CN110219072B - Method for recycling soluble textiles - Google Patents
Method for recycling soluble textiles Download PDFInfo
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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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- 239000002608 ionic liquid Substances 0.000 claims description 14
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- 238000001914 filtration Methods 0.000 claims description 11
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/095—Preparation 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent 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
- D01F6/92—Monocomponent 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
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
Technical Field
The invention relates to the technical field of fiber processing, textile processing and environmental protection, in particular to a technology for recovering, regenerating and recycling soluble textiles.
Background
Countless textiles worldwide become waste products that can no longer be used, or are of low grade, which results in a huge waste of resources and secondary pollution of the environment. The existing textile fiber has no technology and product which can be simply treated and recycled, and the important reason is that the textile raw material composition, color and ready-made clothes accessories are complex; the fabric has compact structure, large fiber damage after opening and low use value.
At present, in the market, only the high-value textiles such as pure-spun cashmere, aramid fiber and the like are subjected to opening and carding to obtain fibers with low strength and short length, and the fibers are recycled with low value.
In the other recycling route, PET bottles are recycled, washed and granulated to obtain PET fibers, but the obtained fiber textiles cannot be used at last and become wastes and pollutants. Or the recycled pure PET clothes are decomposed by high-temperature melting and chemical alcoholysis to obtain PTA (terephthalic acid), but the method has high cost and is only applicable to 100 percent PET fabrics and is not applicable to blending other fabrics which are not PET. This approach suffers from a large limitation.
The applicant's prior patent application CN106065085A discloses a technology for recycling, regenerating and recycling soluble textiles, which adopts polyester soluble fibers with controllable dissolution, and is processed into soluble clothing accessories through conventional weaving, dyeing, after finishing and garment making or injection molding; dissolving the clothes or soluble clothes accessories under certain conditions, filtering a dissolving solution and recovering dissolved substances on one hand to obtain high-purity terephthalic acid and ethylene glycol, reusing the terephthalic acid and the ethylene glycol for polymerization of soluble polyester to obtain soluble polyester chips, and spinning the soluble polyester chips into soluble fibers again for recycling; on the other hand, loose and undissolved textile is treated, including disinfection, stripping or re-dyeing, to become loose fiber aggregate with good quality, and after drying or soft carding, the loose fiber aggregate becomes high-quality textile fiber for recycling. However, the organic solvent used in this method has a slow dissolution rate and causes some damage to the insoluble fibers, thereby affecting the recycling of the fibers.
There is a need in the art for a solvent that dissolves soluble fibers quickly and with little damage to insoluble fibers during the dissolution process, thereby facilitating high quality and efficient reuse of the fibers
Disclosure of Invention
The present invention, on the basis of patent application CN106065085A (the content of which is incorporated herein by reference in its entirety), provides a recycling method with fast dissolution rate of soluble fibers and less damage to insoluble fibers, in view of the above technical problems. In order to solve the technical problems, the invention provides the following technical scheme.
In one aspect of the invention, there is provided 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; the non-dissolved fibers were washed and sterilized to obtain a loose fiber assembly.
Preferably, the raw material for preparing the controlled dissolving fiber comprises terephthalic acid and/or ethylene glycol.
Preferably, the solvent in step a or b comprises an organic component.
Preferably, the organic component is DMSO.
Preferably, the solvent further comprises ethanol; alternatively, preferably, the solvent further comprises water.
More preferably, the solvent further comprises tetrabutylammonium acetate.
DMSO is bipolar, which has a good swelling effect on the fibers. In addition, the combined use of DMSO and tetrabutylammonium acetate greatly increases the dissolution rate of soluble fibers, when tetrabutylammonium acetate is added, because it is a very strong hydrogen bond acceptor due to the strong electronegativity of acetate ions, which advantageously competes with the hydroxyl and acetal oxygen atoms of cellulose, thereby disrupting the hydrogen bond network between cellulose chains.
In a preferred embodiment, the content of ethanol in the solvent is from 40 to 90 wt.%, preferably from 50 to 80 wt.%, based on the total weight of the solvent; the DMSO content is 10-30 wt%, preferably 15-20%; the content of tetrabutylammonium acetate is 0.1-5.0 wt.%, preferably 0.2-2.0 wt.%.
