WO2019047177A1 - 一种含有天然基纤维的废旧涤纶混纺织物的回收方法 - Google Patents

一种含有天然基纤维的废旧涤纶混纺织物的回收方法 Download PDF

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WO2019047177A1
WO2019047177A1 PCT/CN2017/101112 CN2017101112W WO2019047177A1 WO 2019047177 A1 WO2019047177 A1 WO 2019047177A1 CN 2017101112 W CN2017101112 W CN 2017101112W WO 2019047177 A1 WO2019047177 A1 WO 2019047177A1
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polyester
fiber
fibers
natural
recycling
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PCT/CN2017/101112
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English (en)
French (fr)
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葛仪文
姚磊
廖骁
刘洋
卓嘉良
陈学聪
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香港纺织及成衣研发中心
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Priority to PCT/CN2017/101112 priority Critical patent/WO2019047177A1/zh
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
    • C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Definitions

  • the invention belongs to the field of textile resource regeneration, and particularly relates to a method for recycling waste polyester blended fabric containing natural fiber.
  • Polyester is an important variety in synthetic fibers and is a fiber made by spinning and post-treating polyethylene terephthalate high polymer (PET).
  • Polyester blended fabric is a textile product made by blending polyester fiber with other fibers of cotton, wool, silk and hemp.
  • the main polyester blend fabrics include polyester-cotton blended fabric, wool-polyester blended fabric, polyester-woven blended fabric, and polyester-viscose.
  • the recycling method of the polyester blended fabric is to separate the polyester with other components such as cotton fibers, and then separately recover them in a targeted manner.
  • the solvents used in the conventional methods are mostly highly toxic, high in cost and harmful to the environment.
  • most of the existing methods are difficult to completely separate the recovered materials and affect the purity of the recovery.
  • the object of the present invention is to provide an efficient method for recovering waste polyester blended fabric containing natural-based fibers.
  • the method for recovering waste polyester blended fabric containing natural-based fibers comprises the following steps:
  • step S3 the solid insoluble matter obtained in the step S1 is immersed in an ester solvent to be dissolved at a temperature of 150 to 210 ° C, and then a C1-C3 fatty alcohol is added to precipitate a polyester solid for recovery;
  • water-soluble tertiary amine oxide used in the step S1 is selected from the group consisting of dimethylethanolamine oxide, trimethylamine oxide, N-methylmorpholine-N-oxide, N-methylpiperidine-N-oxide One or more of N-methylpyrrolidine-N-oxide The combination;
  • the ester solvent used in the step S3 has the structure of the formula (1):
  • R represents a linear or branched alkyl group of C1 to C5, and n represents an integer of 1 to 3.
  • the waste polyester blended fabric has a polyester content of 10% to 90% by weight and a water content of less than 10% by weight.
  • the natural base fiber in the waste polyester blend fabric comprises protein-based fibers and/or cellulose-based fibers, wherein the protein-based fibers comprise silk and/or wool, and the cellulose-based fibers A combination of one or more of cotton fiber, hemp fiber, viscose fiber, modal fiber, lyocell fiber, cuprammonium fiber, acetate fiber.
  • the content of the protein-based fiber in the waste polyester blended fabric is less than 30% by weight.
  • the water-soluble tertiary amine oxide solution in the step S1 has a water content of 10% to 15% by weight.
  • the antioxidant is selected from the group consisting of catechol, 1,2,3-benzenetriol, propyl gallate, 2,6-di-tert-butyl-p-cresol, gallic acid, and gallic acid.
  • the weight ratio of the waste-based polyester blend fabric containing the natural base fiber to the water-soluble tertiary amine oxide solution in the step S1 is 1:99 to 15:85.
  • the process of dissolving the natural base fiber in the step S1 comprises swelling at 60 to 75 ° C for 20 to 30 minutes, and then heating to 80 to 130 ° C for 50 to 90 minutes.
  • the wet spinning process in the step S2 comprises spinning the fiber solution obtained in the step S1 into water and/or ethanol, and mechanically stretching 3 to 10 times to obtain a regenerated natural base fiber. Plain fiber.
  • the ester solvent used in the step S3 is selected from the group consisting of methyl benzoate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate. a combination of one or more of dimethyl terephthalate and dimethyl isophthalate; the weight ratio of the weight of the polyester to the ester solvent in the waste polyester blended fabric is 1:1.1 1:50.
  • the reaction time in the step S3 is 3 to 30 min.
  • the volume ratio of the dissolved polyester solution to the fatty alcohol is 1:15 to 1:50, and after the fatty alcohol is added, the temperature is lowered to 45 to 65 ° C to precipitate. Polyester solid.
  • the fatty alcohol is selected from the group consisting of methanol or ethanol.
  • the step S3 further comprises the step of thickening the obtained polyester solid to reach the requirements of the spinning section.
  • the step S3 further comprises separately separating the polyester solids and recovering the fatty alcohol and the ester solvent.
  • the recycling method of the present invention can completely and completely separate polyester and other natural base fibers, and the recovered polyester and recycled natural-based cellulose fibers have high purity and high recovery rate, and the recovered polyester can basically retain the original physics. Chemical performance and obvious economic advantages.
  • the recycling method of the present invention is advanced in process, and high-quality regenerated protein/cellulose fiber can be obtained by only one dissolution-regeneration process.
