CN110219072B - Method for recycling soluble textiles - Google Patents

Method for recycling soluble textiles Download PDF

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CN110219072B
CN110219072B CN201910625711.0A CN201910625711A CN110219072B CN 110219072 B CN110219072 B CN 110219072B CN 201910625711 A CN201910625711 A CN 201910625711A CN 110219072 B CN110219072 B CN 110219072B
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fiber
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CN110219072A (en
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余燕平
刘卫国
余尔琪
刘俊和
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/09Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
    • C07C29/095Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/09Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters

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Abstract

The invention provides a method for recycling soluble textiles, which uses a solvent to dissolve fabrics containing controllable soluble fibers or fabrics made of the controllable soluble fibers, and filters and recovers the dissolved solution to obtain high-purity terephthalic acid and ethylene glycol which are reused for preparing the controllable soluble fibers; and preparing the undissolved textile fibers into high-quality textile fibers for recycling. The solvent has high dissolving speed and small damage to non-soluble fibers, thereby being beneficial to high-quality and high-efficiency reutilization of the fibers.

Description

可溶解纺织品的再利用方法Reuse method of dissolvable textiles

技术领域technical field

本发明涉及纤维加工、纺织加工、环保技术领域,特别涉及一种可溶解纺织品的回收、再生、循环使用技术。The invention relates to the technical fields of fiber processing, textile processing and environmental protection, in particular to a recovery, regeneration and recycling technology of dissolvable textiles.

背景技术Background technique

全世界无数的纺织品成为废弃产品不能再使用,或者低级的使用,这就会造成资源的巨大浪费和环境的二次污染。现有的纺织纤维没有能够简单处理及回收的技术和产品,其重要原因是纺织品原料构成、颜色、成衣配件复杂;面料结构紧密,开松后纤维损伤大,使用价值低。Countless textiles in the world have become waste products that can no longer be used, or are used in a low-level manner, which will cause huge waste of resources and secondary pollution of the environment. Existing textile fibers do not have technologies and products that can be easily processed and recycled. The main reason is that the composition, color, and garment accessories of textile materials are complex;

目前,市场上仅仅对于纯纺的羊绒、芳纶纤维等价值高的纺织品,进行开松、梳理,获得得强度低和长度短的纤维,进行低价值的回用。At present, only high-value textiles such as pure spun cashmere and aramid fibers are opened and carded in the market to obtain fibers with low strength and short length for low-value reuse.

而另外一种回收路径,是将PET的瓶回收,然后通过洗净、造粒做成PET纤维,但这种制得的纤维纺织品,最后还是不能使用,成为废弃物及污染物。或者是将回收的纯的PET服装,采用高温熔融加化学醇解的分解法,得到PTA(对苯二甲酸),但这种方法成本高,且仅仅是对100% PET的面料,而对于混纺其它非PET的面料,则不适用。这种方法收到局限性大。Another recycling route is to recycle PET bottles, and then wash and pelletize them into PET fibers. However, the fiber textiles produced by this method cannot be used in the end and become waste and pollutants. Or the recycled pure PET clothing is obtained by the decomposition method of high temperature melting and chemical alcoholysis to obtain PTA (terephthalic acid), but this method is expensive, and it is only for 100% PET fabrics, and for blended spinning Other non-PET fabrics are not applicable. This method is very limited.

本申请人的在先专利申请CN106065085A公开了一种可溶解纺织品的回收、再生、循环使用技术,该技术采用聚酯类的溶解可控的可溶纤维,经常规织布、染色、后整理及成衣或者注塑加工成可溶服饰配件;将该衣服或者可溶服饰配件在一定的条件下溶解,一方面对溶解液进行过滤和溶解物回收,获得的高纯度的对苯二甲酸和乙二醇,将对苯二甲酸和乙二醇回用于可溶性聚酯的聚合,获得可溶性聚酯的切片,可重新进行纺丝成可溶解纤维,循环使用;另一方面对已经松散的未溶解的纺织品,经处理,包括消毒、剥色或者再染色,成为品质保持良好的松散纤维聚合体,烘干后,或经轻柔梳理,成为高品质纺织纤维,循环使用。然而,该方法中使用的有机溶剂溶解速度慢,且对非溶纤维存在一定损伤,从而影响到纤维的循环再利用。The applicant's prior patent application CN106065085A discloses a technology for the recovery, regeneration and recycling of dissolvable textiles. Garment or injection molding into soluble clothing accessories; the clothes or soluble clothing accessories are dissolved under certain conditions, and on the one hand, the dissolved liquid is filtered and dissolved substances are recovered to obtain high-purity terephthalic acid and ethylene glycol , terephthalic acid and ethylene glycol are reused for the polymerization of soluble polyester to obtain slices of soluble polyester, which can be re-spun into soluble fibers and recycled; on the other hand, the loose undissolved textiles , After treatment, including sterilization, stripping or re-dyeing, it becomes a loose fiber aggregate with good quality. After drying, or after gentle carding, it becomes a high-quality textile fiber, which can be recycled. However, the organic solvent used in this method has a slow dissolution rate, and has certain damage to the insoluble fibers, thus affecting the recycling and reuse of the fibers.

本领域需要一种在溶解过程中对可溶纤维溶解速度快且对非溶纤维损伤小的溶剂,从而有利于纤维的高品质和高效再利用There is a need in the art for a solvent with fast dissolving speed for soluble fibers and less damage to insoluble fibers during the dissolving process, so as to facilitate high-quality and efficient reuse of fibers

发明内容SUMMARY OF THE INVENTION

本发明在专利申请CN106065085A(通过引用将其内容全部并入本文)的基础上,针对上述技术问题,提供了一种对可溶纤维溶解速度快且对非溶纤维损伤小的再利用方法。为同时解决上述技术问题,本发明提供了以下技术方案。On the basis of patent application CN106065085A (the entire contents of which are incorporated herein by reference), the present invention provides a recycling method for soluble fiber with fast dissolving speed and little damage to insoluble fiber in view of the above-mentioned technical problems. In order to solve the above technical problems at the same time, the present invention provides the following technical solutions.

在本发明的一方面,提供了一种可溶解纺织品的再利用方法,其中所述可溶解纺织品包含可控溶解纤维面料或者由可控溶解纤维面料制成,所述方法包括以下步骤:In one aspect of the present invention, a method for reusing dissolvable textiles is provided, wherein the dissolvable textiles comprise or are made of controlled dissolving fiber fabrics, and the method includes the following steps:

a. 对于可控溶解纤维面料,所述方法包括以下步骤:a. For controlled dissolving fiber fabrics, the method includes the following steps:

将所述可控溶解纤维面料置于容器中,加入溶剂,使其完全溶解,将溶解液进行过滤、酸析和脱气处理,得到对苯二甲酸和乙二醇,排放废水COD达到环保要求;The controllable dissolving fiber fabric is placed in a container, a solvent is added to make it completely dissolved, and the dissolved solution is filtered, acidified and degassed to obtain terephthalic acid and ethylene glycol, and the COD of the discharged wastewater meets environmental protection requirements ;

或者,or,

b. 对于可控溶解纤维与其它非溶纤维的混纺或交织的纤维面料,所述方法包括以下步骤:b. For blended or interwoven fiber fabrics of controlled dissolving fibers and other non-dissolving fibers, the method includes the following steps:

将所述纤维面料置于容器中,加入溶剂,使其溶解,对于溶解液,进行过滤、酸析和脱气处理,得到对苯二甲酸和乙二醇,排放废水COD达到环保要求;对于非溶解纤维,将其进行清洗、消毒,得到松散的纤维集合体。The fiber fabric is placed in a container, a solvent is added to dissolve it, and the dissolving solution is filtered, acidified and degassed to obtain terephthalic acid and ethylene glycol, and the COD of the waste water is discharged to meet environmental protection requirements; The fibers are dissolved, washed and sterilized to obtain loose fiber aggregates.

优选地,所述可控溶解纤维的制备原料包括对苯二甲酸和/或乙二醇。Preferably, the raw materials for the preparation of the controllable dissolving fibers include terephthalic acid and/or ethylene glycol.

优选地,所述步骤a或b中的溶剂包含有机成分。Preferably, the solvent in step a or b contains organic components.

优选地,所述有机成分为DMSO。Preferably, the organic component is DMSO.

优选地,所述溶剂还包含乙醇;或者,优选地,所述溶剂还包含水。Preferably, the solvent further comprises ethanol; or, preferably, the solvent further comprises water.