More preferably, the solvent in step a or b is basic. Further preferably, the solvent comprises NaOH. In a preferred embodiment, the solvent further comprises 0.001 to 5.0 wt%, preferably 0.1 to 1.0 wt%, of NaOH, based on the total weight of the solvent.
In a particularly preferred embodiment, the solvent comprises an ionic liquid. Preferably, the ionic liquid is present in an amount of 0.1 to 10.0 wt%, preferably 0.2 to 5.0 wt%, more preferably 0.5 to 2.0 wt%, based on the total weight of the solvent.
Particularly preferably, the ionic liquid is an ionic liquid of the following formula (I):
The ionic liquid represented by the formula (I) is effective in breaking hydrogen bonds in the fibers and thus in decomposing the fibers efficiently under the adjustment of the pH value of a weak solvent, and also, because of the strong electronegativity of acetate ions, it acts as a strong hydrogen bond acceptor and favorably competes with hydroxyl groups and acetal oxygen atoms of cellulose to break the hydrogen bond network between cellulose chains and thus can effectively dissolve the fibers. In addition, when the ionic liquid shown in the formula (I) is used, due to the strong electron withdrawing effect of Cl atoms and the polarity of hydroxyl groups, the initial decomposition product generated by decomposition can be more uniformly and firmly attached to the pore surfaces of the fibers, so that the further smooth proceeding of fiber dissolution can be promoted, the non-uniformity of dissolution can be prevented, if the concentration of the decomposition agent is high, the uniform proceeding of dissolution can be improved, and the damage to non-dissolved fibers can be further reduced.
In a preferred embodiment of the present invention, the soluble textile is a soluble textile made by the method of:
(1) adding terephthalic acid, isophthalic acid, ethylene glycol, 5-sodium sulfonate-isophthalic acid polyethylene glycol ester, selecting different substance combinations and substance combinations in different proportions for polymerization 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.
Preferably, the spinning temperature is 270-. More preferably, the spinning temperature is 280-.
In a further preferred embodiment of the invention, the loose fibre assembly is blended or interwoven with a controlled dissolving fibre to produce a fibre fabric.
In the invention, more specifically, the preparation of soluble fiber comprises controllable soluble fiber preparation under different media and different dissolving conditions, and comprises filaments, short fibers and fiber strips;
the textile processing comprises the following steps: the textile can be designed and processed by taking 100 percent of soluble fiber as a raw material, can also be processed by blending the soluble fiber with other fibers, comprises clothing accessories for the textile, such as sewing threads, buttons, trademarks, hanging tags, water shuffling and the like, and also comprises soluble substances;
dissolving and recovering the textile: dissolving the soluble fiber substance under a certain condition, and performing high-purity recovery and sewage treatment on the dissolved soluble fiber substance to achieve the purposes of substance recovery and sewage reaching the environmental-friendly discharge standard; for 100% soluble fiber textile, high-purity recovery is realized, and the recovered matter after dissolution can be directly used as a raw material for controllable fiber production and directly used as a polymer raw material for controllable dissolution fiber; for the dissolution of the blending or interweaving product of the controllable soluble fiber, the remaining non-soluble fiber is loose textile due to the dissolution of the controllable soluble fiber;
and (3) retreatment of the remaining textile: according to the using requirement, carrying out disinfection chemical treatment, and carrying out stripping or bleaching or re-dyeing treatment according to the future using requirement, wherein the residual textile becomes loose or even disintegrates due to the dissolution of soluble fiber, and through soft carding, the fiber strength damage is small, the length loss is little, high-quality additional component fiber or bleached or dyed fiber is obtained, the high-quality additional component fiber can be directly used for directly processing new yarn in a spinning mill, the quality of the blended or interwoven textile after other component fiber is recovered is high, and the high-efficiency and high-quality full-cycle recovery and use of the textile can be realized.
The invention can be realized by the following specific technical scheme.