  • the recycling method of the present invention can be applied to all kinds of polyester-blended polyester blended fabrics, and has a wide application range, which fills the gap existing in the prior art.
  • the recycling method of the present invention avoids the use of highly toxic and irritating chemical reagents, and the reagents used can be recycled and recycled, further reducing the process cost and reducing the environmental hazard.
  • the recycling method provided by the invention has the advantages of high efficiency, low cost, environmental friendliness, wide applicability, and the like, and has the potential of industrial application.
  • 1 is a process flow diagram of a method for recovering waste polyester blended fabric containing natural fiber according to the present invention.
  • the invention provides a method for recovering waste polyester blended fabric containing natural-based fibers, comprising the following steps:
  • step S3 the solid insoluble matter obtained in the step S1 is immersed in an ester solvent to be dissolved at a temperature of 150 to 210 ° C, and then a C1-C3 fatty alcohol is added to precipitate a polyester solid for recovery;
  • the water-soluble tertiary amine oxide used in the step S1 is selected from the group consisting of dimethylethanolamine oxide, trimethylamine oxide, and N- a combination of one or more of methylmorpholine-N-oxide, N-methylpiperidine-N-oxide, N-methylpyrrolidine-N-oxide;
  • the ester solvent used in the step S3 has the structure of the formula (1):
  • R represents a linear or branched alkyl group of C1 to C5, and n represents an integer of 1 to 3.
  • the method for recovering waste polyester blended fabric containing natural fiber based on the present invention first dissolves the natural base fiber into a fiber solution and a polyester solid insoluble matter by using a water-soluble tertiary amine oxide solution containing an antioxidant, and is separated by solid-liquid separation. The purpose of thoroughly separating the polyester fiber (insoluble matter) and the natural base fiber (dissolved in the solution) is achieved, and then the obtained polyester solid insoluble matter and the natural base fiber solution are subjected to targeted recovery treatment.
  • the water-soluble tertiary amine oxide used in the invention has extremely low toxicity and can dissolve components such as protein and cellulose without converting it into a derivative, so that cellulose regenerated fiber can be obtained, and the water-soluble tertiary amine oxide can also be obtained. Repeat after recycling.
  • the natural-based fiber solution can be recovered by wet spinning treatment to obtain regenerated natural-based cellulose fibers.
  • the polyester solid insoluble matter is first dissolved using an ester solvent, and the polyester solution obtained by removing the impurities is further treated with a C1-C3 lower aliphatic alcohol to precipitate and recover the polyester solid.
  • the ester solvent used in the recovery method of the present invention is a solvent of a benzoic acid-derived ester, which is small in toxicity, low in cost, and can be easily recycled and reused.
  • Recovery process of the present invention to obtain a high-quality regenerated protein / cellulose fiber, protein-containing side chains on ionic -COO - and -NH 3 +, -OH polar hydrophilic ability to the cellulose fibers can be improved pure
  • the regenerated fiber has defects such as water swellability and fibrillation properties, and brings an excellent hand feeling.
  • steps S2 and S3 can be processed in different sequential orders according to actual conditions, and the order is not limited, and processing can also be performed at the same time.
  • the waste polyester blend fabric containing the natural base fiber may be any of the existing polyester blend fabrics including, but not limited to, polyester-cotton blend fabric, wool-polyester blend fabric, polyester-wool blend fabric, polyester-viscose.
  • the recovery method of the present invention can obtain a high-purity, high-recovery recovery effect.
  • the waste polyester blend fabric may have a polyester content of 10% to 90% by weight.
  • the waste polyester blend fabric may have a polyester content by weight ratio. 30% to 70%.
  • the waste polyester blend fabric has a water content of less than 10% by weight.
  • the natural base fiber in the waste polyester blend fabric containing the natural-based fiber may be any of the existing ones, and may include, for example, a protein-based fiber, a cellulose-based fiber, or both.
  • the protein based fibers include, but are not limited to, silk, wool, and the like, or combinations thereof.
  • the cellulose based fibers include, but are not limited to, cotton fibers, hemp fibers, viscose fibers, modal fibers, lyocell fibers, cuprammonium fibers, acetate fibers, and the like, or any combination.
  • the waste polyester blend fabric comprises protein-based fibers such as silk and wool
  • the protein-based fiber content is less than 30% by weight.
  • the tertiary amine oxide used in the water-soluble tertiary amine oxide solution in step S1 includes, but is not limited to, dimethylethanolamine oxide, trimethylamine oxide, and N-methylmorpholine-N-oxide. And N-methylpiperidine-N-oxide, N-methylpyrrolidine-N-oxide, or the like, or any combination thereof.
  • the water soluble tertiary amine oxide can be N-methylmorpholine-N-oxide.
  • the water-soluble tertiary amine oxide solution may have a water content of 10% to 15% by weight, and in a preferred embodiment, the water content of the water-soluble tertiary amine oxide solution is The weight ratio can be from 12% to 14%.
  • the antioxidant may be selected from common antioxidant species such as citric acid, phenols, aromatic polyhydroxy compounds, etc., specifically including but not limited to catechol, 1, 2, 3- Pyrogallol, propyl gallate, 2,6-di-tert-butyl-p-cresol, gallic acid, methyl, ethyl, propyl or isopropyl ester of gallic acid, etc., may also be any kind of combination, in a preferred
  • the antioxidant may be propyl gallate or propyl gallate.
