CN115197468A - Process for extracting chinlon from waste blended fabric by using selective solvent and product - Google Patents

Process for extracting chinlon from waste blended fabric by using selective solvent and product Download PDF

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Publication number
CN115197468A
CN115197468A CN202210276448.0A CN202210276448A CN115197468A CN 115197468 A CN115197468 A CN 115197468A CN 202210276448 A CN202210276448 A CN 202210276448A CN 115197468 A CN115197468 A CN 115197468A
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chinlon
solvent
selective solvent
waste
blended fabric
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Inventor
赖文钦
方华玉
柯希贤
赵洪亮
陆东东
张俊峰
林飞芳
吴建通
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Fujian Saixian New Materials Co ltd
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Fujian Huafeng New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/04Recovery or working-up of waste materials of polymers
    • C08J11/06Recovery or working-up of waste materials of polymers without chemical reactions
    • C08J11/08Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

The invention provides a process for extracting chinlon from waste blended fabric by using a selective solvent, which comprises the following specific steps: accurately weighing the waste blended fabric, crushing the waste blended fabric, adding the crushed waste blended fabric into a selective solvent, and carrying out heating dissolution reaction and accelerated dissolution to obtain a mixed solution containing the chinlon. The method has the advantages of no need of synergistic effect of other assistants, simple system, high selectivity and high solubility for dissolving the polyamide components in the waste blended fabric, capability of avoiding dissolving other components such as spandex, terylene, cotton and the like in the waste blended fabric, easiness in recovery, high polyamide extraction recovery rate, high polyamide component purity, low toxicity and low cost of a selective solvent system. More importantly, the energy consumption of the whole extraction process is low, and the selective dissolution of the chinlon component at normal temperature in a short time is realized. And the nylon has wide sources and simple extraction method, can efficiently and economically recover the nylon component from the waste nylon blended fabric through conventional dissolution, filtration and drying, and has commercial application prospect.

Description

Process for extracting chinlon from waste blended fabric by using selective solvent and product
Technical Field
The invention relates to the field of a chinlon extraction method, C08J3/12, in particular to a process for extracting chinlon from waste blended fabric by using a selective solvent and a product.
Background
The synthetic fiber is a chemical fiber prepared by spinning, molding and post-treating a meltable high-molecular linear polymer, and mainly comprises terylene, chinlon, acrylon and the like. The nylon is used as the second most synthetic fiber, and the dosage is second to that of the terylene. In chinlon textiles, other types of fibers are often present, such as polyester, spandex and cotton. The separation of components in the nylon blended fabric is difficult to realize by the traditional mechanical method. The prior method for recycling the nylon blended fabric mainly comprises the steps of melting at high temperature by a screw, extruding and granulating, and is used in the field of low-end plastics or used as resin filler. The quality of regenerated products cannot be guaranteed, the regenerated products are mostly low-grade products, the additional value is low, and the reason is that the recycling rate of the existing waste chinlon fabrics is low. In view of the high price of the nylon fiber, the separation, extraction and recovery of the nylon component from the nylon blended fabric are effective ways for solving the problem that the waste nylon fiber blended fabric cannot be reused in a high-value and comprehensive manner.
Gong et al, utilizing the selective dissolution of nylon by N, N-Dimethylformamide (DMF), can separate and recover nylon fiber from nylon/spandex fabric (Simple process for separation and recycling of nylon 6and polyurethane composites from polyamide fiber 6/polyurethane fiber [ J ]. Textille Research Journal,2020,91 (1-2): 004051753189), but this method has no commercial application prospect due to the toxicity of DMF and the expensive solvent recovery cost. National standard GB/T2910.7-2009 section 7 quantitative chemical analysis of textiles: in the polyamide fiber and certain other fiber mixtures, the mass fraction of the chinlon in the chinlon blended fabric can be measured by utilizing the selective dissolution effect of formic acid on the chinlon, but the used formic acid has extremely strong corrosivity and irritation, has larger safety risk for operators, and is not beneficial to large-scale industrial application. Patent CN201110382369.X discloses a method for preparing nylon powder by dissolving waste nylon by using ionic liquid, wherein the waste nylon is dissolved in the ionic liquid, and the nylon is obtained by dissolving the waste nylon at high temperature under pressure, wherein the volume average particle size of the obtained nylon powder is small, but the required high temperature is 120-300 ℃, the pressure is 0.5-2 MPa, and the ionic liquid is expensive. Patent CN201410257570.9 discloses a method for regenerating nylon, which comprises treating nylon-containing material with solvent and depolymerization catalyst, reacting with diamine material and polymerization catalyst, heating and pressurizing to obtain regenerated nylon material, wherein the nylon recovery rate is 96%, the performance of the regenerated nylon material is good, but the nylon material needs to be heated to 100-150 ℃, nitrogen is filled to pressurize to 1-3 MPa, the selective dissolving performance is poor, and non-nylon impurities are taken out before treatment.