更优选地,所述溶剂中还包含四丁基乙酸铵。More preferably, the solvent also contains tetrabutylammonium acetate.

DMSO具有双极性,其对于纤维具有良好的溶胀效果。另外,当加入四丁基乙酸铵时,由于乙酸根离子的强电负性,它是非常强的氢键受体,有利地与纤维素的羟基和缩醛氧原子竞争,从而破坏了纤维素链之间的氢键网络,因此DMSO和四丁基乙酸铵的组合使用极大地提高了可溶纤维的溶解速度。DMSO is bipolar, which has a good swelling effect on fibers. In addition, when tetrabutylammonium acetate is added, due to the strong electronegativity of the acetate ion, it is a very strong hydrogen bond acceptor, which favorably competes with the hydroxyl and acetal oxygen atoms of cellulose, thereby destroying the cellulose The hydrogen bonding network between the chains, so the combined use of DMSO and tetrabutylammonium acetate greatly improves the dissolution rate of soluble fibers.

在一个优选实施方案中,基于溶剂的总重量计,在所述溶剂中,乙醇的含量为40-90 wt%,优选50-80 wt%;DMSO的含量为10-30 wt%,优选15-20%;四丁基乙酸铵的含量为0.1-5.0 wt%,优选0.2-2.0 wt%。In a preferred embodiment, based on the total weight of the solvent, in the solvent, the content of ethanol is 40-90 wt%, preferably 50-80 wt%; the content of DMSO is 10-30 wt%, preferably 15- 20%; the content of tetrabutylammonium acetate is 0.1-5.0 wt%, preferably 0.2-2.0 wt%.

更优选地,所述步骤a或b中的溶剂呈碱性。进一步优选地,所述溶剂中包含NaOH。在一个优选实施方案中,基于溶剂的总重量计,所述溶剂还包含0.001-5.0 wt%,优选0.1-1.0 wt%的NaOH。More preferably, the solvent in step a or b is alkaline. Further preferably, the solvent contains NaOH. In a preferred embodiment, the solvent further comprises 0.001-5.0 wt%, preferably 0.1-1.0 wt% NaOH, based on the total weight of the solvent.

在一个特别优选的实施方式中,所述溶剂中包含离子液体。优选地,基于溶剂的总重量计,离子液体的含量为0.1-10.0 wt%,优选0.2-5.0 wt%,更优选0.5-2.0 wt%。In a particularly preferred embodiment, the solvent contains an ionic liquid. Preferably, based on the total weight of the solvent, the content of the ionic liquid is 0.1-10.0 wt%, preferably 0.2-5.0 wt%, more preferably 0.5-2.0 wt%.

特别优选地,所述离子液体为下式(I)所述离子液体:Particularly preferably, the ionic liquid is the ionic liquid of the following formula (I):

Figure 133846DEST_PATH_IMAGE001
式(I)
Figure 133846DEST_PATH_IMAGE001
Formula (I)

式(I)所示的离子液体能够有效破坏纤维中的氢键,从而在弱的溶剂pH值调节下能够使纤维有效分解,此外,同样地,由于乙酸根离子的强电负性,其作为强的氢键受体,有利地与纤维素的羟基和缩醛氧原子竞争,破坏纤维素链之间的氢键网络,从而可以有效使纤维溶解。另外,当使用式(I)所示离子液体时,由于Cl原子的强吸电子作用以及羟基的极性,可以使分解产生的初始分解产物更均匀和牢固地附着在纤维的孔隙表面,从而可以促进纤维溶解的进一步顺利进行,这可防止溶解的不均匀性如具备分解剂浓度高,可以提高溶解的匀速进行,并且可以进一步减少对非溶纤维的损伤。The ionic liquid represented by formula (I) can effectively break the hydrogen bonds in the fibers, so that the fibers can be effectively decomposed under weak solvent pH adjustment. In addition, similarly, due to the strong electronegativity of acetate ions, it acts as a A strong hydrogen bond acceptor, which favorably competes with the hydroxyl and acetal oxygen atoms of cellulose, disrupts the hydrogen bond network between the cellulose chains, which can effectively dissolve fibers. In addition, when the ionic liquid represented by formula (I) is used, due to the strong electron-withdrawing effect of the Cl atom and the polarity of the hydroxyl group, the initial decomposition products generated by the decomposition can be more uniformly and firmly attached to the pore surface of the fiber, so that the Promote the further smooth progress of fiber dissolution, which can prevent the non-uniformity of dissolution. For example, with a high concentration of disintegrating agent, the uniform speed of dissolution can be improved, and the damage to insoluble fibers can be further reduced.

在本发明的一个优选实施方式中,所述可溶解纺织品为通过以下方法制得的可溶解纺织品:In a preferred embodiment of the present invention, the dissolvable textile is a dissolvable textile prepared by the following method:

(1)加入取对苯二甲酸、间苯二甲酸、乙二醇、5-磺酸钠-间苯二甲酸聚乙二醇酯,从中选择不同的以上物质组合以及不同比例的物质组合进行聚合,获得切片,所述切片为可碱溶解切片,然后依次进行铸带、冷却、切粒和干燥,得到料粒;(1) Add terephthalic acid, isophthalic acid, ethylene glycol, 5-sodium sulfonate-isophthalic acid polyethylene glycol ester, and select different combinations of the above substances and combinations of substances in different proportions for polymerization , obtain slices, and described slices are the soda-dissolving slices, and then successively carry out casting, cooling, dicing and drying to obtain pellets;

(2)将料粒进行纺丝,制备可控溶解纤维,将所述可控溶解纤维用于制成可溶解纺织品。(2) spinning the pellets to prepare controllable dissolving fibers, and using the controllable dissolving fibers to make dissolvable textiles.

优选地,所述纺丝温度为270-300℃。更优选地,所述纺丝温度为280-290℃。Preferably, the spinning temperature is 270-300°C. More preferably, the spinning temperature is 280-290°C.

在本发明的进一步优选实施方式中,将所述松散的纤维集合体与可控溶解纤维通过混纺或交织制备纤维面料。In a further preferred embodiment of the present invention, a fiber fabric is prepared by blending or interlacing the loose fiber aggregate with the controlled dissolving fiber.

在本发明中,更具体地,可溶纤维的制备包括有在不同介质下、不同溶解条件下的可控可溶纤维制备,有长丝、短纤维及纤维条;In the present invention, more specifically, the preparation of soluble fibers includes controllable preparation of soluble fibers under different media and different dissolution conditions, including filaments, short fibers and fiber strands;

纺织品加工包括:可以是100%可溶纤维为原料的纺织品设计加工,也可以是可溶纤维与其它纤维混纺的纺织品加工,包括纺织品用的服饰辅料,如缝纫线、纽扣、商标、吊牌及水洗牌等,也为可溶解物质构成;Textile processing includes: textile design and processing that can be 100% soluble fiber as raw material, or textile processing of soluble fiber blended with other fibers, including clothing accessories for textiles, such as sewing threads, buttons, trademarks, hang tags and water. Shuffle, etc., also composed of soluble substances;

纺织品溶解回收:在一定条件下溶解,对溶解后的可溶纤维物质,进行高纯度的回收和污水处理,达到物质回收及污水达到环保排放标准目的;对于100%的可溶纤维纺织品,实现高纯度的回收,溶解后的回收物可直接作为可控纤维生产的原料,直接用于可控溶解纤维的聚合物原料;对于可控溶解纤维的混纺或者交织产品溶解,由于可控可溶解纤维的溶解,剩余的非溶解纤维为松散的纺织品;Textile dissolution and recycling: Dissolve under certain conditions, carry out high-purity recycling and sewage treatment for the dissolved soluble fiber material, so as to achieve the purpose of material recovery and sewage reaching environmental protection discharge standards; for 100% soluble fiber textiles, high Purity recovery, the dissolved recyclate can be directly used as the raw material for controllable fiber production, and directly used as the polymer raw material for controllable fiber dissolution; for the dissolution of the blended or interwoven products of the controllable dissolvable fiber, due to the controllable dissolvable fiber Dissolved, the remaining non-dissolved fibers are loose textiles;

剩余纺织品再处理:按使用的要求,进行消毒化学处理,及按未来使用要求,进行剥色或者漂白或者再染色处理,由于可溶纤维的溶解,剩余纺织品将变得松散,甚至解体,通过轻柔梳理,纤维强度损伤很小,长度损失很少,获得高品质的另外组分纤维或者漂白或者染色的纤维,可以直接用于纺纱厂直接加工新的纱线,混纺或者交织纺织品的其它组分纤维回收后的品质高,也可直接为纺纱厂原料,即可实现纺织品高效、高品质的全循环回收和使用。Reprocessing of residual textiles: disinfection chemical treatment according to the requirements of use, and stripping or bleaching or re-dyeing treatment according to future use requirements, due to the dissolution of soluble fibers, the remaining textiles will become loose or even disintegrated. Carding, with little damage to fiber strength and little loss of length, to obtain high-quality additional component fibers or bleached or dyed fibers that can be used directly in spinning mills to process new yarns, blends or other components of interwoven textiles The recovered fibers are of high quality and can also be directly used as raw materials for spinning mills, which can achieve efficient and high-quality full-cycle recycling and use of textiles.