  • the weight of the antioxidant may be from 0.5% to 3% by weight of the water-soluble tertiary amine oxide solution.
  • the weight of the antioxidant may be water-soluble tertiary amine oxidation. 1% to 2% by weight of the solution.
  • the weight ratio of the waste polyester blend fabric containing the natural base fiber to the water-soluble tertiary amine oxide solution may be 1:99 to 15:85.
  • the waste polyester blend fabric The weight ratio to the water soluble tertiary amine oxide solution may range from 10:90 to 13:87.
  • the dissolution process of the natural base fiber can be carried out under heating conditions, for example, the following process: swelling at 60 to 75 ° C for 20 to 30 minutes, and then heating to 80 to 130 ° C for 50 to 90 minutes, in
  • the fiber dissolution may also be a process of swelling for 20 to 30 minutes before 60 to 75 ° C, followed by heating to 90 to 100 ° C for 60 to 80 minutes.
  • the wet spinning process in step S2 may be an existing wet spinning process.
  • the fiber solution obtained in step S1 can be continuously extruded into water and/or ethanol through a spinneret, mechanically stretched by 3 to 10 times, and molecularly oriented, thereby producing a fiber solution. Recycled recycled natural base cellulose fibers.
  • the remaining antioxidant-containing water-soluble tertiary amine oxide solution may be recovered and purified by, for example, an ion exchange column. After processing, Can be recycled.
  • the ester solvent used in the step S3 has the structure of the above formula (1), wherein R may represent a methyl group, an ethyl group, a propyl group, an isopropyl group, a n-butyl group, an isobutyl group or a secondary group.
  • R may represent a methyl group, an ethyl group, a propyl group, an isopropyl group, a n-butyl group, an isobutyl group or a secondary group.
  • Butyl, tert-butyl, n-pentyl, isopentyl, neopentyl, tert-amyl and the like may preferably be a methyl group, an ethyl group, a propyl group, an isopropyl group or an n-butyl group.
  • n may represent an integer of 1, 2 or 3, preferably an integer of 1 or 2, that is, one or two carboxylate groups on the benzene ring, and two or more when n represents an integer other than 1.
  • the substituent group can be located at any possible substitution position on the phenyl ring.
  • the ester solvent includes, but is not limited to, methyl benzoate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate, Dimethyl phthalate, dimethyl isophthalate, and the like may be used in any combination.
  • the amount of the polyester solvent may be from 1:1.1 to 1:50 by weight of the polyester in the waste polyester blend fabric, or may be adjusted by a person skilled in the art according to actual conditions. .
  • the weight ratio of the polyester to the ester solvent may be from 1:15 to 1:20.
  • the polyester dissolution reaction in the step S3 is generally such that the polyester solids are completely dissolved, and the reaction time and temperature can be adjusted by those skilled in the art according to actual conditions.
  • the reaction time may be from 3 to 60 minutes, and in a preferred embodiment, the reaction time may be from 5 to 15 minutes.
  • the reaction temperature may be from 150 to 210 ° C. In a preferred embodiment, the reaction temperature may be from 170 to 190 ° C.
  • the C1-C3 fatty alcohol in the step S3 may be a common lower aliphatic alcohol such as methanol, ethanol, propanol or isopropanol.
  • the fatty alcohol may be methanol or ethanol.
  • the volume ratio of the dissolved polyester solution to the lower aliphatic alcohol such as methanol or ethanol may be from 1:15 to 1:50.
  • the polyester solution and the lower aliphatic alcohol are in a preferred embodiment. The volume ratio can be from 1:20 to 1:25.
  • the fatty alcohol may be added to the dissolved polyester solution, or the dissolved polyester solution may be poured into the fatty alcohol.
  • the polyester solution after adding a lower aliphatic alcohol such as methanol or ethanol, the polyester solution can be cooled to 45 to 65 ° C to precipitate a polyester solid.
  • the precipitated polyester solids may also be treated by granulation, pre-crystallization, drying, solid phase thickening, etc. to increase the number average molecular weight of the polyester, such as tackifying
  • the number average molecular weight is up to 20,000 or more, thereby meeting the requirements of spinning slicing.
  • the lower aliphatic alcohol after the treatment of the polyester solids is collected, and the ester solvent contained therein and the fatty alcohol itself may be separately recovered or purified for recycling. Since the ester solvent used in the present invention has a boiling point much higher than that of the lower aliphatic alcohol, it can be cooled, crystallized, distilled, rectified, etc., which are common in the art. Recovery of ester solvents and fatty alcohols.
  • the remaining fatty alcohol solution is further cooled to 20-40 ° C to precipitate the ester solvent crystals. In a preferred embodiment, the temperature is lowered to 20-25.
  • the remaining fatty alcohol can be recycled by distillation or the like.
  • the ester solvent and the fatty alcohol may also be recovered by distillation or rectification.
  • the operation of the separation step of solid-liquid separation, filtration or the like may be carried out by operations conventional in the art including, but not limited to, suction filtration, (high speed) centrifugation, precipitation, or a combination thereof.