Disclosure of Invention
The invention provides a process and a product for extracting chinlon from waste blended fabric by using a selective solvent, solves the technical problems that a solvent system is expensive, the recovery rate is high and the energy consumption in the extraction process cannot be considered at the same time in the prior art, and achieves the technical effects that the solvent system is low in toxicity, cheap and easy to recover, the energy consumption in the extraction process is low and the chinlon extraction rate is high.
The invention provides a process for extracting chinlon from waste blended fabrics by using a selective solvent, which comprises the following specific steps of:
(1) Accurately weighing waste blended fabric, adding the waste blended fabric into a selective solvent, carrying out heating dissolution reaction and accelerated dissolution to obtain a mixed solution containing nylon, and removing insoluble substances through solid-liquid separation to obtain a nylon solution;
(2) And (2) adding a poor solvent into the nylon solution obtained in the step (1), performing solid-liquid separation to obtain nylon powder, cleaning, drying to constant weight, and collecting to obtain nylon.
In some preferred embodiments, the waste blended fabric contains a nylon fiber component and/or a non-nylon fiber component.
In some preferred embodiments, the nylon fiber component is selected from one or more of nylon 6 fiber, nylon 66 fiber, nylon 610 fiber, nylon 12 fiber, nylon 612 fiber, nylon 46 fiber; preferably, the nylon fiber is nylon 6 fiber.
In some preferred embodiments, the non-nylon fiber component is selected from one or more of cotton fiber, hemp fiber, bamboo fiber, viscose fiber, polyester fiber, spandex fiber, acrylic fiber, and vinylon fiber; preferably, the non-nylon fiber component is selected from one or more of cotton fiber, polyester fiber and spandex fiber.
In some preferred embodiments, the selective solvent is selected from one or more of a flammable solvent, water, an ionic liquid, a chloride, an azo-based compound; preferably, the selective solvent is selected from one or more of a flammable solvent, water, chloride; further preferably, the selective solvent is a mixture of a flammable solvent, water and a chloride.
In some preferred embodiments, the flammable solvent has a boiling point of 50 to 240 ℃; preferably, the combustible solvent is selected from one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol and benzyl alcohol; further preferably, the flammable solvent is ethanol.
In some preferred embodiments, the chloride is selected from one or more of magnesium chloride, potassium chloride, calcium chloride, sodium chloride, barium chloride, ferric chloride; preferably, the chloride is calcium chloride.
In some preferred embodiments, the mass concentration of chloride in the selective solvent is from 22.0 to 100wt%; further preferably, the mass concentration of the chloride in the mixed solvent-selective solvent is 23.0 to 30.0wt%. The inventor discovers that if the mass concentration of the chloride is too high, the excessive dissolution of the chinlon 6 can be caused, the chinlon structure is damaged, the recycled chinlon cannot be reused, and meanwhile, a small part of other components in the waste blended fabric can be dissolved, so that the recovery efficiency of the chinlon 6 is reduced, and if the mass concentration of the chloride is too low, the chinlon 6 in the waste blended fabric can not be dissolved sufficiently under the condition, so that the extraction efficiency of the chinlon 6 is reduced, therefore, only the chloride-containing selective solvent obtained by proportioning water and ethanol with a specific concentration can perform the best extraction and recycling effects on the chinlon 6 in the waste blended fabric.