A technology for recovering, regenerating and recycling soluble textiles comprises the following process steps:
a. preparing soluble fiber and soluble clothing accessories with controllable dissolving conditions:
in the polymerization process of polyester raw materials, adding terephthalic acid, isophthalic acid, ethylene glycol, 5-sodium sulfonate-isophthalic acid polyethylene glycol ester with different proportions of the total weight of the polymer, selecting different substance combinations and substance combinations with different proportions for polymerization to obtain alkali-dissolving slices under different alkali-dissolving conditions, wherein the intrinsic viscosity of the alkali-dissolving slices is 0.40-0.80, and finally completing the processes of casting, cooling, granulating, drying and screening in sequence;
(1) preparing controllable dissolving fibers according to a conventional spinning process, wherein the controllable dissolving fibers comprise filaments, short fibers and fiber strips, and also comprise differentiated and colored fibers of the fibers, so as to be used for producing various textiles such as ready-made clothes, non-woven fabrics, electrostatic flocking and the like;
(2) preparing sewing thread with controllable dissolved fiber by conventional process, wherein the sewing thread can be pure spinning or blended yarn of soluble short fiber, or soluble filament fiber yarn and plied yarn;
(3) according to the conventional injection molding, color master batch adding and molding processes, the dissoluble slices with controllable dissolution conditions are adopted to produce hard dissoluble clothing accessories, including zippers, buttons, logo in film form, water washing hang tags, component hang tags, trademark hang tags and the like;
or,
b. textile dyeing containing soluble fiber and preparation of finished products:
(1) 100% of the finished product of the controllable dissolving fiber:
(1-1) using 100% of controlled dissolving fiber, or staple fiber yarn, or filament yarn, using conventional weaving process, if necessary in dyeing process, i.e. without adding dissolving medium, such as alkali substance, the rest process is the same as the conventional polyester process;
(1-2) 100% of finished products of elastic fibers such as controllable soluble fibers and spandex are processed by a conventional weaving process, if necessary, in a dyeing processing process, namely, no dissolved medium such as alkali substances are added, and the rest processes are the same as the conventional polyester processing process;
(2) finished products of blending or interweaving of the controlled dissolving fibers with other non-dissolving fibers:
(2-1) blending or interweaving the controllable soluble fiber and other non-soluble fibers, such as cotton, wool, hemp and other chemical fibers, into a finished product, and using a conventional weaving process, wherein a dissolved medium is not added in the dyeing process if needed, and the rest processes are the same as the conventional polyester blending or interweaving process;
(2-2) blending or interweaving the controllable dissolved fiber with other non-dissolved fiber to obtain finished products of elastic fibers such as cotton, wool, hemp and other chemical fibers, blending and interweaving the elastic fibers such as spandex, and the like by using a conventional weaving process, wherein the conventional weaving process is adopted, if a dyeing process is needed, a dissolved medium is not added, and the rest processes are the same as the conventional polyester blending or interweaving process;
c. dissolution and recovery of finished products containing soluble fibres and soluble garment accessories (said soluble garment accessories can also be considered as one form of presence of soluble fibres):
(1) dissolving and recycling 100% of the soluble fiber fabric and soluble clothing accessories:
(1-1) dissolving 100% of the controllable soluble fiber fabric or soluble clothing accessories in various cylinder bodies directly under certain solvent conditions. For the dissolved solution, high-purity terephthalic acid, ethylene glycol and NaOH are obtained after membrane filtration, acid precipitation, gasification (namely degassing) and other processes, and the COD of the discharged wastewater meets the environmental protection requirement;
(1-2) the fiber fabric or soluble clothing accessories of 100 percent of controllable soluble fiber and elastic fiber such as spandex and the like are directly and completely dissolved in various cylinder bodies under the condition of a certain solvent. For the dissolved solution, high-purity terephthalic acid, ethylene glycol and NaOH are obtained after membrane filtration, acid precipitation, gasification and other processes, and the COD (chemical oxygen demand) of the discharged wastewater meets the environmental protection requirement; for elastic fibers such as spandex and the like which are not dissolved, the elastic fibers are intercepted on a filter grid, the content of the elastic fibers is low, the elastic fibers are kept in a continuous spandex form, and the elastic fibers are easy to identify and take away; or spandex elastic fiber is dissolved by using elastic fiber solvents such as spandex and the like, and the solvent amount of the part is small, so that the part can be recycled;