  • the column was subjected to purification of a 4-methylmorpholine-N-oxide solution containing propyl gallate.
  • the separated solid insoluble matter was immersed in 50 ml of dimethyl terephthalate at 170 ° C for 15 min, and then slowly poured into methanol.
  • the temperature was lowered to 50 ° C, the precipitated polyester particles were collected by high-speed centrifugation.
  • the temperature is further lowered to 25 ° C, the precipitated dimethyl terephthalate particles are collected, and the remaining methanol solution is recovered by distillation.
  • the column was subjected to purification of a 4-methylmorpholine-N-oxide solution containing propyl gallate.
  • the separated solid insoluble matter was immersed in 190 ° C, 60 ml of butyl benzoate for 5 min, and then slowly poured into ethanol.
  • the temperature was lowered to 60 ° C, the precipitated polyester particles were collected by high-speed centrifugation, and then weak Distillation treatment was carried out to obtain distilled product ethanol, and the residue was butyl benzoate.

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Abstract

提供了一种含有天然基纤维的废旧涤纶混纺织物的回收方法，将废旧涤纶混纺织物置于含有抗氧化剂的水溶性叔胺氧化物溶液中，以使天然基纤维溶解形成纤维溶液和固体不溶物，然后回收纤维溶液得到再生天然基纤维素纤维，并且通过向固体不溶物中依次加入酯类溶剂和脂肪醇回收涤纶固体。该回收方法可分离涤纶与其他天然基纤维，适用于所有的涤纶混纺织物，对涤纶与再生天然基纤维素纤维的回收率高，避免了使用毒性大、刺激性大的化学试剂，所使用的试剂还可回收循环利用。该回收方法具有高效率、低成本、环境友好、适用范围广等优点，具有工业化应用的潜力。

Description

一种含有天然基纤维的废旧涤纶混纺织物的回收方法 技术领域
本发明属于纺织资源再生领域，具体涉及一种含有天然基纤维的废旧涤纶混纺织物的回收方法。
背景技术
涤纶是合成纤维中的一个重要品种，是将聚对苯二甲酸乙二醇酯高聚物(PET)经纺丝和后处理制成的纤维。涤纶混纺织物是将涤纶纤维与其它棉、毛、丝、麻等纤维混合纺纱织成的纺织产品，主要的涤纶混纺织物包括涤棉混纺织物、毛涤混纺织物、涤麻混纺织物、涤粘混纺织物、“三合一”混纺织物(涤纶与两种纤维混纺的织物，如涤毛麻、涤麻棉、涤粘毛、涤棉粘等)。当如此多种类的涤纶混纺织物成为了废旧纺织品之后，亟需找到一种环保、节能、高效的方法将其中的涤纶以及其他混纺的天然基纤维尽可能的回收再利用，以实现一定的经济收益，达到资源的可持续发展。
现有的研究多集中在涤棉混纺织物的回收再利用，极少涉及其他纤维与涤纶混纺织物的回收再利用，尤其是天然基纤维与涤纶混纺织物。通常而言，涤纶混纺织物的回收再利用方法是将涤纶与其他成分如棉纤维等进行分离，然后分别针对性地回收。但是，现有的方法使用的溶剂多为毒性较高的种类，成本高且危害环境，此外，现有的方法大多难以实现回收物的彻底分离，影响回收纯度。
发明内容
为克服现有废旧涤纶混纺织物回收技术中存在的空白及缺陷，本发明的目的是提供一种高效的含有天然基纤维的废旧涤纶混纺织物的回收方法。
本发明提供的含有天然基纤维的废旧涤纶混纺织物的回收方法包括以下步骤：