本发明可以通过以下具体技术方案来实现。The present invention can be realized by the following specific technical solutions.

一种可溶解纺织品的回收、再生、循环使用技术,包括有以下工艺步骤,具体为:A recovery, regeneration and recycling technology for dissolvable textiles, comprising the following process steps, specifically:

a. 溶解条件可控的可溶纤维以及可溶服饰配件制备:a. Preparation of soluble fibers and soluble apparel accessories with controlled dissolution conditions:

在聚酯原料聚合过程中,加入聚合物总重量不同比例的对苯二甲酸、间苯二甲酸、乙二醇、5-磺酸钠-间苯二甲酸聚乙二醇酯,选择不同的以上物质组合以及不同比例的物质组合进行聚合,获得不同碱溶解条件下的碱溶解切片,碱溶解切片的特性粘度为0.40-0.80,碱溶解切片最后依次完成铸带、冷却、切粒、干燥以及筛选工序;During the polymerization of the polyester raw material, add terephthalic acid, isophthalic acid, ethylene glycol, 5-sodium sulfonate-polyethylene glycol isophthalate in different proportions of the total weight of the polymer, and select the above The combination of substances and different proportions of substances are polymerized to obtain alkali-dissolved slices under different alkali-dissolving conditions. The intrinsic viscosity of the alkali-dissolved slices is 0.40-0.80. The alkali-dissolved slices are finally completed in sequence. Casting, cooling, dicing, drying and screening process;

(1)按常规纺丝工艺,制备可控溶解纤维,该可控溶解纤维包括有长丝、短纤维及纤维条,也包括这些纤维的差别化和有色纤维,以用于生产成衣、无纺布、静电植绒等各种纺织品;(1) According to the conventional spinning process, controllable dissolving fibers are prepared. The controllable dissolving fibers include filaments, short fibers and fiber strips, as well as differentiated and colored fibers of these fibers, which are used in the production of garments, nonwovens Cloth, electrostatic flocking and other textiles;

(2)按常规工艺,制备可控溶解纤维的缝纫线,可以是可溶短纤维的纯纺或者是混纺纱,或可溶长丝纤维纱及合股的纱;(2) According to the conventional process, the sewing thread of controllable dissolving fiber is prepared, which can be pure spinning or blended yarn of soluble short fiber, or soluble filament yarn and plied yarn;

(3)按常规的注塑、加入色母粒和成型工艺,采用可控溶解条件的可溶解切片,生产硬质可溶服饰配件,包括拉链、纽扣及膜形态的logo、水洗吊牌、成分吊牌、商标吊牌等;(3) According to the conventional injection molding, adding color masterbatch and molding process, using soluble slices with controllable dissolution conditions to produce hard soluble clothing accessories, including zippers, buttons and logos in the form of films, wash tags, ingredient tags, Trademark hang tags, etc.;

或者,or,

b. 含可溶纤维的纺织染及成品的制备:b. Preparation of textile dyes and finished products containing soluble fibers:

(1)100%的可控溶解纤维成品:(1) 100% Controllable Dissolving Fiber Finished Products:

(1-1)使用100%的可控溶解纤维,或短纤维纱,或长丝纱,用常规织造工艺,如有需要染色加工过程中,即不加入溶解的介质,如碱类物质,其余工艺与常规聚酯的加工工艺相同;(1-1) Use 100% controlled dissolving fiber, or staple fiber yarn, or filament yarn, use conventional weaving process, if necessary, during dyeing process, that is, do not add dissolved media, such as alkali substances, and the rest The process is the same as that of conventional polyester;

(1-2)100%的可控溶解纤维加氨纶等弹性纤维的成品,用常规织造工艺,如有需要染色加工过程中,即不加入溶解的介质,如碱类物质,其余工艺,与常规聚酯的加工工艺相同;(1-2) The finished product of 100% controllable dissolving fiber plus spandex and other elastic fibers, using the conventional weaving process, if necessary, during the dyeing process, that is, without adding dissolving media, such as alkali substances, the rest of the process is the same as the conventional The processing technology of polyester is the same;

(2)可控溶解纤维与其它非溶纤维的混纺或交织的成品:(2) Blended or interwoven products of controllable soluble fibers and other insoluble fibers:

(2-1)将可控溶解纤维与其它非溶纤维的混纺或交织,如棉、毛、麻及其它化学纤维混纺交织成成品,用常规织造工艺,如有需要染色加工过程中,即不加入溶解的介质,其余工艺与常规聚酯混纺或交织加工工艺相同;(2-1) Blend or interweave controllable soluble fibers with other insoluble fibers, such as cotton, wool, hemp and other chemical fibers, into finished products, and use conventional weaving techniques, if necessary, during dyeing and processing. Add the dissolved medium, and the rest of the process is the same as the conventional polyester blending or interweaving process;

(2-2)将可控溶解纤维与其它非溶纤维的混纺或交织的加氨纶等弹性纤维的成品,如棉、毛、麻及其它化学纤维混纺交织加氨纶等弹性纤维成品,用常规织造工艺,如有需要染色加工过程中,即不加入溶解的介质,其余工艺与常规聚酯混纺或交织加工工艺相同;(2-2) The finished product of blending or interweaving controllable soluble fiber and other insoluble fibers with spandex and other elastic fibers, such as cotton, wool, hemp and other chemical fibers blended and interwoven with spandex and other elastic fiber products, using conventional weaving Process, if necessary, during the dyeing process, that is, without adding dissolved medium, the rest of the process is the same as the conventional polyester blending or interweaving process;

c. 含可溶纤维及可溶服装配件(所述可溶服装配件也可以看作是可溶纤维的一种存在形式)成品的溶解、回收:c. Dissolution and recovery of finished products containing soluble fiber and soluble clothing accessories (the soluble clothing accessories can also be regarded as a form of soluble fiber):

(1)100%的可控溶解纤维面料以及可溶服装配件的溶解、回收:(1) Dissolution and recycling of 100% controllable dissolving fiber fabrics and dissolving clothing accessories:

(1-1)将100%的可控溶解纤维面料或者可溶服饰配件,直接在各种缸体内,在一定的溶剂条件下,完全溶解。对于溶解液,经膜法过滤和酸析、气化(即脱气)等工艺后,获得高纯度的对苯二甲酸和乙二醇和NaOH,排放废水COD达到环保要求;(1-1) Dissolve 100% controlled dissolving fiber fabrics or dissolving clothing accessories directly in various cylinders under certain solvent conditions. For the dissolved liquid, after membrane filtration, acid precipitation, gasification (ie degassing) and other processes, high-purity terephthalic acid, ethylene glycol and NaOH are obtained, and the COD of the discharged wastewater meets the environmental protection requirements;

(1-2)将100%的可控溶解纤维加氨纶等弹性纤维的纤维面料或者可溶服饰配件,直接在各种缸体内,在一定的溶剂条件下,完全溶解。对于溶解液,经膜法过滤和酸析、气化等工艺后,获得高纯度的对苯二甲酸和乙二醇和NaOH,排放废水COD达到环保要求;对于没有溶解氨纶等弹性纤维,则在过滤格栅被拦截,该部分含量少,保持成连续式的氨纶形态,容易识别及易被取走;或者再用氨纶等弹性纤维溶剂溶解氨纶弹性纤维,这部分的溶剂量少,可以回收再循环使用;(1-2) 100% controllable dissolving fiber plus elastic fibers such as spandex or soluble clothing accessories are directly dissolved in various cylinders under certain solvent conditions. For the dissolved solution, after membrane filtration, acid precipitation, gasification and other processes, high-purity terephthalic acid, ethylene glycol and NaOH are obtained, and the COD of the discharged wastewater meets the environmental protection requirements; for elastic fibers such as spandex that are not dissolved, filter The grille is intercepted, the content of this part is small, and it is kept in the form of continuous spandex, which is easy to identify and take away; or use spandex and other elastic fiber solvents to dissolve the spandex elastic fibers. This part has a small amount of solvent and can be recycled and recycled. use;