In some preferred embodiments, the mass concentration of the flammable solvent in the mixed solvent-selective solvent is 5.0 to 100wt%; preferably, the mass concentration of the combustible solvent in the selective solvent is 9.5-100 wt%; further preferably, the mass concentration of the combustible solvent in the selective solvent is 37.0-70.0 wt%; still more preferably, the mass concentration of the flammable solvent in the mixed solvent-selective solvent is 40.0 to 61.0wt%.
In some preferred embodiments, the mass ratio of water to ethanol in the selective solvent is (0-2): 1; preferably, the mass ratio of water to ethanol in the selective solvent is (0-1): 1; further preferably, the mass ratio of water to ethanol in the selective solvent is (0.2-0.9): 1.
in some preferred embodiments, the mass ratio of the waste blended fabric to the selective solvent is 1: (5-75); preferably, the mass ratio of the waste blended fabric to the selective solvent is 1: (5-50); further preferably, the mass ratio of the waste blended fabric to the selective solvent is 1: (10-40); still more preferably, the mass ratio of the waste blended fabric to the selective solvent is 1:20.
in some preferred embodiments, the specific conditions of the heating dissolution reaction are that the heating dissolution temperature is 0-60 ℃, and the reaction time is 30-240 min; preferably, the specific conditions of the heating dissolution reaction are that the heating dissolution temperature is 10-40 ℃, and the reaction time is 30-100 min. In the research process, the inventor finds that the dissolution speed is slow when the temperature is lower than 10 ℃; when the temperature is higher than 40 ℃, the dissolving speed is high, the single dissolving of the chinlon 6 in the waste blended fabric is not facilitated, and the other components can be dissolved at a small part, and the most preferable condition is that the dissolving is carried out within the room temperature range, so that an external extra heat source can be saved, and the energy consumption is saved. Meanwhile, through multiple experiments, the inventor finds that the reaction effect is optimal when the reaction time is controlled to be 30-100min, because the reaction time is too short and the dissolution is incomplete; over time, complete dissolution may also be achieved, but efficiency is compromised.
In some preferred embodiments, the accelerated dissolution means is selected from one or more of standing, stirring, shaking, sonication; preferably, the dissolution accelerating means is stirring.
In some preferred embodiments, the separation step is selected from one or more of filtration, centrifugation, decantation, gravity settling; preferably, the separating step is filtration;
in some preferred embodiments, the poor solvent is selected from one or more of methanol, ethanol, propanol, diethyl ether, water, butanol; preferably, the poor solvent is water.
In some preferred embodiments, the volume ratio of the nylon solution to the poor solvent in the step (2) is 1: (1-100); further preferably, the volume ratio of the chinlon solution to the poor solvent in the step (2) is 1: (2 to 20).
In some preferred embodiments, the drying temperature in the step (2) is 95-120 ℃ and the drying time is 3-6 h; preferably, the drying temperature in the step (2) is 105 ℃ and the drying time is 4h.
The invention provides a chinlon extracted from waste blended fabric by using a selective solvent in a second aspect.
Has the advantages that:
(1) Through selecting ethanol, water, calcium chloride as selective solvent in this application, do not need the synergism of other auxiliaries, the system is simple, has high selectivity to the dissolution of polyamide fibre component in old and useless blended fabric, and the solubility is high moreover, can avoid the dissolution of other components such as spandex, dacron, cotton in old and useless blended fabric simultaneously, easily retrieves, has very high polyamide fibre and draws the purity of recovery rate and polyamide fibre component height, has commercial application prospect.