S1：将含有天然基纤维的废旧涤纶混纺织物置于含有抗氧化剂的水溶性叔胺氧化物溶液中，以使天然基纤维溶解形成纤维溶液和固体不溶物；
S2：将步骤S1所得的纤维溶液通过湿法纺丝回收再生天然基纤维素纤维；以及
S3：将步骤S1所得的固体不溶物浸入酯类溶剂中于150～210℃的温度下反应至溶解，然后加入C1～C3的脂肪醇以析出涤纶固体进行回收；
其中，所述步骤S1中使用的水溶性叔胺氧化物选自氧化二甲基乙醇胺、氧化三甲胺、N-甲基吗啉-N-氧化物、N-甲基哌啶-N-氧化物、N-甲基吡咯烷-N-氧化物中的一种或多种 的组合；
所述步骤S3中使用的酯类溶剂具有式(1)结构：
Figure PCTCN2017101112-appb-000001
式(1)中，R表示C1～C5的直链或支链烷基，n表示1～3的整数。
本发明的回收方法中，所述废旧涤纶混纺织物的含涤量按重量比为10％～90％，含水量按重量比低于10％。
本发明的回收方法中，所述废旧涤纶混纺织物中的天然基纤维包括蛋白质基纤维和/或纤维素基纤维，其中，所述蛋白质基纤维包括蚕丝和/或羊毛，所述纤维素基纤维包括棉纤维、麻纤维、粘胶纤维、莫代尔纤维、莱塞尔纤维、铜氨纤维、醋酸纤维中的一种或多种的组合。
本发明的回收方法中，所述废旧涤纶混纺织物中的蛋白质基纤维含量按重量比低于30％。
本发明的回收方法中，所述步骤S1中的水溶性叔胺氧化物溶液的含水率按重量比为10％～15％。
本发明的回收方法中，所述抗氧化剂选自邻苯二酚、1，2，3-苯三酚、没食子酸丙酯、2，6-二叔丁基对甲酚、五倍子酸、五倍子酸的甲、乙、丙或异丙酯中的一种或多种的组合，所述抗氧化剂的重量比为0.5％～3％。
本发明的回收方法中，所述步骤S1中的含有天然基纤维的废旧涤纶混纺织物与水溶性叔胺氧化物溶液的重量比为1﹕99～15﹕85。
本发明的回收方法中，所述步骤S1中天然基纤维溶解的过程包括先于60～75℃下溶胀20～30min，之后升温至80～130℃溶解50～90min。
本发明的回收方法中，所述步骤S2中的湿法纺丝过程包括将步骤S1所得的纤维溶液喷丝至水和/或乙醇中，机械拉伸3～10倍，制得再生天然基纤维素纤维。
本发明的回收方法中，所述步骤S3中使用的酯类溶剂选自苯甲酸甲酯、苯甲酸乙酯、苯甲酸丙酯、苯甲酸异丙酯、苯甲酸丁酯、苯甲酸异丁酯、对苯二甲酸二甲酯、间苯二甲酸二甲酯中的一种或多种的组合；所述废旧涤纶混纺织物中的涤纶重量与所述酯类溶剂的重量比为1﹕1.1～1﹕50。
本发明的回收方法中，所述步骤S3中的反应时间为3～30min。
本发明的回收方法中，所述步骤S3中，溶解后的涤纶溶液与所述脂肪醇的体积比为1﹕15～1﹕50，加入所述脂肪醇后，降温至45～65℃以析出涤纶固体。
本发明的回收方法中，所述脂肪醇选自甲醇或乙醇。
本发明的回收方法中，所述步骤S3还包括将所得的涤纶固体进行增粘至达到纺丝切片的要求。
本发明的回收方法中，所述步骤S3还包括将所述涤纶固体分离回收之后再分别回收所述脂肪醇和所述酯类溶剂。
本发明的含有天然基纤维的废旧涤纶混纺织物的回收方法具有以下优点：
(1)本发明的回收方法可完全、彻底地分离涤纶与其他的天然基纤维，回收的涤纶与再生天然基纤维素纤维纯度高，回收率高，回收所得的涤纶基本能保留原有的物理、化学性能，经济优势明显。
(2)本发明的回收方法工艺过程先进，仅通过一次溶解-再生过程便可得到高质量的再生蛋白质/纤维素纤维。
(3)本发明的回收方法可适用于所有种类的含有涤纶的涤纶混纺织物，适用范围广，填补了现有技术存在的空白。
(4)本发明的回收方法避免了使用毒性大、刺激性大的化学试剂，而且所使用的试剂还可回收循环利用，进一步降低了工艺成本，减轻了对环境的危害。
总之，本发明提供的回收方法具有高效率、低成本、环境友好、适用性广等优点，具有工业化应用的潜力。
附图说明
图1为本发明所述的含有天然基纤维的废旧涤纶混纺织物回收方法的工艺流程图。
具体实施方式
本发明提供了一种含有天然基纤维的废旧涤纶混纺织物的回收方法，包括以下步骤：
S1：将含有天然基纤维的废旧涤纶混纺织物置于含有抗氧化剂的水溶性叔胺氧化物溶液中，以使天然基纤维溶解形成纤维溶液和固体不溶物；
S2：将步骤S1所得的纤维溶液通过湿法纺丝回收再生天然基纤维素纤维；以及
S3：将步骤S1所得的固体不溶物浸入酯类溶剂中于150～210℃的温度下反应至溶解，然后加入C1～C3的脂肪醇以析出涤纶固体进行回收；
其中，步骤S1中使用的水溶性叔胺氧化物选自氧化二甲基乙醇胺、氧化三甲胺、N- 甲基吗啉-N-氧化物、N-甲基哌啶-N-氧化物、N-甲基吡咯烷-N-氧化物中的一种或多种的组合；
步骤S3中使用的酯类溶剂具有式(1)结构：
Figure PCTCN2017101112-appb-000002
