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WO2024016698A1 - 一种菌草纺丝用浆及其制备方法和应用 - Google Patents

一种菌草纺丝用浆及其制备方法和应用 Download PDF

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Publication number
WO2024016698A1
WO2024016698A1 PCT/CN2023/082466 CN2023082466W WO2024016698A1 WO 2024016698 A1 WO2024016698 A1 WO 2024016698A1 CN 2023082466 W CN2023082466 W CN 2023082466W WO 2024016698 A1 WO2024016698 A1 WO 2024016698A1
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WIPO (PCT)
Prior art keywords
juncao
spinning
preparation
pulp
temperature
Prior art date
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PCT/CN2023/082466
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English (en)
French (fr)
Inventor
谢跃亭
邵长金
张政峰
姚法全
邢善静
肖俊江
胡益杰
丁坤
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新乡化纤股份有限公司
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Application filed by 新乡化纤股份有限公司 filed Critical 新乡化纤股份有限公司
Priority to EP23737848.4A priority Critical patent/EP4332280A4/en
Priority to US18/263,962 priority patent/US12071725B2/en
Publication of WO2024016698A1 publication Critical patent/WO2024016698A1/zh

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00—Fibrous raw materials or their mechanical treatment
    • D21B1/02—Pretreatment of the raw materials by chemical or physical means
    • D21B1/023—Cleaning wood chips or other raw materials
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/003—Pulping cellulose-containing materials with organic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes
    • D21C3/222—Use of compounds accelerating the pulping processes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/12—Bleaching ; Apparatus therefor with halogens or halogen-containing compounds
    • D21C9/14—Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with ClO2 or chlorites
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10—Bleaching ; Apparatus therefor
    • D21C9/16—Bleaching ; Apparatus therefor with per compounds
    • D21C9/163—Bleaching ; Apparatus therefor with per compounds with peroxides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres

Definitions

  • the invention belongs to the technical field of new chemical textile materials, and specifically relates to a pulp for Juncao spinning and its preparation method and application.
  • Juncao Since the introduction of Juncao plants into my country, scientific and technological personnel have vigorously developed the Juncao industry technology of "replacing wood with grass.” At present, Juncao has been widely used in planting edible and medicinal fungi, improving soil moisture retention properties, and planting saline-alkali land, etc. to further reduce the degree of desertification in my country's land and improve the green development of the ecological environment. Juncao planting can achieve comprehensive utilization of agricultural resources such as water resources, light, and heat energy, and its growth cycle is much shorter than that of forest resources such as trees. Juncao has a high yield, and its roots can continue to thrive after being cut down and harvested. It can promote the development of the plant recycling industry chain and bring extensive economic benefits to society. For example, the Juncao variety "Oasis No. 1", which is currently widely planted in northern my country, has the advantages of having a yield of more than 25 tons per mu, can survive normally at minus 30 degrees Celsius, and can grow without water for 120 consecutive days.
  • the purpose of the present invention is to provide a pulp for Juncao spinning and its preparation method and application.
  • a first aspect of the present invention provides a method for preparing pulp for Juncao spinning.
  • the specific steps are as follows: placing Juncao in a solution prepared from alkali, a catalyst and an auxiliary agent, cooking it, and then obtaining Juncao spinning pulp through a pulping process.
  • the metal chloride salt is at least one of cobalt chloride, calcium chloride, ferric chloride, ferrous chloride and nickel chloride.
  • the polyether water-soluble organic substance is aromatic polyoxyethylene ether, polyoxyethylene or polyvinyl ether.
  • the polyether water-soluble organic substance is polyethylene oxide.
  • the degree of polymerization of the polyethylene oxide is 9 to 12.
  • the polyethylene oxide has a degree of polymerization of 10.
  • the purity of the polyethylene oxide is 95wt% to 99wt%.
  • the purity of the polyethylene oxide is 95wt%.
  • the bicarbonate is sodium bicarbonate or potassium bicarbonate.
  • the bicarbonate is replaced by carbonate; the carbonate is potassium carbonate or sodium carbonate.
  • the Juncao is calculated as dry Juncao
  • the polyether water-soluble organic matter is calculated as active ingredients
  • the added amount of the catalyst is 0.01wt% to 0.3wt% of Juncao
  • the bicarbonate is The added amount is 0.01wt% to 0.1wt% of the Juncao
  • the volume/mass ratio of the polyether water-soluble organic matter to the Juncao is (1-12)/(2-3) mL/kg.