(2)可控溶解纤维与其它非溶纤维的混纺或交织纤维面料或者可溶服饰配件的溶解、回收:(2) Dissolving and recycling of blended or interwoven fiber fabrics or soluble clothing accessories of controllable soluble fibers and other insoluble fibers:

将该类纺织品,直接在各种缸体内,在一定的溶剂介质溶度条件下,溶解可控溶解纤维;同时清洗、消毒非溶解纤维,而对于非溶解纤维,由于可溶解纤维的溶解,使非溶解纤维成为松散的纤维集合体;Such textiles are directly placed in various cylinders, under the condition of certain solvent medium solubility, to dissolve controllable soluble fibers; at the same time, clean and sterilize insoluble fibers. For insoluble fibers, due to the dissolution of soluble fibers, Make insoluble fibers into loose fiber aggregates;

对于溶解液,经格栅过滤、膜法过滤和酸析、气化等工艺后,获得高纯度的对苯二甲酸和乙二醇和NaOH,所排放废水的COD达到环保要求;For the dissolved liquid, after grid filtration, membrane filtration, acid precipitation, gasification and other processes, high-purity terephthalic acid, ethylene glycol and NaOH are obtained, and the COD of the discharged wastewater meets environmental protection requirements;

对于可控溶解纤维与其它非溶纤维的混纺或交织加氨纶等弹性纤维的成品,如棉、毛、麻及其它化学纤维混纺交织加氨纶等弹性纤维成品,直接在各种缸体内,在一定的溶剂介质溶度条件下,溶解可控溶解纤维及氨纶等弹性纤维,这种溶剂可以是一种或者是分别溶解可控溶解纤维及溶解氨纶等弹力纤维的溶解复合;也可以在缸内溶解可控溶解纤维;然后,再用氨纶等弹性纤维溶剂溶解氨纶弹性纤维,这部分的溶剂,可以回收再循环使用;For the finished products of blended or interwoven elastic fibers such as controllable soluble fibers and other non-soluble fibers, such as cotton, wool, hemp and other chemical fibers blended and interwoven with elastic fibers such as spandex, directly in various cylinders, in Under a certain solubility of the solvent medium, it can dissolve elastic fibers such as controllable dissolving fibers and spandex. Dissolve controllable dissolving fibers; then, use spandex and other elastic fiber solvents to dissolve spandex elastic fibers, and this part of the solvent can be recovered and recycled;

对于已经是松散的非溶解的纤维集合体,可以进行再生处理,可以用消毒液助剂,消毒处理;或直接烘干、轻柔梳理后,为杂色纤维使用;或按再生使用要求,剥色后,漂白处理,烘干、轻柔梳理后,成为漂白纤维;或将剥色后纤维,再经染色,烘干、轻柔梳理后,成为有色纤维使用。由于是松散的纤维集合体,经轻柔梳理后,纤维的强度和长度,损伤很小,保证了非溶解纤维的可纺性和服用性能;For the already loose and non-dissolving fiber aggregates, it can be regenerated, and disinfectant can be used for disinfection; or directly dried and gently combed, it can be used for variegated fibers; or according to the requirements of regeneration, stripping After bleaching, drying, and gentle carding, it becomes bleached fiber; or the peeled fiber is dyed, dried, and gently carded to become colored fiber. Because it is a loose fiber aggregate, after gentle carding, the strength and length of the fiber are less damaged, which ensures the spinnability and wearability of the non-dissolving fiber;

d. 获得高纯度化工原料及高品质纤维材料:d. Obtain high-purity chemical raw materials and high-quality fiber materials:

经上述处理后的回收的化工原料:1、对苯二甲酸和乙二醇和NaOH,纯度高,符合工业使用;2、一次处理的再生纤维的强度保存率高,再生纤维的长度无任何损失。The recovered chemical raw materials after the above treatment: 1. The terephthalic acid, ethylene glycol and NaOH have high purity and are suitable for industrial use; 2. The strength preservation rate of the once-treated regenerated fiber is high, and the length of the regenerated fiber is not lost.

其中,所述步骤a的纺丝温度为270-300℃,注塑温度 150-250℃。Wherein, the spinning temperature in the step a is 270-300°C, and the injection temperature is 150-250°C.

其中,所述步骤c中所采用的碱溶液为氢氧化钠溶液或者低碱、无碱的高温纯水溶液或者有机溶剂。Wherein, the alkali solution adopted in the step c is sodium hydroxide solution or a low-alkali, alkali-free high-temperature pure aqueous solution or an organic solvent.

本发明的有益效果为:本发明所述的一种可溶解纺织品的回收、再生、循环使用技术,对于纺织品经溶解后的溶解液,经格栅过滤、膜法过滤和酸析、气化等工艺后,获得高纯度的对苯二甲酸和乙二醇和NaOH,排放废水COD达到环保要求;对于可溶纤维的混纺或者交织物,可通过纺织品中的可溶纤维的溶解,使紧密的纺织品,变为松散的非溶解纤维的集合体;对于非溶解的纤维集合体,可以进行再生处理,经消毒处理,或直接烘干、轻柔梳理后,为杂色纤维使用,或按再生使用要求,剥色后,漂白处理,烘干、轻柔梳理后,成为漂白纤维,或将剥色后纤维,再经染色,烘干、轻柔梳理后,成为有色纤维使用,由于是松散的纤维集合体,经对纤维的强度和长度的损伤很小的轻柔梳理后,就可以使用,保证了非溶解纤维的可纺性和服用性能。本发明使无价值及成为环境污染物的纺织品,成为有价值的商品,即减少对环境的污染,还可以循环使用。The beneficial effects of the present invention are as follows: the recovery, regeneration and recycling technology of dissolvable textiles described in the present invention, for the dissolving liquid after the textiles are dissolved, through grid filtration, membrane filtration, acid precipitation, gasification, etc. After the process, high-purity terephthalic acid, ethylene glycol and NaOH are obtained, and the COD of the discharged wastewater meets the environmental protection requirements; for the blended or interwoven fabrics of soluble fibers, the soluble fibers in the textiles can be dissolved to make the tight textiles, It becomes a loose aggregate of non-dissolving fibers; for the non-dissolving fiber aggregate, it can be regenerated, disinfected, or directly dried and gently combed, and then used for variegated fibers, or peeled off according to the requirements of regeneration. After coloring, bleaching treatment, drying, and gentle carding will become bleached fibers, or the fibers after stripping will be dyed, dried, and gently combed to become colored fibers. It can be used after gentle carding with little damage to the strength and length of the fiber, which ensures the spinnability and wearability of the non-dissolving fiber. The invention makes the textiles, which are worthless and become environmental pollutants, become valuable commodities, that is, the pollution to the environment is reduced, and the textiles can be recycled.

附图说明Description of drawings

下面利用附图来对本发明进行进一步的说明,但是附图中的实施例不构成对本发明的任何限制。The present invention is further described below with reference to the accompanying drawings, but the embodiments in the accompanying drawings do not constitute any limitation to the present invention.

图1为本发明的碱溶解液回收结构示意图;Fig. 1 is the alkali dissolving liquid recovery structure schematic diagram of the present invention;

图2为根据现有技术方法纤维在溶解20min时的TEM图(对比例1);Figure 2 is a TEM image of fibers dissolved for 20 min according to the prior art method (Comparative Example 1);

图3为根据本发明的方法纤维在溶解20min时的TEM图(实施例1)。Figure 3 is a TEM image of the fibers according to the method of the present invention when they are dissolved for 20 min (Example 1).

具体实施方式Detailed ways

下面结合具体的实施方式来对本发明进行说明。The present invention will be described below with reference to specific embodiments.