式(1)中，R表示C1～C5的直链或支链烷基，n表示1～3的整数。
参照图1，本发明的含有天然基纤维的废旧涤纶混纺织物的回收方法首先使用含有抗氧化剂的水溶性叔胺氧化物溶液将天然基纤维溶解形成纤维溶液以及涤纶固体不溶物，通过固液分离达到彻底分离涤纶纤维(不溶物)和天然基纤维(溶于溶液)的目的，然后再对所得的涤纶固体不溶物和天然基纤维溶液进行针对性回收处理。本发明使用的水溶性叔胺氧化物毒性极低，能溶解蛋白质、纤维素等成分而不会将其转变成衍生物，因此可再制得纤维素再生纤维，水溶性叔胺氧化物也可回收之后重复使用。
进一步地，天然基纤维溶液可通过湿法纺丝处理得到再生天然基纤维素纤维进行回收。涤纶固体不溶物首先使用酯类溶剂进行溶解，除去杂质后所得的涤纶溶液再使用C1～C3的低级脂肪醇处理，使得涤纶固体析出而回收。本发明的回收方法使用的酯类溶剂为苯甲酸衍生酯的溶剂，毒性小，成本低，也可方便地回收再利用。
本发明回收方法得到的是高质量的再生蛋白质/纤维素纤维，蛋白质侧链上含有离子-COO-和-NH3 +，亲水能力强于纤维素上的极性-OH，可改善纯纤维素再生纤维的水溶胀性和原纤化特性等缺陷，并带来优异的手感。
在实际应用中，步骤S2、S3可根据实际情况按不同的先后顺序进行处理，顺序不限，也可同时进行处理。
在本发明的回收方法中，含有天然基纤维的废旧涤纶混纺织物可以为现有的任意种类的涤纶混纺织物，包括但不限于涤棉混纺织物、毛涤混纺织物、涤麻混纺织物、涤粘混纺织物、“三合一”混纺织物等，本发明的回收方法都可以得到高纯度、高回收率的回收效果。在根据本发明的一个实施方式中，废旧涤纶混纺织物的含涤量按重量比可以为10％～90％，在一个优选的实施方式中，废旧涤纶混纺织物的含涤量按重量比可以为30％～70％。在根据本发明的一个实施方式中，废旧涤纶混纺织物的含水量按重量比低于10％。
在本发明的回收方法中，含有天然基纤维的废旧涤纶混纺织物中的天然基纤维可以为现有的任意种类，例如可包括蛋白质基纤维、纤维素基纤维或同时包含二者。在根据本发明的一个实施方式中，蛋白质基纤维包括但不限于蚕丝、羊毛等，或为其组合。在根据本 发明的另一个实施方式中，纤维素基纤维包括但不限于棉纤维、麻纤维、粘胶纤维、莫代尔纤维、莱塞尔纤维、铜氨纤维、醋酸纤维等，或为任意组合。在一个优选的实施方式中，当废旧涤纶混纺织物中包含蛋白质基纤维如蚕丝、羊毛时，蛋白质基纤维含量按重量比低于30％。
在本发明的回收方法中，步骤S1中的水溶性叔胺氧化物溶液使用的叔胺氧化物包括但不限于氧化二甲基乙醇胺、氧化三甲胺、N-甲基吗啉-N-氧化物、N-甲基哌啶-N-氧化物、N-甲基吡咯烷-N-氧化物等，或为任意组合。在一个优选的实施方式中，水溶性叔胺氧化物可以为N-甲基吗啉-N-氧化物。在根据本发明的一个实施方式中，水溶性叔胺氧化物溶液的含水率按重量比可以为10％～15％，在一个优选的实施方式中，水溶性叔胺氧化物溶液的含水率按重量比可以为12％～14％。
在本发明的回收方法中，抗氧化剂可以选用常见的抗氧化剂种类如鞣酸类、酚类、芳族多羟基化合物等，具体地，包括但不限于邻苯二酚、1，2，3-苯三酚、没食子酸丙酯、2，6-二叔丁基对甲酚、五倍子酸、五倍子酸的甲、乙、丙或异丙酯等，也可为任意种类的组合，在一个优选的实施方式中，抗氧化剂可以为没食子酸丙酯或五倍子酸丙酯。在根据本发明的一个实施方式中，抗氧化剂的重量可以为水溶性叔胺氧化物溶液重量的0.5％～3％，在一个优选的实施方式中，抗氧化剂的重量可以为水溶性叔胺氧化物溶液重量的1％～2％。
在本发明的回收方法中，含有天然基纤维的废旧涤纶混纺织物与水溶性叔胺氧化物溶液的重量比可以为1﹕99～15﹕85，在一个优选的实施方式中，废旧涤纶混纺织物与水溶性叔胺氧化物溶液的重量比可以为10﹕90～13﹕87。
在本发明的回收方法中，天然基纤维的溶解过程可以在加热条件下进行，例如以下过程：先于60～75℃下溶胀20～30min，之后升温至80～130℃溶解50～90min，在一个优选的实施方式中，纤维溶解还可以为以下过程：先于60～75℃下溶胀20～30min，之后升温至90～100℃溶解60～80min。
在本发明的回收方法中，步骤S2中的湿法纺丝过程可以为现有的湿法纺丝工艺。在一个优选的实施方式中，可以为以下过程：将步骤S1所得的纤维溶液通过喷丝头连续挤入水和/或乙醇中，机械拉伸3～10倍，使分子取向，由此制得可回收的再生天然基纤维素纤维。
在本发明的回收方法中，如图1所示，步骤S2回收再生天然基纤维素纤维之后，还可回收剩余的含抗氧化剂的水溶性叔胺氧化物溶液，通过如离子交换柱等的纯化处理后， 可以循环再利用。
