CN103374144A - Method for extracting polyester material from waste textiles or similar wastes containing polyester - Google Patents
Method for extracting polyester material from waste textiles or similar wastes containing polyester Download PDFInfo
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- CN103374144A CN103374144A CN2012101162983A CN201210116298A CN103374144A CN 103374144 A CN103374144 A CN 103374144A CN 2012101162983 A CN2012101162983 A CN 2012101162983A CN 201210116298 A CN201210116298 A CN 201210116298A CN 103374144 A CN103374144 A CN 103374144A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention relates to a method for extracting a polyester material from waste textiles or similar wastes containing polyester, particularly relates to purification of polyester from colored polyester fabric leftovers or polyester-containing blended fabric leftovers and belongs to the technical field of high polymer chemistry and polymers. The method is characterized by comprising the following steps of: firstly, selecting an organic solvent having a boiling point not exceeding 215 DEG C for decontamination and decoloration, decontaminating and decoloring wastes by using the organic solvent and dissolving the wastes by using the organic solvent to remove partial hetero fibers; secondly, dissolving polyester in the wastes by using a polyester solvent having a boiling point not exceeding 215 DEG C, and filtering out insoluble natural fibers and the like; and finally, mixing the polymer mixed solution with a precipitator so that polymer is separated out. The method for purifying the polymer without decomposing monomers is easy to control in technique, high in yield, obvious in energy saving and low in consumption; the polyester material is controllable in viscosity, appropriate in whiteness and friendly to production environment; the solvent is low in boiling point and easy to recover; and basically, no three wastes are discharged.
Description
Technical field
The present invention relates to a kind of method of from the waste spinning fabric that contains polyester or similar waste material, extracting polyester material, relate in particular to colored terylene cloth angle or contain and wash the polyester of purifying in the blended fabric angle, belong to polymer chemistry and technical field of polymer.
Background technology
Utilize at present the mode that contains polyester waste spinning fabric a lot, colored terylene cloth angle or contain and wash multiplex the blooming in blended fabric angle and do filler, utility value is lower.As for terylene waste, enterprise of domestic a lot of factories is that the plain modes such as, cleaning assorted by choosing, heating are made foam material, be incorporated into melt-spinning in the polyester slice virgin material with certain proportion, but what can have influence on quality and the class of product; Nonetheless, still raised the price of terylene waste.
Also have terylene waste is resolved into first the monomer of PTA, DMT, EG and so on by modes such as alcoholysis, and then regroup into PET.This is a kind of preferably way of recycling, and Japanese Supreme Being people group is exactly the mark post of this respect, and they successfully realize magnificent the turning round from the silk to the silk by the complete circular form chemical recovery regeneration techniques of PET waste silk → DMT → PTA → PET resin → PET silk.Certainly, thisly separate first that the mode energy consumption of gathering afterwards is inevitable greatly, complex procedures is that obvious, high-precision technology control is essential especially; And domestic present situation is terylene waste price height enterprise, if again by this mode of gathering afterwards of separating first, is to make returned enterprise be difficult to maintain in fact.
Perhaps, utilize relatively quickly and easily the waste spinning fabric that contains polyester, especially to colored terylene cloth angle or contain and wash the blended fabric angle, extract polyester by not resolving into monomer, be only a good approach that really meets national conditions, save energy.