实施例1Example 1

100%的可控可溶纤维面料以及可溶服装配件的溶解、回收和再利用技术,其包括有以下工艺步骤,具体为:The technology for dissolving, recycling and reusing 100% controllable soluble fiber fabrics and soluble clothing accessories includes the following process steps, specifically:

a. 在聚酯原料聚合过程中,加入聚合物总重量为6%的5-磺酸钠-间苯二甲酸聚乙二醇酯以及聚合物总重量为4%的间苯二甲酸,打浆搅拌并同时加温至230℃;而后移至反应釜并再加入聚合物总重量为10%的聚乙二醇,使其稀释并降温至210℃;继续往反应釜中加入聚乙二醇,这部分聚乙二醇占聚合物总重量的10%,在50分钟内加完聚乙二醇并同时搅拌,常压下升温至230℃并使得混合物料在真空状态下聚合,聚合后的碱降解切片最后依次完成铸带、冷却、切粒、干燥以及筛选工序,其中,碱降解切片的特性粘度为0.65;a. in the polyester raw material polymerization process, adding the 5-sodium sulfonate-isophthalic acid polyethylene glycol ester that the total polymer weight is 6% and the isophthalic acid that the total polymer weight is 4%, beating and stirring And at the same time be heated to 230 ℃; Then move to the reaction kettle and then add the polyethylene glycol that the total weight of the polymer is 10%, so that it is diluted and cooled to 210 ℃; Continue to add polyethylene glycol in the reaction kettle, this Part of the polyethylene glycol accounts for 10% of the total weight of the polymer. The polyethylene glycol is added within 50 minutes and stirred at the same time. The temperature is raised to 230 ° C under normal pressure and the mixture is polymerized in a vacuum state. The alkali after polymerization is degraded. The slicing finally completes the steps of casting, cooling, dicing, drying and screening in sequence, wherein the intrinsic viscosity of the alkali-degraded slicing is 0.65;

将上述碱降解切片制备碱溶降解长丝纤维,该易碱溶降解纤维为长丝纤维:其中,纺丝及纺丝后处理工序为:经常规的POY纺丝工艺,纺丝温度290℃,获得在碱溶液下可以溶解的POY长丝,然后,在加弹机上,生产出低弹丝DTY;其中,纤维指标:15.5tex/48F细度、3.6cn/dtex强度、25%断裂伸长率.经常规纺丝工艺,生产FDY长丝,150D/48F,强度4.0cn/dtex强度、20%断裂伸长率;The alkali-soluble degradable filament fiber is prepared by the above-mentioned alkali degradation slices, and the easily alkali-soluble degradable fiber is a filament fiber: wherein, the spinning and post-spinning treatment procedures are: through the conventional POY spinning process, the spinning temperature is 290 ° C, Obtain POY filaments that can be dissolved in alkaline solution, and then, on the texturing machine, produce low elastic yarn DTY; among them, fiber index: 15.5tex/48F fineness, 3.6cn/dtex strength, 25% elongation at break .By conventional spinning process, produce FDY filament, 150D/48F, strength 4.0cn/dtex strength, 20% elongation at break;

b. 上述DTY长丝,经常规工艺,生产出各种面料及成衣、纺织品:b. The above DTY filaments, through conventional processes, produce various fabrics, garments and textiles:

(1)上述FDY长丝经合股并线后,做纺织品的缝纫线;(1) After the above-mentioned FDY filaments are plied and stitched, they are used as sewing threads for textiles;

(2)上述成衣、纺织品配上服饰配件,该配件为可溶切片经常规的注塑、加色母粒着色和成型工艺的硬质可溶服饰配件,包括拉链、纽扣及膜形态的logo及水g洗吊牌、成分吊牌、商标吊牌;(2) The above garments and textiles are equipped with clothing accessories, which are hard soluble clothing accessories with soluble chips that have undergone conventional injection molding, masterbatch coloring and molding processes, including zippers, buttons, and film-shaped logos and water. g Shuffle tags, ingredient tags, trademark tags;

c. 在封闭的染整厂普通溢流缸中,加入溶剂,溶解温度为110℃,溶解时间为60分钟,浴比:1:10,将可溶纤维溶解,所述溶剂的组成为,基于溶剂的总重量计,乙醇的含量为70.0 wt%,;DMSO的含量为25.0 wt%,四丁基乙酸铵的含量为2.0 wt%,0.2 wt%的NaOH,2.8wt%式(I)所示离子液体;c. In a closed common overflow tank of dyeing and finishing plant, add a solvent, the dissolving temperature is 110°C, the dissolving time is 60 minutes, the liquor ratio is 1:10, and the soluble fibers are dissolved. The composition of the solvent is based on Based on the total weight of the solvent, the content of ethanol is 70.0 wt%, the content of DMSO is 25.0 wt%, the content of tetrabutylammonium acetate is 2.0 wt%, 0.2 wt% of NaOH, 2.8 wt% shown in formula (I) ionic liquid;

d. 如图1所示,将可控溶溶解纤维纺织品,在缸中的碱溶解液中溶解,溶解液经格栅后引入至调节池中,调节池中的碱溶解液依次经过预处理以及膜系统,且经过膜系统的碱溶解液进入至酸析罐中,且通过加酸泵往酸析罐中抽送酸液,酸液与碱溶解液在酸析罐中搅拌后获得PH值为3-4的废水,在此过程中,对苯二甲酸析出;待酸液与碱溶解液于酸析罐中充分反应后,将酸析罐中的废水引入至离心过滤机进行过滤,以分离出对苯二甲酸。经离心过滤机进行过滤脱水后,分离出的对苯二甲酸再根据不同的要求,洗涤或不洗涤,装袋储存等待出运。将酸析过的滤液,再经过过滤膜系统,分离出乙二醇。其中,格栅主要是拦截水中较大颗粒物及其它大径污染物,如杂质等漂浮物,调节池用于缓冲水量、均匀水质、沉淀较大的固体颗粒物,以利于后序工艺进行处理。经离心过滤机的滤出液大幅度降低污水COD,滤液可生化。再经膜系统过滤乙二醇后,COD进一步降低,满足印染废水排放要求,且进入工厂的生化污水处理系统。d. As shown in Figure 1, the controllable dissolving fiber textile is dissolved in the alkaline dissolving solution in the tank, and the dissolving solution is introduced into the adjustment tank after passing through the grid, and the alkaline dissolving solution in the adjustment tank is sequentially pretreated and Membrane system, and the alkali solution passing through the membrane system enters the acid precipitation tank, and the acid solution is pumped into the acid precipitation tank through the acid pump, and the acid solution and the alkali solution are stirred in the acid precipitation tank to obtain a pH value of 3 -4 waste water, during this process, terephthalic acid is precipitated; after the acid solution and the alkali solution are fully reacted in the acid precipitation tank, the wastewater in the acid precipitation tank is introduced into a centrifugal filter for filtration to separate out terephthalic acid. After being filtered and dehydrated by a centrifugal filter, the separated terephthalic acid can be washed or not washed according to different requirements, and stored in bags for shipment. The acid-precipitated filtrate is then passed through a filter membrane system to separate out ethylene glycol. Among them, the grille mainly intercepts larger particles and other large-diameter pollutants in the water, such as impurities and other floating objects, and the adjustment tank is used to buffer the water volume, uniform water quality, and precipitate larger solid particles, so as to facilitate the subsequent processing. The filtrate of the centrifugal filter can greatly reduce the COD of sewage, and the filtrate can be biochemical. After the ethylene glycol is filtered by the membrane system, the COD is further reduced, which meets the discharge requirements of printing and dyeing wastewater, and enters the biochemical wastewater treatment system of the factory.