  • the alkali solution is potassium hydroxide solution or sodium hydroxide solution, and the alkali solution concentration is 105-120g/L.
  • the cooking temperature is 160-175°C, and the cooking time is 4-6 hours.
  • the Juncao is pretreated before cooking.
  • the pretreatment process is as follows: cutting the Juncao into sections, sterilizing and drying, screening the internodes, preheating at high temperature and then performing the cooking process, which can reduce the preparation time. Sugar content of the slurry.
  • the disinfectant used in the disinfection is at least one of alcohol solution, acid solution or glycol derivatives; the temperature of the disinfection is 25-45°C.
  • the high-temperature preheating temperature is 135-175°C and the time is 30-120 minutes.
  • the high-temperature preheating can promote the production of organic acids by the fungus itself, facilitate the precipitation of hemicellulose, and save cost, which is conducive to the mass production of pulp for Juncao spinning.
  • the fungi need to be repeatedly washed with water to remove impurities before the cooking process is carried out; the temperature of the washing is 30 to 100°C.
  • the steps of obtaining pulp for Juncao spinning through the pulping process include: beating, bleaching, sheet making, and shaping to obtain Pulp for Juncao spinning.
  • the beating speed is 8.0 to 8.5 r/s
  • the beating temperature is 15 to 35°C
  • the belt rotation speed ratio is 260 to 285
  • the beating time is 0.5 to 1 hour.
  • the bleaching agent used in the bleaching is any one of hydrogen peroxide, chlorine dioxide, sodium hypochlorite and calcium hypochlorite.
  • the bleaching time is 10 to 60 minutes, and the bleaching temperature is 30 to 70°C.
  • a gray-removing iron agent needs to be added, and then the pulp for Juncao spinning can be obtained by papermaking and shaping.
  • desalted water is used to form the slurry, and the spraying volume of desalted water is 30 to 45 m 3 /h.
  • the dosage of the gray iron removal agent is 0.01% to 0.08% of the absolute dry slurry.
  • a second aspect of the present invention provides a Juncao spinning pulp prepared by the above method.
  • the third aspect of the present invention provides the application of the above-mentioned Juncao spinning pulp in spinning.
  • the present invention has the following advantages:
  • the Juncao is first subjected to high-temperature preheating treatment, and then the Juncao is cooked under the action of an appropriate amount of catalysts and auxiliaries, and finally the pulp for Juncao spinning is obtained through the pulping process.
  • the invention realizes the research and development of efficiently preparing Juncao spinning pulp, greatly improves the comprehensive added value of Juncao, has broad prospects, and can bring better economic benefits to enterprises for mass production.
  • metal chloride is selected as the catalyst, and polyether water-soluble organic matter and/or bicarbonate (or replaced by carbonate) is used as the auxiliary agent.
  • Metal chloride salts can break the glycosidic bonds in cellulose during the alkalization process, thereby accelerating the degradation of cellulose.
  • Polyether water-soluble organic substances can significantly reduce the surface tension of the alkali solution and promote the penetration of the alkali solution into the cellulose molecules.
  • Bicarbonate or carbonate solutions can penetrate into the cellulose crystallization area and increase the amount of fiber voids.
  • the present invention adds catalysts and auxiliaries to the reaction system at the same time, especially when polyether water-soluble organic matter and bicarbonate (or carbonate) are compounded as auxiliaries, their synergistic effect can be used to enhance the penetration and dispersion of the Juncao fiber. , accelerate the oxidative degradation of fiber, Reduce its degree of polymerization and effectively reduce fiber viscosity, which is conducive to efficient extraction of Juncao fiber.
  • the present invention selects internodal Juncao for production and research, and eliminates nodules and mildewed materials, so that the internodal part of Juncao accounts for more than 98% of the input raw materials.
  • the prepared Juncao spinning slurry has higher quality, and the slurry The physical and chemical indicators are good (fiber viscosity 14-20mPa.s, ⁇ -cellulose content above 91%).
  • the preparation method provided by the present invention has a low degree of corrosion on production equipment, a safe and stable operation process, and an environmentally friendly and pollution-free preparation process. It can realize the absolute advantage of high-value reuse of Juncao raw materials and help the chemical fiber industry to save energy and reduce emissions.