Application number is 201010549439.1 patent application, attempts exactly to realize a kind of trial of this purpose.It is organic solvent and some catalyzer with some known energy dissolved polyesters, will be without polyster fibre, polyester piece good and dissolving or the alcoholysis such as BLENDED FABRIC waste material, clothes of sorting, filter insolubles, then solution is distilled, reclaim solvent, " residuum of distillation is mainly polyethylene terephthalate or its degradation product, adopts the further processing treatment of other technologies, realizes the recycling of polyster fibre, polyester piece good and BLENDED FABRIC waste material thereof ".Application documents do not describe in detail said other technologies, only mention in an embodiment the solvent Distillation recovery after, " remaining liquid is carried out liquid-phase tackifying polymerization, spinning with other technologies ".Carefully look in full, waste material from its operation and employing, in the residuum of distillation or also have the pollution in easy molten cellulosic, the waste material, oil or initial thin dust that clings etc. in dyestuff, spinning finishing agent, textile finish oil, the BLENDED FABRIC waste material, these to the later spinning of polyester with become yarn quality all will bring to seriously influence.Such method in fact an elimination some natural fibers, viscose fiber and foreign material etc., or not as directly classified filtering behind the waste material hot melt being come to such an extent that save time, the saving of labor, save the industrial chemicals loss.Because it is original just very bothersome that certain density polyester liquid will distillate organic solvent, and the residuum of distillation still will be done some processing, though and organic solvent recyclable, loss is inevitable.Discuss, application documents are not described further said other technologies should belong to normal, but behind its solvent Distillation recovery described later, " liquid phase " mentioned perhaps will make polyester reach molten state by high temperature and could realize.In addition, its selected organic solvent is high poison even hypertoxic a bit, and some boiling point is higher or increase energy consumption etc.
As for the author's patent application in 1988 " method of utilizing the chemical fabric angle to manufacture a product ", then more without how many actual values.Just hoped originally and made the again corrosion resistant pesticide bottle of anti-collision of a kind of cheapness that because chemical fabric at that time mostly is pure terylene, and its cloth horn scraps was not substantially to utilize.
Summary of the invention
Purpose of the present invention is to attempt to draw a kind ofly just can extract relatively pure polyester material among the waste spinning fabric or similar waste material that contain polyester without decomposing monomer and repolymerization, and the method that energy consumption is low, leaching process does not cause again environmental pollution.
In order to achieve the above object, the invention provides a kind of method of extracting polyester material from the waste spinning fabric that contains polyester or similar waste material, particularly colored terylene cloth angle or contain and wash the polyester of purifying in the blended fabric angle comprises the following steps:
(a) selecting the organic solvent of 20 ℃-215 ℃ of boiling points is the decontamination decolouring solvent of main component, carry out the decontamination decolouring with 20 ℃-178 ℃ of solution temperatures to containing polyester waste spinning fabric or similar waste material, some easy molten fiber outside the polyester that simultaneously dissolving may exist etc., then solid-liquid separation, and from contaminated liquid, reclaim organic solvent in modes such as distillation or fractionation, in order to recycling;
(b) selecting the organic solvent of 20 ℃-215 ℃ of boiling points is the polyester solvent of main component, will be under 20 ℃ of-208 ℃ of temperature the decontamination decolouring contain polyester waste spinning fabric or similar waste material fully dissolves, then with solution filter, collect the polyester mixing solutions, the undissolved thing that leaches deals with in addition;
(c) the polyester mixing solutions is mixed mutually with the precipitating agent, cause polyester to be separated out in modes such as precipitation or suspensions, then refilter, filtrate collection is in order to recycling, the polyester filter cake is lower than the cleaning solvent flushing of polyester solvent again with boiling point, then with the polyester filtration cakes torrefaction, namely get polyester material; Can be together with the recovery and rinsing solvent when dry, comprise from the contaminated liquid of wash distillating the raffinate that is left behind the cleaning solvent with mode recovery and rinsing solvents such as distillations, can with the filtrate merging of collecting above, recycle in order to follow-up.
Preferably, the solvent component of said decontamination decolouring solvent, consistent with the solvent component after said polyester solvent adds said precipitating agent; Like this, step (c) contains the filtrate of polyester solvent and precipitating agent, can be without distillation or fractionation, and just conduct decontamination decolouring solvent next time uses.
Preferably, the solvent component of said decontamination decolouring solvent, consistent with the solvent component of said polyester solvent.
Preferably, also be included in the step (b), carry out synchronously the polyester adhesiveness increasing and modifying with dissolved polyester and process.