在本发明的回收方法中，步骤S3使用的酯类溶剂具有上述式(1)结构，其中，R可表示甲基、乙基、丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基、异戊基、新戊基、叔戊基等，优选可以为甲基、乙基、丙基、异丙基、正丁基。n可表示1、2或3的整数，优选为1或2的整数，即苯环上具有一或两个羧酸酯基团，当n表示不为1的整数时，两个或两个以上的取代基团可以位于苯环上任意可能的取代位置。在根据本发明的一个实施方式中，酯类溶剂包括但不限于苯甲酸甲酯、苯甲酸乙酯、苯甲酸丙酯、苯甲酸异丙酯、苯甲酸丁酯、苯甲酸异丁酯、对苯二甲酸二甲酯、间苯二甲酸二甲酯等，也可为任意种类的组合。
在本发明的回收方法中，按照废旧涤纶混纺织物中涤纶的重量计算，其与酯类溶剂的用量可以为1﹕1.1～1﹕50的重量比，也可根据实际情况由本领域技术人员进行调节。在根据本发明的一个优选实施方式中，涤纶与酯类溶剂的重量比可以为1﹕15～1﹕20。
在本发明的回收方法中，步骤S3中的涤纶溶解反应一般应使涤纶固体溶解完全，可由本领域技术人员根据实际情况调节反应时间和温度。在根据本发明的一个实施方式中，反应时间可以为3～60分钟，在一个优选的实施方式中，反应时间可以为5～15分钟。在根据本发明的一个实施方式中，反应温度可以为150～210℃，在一个优选的实施方式中，反应温度可以为170～190℃。涤纶溶解反应完成后，可进行过滤除去杂质，得到涤纶溶液。
在本发明的回收方法中，步骤S3中的C1～C3脂肪醇可以为甲醇、乙醇、丙醇、异丙醇等常见的低级脂肪醇。在根据本发明的一个实施方式中，脂肪醇可以为甲醇或乙醇。在根据本发明的一个实施方式中，溶解后的涤纶溶液与甲醇、乙醇等低级脂肪醇的体积比可以为1﹕15～1﹕50，在一个优选的实施方式中，涤纶溶液与低级脂肪醇的体积比可以为1﹕20～1﹕25。在根据本发明的一个实施方式中，脂肪醇可以加入到溶解后的涤纶溶液中，也可将溶解后的涤纶溶液倒入脂肪醇中。在根据本发明的一个实施方式中，加入甲醇、乙醇等低级脂肪醇之后，可将涤纶溶液降温至45～65℃以析出涤纶固体。
在本发明的回收方法中，为达到更高的回收要求，对于析出的涤纶固体还可通过造粒、预结晶、干燥、固相增粘等处理以提高涤纶的数均分子量，如可增粘至数均分子量达20000以上，从而达到纺丝切片的要求。
在本发明的回收方法中，如图1所示，收集处理涤纶固体之后的低级脂肪醇，还可分别对于其中所含的酯类溶剂以及脂肪醇本身进行回收或提纯以循环利用。由于本发明使用的酯类溶剂沸点远高于低级脂肪醇，因此可通过降温析晶、蒸馏、精馏等本领域常见方式 回收酯类溶剂和脂肪醇。在根据本发明的一个实施方式中，分离出涤纶固体后，再将剩余的脂肪醇溶液继续降温至20～40℃以析出酯类溶剂晶体，在一个优选的实施方式中，降温至20～25℃以析出酯类溶剂晶体，回收酯类溶剂晶体后，剩余的脂肪醇通过蒸馏等方式提纯后可循环利用。在根据本发明的另一个实施方式中，也可采用蒸馏或精馏方式回收酯类溶剂以及脂肪醇。
在本发明的回收方法中，固液分离、过滤等分离步骤的操作可选用本领域常见的操作，包括但不限于抽滤法、(高速)离心法、沉淀法、或它们的组合。
为使本发明的目的、技术方案和优点更加清楚，下面将进一步描述本发明的示例性实施例的技术方案。
以下实施例所使用的化学试剂如无特别说明则为市售商品，以下实施例所使用的操作或仪器如无特别说明则为本领域常见的操作或仪器。以下实施例中所述的比例、比值、含量等如无特别说明则为重量比。
实施例1
将含水量5％、含涤量50％、含毛量10％的废旧涤毛棉混纺织物10g，置于65℃的含0.5g没食子酸丙酯和12％去离子水的4-甲基吗啉-N-氧化物溶液45ml中溶胀30min，然后升温到100℃，使其中的天然基纤维充分溶解60min。利用真空抽滤法对混合物进行固液分离，将得到的蛋白质/纤维素纺丝原液从喷丝头连续挤入水中，机械拉伸3倍，制得再生蛋白质/纤维素纤维，回收并用离子交换柱进行纯化含有没食子酸丙酯的4-甲基吗啉-N-氧化物溶液。而分离出的固体不溶物则浸入到170℃、50ml的对苯二甲酸二甲酯中15min后，然后缓慢倒入甲醇中，当温度降至50℃时，利用高速离心法收集析出的涤纶颗粒，再继续降温至25℃时，收集析出的对苯二甲酸二甲酯颗粒，并再通过蒸馏法回收剩余的甲醇溶液。
实施例2
将含水量8％、含涤量30％、含毛量15％的废旧涤粘毛混纺织物10g，置于75℃的含1g五倍子酸丙酯和14％去离子水的4-甲基吗啉-N-氧化物溶液50ml中溶胀20min，然后升温到90℃，使其中的天然基纤维充分溶解80min。利用真空抽滤法对混合物进行固液分离，将得到的蛋白质/纤维素纺丝原液从喷丝头连续挤入水中，机械拉伸8倍，制得再生蛋白质/纤维素纤维，回收并用离子交换柱进行纯化含有五倍子酸丙酯的4-甲基吗啉-N-氧化物溶液。而分离出的固体不溶物则浸入到190℃、60ml的苯甲酸丁酯中5min后，然后缓慢倒入乙醇中，当温度降至60℃时，利用高速离心法收集析出的涤纶颗粒，再对乙醇溶液 进行蒸馏处理，得到蒸馏产物乙醇，剩余物为苯甲酸丁酯。