实施例2Example 2

可控可溶纤维与纤维素纤维的混纺纱织物的纤维面料以及可溶服饰配件的溶解、回收和再利用技术,其包括有以下工艺步骤,具体为:The fiber fabric of the blended yarn fabric of controllable soluble fiber and cellulose fiber and the dissolution, recovery and reuse technology of soluble clothing accessories, which include the following process steps, specifically:

a. 将实施例一所制备而成的可控可溶纤维短纤维,与纤维素纤维(如棉、麻及人造纤维)混纺,混纺比65/35,50/50等;纱支按常规的纤维素纤维或混纺的纱线规格;织布按常规工艺;染色采用聚酯与纤维素纤维二浴法的活性染料和分散染料染色工艺;由此,制得面料,包括梭织及针织面料;a. The controllable soluble short fibers prepared in Example 1 are blended with cellulose fibers (such as cotton, hemp and rayon), and the blending ratio is 65/35, 50/50, etc.; Cellulose fiber or blended yarn specifications; weaving according to conventional technology; dyeing using polyester and cellulose fiber two-bath method of reactive dyes and disperse dyes dyeing process; thus, obtained fabrics, including woven and knitted fabrics;

(1)上述短纤维混纺纱经合股并线后,做该类纺织品的缝纫线;(1) After the above-mentioned staple fiber blended yarn is plied and stitched, it is used as a sewing thread for this type of textile;

(2)上述成衣、纺织品配上服饰配件,该配件为可溶切片经常规的注塑、加色母粒着色和成型工艺的硬质可溶服饰配件,包括拉链、纽扣及膜形态的logo及水g洗吊牌、成分吊牌、商标吊牌;(2) The above garments and textiles are equipped with clothing accessories, which are hard soluble clothing accessories with soluble chips that have undergone conventional injection molding, masterbatch coloring and molding processes, including zippers, buttons, and film-shaped logos and water. g Shuffle tags, ingredient tags, trademark tags;

b. 清洗、消毒及溶解:在封闭的缸中溶解,加入溶剂,溶解温度为110℃,溶解时间为60分钟,浴比:1:10,并加入消毒剂、清洗剂,将可溶纤维溶解及消毒和清洗,所述溶剂的组成为,基于溶剂的总重量计,乙醇的含量为70.0 wt%,;DMSO的含量为25.0 wt%,四丁基乙酸铵的含量为2.0 wt%,0.2 wt%的NaOH,2.8 wt%式(I)所示离子液体;b. Cleaning, disinfection and dissolution: dissolve in a closed tank, add solvent, dissolve temperature is 110℃, dissolve time is 60 minutes, bath ratio: 1:10, and add disinfectant and cleaning agent to dissolve soluble fibers and disinfection and cleaning, the composition of the solvent is, based on the total weight of the solvent, the content of ethanol is 70.0 wt%, the content of DMSO is 25.0 wt%, the content of tetrabutylammonium acetate is 2.0 wt%, 0.2 wt% % NaOH, 2.8 wt% ionic liquid shown in formula (I);

如图1所示,对于所排出的溶解液而言,经格栅后引入至调节池中,调节池中的碱溶解液依次经过预处理以及膜系统,且经过膜系统的碱溶解液进入至酸析罐中,且通过加酸泵往酸析罐中抽送酸液,酸液与碱溶解液在酸析罐中搅拌后获得PH值为3-4的废水,在此过程中,对苯二甲酸析出;待酸液与碱溶解液于酸析罐中充分反应后,将酸析罐中的废水引入至离心过滤机进行过滤,以分离出对苯二甲酸。经离心过滤机进行过滤脱水后,分离出的对苯二甲酸再根据不同的要求,洗涤或不洗涤,装袋储存等待出运。将酸析过的滤液,再经过过滤膜系统,分离出乙二醇。其中,格栅主要是拦截水中较大颗粒物及其它大径污染物,如杂质等漂浮物,调节池用于缓冲水量、均匀水质、沉淀较大的固体颗粒物,以利于后序工艺进行处理。经离心过滤机的滤出液大幅度降低污水COD,滤液可生化。再经膜系统过滤乙二醇后,COD进一步降低,满足印染废水排放要求,且进入工厂的生化污水处理系统;As shown in Figure 1, for the discharged dissolved liquid, it is introduced into the adjustment tank after passing through the grid, and the alkaline dissolved liquid in the adjustment tank undergoes pretreatment and the membrane system in turn, and the alkaline dissolved liquid through the membrane system enters the In the acid precipitation tank, the acid solution is pumped into the acid precipitation tank by adding an acid pump, and the acid solution and the alkali solution are stirred in the acid precipitation tank to obtain waste water with a pH value of 3-4. Formic acid is precipitated; after the acid solution and the alkali solution are fully reacted in the acid precipitation tank, the waste water in the acid precipitation tank is introduced into a centrifugal filter for filtration to separate terephthalic acid. After being filtered and dehydrated by a centrifugal filter, the separated terephthalic acid can be washed or not washed according to different requirements, and stored in bags for shipment. The acid-precipitated filtrate is then passed through a filter membrane system to separate out ethylene glycol. Among them, the grille mainly intercepts larger particles and other large-diameter pollutants in the water, such as impurities and other floating objects, and the adjustment tank is used to buffer the water volume, uniform water quality, and precipitate larger solid particles, so as to facilitate the subsequent processing. The filtrate of the centrifugal filter can greatly reduce the COD of sewage, and the filtrate can be biochemical. After the ethylene glycol is filtered by the membrane system, the COD is further reduced, which meets the discharge requirements of printing and dyeing wastewater, and enters the biochemical wastewater treatment system of the factory;

对于非溶解纤维而言,依次进行剥色和漂白,其中采用还原剥色工艺进行剥色处理,经消毒、剥色、漂白的棉纤维松散集合体,可以再按需要按常规漂白棉花的染色工艺染色烘干,也可以直接以漂白松散集合体烘干。最后将上述烘干的棉纤维,轻柔梳理、开松,纤维强度、长度损伤小,保持原有纤维的可纺性和服用性,获得高品质的再生棉纤维,使棉纤维可以后续循环使用生产高品质的纱线。For non-dissolving fibers, color stripping and bleaching are carried out in sequence, in which the color stripping process is carried out by means of reduction and color stripping. Dyeing and drying can also be directly dried with bleached loose aggregates. Finally, the above-mentioned dried cotton fibers are gently combed and opened, the fiber strength and length are less damaged, the spinnability and wearability of the original fibers are maintained, and high-quality regenerated cotton fibers are obtained, so that the cotton fibers can be recycled for subsequent production. High quality yarn.

实施例3Example 3

可控可溶纤维与纤维素纤维的混纺纱加氨纶纤维织物的纤维面料以及可溶服饰配件的溶解、回收和再利用技术,其包括有以下工艺步骤,具体为:The technology for dissolving, recycling and reusing controllable soluble fiber and cellulose fiber blended yarn plus spandex fiber fabric and soluble clothing accessories includes the following process steps, specifically:

a. 将实施例一所制备而成的聚合后原料,经常规纺丝工艺,生产长度38mm、细度1.5D的短纤维(3.6cn/dtex强度、25%断裂伸长率),将可控可溶纤维短纤维,与纤维素纤维(如棉、麻及人造纤维)混纺,混纺比65/35,50/50等,将该纱线与氨纶交织或者并线弹力纱线,按常规织造工艺成梭织或者针织面料;染色采用聚酯与纤维素纤维二浴法的活性染料和分散染料染色工艺;由此,制得面料,包括梭织及针织面料,再缝制为纺织品成品;a. The polymerized raw material prepared in Example 1 is subjected to a conventional spinning process to produce short fibers with a length of 38mm and a fineness of 1.5D (3.6cn/dtex strength, 25% elongation at break), which will be controllable Soluble staple fibers, blended with cellulose fibers (such as cotton, hemp and man-made fibers), the blending ratio is 65/35, 50/50, etc., the yarn is interwoven with spandex or doubling elastic yarn, according to the conventional weaving process into woven or knitted fabrics; dyed by reactive dyes and disperse dyes dyeing process of polyester and cellulose fiber two-bath method; thus, fabrics are prepared, including woven and knitted fabrics, and then sewn into finished textile products;

(1)上述短纤维混纺纱经合股并线后,做该类纺织品的缝纫线;(1) After the above-mentioned staple fiber blended yarn is plied and stitched, it is used as a sewing thread for this type of textile;

(2)上述成衣、纺织品配上服饰配件,该配件为可溶切片经常规的注塑、加色母粒着色和成型工艺的硬质服饰配件,包括拉链、纽扣及膜形态的logo及水g洗吊牌、成分吊牌、商标吊牌;(2) The above-mentioned garments and textiles are equipped with clothing accessories, which are hard clothing accessories with soluble chips that have undergone conventional injection molding, masterbatch coloring and molding processes, including zippers, buttons, and film-shaped logos and washing with water. Tag, ingredient tag, trademark tag;

b. 清洗、消毒及溶解:在封闭的缸中加入溶剂,溶解温度为110℃,溶解时间为60分钟,浴比为1:10,并添加消毒剂、清洗剂,将可溶纤维溶解及消毒和清洗,所述溶剂的组成为,基于溶剂的总重量计,乙醇的含量为70.0 wt%,;DMSO的含量为25.0 wt%,四丁基乙酸铵的含量为2.0 wt%,0.2 wt%的NaOH,2.8 wt%式(I)所示离子液体;b. Cleaning, disinfection and dissolving: add solvent in a closed tank, the dissolving temperature is 110°C, the dissolving time is 60 minutes, the bath ratio is 1:10, and disinfectant and cleaning agent are added to dissolve and disinfect the soluble fibers and cleaning, the composition of the solvent is, based on the total weight of the solvent, the content of ethanol is 70.0 wt%, the content of DMSO is 25.0 wt%, the content of tetrabutylammonium acetate is 2.0 wt%, and the content of 0.2 wt% NaOH, 2.8 wt% ionic liquid represented by formula (I);