Preferably, the decontamination bleaching temperature in the said step (a) is 20 ℃-158 ℃.
Preferably, the temperature of dissolved polyester is 20 ℃-188 ℃ in the said step (b).
Preferably, the temperature of dissolved polyester is 20 ℃-178 ℃ in the said step (b).
Preferably, the main component of said decontamination decolouring solvent is one or more in the main component of following polyester solvent, and in the following precipitating agent one or more; The main component of said polyester solvent is one or more in N-Methyl pyrrolidone, Isosorbide-5-Nitrae-Ding lactones, N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, diethylformamide, orthodichlorobenzene, the meta-cresol; In the isomers that said precipitating agent is 2-picoline, propyl alcohol, sec-butyl alcohol, isopropylcarbinol, butanols, pyridine, amylalcohol, amylalcohol, the dioxan one or more; Said cleaning solvent is one or more in chloroform, methylene dichloride, tetracol phenixin, methyl alcohol, the ethanol.
Preferably, the main component of said decontamination decolouring solvent is one or more in the isomers, amylalcohol, dioxan of N-Methyl pyrrolidone, Isosorbide-5-Nitrae-Ding lactones, N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, diethylformamide, orthodichlorobenzene, meta-cresol, 2-picoline, propyl alcohol, sec-butyl alcohol, isopropylcarbinol, butanols, pyridine, amylalcohol.
The present invention at first carries out the decontamination decolouring to containing polyester waste spinning fabric or similar waste material, effectively remove pollution, oil, spinning finishing agent and the initial thin dust that clings etc. in the waste material, remove simultaneously most of dyestuff, and some easy molten fiber outside the dissolving polyester that may exist etc. carries out initial gross separation; Then adopt the polyester solvent that does not dissolve natural fiber waste material to be dissolved the natural and viscose fiber that elimination may exist etc.; Agent makes polyester separate out as precipitating to adopt the solvent that is difficult for dissolved polyester again, and a small amount of easy molten cellulosic and excess dye outside the polyester that may exist are still stayed in the mixing solutions, thereby reaches the purpose of the relatively pure polyester material of extraction.Adopting the organic solvent of moderate boiling point as the main component of decontamination decolouring solvent and polyester solvent, is a bright spot of the present invention, like this from decontamination decolouring, dissolved polyester to solvent recuperation, all reaches the actual effect of energy-and time-economizing; Especially select the solvent component of decontamination decolouring solvent, when consistent with the solvent component after the polyester solvent adds said precipitating agent, only need once to the solvent Distillation recovery, just may be used on two procedures, further energy-and time-economizing, and because also having precipitating operation etc. behind the dissolved polyester, so how many impacts are the whiteness of final polyester material etc. be there is no.Can find out obviously that from step of the present invention high recovery of solvent is feasible; Insoluble cottonly fine and so on leach thing and also can treatedly remake his usefulness, so substantially form without " three wastes ".
Embodiment
Embodiment 1
With blue woven dacron angle 45g, polyester-mixed cotton cloth angle 3g with wash sticky cloth angle 2g, put in the decontamination decolouring solvent of 310g N,N-DIMETHYLACETAMIDE, be warming up to 135 ℃-140 ℃ and keep 8min-15min, then solid-liquid separation, the cloth angle is extracted substantially, at this moment find that the cloth angle has been the pale blue whiting, and liquid is blue ink look (contaminated liquid distillating recovering solvent); Again get again the 290g N,N-DIMETHYLACETAMIDE and be warming up to 160 ℃, inwardly drop into treated cloth angle, then pressurization is warming up to 168 ℃-178 ℃ and keep 12-20min, the polyester composition is fully dissolved, then leach insolubles, when solution temperature drops to 130 ℃, the propyl alcohol temperature about itself and 500g normal temperature is closed, polyester is separated out as main take more solid bulk at once, and small part is with granular precipitation in small, broken bits; Then filter, this filtrate is collected separately and is prepared next embodiment use, and filter cake is dry by about 100 ℃ with the chloroform flushing again, namely gets the white polyester material.Polyester material is manual hot candied behind hot melt, and its wire-drawing effect of visual inspection slightly is inferior to the hot melt effect at initial woven dacron angle, but difference not too.This embodiment comprises that also the chloroform equal solvent reclaims routinely and reasonably recycles.