  • the present invention provides new ideas for the development and utilization of Juncao raw materials. According to the characteristics of Juncao raw materials such as wide planting area and extremely rich output, it can meet the domestic textile enterprises’ demand for plant cellulose and will significantly reduce the consumption of chemical fiber enterprises. Material cost of plant fibers. At the same time, under the national strategic layout, through the high-value utilization of biomass Juncao, "replacing wood with grass” can reduce the felling of forest trees, which can further protect the ecological environment and meet the requirements of the national efficient development strategy.
  • Spinning pulp generally needs to meet the following standards: fiber viscosity (cupra ammonia solution method) ⁇ 20mPa.s, ⁇ -cellulose content ⁇ 90.0%, polypentose content ⁇ 7%, reactivity (viscose filtration method) ⁇ 500s.
  • fiber viscosity is 14mPa.s ⁇ 20mPa.s
  • ⁇ -cellulose content is 91.0% ⁇ 94.0%
  • polypentane content is 91.0% ⁇ 94.0%.
  • the sugar content is ⁇ 4.92%
  • the resin content is ⁇ 0.13%
  • the reaction performance is within 0 to 250 seconds, which meets the standards for spinning pulp.
  • step (3) Perform beating treatment on the primary Juncao pulp obtained in step (3).
  • the beating temperature is 30°C and the beating time is 0.5h.
  • a gray iron removal agent is added, and the Juncao spinning is obtained by papermaking and pressing. Silk pulp.
  • the present invention uses the copper ammonia solution method to measure fiber viscosity, and the viscose filtration method to measure the reaction performance of Juncao spinning slurry.
  • Reaction performance reflects the degree of dissolution or uniformity of pulp.
  • Fiber glue prepared from dissolving pulp with low reactivity often contains varying degrees of undissolved/semi-dissolved components, which can easily block the micropores of the spinning nozzle and cause processing difficulties. , affects the quality of the finished yarn, increases the carbon disulfide consumption per unit product, and brings negative impacts to viscose fiber production in terms of cost, efficiency, product quality, environmental protection and other aspects.
  • the physical and chemical indicators of the Juncao spinning slurry obtained in this example are as follows: fiber viscosity 14.5 mPa.s, ⁇ -cellulose content 91.3%, polypentose content 4.92%, resin content 0.13%, and reaction performance 52s.
  • step (3) Perform beating treatment on the primary Juncao pulp obtained in step (3).
  • the beating temperature is 30°C and the beating time is 0.5h.
  • a gray iron removal agent is added, and the Juncao pulp is made and pressed to obtain Juncao. Spinning pulp.
  • the physical and chemical indicators of the obtained Juncao spinning pulp are as follows: cupro ammonia viscosity 14.3 mPa.s, ⁇ -cellulose content 91.4%, polypentose content 4.7%, resin content 0.07%, and reaction performance 234s.
  • step (3) Perform beating treatment on the primary Juncao pulp obtained in step (3).
  • the beating temperature is 30°C and the beating time is 0.5h.
  • a gray iron removal agent is added, and the Juncao pulp is made and pressed to obtain Juncao. Spinning pulp.
  • the physical and chemical indicators of the obtained Juncao spinning pulp are as follows: cupro ammonia viscosity 18.7 mPa.s, ⁇ -cellulose content 91.7%, polypentose content 5.28%, resin content 0.08%, reaction performance 22s.
  • step (3) Perform beating treatment on the primary Juncao pulp obtained in step (3).
  • the beating temperature is 30°C and the beating time is 0.5h.
  • a gray iron removal agent is added, and the Juncao pulp is made and pressed to obtain Juncao. Spinning pulp.
  • the physical and chemical indicators of the obtained Juncao spinning pulp are as follows: fiber viscosity 19.8 mPa.s, ⁇ -cellulose content 93.8%, polypentose content 6.66%, resin content 0.16%, reaction performance ⁇ 500s.
  • Comparative Example 1 The content of Comparative Example 1 is basically the same as that of Example 1, except that no catalyst is added during the cooking process.
  • the physical and chemical indicators of the Juncao spinning slurry prepared in Comparative Example 1 are as follows: fiber viscosity 21.7 mPa.s, ⁇ -cellulose content 91.8%, polypentose content 4.38%, resin content 0.13%, and reaction performance >500s.
  • Comparative Example 2 The content of Comparative Example 2 is basically the same as that of Example 1, except that no auxiliary agent is added during the cooking process.
  • the physical and chemical indicators of the Juncao spinning slurry prepared in Comparative Example 2 are as follows: fiber viscosity 22.4 mPa.s, ⁇ -cellulose content 92.6%, polypentose content 5.51%, resin content 0.14%, and reaction performance >500s.