如图1所示,对于所排出的溶解液而言,经格栅后引入至调节池中,调节池中的碱溶解液依次经过预处理以及膜系统,且经过膜系统的碱溶解液进入至酸析罐中,且通过加酸泵往酸析罐中抽送酸液,酸液与碱溶解液在酸析罐中搅拌后获得PH值为3-4的废水,在此过程中,对苯二甲酸析出;待酸液与碱溶解液于酸析罐中充分反应后,将酸析罐中的废水引入至离心过滤机进行过滤,以分离出对苯二甲酸。经离心过滤机进行过滤脱水后,分离出的对苯二甲酸再根据不同的要求,洗涤或不洗涤,装袋储存等待出运。将酸析过的滤液,再经过过滤膜系统,分离出乙二醇。其中,格栅主要是拦截水中较大颗粒物及其它大径污染物,如杂质等漂浮物,调节池用于缓冲水量、均匀水质、沉淀较大的固体颗粒物,以利于后序工艺进行处理。经离心过滤机的滤出液大幅度降低污水COD,滤液可生化。再经膜系统过滤乙二醇后,COD进一步降低,满足印染废水排放要求,且进入工厂的生化污水处理系统;As shown in Figure 1, for the discharged dissolved liquid, it is introduced into the adjustment tank after passing through the grid, and the alkaline dissolved liquid in the adjustment tank undergoes pretreatment and the membrane system in turn, and the alkaline dissolved liquid through the membrane system enters the In the acid precipitation tank, the acid solution is pumped into the acid precipitation tank by adding an acid pump, and the acid solution and the alkali solution are stirred in the acid precipitation tank to obtain waste water with a pH value of 3-4. Formic acid is precipitated; after the acid solution and the alkali solution are fully reacted in the acid precipitation tank, the waste water in the acid precipitation tank is introduced into a centrifugal filter for filtration to separate terephthalic acid. After being filtered and dehydrated by a centrifugal filter, the separated terephthalic acid can be washed or not washed according to different requirements, and stored in bags for shipment. The acid-precipitated filtrate is then passed through a filter membrane system to separate out ethylene glycol. Among them, the grille mainly intercepts larger particles and other large-diameter pollutants in the water, such as impurities and other floating objects, and the adjustment tank is used to buffer the water volume, uniform water quality, and precipitate larger solid particles, so as to facilitate the subsequent processing. The filtrate of the centrifugal filter can greatly reduce the COD of sewage, and the filtrate can be biochemical. After the ethylene glycol is filtered by the membrane system, the COD is further reduced, which meets the discharge requirements of printing and dyeing wastewater, and enters the biochemical wastewater treatment system of the factory;

对于在缸中的非溶解纤维,加入二甲基乙酰胺(DMAC)液体,浴比为1:1,温度为95℃,时间为30分钟,而后排出二甲基乙酰胺(DMAC)液体并通过液体收集器储存,以待下一缸循环使用;非溶解纤维再依次进行剥色和漂白,其中采用还原剥色工艺进行剥色处理,经消毒、剥色、漂白的棉纤维松散集合体,可以再按需要按常规漂白棉花的染色工艺染色烘干,也可以直接以漂白松散集合体烘干。最后将上述烘干的棉纤维,轻柔梳理、开松,纤维强度、长度损伤小,保持原有纤维的可纺性和服用性,获得高品质的再生棉纤维,使棉纤维可以后续循环使用生产高品质的纱线。For the non-dissolved fibers in the tank, add dimethylacetamide (DMAC) liquid, the liquor ratio is 1:1, the temperature is 95 ℃, the time is 30 minutes, and then the dimethylacetamide (DMAC) liquid is discharged and passed through The liquid collector is stored for recycling in the next tank; the non-dissolved fibers are then stripped and bleached in sequence, and the color stripping process is carried out by using the reduction stripping process. Then, it can be dyed and dried according to the dyeing process of conventional bleached cotton as required, or it can be directly dried with bleached loose aggregates. Finally, the above-mentioned dried cotton fibers are gently combed and opened, the fiber strength and length are less damaged, the spinnability and wearability of the original fibers are maintained, and high-quality regenerated cotton fibers are obtained, so that the cotton fibers can be recycled for subsequent production. High quality yarn.

实施例4Example 4

可控可溶纤维与毛纤维的混纺织物的成品的溶解、回收和再利用技术,其包括有以下工艺步骤,具体为:The technology for dissolving, recycling and reusing the finished product of the blended fabric of controllable soluble fiber and wool fiber includes the following process steps, specifically:

a. 在聚酯原料聚合过程中,加入聚合物总重量为10%的5-磺酸钠-间苯二甲酸聚乙二醇酯以及聚合物总重量为4%的间苯二甲酸,打浆搅拌并同时加温至230℃;而后移至反应釜并再加入聚合物总重量为15%的聚乙二醇,使其稀释并降温至210℃;继续往反应釜中加入聚乙二醇,这部分聚乙二醇占聚合物总重量的15%,在50分钟内加完聚乙二醇并同时搅拌,常压下升温至230℃并使得混合物料在真空状态下聚合,聚合后的碱降解切片最后依次完成铸带、冷却、切粒、干燥以及筛选工序,其中,碱降解切片的特性粘度为0.55;a. in the polyester raw material polymerization process, adding the 5-sodium sulfonate-isophthalic acid polyethylene glycol ester that the total polymer weight is 10% and the isophthalic acid that the total polymer weight is 4%, beating and stirring And at the same time be heated to 230 ℃; Then move to the reaction kettle and add the polyethylene glycol that the total weight of the polymer is 15%, make it diluted and be cooled to 210 ℃; Continue to add polyethylene glycol in the reaction kettle, this Part of the polyethylene glycol accounts for 15% of the total weight of the polymer. The polyethylene glycol was added within 50 minutes and stirred at the same time. The temperature was raised to 230 ° C under normal pressure and the mixture was polymerized in a vacuum state, and the alkali after the polymerization was degraded. The slicing finally completes the steps of casting, cooling, dicing, drying and screening in sequence, wherein the intrinsic viscosity of the alkali-degraded slices is 0.55;

将上述碱降解切片制备低碱易碱容短纤维,纺丝温度275℃。该低碱易溶解纤维为毛型纤维,长度为110mm,强度2.5cn/dtex,断裂伸长率 30%,后经梳理制条后,制得20克/5米的纤维条。在毛纺生产中,与羊毛条并条混合成纱,混纺比例为50可溶纤维/50羊毛纤维,Nm为60Nm,并按常规工艺织布及无碱态下染色成面料及成纺织品;The above alkali-degraded chips were used to prepare low-alkali-easy-alkali-tolerant short fibers, and the spinning temperature was 275°C. The low-alkali easily soluble fiber is wool-type fiber, with a length of 110 mm, a strength of 2.5 cn/dtex, and an elongation at break of 30%. After carding and slivering, a fiber sliver of 20 g/5 m is obtained. In the production of wool spinning, it is mixed with wool tops to form yarns, the blending ratio is 50 soluble fibers/50 wool fibers, and the Nm is 60 Nm, and the fabrics and textiles are woven according to the conventional process and dyed in an alkali-free state;

(1)上述毛混纺纱经合股并线后,做毛混纺纺织品的缝纫线。(1) After the above-mentioned wool blended yarn is plied and stitched, it is used as a sewing thread for wool blended textiles.