Embodiment 2
The filtrate of collecting separately among the embodiment 1 is added thermal distillation, only distillate propyl alcohol, raffinate directly replaces decontamination decolouring solvent to use, then at unclassified stores, temperature and time etc. all under the equal condition, repeat the operation of embodiment 1, obtain at last the whiteness etc. and embodiment 1 no significant difference of polyester material.This embodiment main purpose is to state the method that solvent rationally recycles, and is beneficial to further energy-and time-economizing impairment consumption.
Embodiment 3
With slightly with blue woven dacron angle 45g, the polyester-mixed cotton cloth angle 3g of greasy dirt with wash sticky cloth angle 2g, put in the decontamination decolouring solvent that 310g methyl-sulphoxide and 500g butanols be made into, be warming up to 130 ℃-135 ℃ and keep 8min-15min, then at this moment solid-liquid separation and the cloth angle extracted substantially finds that the cloth angle has been the pale blue whiting and mixed solution is blue ink look (contaminated liquid distillating recovering solvent); Again get again the 290g methyl-sulphoxide and be warming up to 160 ℃, inwardly drop into treated cloth angle, continue to be warming up to 177 ℃-182 ℃ and keep 10min-18min, the polyester composition is fully dissolved, then leach insolubles (reticulating), when solution temperature drops to 140 ℃, the butanols temperature about itself and 500g normal temperature is closed, polyester is namely separated out the broken pasty state of band small part so that loose bulk and wadding are flower-shaped as main; Then filter, this filtrate is collected separately and is prepared next embodiment use, and filter cake is dry by about 100 ℃ with the chloroform flushing again, namely gets the white polyester material.Polyester material is manual hot candied behind hot melt, the hot melt effect at its wire-drawing effect of visual inspection and initial woven dacron angle is quite approaching, but relatively relatively poor because of the polyester precipitating situation of this embodiment, the filtration unit that in addition adopts is insuperior again, a small amount of loss is arranged in filtrate and cause polyester material.This embodiment comprises that equally solvent reclaims routinely and reasonably recycles.
Embodiment 4
The filtrate of collecting separately among the embodiment 3 is directly replaced decontamination decolouring solvent, all under the equal condition, repeat the operation of embodiment 3 at unclassified stores, temperature and time, obtain at last the whiteness etc. and embodiment 3 basic indifferences of polyester material.
Embodiment 5
With blue woven dacron angle 45g, polyester-mixed cotton cloth angle 3g with wash sticky cloth angle 2g, put in the decontamination decolouring solvent of 310g methyl-sulphoxide, be warming up to 118 ℃-128 ℃ and keep 8min-15min, then solid-liquid separation and the cloth angle extracted substantially, at this moment find that the cloth angle has been pale blue whiting (it is lower to play the temperature of decolorization with methyl-sulphoxide separately), and liquid is blue ink look (contaminated liquid Distillation recovery methyl-sulphoxide); Simultaneously get again the 290g methyl-sulphoxide and be warming up to 160 ℃, inwardly drop into treated cloth angle, continue to be warming up to 177 ℃-182 ℃ and keep 10min-18min, the polyester composition is fully dissolved, then leach insolubles, when solution temperature drops to 140 ℃, the butanols temperature about itself and 500g normal temperature is closed, polyester is namely separated out the broken pasty state of band small part so that loose bulk and wadding are flower-shaped as main; Then filter, this filtrate is collected separately and is prepared next embodiment use, and filter cake is dry by about 100 ℃ with the chloroform flushing again, namely gets the white polyester material.Polyester material is manual hot candied behind hot melt, the hot melt effect at its wire-drawing effect of visual inspection and initial woven dacron angle is quite approaching, but relatively relatively poor because of the polyester precipitating situation of this embodiment, the filtration unit that in addition adopts is insuperior again, and causing polyester material has a small amount of loss.This embodiment comprises that equally solvent reclaims routinely and reasonably recycles.