(2) dissolving and recycling the blended or interwoven fiber fabric of the controllable dissolving fiber and other non-dissolving fiber or soluble clothing accessories:
directly dissolving the textile in various cylinder bodies under the condition of certain solvent medium solubility to dissolve controllable dissolving fibers; simultaneously, the non-soluble fiber is cleaned and disinfected, and for the non-soluble fiber, the non-soluble fiber becomes a loose fiber aggregate due to the dissolution of the soluble fiber;
for the dissolved solution, after the processes of grid filtration, membrane filtration, acid precipitation, gasification and the like, high-purity terephthalic acid, ethylene glycol and NaOH are obtained, and the COD of the discharged wastewater meets the environmental protection requirement;
for the controllable dissolved fiber and other non-soluble fiber blending or interweaving plus spandex and other elastic fiber finished products, such as cotton, wool, hemp and other chemical fiber blending interweaving plus spandex and other elastic fiber finished products, directly dissolving the controllable dissolved fiber and spandex and other elastic fibers in various cylinder bodies under a certain solvent medium solubility condition, wherein the solvent can be one or the dissolution composition of respectively dissolving the controllable dissolved fiber and the elastic fibers such as the dissolved spandex and the like; controllable dissolving fiber can be dissolved in the cylinder; then, spandex elastic fiber is dissolved by using elastic fiber solvents such as spandex and the like, and the solvent of the part can be recycled;
the loose and non-soluble fiber aggregate can be subjected to regeneration treatment, and can be subjected to disinfection treatment by using a disinfectant auxiliary agent; or directly drying and lightly carding to obtain variegated fiber; or according to the regeneration use requirement, after stripping, bleaching treatment, drying and soft carding, the bleached fiber is formed; or the stripped fiber is dyed, dried and lightly carded to form the colored fiber for use. Because the fiber is a loose fiber aggregate, the strength, the length and the damage of the fiber are small after the fiber is lightly carded, and the spinnability and the service performance of the non-soluble fiber are ensured;
d. obtaining high-purity chemical raw materials and high-quality fiber materials:
the recovered chemical raw materials after the treatment comprise: 1. terephthalic acid, ethylene glycol and NaOH have high purity, and are in line with industrial use; 2. the strength preservation rate of the regenerated fiber treated at one time is high, and the length of the regenerated fiber is not lost.
Wherein the spinning temperature in the step a is 270-300 ℃, and the injection molding temperature is 150-250 ℃.
Wherein, the alkali solution adopted in the step c is sodium hydroxide solution or low-alkali or alkali-free high-temperature pure water solution or organic solvent.
The invention has the beneficial effects that: the soluble textile recovery, regeneration and recycling technology provided by the invention is used for obtaining high-purity terephthalic acid, ethylene glycol and NaOH after processes such as grid filtration, membrane filtration, acid precipitation, gasification and the like are carried out on a dissolved solution obtained after the textile is dissolved, and the COD (chemical oxygen demand) of discharged wastewater meets the environmental protection requirement; for the blending or interweaving fabric of the soluble fiber, the compact textile can be changed into the aggregation of loose non-soluble fiber through the dissolution of the soluble fiber in the textile; the non-soluble fiber aggregate can be regenerated and used as variegated fiber after disinfection treatment or direct drying and soft carding, or can be used as bleached fiber after stripping, bleaching treatment, drying and soft carding according to the regeneration use requirement, or can be used as colored fiber after the stripping fiber is dyed, dried and soft carded, and can be used after the soft carding with little damage to the strength and the length of the fiber due to the loose fiber aggregate, thereby ensuring the spinnability and the service performance of the non-soluble fiber. The invention makes the textile which has no value and becomes the environmental pollutant become a valuable commodity, namely reduces the pollution to the environment and can be recycled.
Drawings
The invention will be further described with reference to the drawings to which, however, the embodiments shown in the drawings do not constitute any limitation.
FIG. 1 is a schematic view of the recovery structure of an alkali dissolving solution according to the present invention;
FIG. 2 is a TEM image of a fiber at 20min dissolution according to a prior art method (comparative example 1);
FIG. 3 is a TEM image of the fibers at 20min dissolution according to the process of the invention (example 1).
Detailed Description
The present invention will be described below with reference to specific embodiments.