  • Comparative Example 3 The content of Comparative Example 3 is basically the same as that of Example 1, except that no catalyst or auxiliary agent is added during the cooking process.
  • the physical and chemical indicators of the Juncao spinning slurry prepared in Comparative Example 3 are as follows: fiber viscosity 125.7 mPa.s, ⁇ -cellulose content 88.2%, polypentose content 16.68%, and reaction performance >500s.
  • the fiber viscosity of the pulp for Juncao spinning can be maintained in the range of 14.0 to 15.0 mPa.s, and the reaction performance is excellent.

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Abstract

一种菌草纺丝用浆及其制备方法和应用，制备方法为：将菌草置于由碱液、催化剂和助剂配制的溶液中蒸煮，再通过制浆过程得到菌草纺丝用浆。实现了高效制备菌草纺丝用浆，与现有技术对比，菌草纺丝用浆品质较高，浆料物化指标良好，对生产设备腐蚀程度偏低，操作过程安全、稳定、环保，将大幅度提升菌草的综合附加值，可供企业量产化投产。

Description

一种菌草纺丝用浆及其制备方法和应用
本申请要求于于2022年7月22日提交中国专利局、申请号为CN202210862610.7、发明名称为“一种菌草纺丝用浆及其制备方法和应用”的中国专利申请以及2022年8月30日提交中国专利局、申请号为CN202211048526.8、发明名称为“一种菌草纺丝用浆及其制备方法和应用”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明属于化学纺织新材料技术领域，具体涉及一种菌草纺丝用浆及其制备方法和应用。
背景技术
自菌草植物引入我国后，科技人员大力发展“以草代木”菌草产业技术。目前，菌草已经广泛应用于食药用菌种植、提升土壤水分保持特性、盐碱土地种植等方面，以进一步降低我国土地荒漠化程度，改善生态环境绿色发展。菌草种植可以实现水资源、光照、热能等农业资源的综合利用，其生长周期远低于树木等森林资源。菌草产量高，经砍伐收割后根系可继续繁衍生长，能够促进植物循环利用产业链发展，为社会带来广泛的经济效益。例如，目前广泛种植于我国北方的菌草品种“绿洲一号”，自身具备亩产高达25余吨、零下30℃正常生存、可连续120天断水生长等优势。
现阶段，生物质菌草纤维素仅用于农业种植、生态修复，还未曾应用于化纤纺织新材料领域，具有可观的综合利用价值。而纺织用化纤、木浆粕成本高，下游纺织企业生产价格成本高。另外，由于受疫情影响，国外木浆、棉浆无法及时供应国内厂家生产使用，造成国内货存量不足，因此，开发能够替代木浆、棉浆的菌草纤维纺丝用浆具有重要意义。
发明内容
针对现有技术中存在的问题和不足，本发明的目的旨在提供一种菌草纺丝用浆及其制备方法和应用。
为实现上述目的，本发明采用以下技术方案：
本发明第一方面提供一种菌草纺丝用浆的制备方法，具体步骤为：将菌草置于由碱液、催化剂和助剂配制的溶液中蒸煮，再通过制浆过程得到菌草纺丝用浆；所述催化剂为金属氯化盐，所述助剂为聚醚类水溶性有机物和/或碳酸氢盐。
优选地，所述金属氯化盐为氯化钴、氯化钙、氯化铁、氯化亚铁和氯化镍的至少一种。