Embodiment 6
The filtrate of collecting separately among the embodiment 5 is added thermal distillation, only distillate butanols, raffinate directly replaces decontamination decolouring solvent to use, then at unclassified stores, temperature and time all under the equal condition, repeat the operation of embodiment 5, the whiteness etc. that obtains at last polyester material is as good as substantially with embodiment 5.
Claims (10)
1. from the waste spinning fabric that contains polyester or similar waste material, extract the method for polyester material, relate in particular to colored terylene cloth angle or contain and wash the polyester of purifying in the blended fabric angle, it is characterized in that, comprise the following steps:
(a) selecting the organic solvent of 20 ℃-215 ℃ of boiling points is the decontamination decolouring solvent of main component, carry out the decontamination decolouring with 20 ℃-178 ℃ of solution temperatures to containing polyester waste spinning fabric or similar waste material, some easy molten fiber outside the polyester that simultaneously dissolving may exist etc., then solid-liquid separation, and from contaminated liquid, reclaim organic solvent in modes such as distillation or fractionation, in order to recycling;
(b) selecting the organic solvent of 20 ℃-215 ℃ of boiling points is the polyester solvent of main component, will be under 20 ℃ of-208 ℃ of temperature the decontamination decolouring contain polyester waste spinning fabric or similar waste material fully dissolves, then with solution filter, collect the polyester mixing solutions, the undissolved thing that leaches deals with in addition;
(c) the polyester mixing solutions is mixed mutually with the precipitating agent, cause polyester to be separated out in modes such as precipitation or suspensions, then refilter, filtrate collection is in order to recycling, the polyester filter cake is lower than the cleaning solvent flushing of polyester solvent again with boiling point, then with the polyester filtration cakes torrefaction, namely get polyester material; Can be together with the recovery and rinsing solvent when dry, comprise from the contaminated liquid of wash distillating the raffinate that is left behind the cleaning solvent with mode recovery and rinsing solvents such as distillations, can with the filtrate merging of collecting above, recycle in order to follow-up.
2. the method for from the waste spinning fabric that contains polyester or similar waste material, extracting polyester material as claimed in claim 1, it is characterized in that, the solvent component of said decontamination decolouring solvent, consistent with the solvent component after said polyester solvent adds said precipitating agent; Like this, step (c) contains the filtrate of polyester solvent and precipitating agent, can be without distillation or fractionation, and just conduct decontamination decolouring solvent next time uses.
3. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 is characterized in that, the solvent component of said decontamination decolouring solvent is consistent with the solvent component of said polyester solvent.
4. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 characterized by further comprising in step (b), carries out synchronously the polyester adhesiveness increasing and modifying with dissolved polyester and processes.
5. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 is characterized in that the decontamination bleaching temperature in the said step (a) is 20 ℃-158 ℃.
6. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 is characterized in that, the temperature of dissolved polyester is 20 ℃-188 ℃ in the said step (b).
7. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 is characterized in that, the temperature of dissolved polyester is 20 ℃-178 ℃ in the said step (b).
8. the method for extracting polyester material from the waste spinning fabric that contains polyester or similar waste material as claimed in claim 1 is characterized in that in step (b), the mode dissolved polyester that adopts pressurization to heat up.