Example 1
The dissolving, recovering and recycling technology of 100% of controllable soluble fiber fabric and soluble clothing accessories comprises the following process steps:
a. in the process of polymerizing polyester raw materials, adding 5-sodium sulfonate-isophthalic acid polyethylene glycol ester with the total weight of polymer being 6 percent and isophthalic acid with the total weight of polymer being 4 percent, pulping, stirring and simultaneously heating to 230 ℃; then moving to a reaction kettle, adding polyethylene glycol with the total weight of 10 percent of the polymer, diluting the mixture, and cooling to 210 ℃; continuously adding polyethylene glycol into the reaction kettle, wherein the polyethylene glycol accounts for 10% of the total weight of the polymer, adding the polyethylene glycol within 50 minutes while stirring, heating to 230 ℃ under normal pressure to polymerize the mixed material in a vacuum state, and finally sequentially completing the processes of belt casting, cooling, grain cutting, drying and screening on the polymerized alkali degradation slices, wherein the intrinsic viscosity of the alkali degradation slices is 0.65;
preparing alkali-soluble degradation filament fibers by using the alkali-degradable slices, wherein the easy-alkali-soluble degradation fibers are the filament fibers: the spinning and spinning post-treatment process comprises the following steps: the POY filament yarn which can be dissolved in alkali solution is obtained by a conventional POY spinning process at the spinning temperature of 290 ℃, and then the low-stretch yarn DTY is produced on a texturing machine, wherein the fiber indexes are as follows: producing FDY filament with fineness of 15.5 tex/48F, strength of 3.6cn/dtex and elongation at break of 25 percent by a conventional spinning process, wherein the FDY filament is 150D/48F, the strength of 4.0cn/dtex and the elongation at break of 20 percent;
b. the DTY filament is produced into various fabrics, ready-made clothes and textiles through the conventional process:
(1) the FDY filaments are folded and doubled to be used as sewing threads of textiles;
(2) the ready-made clothes and textiles are matched with clothing accessories, the accessories are hard soluble clothing accessories of soluble slices which are subjected to conventional injection molding, coloring master batch coloring and forming processes, and the accessories comprise zippers, buttons, logo and water g washing tags in film shapes, component tags and trademark tags;
c. adding a solvent into a closed common overflow tank of a dyeing and finishing factory, wherein the dissolving temperature is 110 ℃, the dissolving time is 60 minutes, and the bath ratio is as follows: 1: dissolving soluble fiber, the solvent having a composition such that the content of ethanol is 70.0 wt%, based on the total weight of the solvent; 25.0 wt% of DMSO, 2.0 wt% of tetrabutylammonium acetate, 0.2wt% of NaOH and 2.8wt% of ionic liquid shown in formula (I);
d. as shown in fig. 1, dissolving a controllably soluble fiber textile in an alkali solution in a cylinder, introducing the solution into a regulating reservoir after passing through a grid, sequentially passing through pretreatment and a membrane system for the alkali solution in the regulating reservoir, introducing the alkali solution passing through the membrane system into an acid precipitation tank, pumping acid liquor into the acid precipitation tank by an acid adding pump, stirring the acid liquor and the alkali solution in the acid precipitation tank to obtain wastewater with a PH value of 3-4, and precipitating terephthalic acid in the process; after the acid solution and the alkali solution react sufficiently in the acid precipitation tank, the wastewater in the acid precipitation tank is introduced into a centrifugal filter for filtering so as to separate the terephthalic acid. After the terephthalic acid is filtered and dehydrated by a centrifugal filter, the separated terephthalic acid is washed or not washed according to different requirements, and is bagged, stored and waited for shipment. And (4) separating the ethylene glycol from the acid-separated filtrate through a filter membrane system. Wherein, the grid mainly is the floater such as interception aquatic great particulate matter and other major diameter pollutants, and the equalizing basin is used for buffering water yield, even quality of water, deposit great solid particle to do benefit to the processing of follow-up technology. The filtrate from the centrifugal filter can reduce COD in sewage greatly and the filtrate can be biochemical. After the glycol is filtered by the membrane system, the COD is further reduced, the discharge requirement of the printing and dyeing wastewater is met, and the wastewater enters a biochemical sewage treatment system of a factory.