(2) Chinlon is a synthetic polyamide fiber containing highly polar hydrogen bonds and having poor dissolution effect with alcohols. However, the inventor of the invention finds out through a large number of experiments that the selection of the high-selectivity solvent can increase the solubility of the chinlon material in the waste blended fabric in the mixed solvent, and particularly, the selection of the ternary selective solvent system of ethanol, water and calcium chloride can realize the selective dissolution of chinlon, especially chinlon 6. Presumably, in a polar environment, calcium ions and chloride ions are coordinated with active groups in the chinlon 6 to form a more stable complex, so that hydrogen bonds of the chinlon 6 are damaged, thermal movement of carbonyl is hindered, regular arrangement of molecular chains of the chinlon 6 is damaged, a three-dimensional ordered structure of the chinlon 6 is weakened, and the chinlon is converted into an amorphous structure from a semi-crystalline structure. Unexpectedly, when the mass concentration of the chloride in the selective solvent is 22.0 to 100wt%, the mass concentration of the ethanol is 37.0 to 100wt%, and the mass ratio of water to ethanol in the selective solvent is (0 to 1): 1, the reaction temperature in the reaction and dissolution process can be effectively reduced, the reaction time is shortened, the reaction difficulty is reduced, and the selective dissolution of the chinlon 6 in the waste blended fabric is further improved, so that the aim of extracting the chinlon 6 component from the blended fabric into a selective solvent is fulfilled, and meanwhile, the recovery rate of the chinlon 6 is up to 95%.
(3) The selective solvent system in the invention is low in toxicity and low in price, more importantly, the energy consumption in the whole extraction process is low, and the selective dissolution of the chinlon component at normal temperature in a short time is realized. The nylon has wide sources, the extraction method of the nylon component is simple, the nylon component can be efficiently and economically recovered from the waste nylon blended fabric through conventional dissolution, filtration and drying, and after the nylon 6 powder is cleaned and dried to remove the solvent and moisture, the nylon 6 can be used in the downstream fields of fibers or plastics and the like, thereby being beneficial to realizing the high added value utilization of the waste nylon blended fabric, saving resources and protecting the environment.
Detailed Description
Example 1.
1. A process for extracting chinlon from waste blended fabric by using a selective solvent comprises the following specific steps:
(1) Accurately weighing 1g of waste blended fabric (nylon 6 fiber), adding into 20g of selective solvent, stirring and dissolving at 25 ℃ for 60min to obtain a nylon-containing mixed solution, and removing insoluble substances through solid-liquid separation (filtration) to obtain a nylon 6 solution;
(2) And (2) adding 200g of poor solvent (water) into the nylon 6 solution obtained in the step (1), performing solid-liquid separation (filtration) to obtain nylon 6 powder, cleaning, drying at 105 ℃ for 4 hours, and collecting to obtain the nylon.
The selective solvent is a mixed solution of combustible solvent, water and chloride.
The combustible solvent is ethanol. The chloride is calcium chloride.
The mass concentration of chloride in the mixed solvent is 29.5wt%; the mass concentration of the combustible solvent in the mixed solvent is 61.0wt%; the mass concentration of water in the mixed solvent was 9.5wt%.
The mass ratio of water to ethanol in the mixed solvent is 0.16:1.
2. chinlon extracted from waste blended fabric by using selective solvent.
Example 2.
1. A process for extracting chinlon from waste blended fabric by using a selective solvent is different from the process of the embodiment 1 in that:
the waste blended fabric is a terylene/chinlon 6/spandex fabric.
The content of the nylon-6 fiber is 15wt%; the content of the polyester fiber is 75wt%; the content of spandex fiber was 10wt%.
2. Chinlon extracted from waste blended fabric by using selective solvent.
Example 3.
1. A process for extracting chinlon from waste blended fabric by using a selective solvent is different from the process of the embodiment 1 in that:
the mass concentration of chloride in the mixed solvent is 25wt%; the mass concentration of the combustible solvent in the mixed solvent is 40wt%; the mass concentration of water in the mixed solvent is 35wt%.
The waste blended fabric is cotton/chinlon 6/spandex fabric.
The content of the nylon-6 fiber is 32wt%; the content of cotton fiber is 65wt%; the content of spandex fiber was 3wt%.
