙烯酸体积的1.5%; (1) Preparation of konjac glucomannan acrylate: Take hot water and keep it at 45-50°C, add konjac glucomannan, acrylic acid and concentrated sulfuric acid with a volume concentration of 98% while stirring, and the reaction time is 4h; then, Rotate at a speed of 500r/min and evaporate and concentrate the reaction solution until the water content is 0.5%. Add ethanol with a volume concentration of 60% for precipitation. The precipitate is washed 3 times with ethanol with a volume concentration of 95%, filtered and The precipitate was air-dried at room temperature and crushed to obtain substance A, which was set aside; the mass ratio of the acrylic acid and konjac glucomannan to water was 1:150, and the mass ratio of acrylic acid to konjac glucomannan was 3.5:1. Concentrated sulfuric acid accounts for 1.5% of the volume of acrylic acid;
(2)魔芋葡甘聚糖酯化改性:按质量体积比(g/mL)为1∶250的比例将马来酸单月桂酯溶解于体积浓度为60%的乙醇中, 用体积浓度为20%的稀硫酸调pH值为4; 按马来酸单月桂酯和魔芋葡甘聚糖的质量比为1:15的比例加入魔芋葡甘聚糖, 搅拌均匀,在40℃温度下反应2h , 然后用体积浓度为60%的乙醇洗涤沉淀,过滤后将沉淀物在50℃下真空干燥, 得到物质B,碾碎备用; (2) Esterification modification of konjac glucomannan: Dissolve monolauryl maleate in ethanol with a volume concentration of 60% at a mass volume ratio (g/mL) of 1:250, and use a volume concentration of 20% dilute sulfuric acid to adjust the pH value to 4; add konjac glucomannan according to the mass ratio of monolauryl maleate and konjac glucomannan at a ratio of 1:15, stir evenly, and react at 40°C for 2 hours , and then washed the precipitate with ethanol with a volume concentration of 60%, filtered and dried the precipitate in vacuum at 50°C to obtain substance B, which was crushed for later use;
(3)魔芋葡甘聚糖仿丝浆液的制备: (3) Preparation of konjac glucomannan imitation silk slurry:
(a)取玉米淀粉,按质量体积比(g/mL)为1∶200的比例加入无菌水,在80℃条件下溶胀13h,分散,得到物质C ; (a) Take cornstarch, add sterile water at a ratio of mass volume ratio (g/mL) of 1:200, swell at 80°C for 13 hours, and disperse to obtain substance C;
(b)按质量体积(g/mL)比为1∶200的比例,取壳聚糖加入pH 3.5的乙酸水溶液中,搅拌溶解后在80℃条件下溶胀13h,分散,得到物质D; (b) According to the ratio of mass volume (g/mL) of 1:200, take chitosan and add it to acetic acid aqueous solution with pH 3.5, stir and dissolve, swell at 80°C for 13 hours, and disperse to obtain substance D;
(c)将步骤(1)制得的物质A和步骤(2)制得的物质B按照质量比为1∶1的比例混合,得到AB混合物;将物质C和物质D按照体积比为2∶1的比例混合,得到CD混合液;将AB混合物加到CD混合液中,然后在超声波功率150W、70℃下分散20min,得到魔芋葡甘聚糖仿丝浆液; (c) Mix the substance A prepared in step (1) with the substance B prepared in step (2) according to the mass ratio of 1:1 to obtain the AB mixture; mix substance C and substance D according to the volume ratio of 2: Mix at a ratio of 1 to obtain a CD mixture; add the AB mixture to the CD mixture, and then disperse for 20 minutes at an ultrasonic power of 150W and 70°C to obtain a konjac glucomannan silk-like slurry;
(4) 魔芋葡甘聚糖纤维湿纸巾的制备:将步骤(3)的魔芋葡甘聚糖仿丝浆液经过纤维湿法纺丝全套设备处理,即经过溶解、过滤、脱泡、计量、凝固、拉伸、洗涤、定型、卷绕、干燥后蒸煮熟化、冷冻杀菌后即得到纤维湿纸巾。所述纤维湿法纺丝全套设备,指型号为105,155,215的纤维湿法纺丝全套设备,溶解、过滤、脱泡、计量、凝固、拉伸、洗涤、定型、卷绕、干燥后蒸煮熟化、冷冻杀菌的全过程由纤维湿法纺丝全套设备参照现有技术完成;具体步骤如下: (4) Preparation of konjac glucomannan fiber wet wipes: process the konjac glucomannan silk-like slurry in step (3) through a complete set of fiber wet spinning equipment, that is, dissolve, filter, defoam, measure, and coagulate , Stretching, washing, shaping, winding, drying, cooking, freezing and sterilization to obtain fiber wet wipes. The full set of fiber wet spinning equipment refers to the full set of fiber wet spinning equipment with models 105, 155, and 215. The whole process of cooking, curing and freezing sterilization is completed by a complete set of fiber wet spinning equipment referring to the existing technology; the specific steps are as follows:
(a)纺丝:将步骤(3)的纺丝浆液经180目筛过滤,置于400mm汞柱的负压下脱泡0.8个小时后,以计量泵(压力1兆帕以上,最大流量:1200L/H)输送至纺丝冒(通常为3000至数万孔)挤出,丝束进入凝固浴,凝固浴中置有pH 4.5的体积浓度为98%的乙醇溶液,边凝固边拉伸,拉伸倍数控制在2.0,最后经pH4的体积浓度为70%酸性乙醇洗涤后卷绕,干燥至含水率为5%,成为魔芋葡甘聚糖高吸水性纤维; (a) Spinning: Filter the spinning slurry in step (3) through a 180-mesh sieve, place it under a negative pressure of 400 mm Hg for 0.8 hours, and then use a metering pump (pressure above 1 MPa, maximum flow: 1200L/H) to the spinning head (usually 3000 to tens of thousands of holes) for extrusion, the filaments enter the coagulation bath, and the coagulation bath is equipped with a pH 4.5 ethanol solution with a volume concentration of 98%, stretching while coagulating, The stretching ratio is controlled at 2.0, and finally, after being washed with 70% acidic ethanol with a volume concentration of pH4, it is wound up, dried to a moisture content of 5%, and becomes konjac glucomannan superabsorbent fiber;
(b)蒸煮熟化:将步骤(a)的魔芋葡甘聚糖高吸水性纤维制品置于绝对压力0.4Mpa,温度140℃的水蒸汽中,熟化25min;生丝熟化处理后,萃取丝胶制成丝胶水溶液,将丝胶水溶液装入湿纸巾模具中静置12个h后, 150℃蒸煮5h,制备成型料胚; (b) Cooking and maturing: put the konjac glucomannan superabsorbent fiber product in step (a) in water vapor with an absolute pressure of 0.4Mpa and a temperature of 140°C for 25 minutes; after raw silk maturation, extract sericin Sericin aqueous solution, put the sericin aqueous solution into a wet paper towel mold and let it stand for 12 hours, then cook at 150°C for 5 hours to prepare a molding blank;
(c)冷冻杀菌:在步骤(b)制得的成型料胚上均匀插孔后,将其在0℃条件下冷冻2d后解冻脱水;然后进行第二次冷冻,时间为6d,将冻好的半成品经解冻脱水、漂白、脱硫、杀菌即得新型魔芋葡甘聚糖纤维纸巾。 所述漂白剂为过氧化氢,所述杀菌剂为臭氧或紫外线。 (c) Freezing sterilization: After evenly inserting holes in the molded blanks prepared in step (b), freeze them at 0°C for 2 days and then thaw and dehydrate them; The semi-finished product is thawed and dehydrated, bleached, desulfurized, and sterilized to obtain a new type of konjac glucomannan fiber paper towel. Described bleaching agent is hydrogen peroxide, and described bactericide is ozone or ultraviolet ray.
(d)加湿包装:最后用水刺机将步骤(c)制得的魔芋葡甘聚糖纤维纸巾高压加固缠结,然后加湿、浸泡杀菌消毒液,密封包装。 (d) Humidification packaging: Finally, the konjac glucomannan fiber paper towel prepared in step (c) is reinforced and entangled under high pressure with a hydroentanglement machine, then humidified, soaked in sterilizing solution, and sealed for packaging.
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。 The above descriptions are only preferred embodiments of the present invention, and all equivalent changes and modifications made according to the scope of the patent application of the present invention shall fall within the scope of the present invention.
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| CN106117628A (en) * | 2016-07-28 | 2016-11-16 | 马鞍山市五谷禽业专业合作社 | The starch base composite mulching film that a kind of ageing resistace is excellent |
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