Example 2
The dissolving, recovering and recycling technology of the fiber fabric of the controllable soluble fiber and cellulose fiber blended yarn fabric and the soluble clothing accessories comprises the following process steps:
a. blending the controllable soluble fiber short fiber prepared in the first embodiment with cellulose fiber (such as cotton, hemp and rayon) according to blending ratio of 65/35, 50/50 and the like; the yarn count is according to the specification of conventional cellulose fiber or blended yarn; weaving according to a conventional process; the dyeing adopts a reactive dye and disperse dye dyeing process of a polyester and cellulose fiber two-bath method; thus, the fabric is prepared, including woven and knitted fabrics;
(1) after the short fiber blended yarns are subjected to plying and doubling, sewing threads of the textile are made;
(2) the ready-made clothes and textiles are matched with clothing accessories, the accessories are hard soluble clothing accessories of soluble slices which are subjected to conventional injection molding, coloring master batch coloring and forming processes, and the accessories comprise zippers, buttons, logo and water g washing tags in film shapes, component tags and trademark tags;
b. cleaning, disinfecting and dissolving: dissolving in a closed cylinder, adding a solvent, wherein the dissolving temperature is 110 ℃, the dissolving time is 60 minutes, and the bath ratio is as follows: 1: 10, adding a disinfectant and a cleaning agent, dissolving the soluble fiber, and disinfecting and cleaning, wherein the solvent comprises 70.0 wt% of ethanol based on the total weight of the solvent; 25.0 wt% of DMSO, 2.0 wt% of tetrabutylammonium acetate, 0.2wt% of NaOH and 2.8wt% of ionic liquid shown in formula (I);
as shown in fig. 1, the discharged solution is introduced into a regulating reservoir after passing through a grid, the alkali solution in the regulating reservoir sequentially passes through a pretreatment and a membrane system, the alkali solution passing through the membrane system enters an acid precipitation tank, acid liquor is pumped into the acid precipitation tank by an acid adding pump, and the acid liquor and the alkali solution are stirred in the acid precipitation tank to obtain wastewater with a PH value of 3-4, wherein terephthalic acid is precipitated in the process; after the acid solution and the alkali solution react sufficiently in the acid precipitation tank, the wastewater in the acid precipitation tank is introduced into a centrifugal filter for filtering so as to separate the terephthalic acid. After the terephthalic acid is filtered and dehydrated by a centrifugal filter, the separated terephthalic acid is washed or not washed according to different requirements, and is bagged, stored and waited for shipment. And (4) separating the ethylene glycol from the acid-separated filtrate through a filter membrane system. Wherein, the grid mainly is the floater such as interception aquatic great particulate matter and other major diameter pollutants, and the equalizing basin is used for buffering water yield, even quality of water, deposit great solid particle to do benefit to the processing of follow-up technology. The filtrate from the centrifugal filter can reduce COD in sewage greatly and the filtrate can be biochemical. After the glycol is filtered by the membrane system, COD is further reduced, the discharge requirement of the printing and dyeing wastewater is met, and the wastewater enters a biochemical sewage treatment system of a factory;
for the non-soluble fiber, stripping and bleaching are sequentially carried out, wherein a reduction stripping process is adopted for stripping, and the disinfected, stripped and bleached cotton fiber loose aggregate can be dyed and dried according to the conventional dyeing process for bleaching cotton or directly bleached loose aggregate. And finally, the dried cotton fibers are lightly carded and opened, the damage to the fiber strength and the length is small, the spinnability and the serviceability of the original fibers are kept, and high-quality regenerated cotton fibers are obtained, so that the cotton fibers can be recycled to produce high-quality yarns.