9. such as each described method of from the waste spinning fabric that contains polyester or similar waste material, extracting polyester material in the claim 1,2,4,5,6,7,8, it is characterized in that, the main component of said decontamination decolouring solvent is one or more in the main component of following polyester solvent, and in the following precipitating agent one or more; The main component of said polyester solvent is one or more in N-Methyl pyrrolidone, Isosorbide-5-Nitrae-Ding lactones, N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, diethylformamide, orthodichlorobenzene, the meta-cresol; In the isomers that said precipitating agent is 2-picoline, propyl alcohol, sec-butyl alcohol, isopropylcarbinol, butanols, pyridine, amylalcohol, amylalcohol, the dioxan one or more; Said cleaning solvent is one or more in chloroform, methylene dichloride, tetracol phenixin, methyl alcohol, the ethanol.
10. such as each described method of from the waste spinning fabric that contains polyester or similar waste material, extracting polyester material in the claim 1,4,5,6,7,8, it is characterized in that, the main component of said decontamination decolouring solvent is one or more in the isomers, amylalcohol, dioxan of N-Methyl pyrrolidone, Isosorbide-5-Nitrae-Ding lactones, N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, diethylformamide, orthodichlorobenzene, meta-cresol, 2-picoline, propyl alcohol, sec-butyl alcohol, isopropylcarbinol, butanols, pyridine, amylalcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101162983A CN103374144A (en) | 2012-04-13 | 2012-04-13 | Method for extracting polyester material from waste textiles or similar wastes containing polyester |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101162983A CN103374144A (en) | 2012-04-13 | 2012-04-13 | Method for extracting polyester material from waste textiles or similar wastes containing polyester |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2528494A (en) * | 2014-07-24 | 2016-01-27 | Worn Again Footwear And Accessories Ltd | Recycling process |
| WO2016012755A1 (en) * | 2014-07-24 | 2016-01-28 | Worn Again Footwear And Accessories Limited | Recycling process |
| CN107587362A (en) * | 2016-07-15 | 2018-01-16 | 浙江绿宇环保股份有限公司 | It is a kind of to realize that containing for solvent circulation washs waste textile decoloration process |
| WO2019047176A1 (en) * | 2017-09-08 | 2019-03-14 | 香港纺织及成衣研发中心 | Method for recycling waste polyester-cotton blend fabrics |
| CN109468868A (en) * | 2017-09-08 | 2019-03-15 | 香港纺织及成衣研发中心 | A kind of composite decoloring method of waste and old polyester cotton |
| CN110790980A (en) * | 2019-10-22 | 2020-02-14 | 宁波大发化纤有限公司 | Separation and impurity removal method for blending material in waste polyester fiber product |
-
2012
- 2012-04-13 CN CN2012101162983A patent/CN103374144A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2528494A (en) * | 2014-07-24 | 2016-01-27 | Worn Again Footwear And Accessories Ltd | Recycling process |
| WO2016012755A1 (en) * | 2014-07-24 | 2016-01-28 | Worn Again Footwear And Accessories Limited | Recycling process |
| JP2017522444A (en) * | 2014-07-24 | 2017-08-10 | ウォーン アゲイン フットウェア アンド アクセサリーズ リミテッド | Recycling process |
| GB2528494B (en) * | 2014-07-24 | 2018-01-03 | Worn Again Footwear And Accessories Ltd | Process for extracting polyester and dyes from fabric |
| CN107587362A (en) * | 2016-07-15 | 2018-01-16 | 浙江绿宇环保股份有限公司 | It is a kind of to realize that containing for solvent circulation washs waste textile decoloration process |
| WO2019047176A1 (en) * | 2017-09-08 | 2019-03-14 | 香港纺织及成衣研发中心 | Method for recycling waste polyester-cotton blend fabrics |
| CN109468868A (en) * | 2017-09-08 | 2019-03-15 | 香港纺织及成衣研发中心 | A kind of composite decoloring method of waste and old polyester cotton |
| CN110790980A (en) * | 2019-10-22 | 2020-02-14 | 宁波大发化纤有限公司 | Separation and impurity removal method for blending material in waste polyester fiber product |
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