(2)上述成衣、纺织品配上服饰配件,该配件为可溶切片经常规的注塑、加色母粒着色和成型工艺的硬质服饰配件,包括拉链、纽扣及膜形态的logo及水g 洗吊牌、成分吊牌、商标吊牌;(2) The above-mentioned garments and textiles are equipped with clothing accessories, which are rigid clothing accessories with soluble chips that have undergone conventional injection molding, masterbatch coloring and molding processes, including zippers, buttons, logos in the form of membranes, and water washing. Tag, ingredient tag, trademark tag;

b. 在封闭的缸中加入100%NaOH 1.5g/L,渗透剂 2g/升溶剂,溶解温度为90℃,溶解时间为60分钟,浴比为1:10,将可溶纤维溶解,所述溶剂的组成为,基于溶剂的总重量计,乙醇的含量为70.0 wt%,;DMSO的含量为25.0 wt%,四丁基乙酸铵的含量为2.0 wt%,0.2wt%的NaOH,2.8 wt%式(I)所示离子液体;b. Add 100% NaOH 1.5g/L, penetrant 2g/L solvent to a closed tank, the dissolving temperature is 90°C, the dissolving time is 60 minutes, and the bath ratio is 1:10 to dissolve the soluble fibers. The composition of the solvent is, based on the total weight of the solvent, the content of ethanol is 70.0 wt%, the content of DMSO is 25.0 wt%, the content of tetrabutylammonium acetate is 2.0 wt%, 0.2 wt% of NaOH, 2.8 wt% The ionic liquid represented by formula (I);

如图1所示,对于所排出的溶解液而言,经格栅后引入至调节池中,调节池中的碱溶解液依次经过预处理以及膜系统,且经过膜系统的碱溶解液进入至酸析罐中,且通过加酸泵往酸析罐中抽送酸液,酸液与碱溶解液在酸析罐中搅拌后获得pH值为3-4的废水,在此过程中,对苯二甲酸析出;待酸液与碱溶解液于酸析罐中充分反应后,将酸析罐中的废水引入至离心过滤机进行过滤,以分离出对苯二甲酸。经离心过滤机进行过滤脱水后,分离出的对苯二甲酸再根据不同的要求,洗涤或不洗涤,装袋储存等待出运。将酸析过的滤液,再经过过滤膜系统,分离出乙二醇。其中,格栅主要是拦截水中较大颗粒物及其它大径污染物,如杂质等漂浮物,调节池用于缓冲水量、均匀水质、沉淀较大的固体颗粒物,以利于后序工艺进行处理。经离心过滤机的滤出液大幅度降低污水COD,滤液可生化。再经膜系统过滤乙二醇后,COD进一步降低,满足印染废水排放要求,且进入工厂的生化污水处理系统;As shown in Figure 1, for the discharged dissolved liquid, it is introduced into the adjustment tank after passing through the grid, and the alkaline dissolved liquid in the adjustment tank undergoes pretreatment and the membrane system in turn, and the alkaline dissolved liquid through the membrane system enters the In the acid precipitation tank, the acid solution is pumped into the acid precipitation tank by adding an acid pump, and the acid solution and the alkali solution are stirred in the acid precipitation tank to obtain wastewater with a pH value of 3-4. Formic acid is precipitated; after the acid solution and the alkali solution are fully reacted in the acid precipitation tank, the waste water in the acid precipitation tank is introduced into a centrifugal filter for filtration to separate terephthalic acid. After being filtered and dehydrated by a centrifugal filter, the separated terephthalic acid can be washed or not washed according to different requirements, and stored in bags for shipment. The acid-precipitated filtrate is then passed through a filter membrane system to separate out ethylene glycol. Among them, the grille mainly intercepts larger particles and other large-diameter pollutants in the water, such as impurities and other floating objects, and the adjustment tank is used to buffer the water volume, uniform water quality, and precipitate larger solid particles, so as to facilitate the subsequent processing. The filtrate of the centrifugal filter can greatly reduce the COD of sewage, and the filtrate can be biochemical. After the ethylene glycol is filtered by the membrane system, the COD is further reduced, which meets the discharge requirements of printing and dyeing wastewater, and enters the biochemical wastewater treatment system of the factory;

将未溶解的松散的羊毛纤维集合体,进行剥色、漂白,以获得强度和长度保持良好的再生羊毛纤维。The undissolved loose wool fiber aggregates are stripped and bleached to obtain recycled wool fibers with good strength and length.

对比例1Comparative Example 1

重复实施例1,其与实施例1的区别仅在于在b中,在封闭的缸中加入100%NaOH1.5g/L,渗透剂 2g/升。Example 1 was repeated except that in b, 100% NaOH 1.5g/L and penetrant 2g/L were added in a closed tank.

由图2和图3可以清楚地看出,当采用本发明的溶剂进行溶解处理时,溶解速度更快(即消解得更快),并且对非溶纤维损伤更小(具有更小的图中阴影区域),从而表明本发明的溶剂对可溶纤维溶解速度快且对非溶纤维损伤小的溶剂,这意味着特别有利的经济效益和价值。It can be clearly seen from Figure 2 and Figure 3 that when the solvent of the present invention is used for dissolution treatment, the dissolution rate is faster (that is, the digestion is faster), and the damage to the non-dissolving fiber is smaller (with a smaller figure). Shaded area), thus indicating that the solvent of the present invention has a fast dissolving speed for soluble fibers and a solvent with little damage to insoluble fibers, which means particularly favorable economic benefits and value.

本书面描述使用实例来公开本发明,包括最佳模式,且还使本领域技术人员能够制造和使用本发明。本发明的可授予专利的范围由权利要求书限定,且可以包括本领域技术人员想到的其它实例。如果这种其它实例具有不异于权利要求书的字面语言的结构元素,或者如果这种其它实例包括与权利要求书的字面语言无实质性差异的等效结构元素,则这种其它实例意图处于权利要求书的范围之内。在不会造成不一致的程度下,通过参考将本文中参考的所有引用之处并入本文中。This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to make and use the invention. The patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. If such other examples have structural elements that do not differ from the literal language of the claims, or if such other examples include equivalent structural elements with insubstantial differences from the literal language of the claims, such other examples are intended within the scope of the claims. To the extent that it does not create inconsistency, all citations referenced herein are incorporated herein by reference.

Claims (7)

1. A method of recycling a dissolvable textile, wherein the dissolvable textile comprises or is made from a controlled dissolving fibrous facing, the method comprising the steps of:
a. for controlled dissolving fibrous fabrics, the method comprises the steps of:
placing the controllable dissolving fiber fabric into a container, adding a solvent to completely dissolve the controllable dissolving fiber fabric, filtering, acid-separating and degassing a dissolving solution to obtain terephthalic acid and ethylene glycol, wherein the COD (chemical oxygen demand) of the discharged wastewater meets the environmental protection requirement;
or,
b. for a fibrous fabric having a blend or interweave of controlled dissolving fibers with other non-dissolving fibers, the method comprises the steps of:
placing the fiber fabric in a container, adding a solvent to dissolve the fiber fabric, filtering, acid-separating and degassing a dissolved solution to obtain terephthalic acid and ethylene glycol, wherein the COD (chemical oxygen demand) of the discharged wastewater meets the environmental protection requirement; cleaning and disinfecting the non-soluble fiber to obtain a loose fiber aggregate;
the solvent of the steps a and b comprises ionic liquid, the content of the ionic liquid is 0.1-10.0 wt% based on the total weight of the solvent, and the ionic liquid is the ionic liquid shown in the following formula (I):
Figure FDA0002493244850000011
the solvent in a or b comprises DMSO and tetrabutylammonium acetate, and the content of the DMSO in the solvent is 10-30 wt% and the content of the tetrabutylammonium acetate in the solvent is 0.1-5.0 wt% based on the total weight of the solvent.
2. The method according to claim 1, wherein the solvent further comprises ethanol.
3. The method according to claim 1, wherein the solvent in a or b is basic.
4. The method of claim 1, wherein the soluble textile is a soluble textile made by the method of:
(1) adding terephthalic acid, isophthalic acid, ethylene glycol and 5-sodium sulfonate-isophthalic acid polyethylene glycol ester, selecting different substance combinations and different proportions from the terephthalic acid, the isophthalic acid polyethylene glycol ester to polymerize to obtain slices, wherein the slices are alkali-soluble slices, and then sequentially carrying out tape casting, cooling, grain cutting and drying to obtain material particles;
(2) and spinning the material particles to prepare controllable dissolving fibers, and using the controllable dissolving fibers to prepare soluble textiles.
5. The process according to claim 4, wherein the spinning temperature is 270-300 ℃.
6. The process according to claim 5, wherein the spinning temperature is 280-290 ℃.
7. The method of claim 1, wherein the loose assembly of fibers is blended or interwoven with controlled dissolving fibers to produce a fibrous facing.
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