优选地，所述聚醚类水溶性有机物为芳香基聚氧乙烯醚、聚氧化乙烯或聚乙烯醚。
更为优选的，所述聚醚类水溶性有机物优选为聚氧化乙烯。
优选地，所述聚氧化乙烯的聚合度为9～12。
更为优选地，所述聚氧化乙烯的聚合度为10。
更为优选地，所述聚氧化乙烯的纯度为95wt％～99wt％。
更为优选地，所述聚氧化乙烯的纯度为95wt％。
优选地，所述碳酸氢盐为碳酸氢钠或碳酸氢钾。
优选地，所述碳酸氢盐替换为碳酸盐；所述碳酸盐为碳酸钾或碳酸钠。
优选地，所述菌草以干菌草计，所述聚醚类水溶性有机物以有效成分计，所述催化剂的添加量为菌草的0.01wt％～0.3wt％，所述碳酸氢盐的添加量为所述菌草的0.01wt％～0.1wt％，所述聚醚类水溶性有机物与所述菌草的体积/质量比为(1～12)/(2～3)mL/kg。
优选地，所述碱液为氢氧化钾溶液或氢氧化钠溶液，碱液浓度为105～120g/L。
优选地，所述蒸煮温度为160～175℃，蒸煮时间4～6h。
优选地，蒸煮前先对菌草进行预处理，所述预处理的过程为：将菌草切段、消毒、干燥后，筛选节间菌草，高温预加热后再进行蒸煮过程，可以降低制备浆料的糖分含量。
更为优选地，所述消毒使用的消毒液为醇溶液、酸溶液或二元醇衍生物类中的至少一种；所述消毒的温度为25～45℃。
更为优选地，所述高温预加热的温度为135～175℃，时间为30～120min，所述高温预加热可以促进菌草自身产生有机酸，便于半纤维素的析出，节约 成本，利于菌草纺丝用浆量产化。
更为优选地，所述高温预加热后需要用水反复清洗菌草，除去杂质后再进行蒸煮过程；所述清洗的温度为30～100℃。
优选地，所述通过制浆过程得到菌草纺丝用浆的步骤为：打浆、漂白、抄造、成型，得到菌草纺丝用浆。
更为优选地，所述打浆的转速为8.0～8.5r/s，打浆温度为15～35℃，皮带转动速比为260～285，打浆时间为0.5～1h。
更为优选地，所述漂白使用的漂白剂为过氧化氢、二氧化氯、次氯酸钠和次氯酸钙中的任意一种。
更为优选地，所述漂白的时间为10～60min，漂白温度30～70℃。
更为优选地，打浆、漂白后需加入除灰铁药剂，再经抄造、成型得到菌草纺丝用浆。
更为优选地，采用脱盐水对浆料进行抄造成型，脱盐水的喷洒量为30～45m3/h。
更为优选地，所述除灰铁药剂的用量为绝干浆量的0.01％～0.08％。
本发明第二方面提供了一种由上述方法制备的菌草纺丝用浆。
本发明第三方面提供了上述菌草纺丝用浆在纺丝中的应用。
与现有技术相比，本发明具有以下优点：
1.本发明是先将菌草进行高温预加热处理，然后在适量催化剂与助剂作用下对菌草进行蒸煮，最后通过制浆过程得到菌草纺丝用浆。本发明实现了高效制备菌草纺丝用浆的研发，大幅度提升了菌草的综合附加值，前景广阔，能为企业量产化投产带来更好的经济效益。
2.本发明选择金属氯化盐作为催化剂，聚醚类水溶性有机物和/或碳酸氢盐(或替换为碳酸盐)作为助剂。金属氯化盐在碱化过程中能够促使纤维素内的糖苷键断裂，从而加速纤维素的降解。聚醚类水溶性有机物能够显著降低碱液的表面张力，促进碱液向纤维素分子间渗透，碳酸氢盐或碳酸盐溶液可以渗入纤维素结晶区，增大纤维空隙量。本发明将催化剂和助剂同时加入反应体系，尤其是聚醚类水溶性有机物与碳酸氢盐(或碳酸盐)复配作为助剂时，可利用其协同作用加强菌草纤维的渗透与疏散，加速纤维氧化降解， 减小其聚合度，有效降低纤维粘度，有利于高效提取菌草纤维。
3.本发明挑选节间菌草进行生产研发，剔除了结节及霉变物料，使得菌草节间部分占投入原料的98％以上，制备的菌草纺丝用浆品质较高，浆料物化指标良好(纤维粘度14～20mPa.s，α-纤维素含量91％以上)。同时，本发明提供的制备方法对生产设备腐蚀程度偏低，操作过程安全、稳定，制备过程环保无污染，可实现菌草原料高值化再利用的绝对优势，助力化纤行业节能减排行动。