虽然为了说明本发明，已经公开了本发明的优选实施方案，但是本领域的技术人员应当理解，在不脱离权利要求书所限定的本发明构思和范围的情况下，可以对本发明做出各种修改、添加和替换。

Claims (15)

  1. 一种含有天然基纤维的废旧涤纶混纺织物的回收方法，其特征在于，包括以下步骤：
    S1：将含有天然基纤维的废旧涤纶混纺织物置于含有抗氧化剂的水溶性叔胺氧化物溶液中，以使天然基纤维溶解形成纤维溶液和固体不溶物；
    S2：将步骤S1所得的纤维溶液通过湿法纺丝回收再生天然基纤维素纤维；以及
    S3：将步骤S1所得的固体不溶物浸入酯类溶剂中于150～210℃的温度下反应至溶解，然后加入C1～C3的脂肪醇以析出涤纶固体进行回收；
    其中，所述步骤S1中使用的水溶性叔胺氧化物选自氧化二甲基乙醇胺、氧化三甲胺、N-甲基吗啉-N-氧化物、N-甲基哌啶-N-氧化物、N-甲基吡咯烷-N-氧化物中的一种或多种的组合；
    所述步骤S3中使用的酯类溶剂具有式(1)结构：
    Figure PCTCN2017101112-appb-100001
    式(1)中，R表示C1～C5的直链或支链烷基，n表示1～3的整数。
  2. 根据权利要求1所述的回收方法，其特征在于，所述废旧涤纶混纺织物的含涤量按重量比为10％～90％，含水量按重量比低于10％。
  3. 根据权利要求2所述的回收方法，其特征在于，所述废旧涤纶混纺织物中的天然基纤维包括蛋白质基纤维和/或纤维素基纤维，其中，所述蛋白质基纤维包括蚕丝和/或羊毛，所述纤维素基纤维包括棉纤维、麻纤维、粘胶纤维、莫代尔纤维、莱塞尔纤维、铜氨纤维、醋酸纤维中的一种或多种的组合。
  4. 根据权利要求3所述的回收方法，其特征在于，所述废旧涤纶混纺织物中的蛋白质基纤维含量按重量比低于30％。
  5. 根据权利要求1所述的回收方法，其特征在于，所述步骤S1中的水溶性叔胺氧化物溶液的含水率按重量比为10％～15％。
  6. 根据权利要求1所述的回收方法，其特征在于，所述抗氧化剂选自邻苯二酚、1，2，3-苯三酚、没食子酸丙酯、2，6-二叔丁基对甲酚、五倍子酸、五倍子酸的甲、乙、丙 或异丙酯中的一种或多种的组合，所述抗氧化剂的重量比为0.5％～3％。
  7. 根据权利要求1所述的回收方法，其特征在于，所述步骤S1中的含有天然基纤维的废旧涤纶混纺织物与水溶性叔胺氧化物溶液的重量比为1﹕99～15﹕85。
  8. 根据权利要求1所述的回收方法，其特征在于，所述步骤S1中天然基纤维溶解的过程包括先于60～75℃下溶胀20～30min，之后升温至80～130℃溶解50～90min。
  9. 根据权利要求1所述的回收方法，其特征在于，所述步骤S2中的湿法纺丝过程包括将步骤S1所得的纤维溶液喷丝至水和/或乙醇中，机械拉伸3～10倍，制得再生天然基纤维素纤维。
  10. 根据权利要求1所述的回收方法，其特征在于，所述步骤S3中使用的酯类溶剂选自苯甲酸甲酯、苯甲酸乙酯、苯甲酸丙酯、苯甲酸异丙酯、苯甲酸丁酯、苯甲酸异丁酯、对苯二甲酸二甲酯、间苯二甲酸二甲酯中的一种或多种的组合；所述废旧涤纶混纺织物中的涤纶重量与所述酯类溶剂的重量比为1﹕1.1～1﹕50。
  11. 根据权利要求1所述的回收方法，其特征在于，所述步骤S3中的反应时间为3～30min。
  12. 根据权利要求1所述的回收方法，其特征在于，所述步骤S3中，溶解后的涤纶溶液与所述脂肪醇的体积比为1﹕15～1﹕50，加入所述脂肪醇后，降温至45～65℃以析出涤纶固体。
  13. 根据权利要求12所述的回收方法，其特征在于，所述脂肪醇选自甲醇或乙醇。
  14. 根据权利要求1所述的回收方法，其特征在于，所述步骤S3还包括将所得的涤纶固体进行增粘至达到纺丝切片的要求。
  15. 根据权利要求1所述的回收方法，其特征在于，所述步骤S3还包括将所述涤纶固体分离回收之后再分别回收所述脂肪醇和所述酯类溶剂。
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WO2023180181A1 (en) * 2022-03-21 2023-09-28 Phoenxt Pty. Ltd Regenerating cellulose from waste textile

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