Example 3
The dissolving, recovering and reusing technology of the blended yarn of the controllable soluble fiber and the cellulose fiber and the fiber fabric of the spandex fiber fabric and the soluble clothing accessories comprises the following process steps:
a. the polymerized raw material prepared in the first embodiment is produced into short fiber (3.6 cn/dtex strength and 25% elongation at break) with the length of 38mm and the fineness of 1.5D by a conventional spinning process, the controllable soluble fiber short fiber is blended with cellulose fiber (such as cotton, hemp and artificial fiber) according to the blending ratio of 65/35, 50/50 and the like, and the yarn is interwoven with spandex or is doubled with elastic yarn to form woven or knitted fabric according to the conventional weaving process; the dyeing adopts a reactive dye and disperse dye dyeing process of a polyester and cellulose fiber two-bath method; therefore, the fabric is prepared, and comprises a woven fabric and a knitted fabric, and then the fabric is sewn into a finished textile product;
(1) after the short fiber blended yarns are subjected to plying and doubling, sewing threads of the textile are made;
(2) the ready-made clothes and textiles are matched with clothing accessories which are hard clothing accessories of soluble slices through conventional injection molding, coloring master batch coloring and forming processes, and the accessories comprise zippers, buttons, logo and water g washing tags in film shapes, component tags and trademark tags;
b. cleaning, disinfecting and dissolving: adding a solvent into a closed cylinder, wherein the dissolving temperature is 110 ℃, the dissolving time is 60 minutes, and the bath ratio is 1: 10, adding a disinfectant and a cleaning agent, dissolving soluble fiber, and disinfecting and cleaning, wherein the solvent comprises 70.0 wt% of ethanol based on the total weight of the solvent; 25.0 wt% of DMSO, 2.0 wt% of tetrabutylammonium acetate, 0.2wt% of NaOH and 2.8wt% of ionic liquid shown in formula (I);
as shown in fig. 1, the discharged solution is introduced into a regulating reservoir after passing through a grid, the alkali solution in the regulating reservoir sequentially passes through a pretreatment and a membrane system, the alkali solution passing through the membrane system enters an acid precipitation tank, acid liquor is pumped into the acid precipitation tank by an acid adding pump, and the acid liquor and the alkali solution are stirred in the acid precipitation tank to obtain wastewater with a PH value of 3-4, wherein terephthalic acid is precipitated in the process; after the acid solution and the alkali solution react sufficiently in the acid precipitation tank, the wastewater in the acid precipitation tank is introduced into a centrifugal filter for filtering so as to separate the terephthalic acid. After the terephthalic acid is filtered and dehydrated by a centrifugal filter, the separated terephthalic acid is washed or not washed according to different requirements, and is bagged, stored and waited for shipment. And (4) separating the ethylene glycol from the acid-separated filtrate through a filter membrane system. Wherein, the grid mainly is the floater such as interception aquatic great particulate matter and other major diameter pollutants, and the equalizing basin is used for buffering water yield, even quality of water, deposit great solid particle to do benefit to the processing of follow-up technology. The filtrate from the centrifugal filter can reduce COD in sewage greatly and the filtrate can be biochemical. After the glycol is filtered by the membrane system, COD is further reduced, the discharge requirement of the printing and dyeing wastewater is met, and the wastewater enters a biochemical sewage treatment system of a factory;
adding Dimethylacetamide (DMAC) liquid into the undissolved fibers in the vat at a bath ratio of 1:1 and a temperature of 95 ℃ for 30 minutes, and then discharging the DMAC liquid and storing the DMAC liquid by a liquid collector for recycling in the next vat; the non-dissolved fiber is sequentially stripped and bleached, wherein a reduction stripping process is adopted for stripping treatment, and the disinfected, stripped and bleached cotton fiber loose aggregate can be dyed and dried according to the dyeing process of conventional bleached cotton or directly dried by the bleached loose aggregate. And finally, the dried cotton fibers are lightly carded and opened, the damage to the fiber strength and the length is small, the spinnability and the serviceability of the original fibers are kept, and high-quality regenerated cotton fibers are obtained, so that the cotton fibers can be recycled to produce high-quality yarns.
Example 4
The dissolving, recovering and reusing technology of the finished product of the controllable soluble fiber and wool fiber blended fabric comprises the following process steps:
a. in the process of polymerizing polyester raw materials, adding 5-sodium sulfonate-isophthalic acid polyethylene glycol ester with the total weight of polymer being 10 percent and isophthalic acid with the total weight of polymer being 4 percent, pulping, stirring and simultaneously heating to 230 ℃; then moving to a reaction kettle, adding polyethylene glycol with the total weight of 15 percent of the polymer, diluting the mixture, and cooling to 210 ℃; continuously adding polyethylene glycol into the reaction kettle, wherein the polyethylene glycol accounts for 15% of the total weight of the polymer, adding the polyethylene glycol within 50 minutes while stirring, heating to 230 ℃ under normal pressure to polymerize the mixed material in a vacuum state, and finally sequentially completing the processes of belt casting, cooling, grain cutting, drying and screening on the polymerized alkali degradation slices, wherein the intrinsic viscosity of the alkali degradation slices is 0.55;
the alkali degradation slice is used for preparing low-alkali easy-alkali-soluble short fiber, and the spinning temperature is 275 ℃. The low-alkali easily-soluble fiber is wool-type fiber, the length of the fiber is 110mm, the strength of the fiber is 2.5cn/dtex, the elongation at break of the fiber is 30 percent, and the fiber is carded into strips to prepare 20 g/5 m fiber strips. In the wool spinning production, the wool spinning yarn is blended with wool top drawing to form yarn, the blending ratio is 50 soluble fiber/50 wool fiber, the Nm is 60Nm, and the yarn is woven by a conventional process and dyed into fabric and textile under an alkali-free state;
(1) the wool blended yarn is folded and doubled to be used as a sewing thread of the wool blended textile.