4.本发明为菌草原料的开发利用提供了新思路，根据菌草原料具有种植区域广、产量极为丰富等特点，可满足国内纺织企业对植物纤维素的用量需求，将大幅度降低化纤企业植物纤维的物料成本。同时，在国家战略布局下，通过生物质菌草的高值化利用，“以草代木”减少森林树木砍伐，能够进一步保护生态环境，符合国家高效发展战略要求。
5.纺丝用浆一般需达到以下标准：纤维粘度(铜氨溶液法)＜20mPa.s，α-纤维素含量≥90.0％，多戊糖含量＜7％，反应性能(黏胶过滤法)＜500s。本发明通过在蒸煮过程添加催化剂和助剂，制得具有优良性能的菌草纺丝用浆，其纤维粘度为14mPa.s～20mPa.s，α-纤维素含量91.0％～94.0％，多戊糖含量＜4.92％，树脂含量＜0.13％，反应性能处于0～250s内，符合纺丝用浆的标准。
具体实施方式
以下通过具体的实施例对本发明作进一步说明，但并不限制本发明的范围。
实施例1：
一种菌草纺丝用浆的制备方法，具体步骤如下：
(1)取菌草干草或鲜草，将其切段制成边长为1～2.5cm的块状物料，使用浓度为50％～95％的乙醇溶液对菌草消毒；用水反复冲洗消毒后的菌草；烘干菌草；挑选节间菌草，使菌草节间部分占投入原料98％以上，备用；
(2)取2kg备好的菌草原料置于蒸煮容器中，采用蒸汽与水混合介质对菌草原料进行预加热处理，预加热温度为170℃，保温时间100min；
(3)将预加热处理后的菌草用水去除杂质后再次投入蒸煮容器内，相 继加入浓度为120g/L的氢氧化钠溶液8L、氯化亚铁2g、聚氧化乙烯(聚合度＝10，纯度＝95wt％)5mL和碳酸氢钠2.5g，于170℃下蒸煮5h，得到菌草初制浆料；
(4)对步骤(3)得到的菌草初制浆料进行打浆处理，打浆温度30℃，打浆时间0.5h；再经过漂白处理后加入除灰铁药剂，抄造、压榨成型，得到菌草纺丝用浆。
本发明采用铜氨溶液法测定纤维粘度，黏胶过滤法测定菌草纺丝用浆的反应性能。
黏胶过滤法的具体操作为：浆粕样品首先被溶解于NaOH和二硫化碳的混合液形成黏胶，然后采用10000孔/cm2的滤网对黏胶液进行过滤，滤网下放一个量筒，当量筒内滤液到达25ml时掐秒表，到达50ml时记录时间，记S1，到达125ml时再次掐秒表，到达150ml时记录时间，记S2。反应性能＝S2-S1。
反应性能反映的是浆粕的溶解程度或均匀程度，反应性能低下的溶解浆制备的纤维胶液往往含有不同程度的未溶解/半溶解组分，容易堵塞纺丝喷嘴的微孔，造成加工困难，影响成丝品质，并增加单位产品的二硫化碳耗用量，给黏胶纤维生产带来成本、效率、产品质量、环保等多方面的负面影响。
本实施例所得菌草纺丝用浆各物化指标如下：纤维粘度14.5mPa.s，α-纤维素含量91.3％，多戊糖含量4.92％，树脂含量0.13％，反应性能52s。
实施例2：
一种菌草纺丝用浆的制备方法，具体步骤如下：
(1)取菌草干草或鲜草，将其切段制成边长为1～2.5cm块状物料，使用浓度为50％～95％的乙醇溶液对菌草消毒；用水反复冲洗消毒后的菌草；烘干菌草；挑选节间菌草，使节间部分占投入原料98％以上，备用；
(2)取2kg备好的菌草原料置于蒸煮容器中，采用蒸汽与水混合介质对菌草原料进行预加热处理，预加热处理温度为170℃，保温时间为2h；
(3)将预加热处理后的菌草用水去除杂质后再次投入蒸煮容器内，相继加入浓度为120g/L的氢氧化钾溶液8L、氯化亚铁4.0g、聚氧化乙烯(聚合度＝10，纯度＝95wt％)10mL和碳酸氢钠2.5g，于170℃下蒸煮5h，得 到菌草初制浆料；
(4)对步骤(3)得到的菌草初制浆料进行打浆处理，打浆温度30℃，打浆时间为0.5h；再经过漂白处理后加入除灰铁药剂，抄造、压榨成型，得到菌草纺丝用浆。
所得菌草纺丝用浆各物化指标如下：铜氨粘度14.3mPa.s，α-纤维素含量91.4％，多戊糖含量4.7％，树脂含量0.07％，反应性能234s。
实施例3：
一种菌草纺丝用浆的制备方法，具体步骤如下：