(2) The ready-made clothes and textiles are matched with clothing accessories which are hard clothing accessories of soluble slices through conventional injection molding, coloring master batch coloring and forming processes, and the accessories comprise zippers, buttons, logo and water g washing tags in film shapes, component tags and trademark tags;
b. adding 1.5 g/L100% NaOH and 2 g/L penetrant into a closed cylinder, wherein the dissolving temperature is 90 ℃, the dissolving time is 60 minutes, and the bath ratio is 1: dissolving soluble fiber, the solvent having a composition such that the content of ethanol is 70.0 wt%, based on the total weight of the solvent; 25.0 wt% of DMSO, 2.0 wt% of tetrabutylammonium acetate, 0.2wt% of NaOH and 2.8wt% of ionic liquid shown in formula (I);
as shown in fig. 1, the discharged solution is introduced into an adjusting tank through a grid, the alkali solution in the adjusting tank sequentially passes through pretreatment and a membrane system, the alkali solution passing through the membrane system enters an acid precipitation tank, acid liquor is pumped into the acid precipitation tank through an acid adding pump, and the acid liquor and the alkali solution are stirred in the acid precipitation tank to obtain wastewater with a pH value of 3-4, wherein terephthalic acid is precipitated in the process; after the acid solution and the alkali solution react sufficiently in the acid precipitation tank, the wastewater in the acid precipitation tank is introduced into a centrifugal filter for filtering so as to separate the terephthalic acid. After the terephthalic acid is filtered and dehydrated by a centrifugal filter, the separated terephthalic acid is washed or not washed according to different requirements, and is bagged, stored and waited for shipment. And (4) separating the ethylene glycol from the acid-separated filtrate through a filter membrane system. Wherein, the grid mainly is the floater such as interception aquatic great particulate matter and other major diameter pollutants, and the equalizing basin is used for buffering water yield, even quality of water, deposit great solid particle to do benefit to the processing of follow-up technology. The filtrate from the centrifugal filter can reduce COD in sewage greatly and the filtrate can be biochemical. After the glycol is filtered by the membrane system, COD is further reduced, the discharge requirement of the printing and dyeing wastewater is met, and the wastewater enters a biochemical sewage treatment system of a factory;
the undissolved loose wool fiber aggregate is stripped and bleached to obtain regenerated wool fiber with good strength and length.
Comparative example 1
Example 1 was repeated, differing from example 1 only in that in b, 100% naoh1.5g/L, penetrant 2 g/L were added in a closed cylinder.
As is clear from fig. 2 and 3, when the dissolution treatment is performed with the solvent of the present invention, the dissolution rate is faster (i.e., digestion is faster) and the damage to the insoluble fiber is smaller (smaller shaded area in the figure), indicating that the solvent of the present invention has a fast dissolution rate for the soluble fiber and a small damage to the insoluble fiber, which means particularly advantageous economic benefits and values.
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. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims. All citations referred to herein are incorporated herein by reference to the extent that no inconsistency is made.
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):
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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| EP1889889A3 (en) * | 2004-03-08 | 2010-09-22 | Nitto Denko Corporation | Pressure-sensitive adhesive composition, pressure-sensitive adhesive sheets and surface protecting film |
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| US8449652B2 (en) * | 2004-08-05 | 2013-05-28 | University Of Wyoming | Poly(ionic liquid)s as new materials for CO2 separation and other applications |
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