(1)取菌草干草或鲜草，将其切段制成边长为1～2.5cm块状物料，使用浓度为50％～95％的乙醇溶液对菌草消毒；用水反复冲洗消毒后的菌草；烘干菌草；挑选节间菌草，使得节间部分占投入原料98％以上，备用；
(2)取2kg备好的菌草原料置于蒸煮容器中，采用蒸汽与水混合介质对菌草原料进行预加热处理，预加热处理温度为169℃，保温时间为100min；
(3)将预加热处理后的菌草用水去除杂质后再次投入蒸煮容器内，相继加入浓度为115g/L的氢氧化钾溶液8L、氯化亚铁3g和聚氧化乙烯(聚合度＝10，纯度＝95wt％)10mL，于170℃下蒸煮6h，得到菌草初制浆料；
(4)对步骤(3)得到的菌草初制浆料进行打浆处理，打浆温度30℃，打浆时间为0.5h；再经过漂白处理后加入除灰铁药剂，抄造、压榨成型，得到菌草纺丝用浆。
所得菌草纺丝用浆各物化指标如下：铜氨粘度18.7mPa.s，α-纤维素含量91.7％，多戊糖含量5.28％，树脂含量0.08％，反应性能22s。
实施例4：
一种菌草纺丝用浆的制备方法，具体步骤如下：
(1)取菌草干草或鲜草，将其切段制成边长为1～2.5cm块状物料，使用浓度为50％～95％的乙醇溶液对菌草消毒；用水反复冲洗消毒后的菌草；烘干菌草；挑选节间菌草，使得节间部分占投入原料98％以上，备用；
(2)取2kg备好的菌草原料置于蒸煮容器中，采用蒸汽与水混合介质对菌草原料进行预加热处理，预加热处理温度为170℃，保温时间为1h；
(3)将预加热处理后的菌草用水去除杂质后再次投入蒸煮容器内，相 继加入浓度为120g/L的氢氧化钾溶液8L、氯化亚铁4.0g和聚氧化乙烯(聚合度＝10，纯度＝95wt％)6mL，于169℃下蒸煮4.5h，得到菌草初制浆料；
(4)对步骤(3)得到的菌草初制浆料进行打浆处理，打浆温度30℃，打浆时间为0.5h；再经过漂白处理后加入除灰铁药剂，抄造、压榨成型，得到菌草纺丝用浆。
所得菌草纺丝用浆各物化指标如下：纤维粘度19.8mPa.s，α-纤维素含量93.8％，多戊糖含量6.66％，树脂含量0.16％，反应性能<500s。
对比例1：
对比例1的内容与实施例1基本相同，其不同之处在于，蒸煮过程中不加催化剂。
对比例1制备的菌草纺丝用浆的物化指标如下：纤维粘度21.7mPa.s，α-纤维素含量91.8％，多戊糖含量4.38％，树脂含量0.13％，反应性能>500s。
对比例2：
对比例2的内容与实施例1基本相同，不同之处在于，蒸煮过程中不加助剂。
对比例2制备的菌草纺丝用浆的物化指标如下：纤维粘度22.4mPa.s，α-纤维素含量92.6％，多戊糖含量5.51％，树脂含量0.14％，反应性能>500s。
对比例3：
对比例3的内容与实施例1基本相同，不同之处在于，蒸煮过程中不加催化剂和助剂。
对比例3制备的菌草纺丝用浆的物化指标如下：纤维粘度125.7mPa.s，α-纤维素含量88.2％，多戊糖含量16.68％，反应性能>500s。
通过上述实验结果可知，对比例3在蒸煮过程中未加入催化剂和助剂，制备的浆料纤维粘度较大，α-纤维素含量较低，不符合纺丝用浆的标准。在加入催化剂(对比例2)或助剂(对比例1)后，浆料的纤维粘度明显降低，但反应性能不符合纺丝用浆标准。而当同时加入催化剂和助剂(实施例1～4)后，所得菌草纺丝用浆的纤维粘度可降低至14～20mPa.s，尤其当助剂为聚 醚类水溶性有机物与碳酸氢盐的混合物(实施例1～2)时，菌草纺丝用浆的纤维粘度可保持在14.0～15.0mPa.s范围，且反应性能优异。
上述结果说明，在蒸煮过程中催化剂和助剂对浆料的纤维粘度、树脂含量、反应性能等均有较大影响，这是由于催化剂在碱化过程中能够促使纤维素内的糖苷键断裂，从而促进纤维素的降解。聚醚类水溶性有机物可以有效降低碱液的表面张力，有利于碱液向纤维素分子间渗透，碳酸氢盐溶液可以渗入纤维素结晶区，增大纤维空隙量。因此，将催化剂和助剂同时加入反应体系，尤其聚醚类水溶性有机物与碳酸氢盐复配作为助剂时，可利用其协同作用加强菌草纤维的渗透与疏散，加速纤维氧化降解，减小其聚合度，有效降低纤维粘度，提升反应性能。
上述实施例为本发明的具体实施方式，但本发明的实施方式并不受上述实施例的限制，其它任何不超出本发明设计思路组合、改变、修饰、替代、简化，均落入本发明的保护范围之内。

Claims (18)

  1. 一种菌草纺丝用浆的制备方法，其特征在于，将菌草置于由碱液、催化剂和助剂配制的溶液中蒸煮，再通过制浆过程得到菌草纺丝用浆；所述催化剂为金属氯化盐，所述助剂为聚醚类水溶性有机物和/或碳酸氢盐。
  2. 根据权利要求1所述的制备方法，其特征在于，所述金属氯化盐为氯化钴、氯化钙、氯化铁、氯化亚铁和氯化镍中的至少一种。
  3. 根据权利要求1所述的制备方法，其特征在于，所述聚醚类水溶性有机物为芳香基聚氧乙烯醚、聚氧化乙烯或聚乙烯醚。
  4. 根据权利要求3所述的制备方法，其特征在于，所述聚氧化乙烯的聚合度为9～12。
  5. 根据权利要求1所述的制备方法，其特征在于，所述碳酸氢盐为碳酸氢钠或碳酸氢钾。
  6. 根据权利要求1所述的制备方法，其特征在于，所述碳酸氢盐替换为碳酸盐；所述碳酸盐为碳酸钾或碳酸钠。
  7. 根据权利要求1～6任一项所述的制备方法，其特征在于，所述菌草以干菌草计，所述聚醚类水溶性有机物以有效成分计，所述催化剂的添加量为所述菌草的0.01wt％～0.3wt％，所述碳酸氢盐的添加量为所述菌草的0.01wt％～0.1wt％，所述聚醚类水溶性有机物与所述菌草的体积/质量比为(1～12)/(2～3)mL/kg。
  8. 根据权利要求1所述的制备方法，其特征在于，所述碱液为氢氧化钾溶液或氢氧化钠溶液；所述碱液的浓度为105～120g/L。
  9. 根据权利要求1或5所述的制备方法，其特征在于，所述蒸煮的温度为160～175℃，蒸煮时间4～6h。
  10. 根据权利要求1所述的制备方法，其特征在于，所述蒸煮前先对菌草进行预处理，所述预处理的过程为：将菌草切段、消毒、干燥后，筛选节间菌草，高温预加热；所述高温预加热的温度为135～175℃。
  11. 根据权利要求10所述的制备方法，其特征在于，所述消毒使用的消毒液为醇溶液、酸溶液或二元醇衍生物类中的至少一种；所述消毒的温度为25～45℃。
  12. 根据权利要求10或11所述的制备方法，其特征在于，所述高温预 加热后，用水反复清洗菌草，所述清洗的温度为30～100℃；
    所述高温预加热的时间为30～120min。
  13. 根据权利要求1所述的制备方法，其特征在于，所述通过制浆过程得到菌草纺丝用浆的步骤为：打浆、漂白、抄造、成型，得到菌草纺丝用浆。
  14. 根据权利要求13所述的制备方法，其特征在于，所述打浆的转速为8.0～8.5r/s，打浆温度为15～35℃，皮带转动速比为260～285，打浆时间为0.5～1h；
    所述漂白使用的漂白剂为过氧化氢、二氧化氯、次氯酸钠和次氯酸钙中的任意一种；所述漂白的时间为10～60min，漂白温度30～70℃；
    所述抄造为采用脱盐水对浆料进行抄造，脱盐水的喷洒量为30～45m3/h。
  15. 根据权利要求13或14所述的制备方法，其特征在于，所述通过制浆过程得到菌草纺丝用浆的步骤为：打浆、漂白后加入除灰铁药剂，再经抄造、成型，得到菌草纺丝用浆；所述除灰铁药剂的用量为绝干浆量的0.01％～0.08％。
  16. 一种利用权利要求1～15任一所述方法制备的菌草纺丝用浆。
  17. 根据权利要求16所述的菌草纺丝用浆，其特征在于，所述菌草纺丝用浆的纤维粘度14～20mPa.s，α-纤维素含量91％以上，多戊糖含量＜4.92％，树脂含量＜0.13％，反应性能为0～250s；所述纤维粘度采用铜氨溶液法测试得到；所述反应性能采用黏胶过滤法测试得到。
  18. 权利要求16或17所述的菌草纺丝用浆在纺丝中的应用。
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