And (3) performance testing:
1. solubility: respectively putting 0.5g of nylon-6 fiber, cotton fiber, polyester fiber and spandex fiber into 10g of calcium chloride/ethanol/water (specific ratio shown in the following table) selective solvent, stirring for 60min at 25 ℃, and observing the dissolution condition of the fibers, as shown in table 1:
TABLE 1 dissolution of different fibres in calcium chloride/ethanol/water solvent
Figure BDA0003555920870000061
Figure BDA0003555920870000071
2. And (3) recovery rate: the powders obtained in the examples were weighed and the recovery = m according to the formula 2 /(m 1 X chinlon content) x 100%, wherein: m is 1 The mass of the waste blended fabric added before dissolution; m is 2 The mass of the solid obtained after drying. The specific results are shown in table 2:
table 2 example recovery test results
Example 1 Example 2 Example 3
Mass/g of waste blended fabric 1 1 1
Mass/g of solid powder 0.95 0.14 0.3
Percent recovery% 95 93 94

Claims (10)

1. A process for extracting chinlon from waste blended fabric by using a selective solvent is characterized by comprising the following specific steps:
(1) Accurately weighing waste blended fabric, adding the waste blended fabric into a selective solvent, carrying out heating dissolution reaction and accelerated dissolution to obtain a mixed solution containing nylon, and removing insoluble substances through solid-liquid separation to obtain a nylon solution;
(2) Adding a poor solvent into the nylon solution obtained in the step (1), performing solid-liquid separation to obtain nylon powder, cleaning, drying to constant weight, and collecting to obtain nylon;
the selective solvent is selected from one or more of flammable solvent, water, ionic liquid, chloride and azo compounds.
2. The process for extracting chinlon from waste blended fabric by using the selective solvent as claimed in claim 1, wherein the selective solvent is a mixed solution of a combustible solvent, water and a chloride.
3. The process for extracting chinlon from waste blended fabrics by using the selective solvent as claimed in claim 2, wherein the mass concentration of chloride in the selective solvent is 22.0-100 wt%, the mass concentration of the combustible solvent is 37.0-100 wt%, and the mass ratio of water to the combustible solvent is (0-1): 1.
4. the process for extracting chinlon from waste blended fabrics by using selective solvent as claimed in any one of claims 1 to 3, wherein the boiling point of the flammable solvent is 50-240 ℃.
5. The process for extracting chinlon from waste blended fabrics by using selective solvent as claimed in claim 4, wherein the flammable solvent is selected from one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol and benzyl alcohol.
6. The process for extracting chinlon from waste blended fabrics by using selective solvent according to any one of claims 1-3, wherein the chloride is selected from one or more of magnesium chloride, potassium chloride, calcium chloride, sodium chloride, barium chloride and ferric chloride.
7. The process for extracting chinlon from waste blended fabrics by using selective solvent as claimed in claim 5, wherein the chloride is calcium chloride.
8. The process for extracting chinlon from waste blended fabric by using selective solvent as claimed in claim 1, wherein the mass ratio of the waste blended fabric to the selective solvent is 1: (5 to 50).
9. The process for extracting chinlon from waste blended fabrics by using the selective solvent as claimed in claim 1, wherein the specific conditions of the heating and dissolving reaction are that the heating and dissolving temperature is 0-60 ℃ and the reaction time is 30-240 min.
10. A chinlon obtained by the process for extracting chinlon from waste blended fabrics with a selective solvent according to any one of claims 1-9.
CN202210276448.0A 2022-03-21 2022-03-21 Process for extracting chinlon from waste blended fabric by using selective solvent and product Pending CN115197468A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09309956A (en) * 1996-05-22 1997-12-02 Asahi Chem Ind Co Ltd Agglomerate of polyamide particles and its production
WO2000029463A1 (en) * 1998-11-13 2000-05-25 Stefandl Roland E Improved process for recycling and recovery of purified nylon polymer
JP2009286867A (en) * 2008-05-28 2009-12-10 Univ Kansai Method for recovering aliphatic polyamide from composite of aliphatic polyamide fiber base fabric
CN101745999A (en) * 2009-12-23 2010-06-23 陈学玺 Clean production process for reclaiming nylon 66 from waste tire cords
CN105367818A (en) * 2015-11-08 2016-03-02 韶关市连邦环保新材料股份有限公司 Method for preparing pure product nylon 6 by taking nylon 6 waste material as raw material
CN109881306A (en) * 2019-01-21 2019-06-14 五邑大学 A kind of blended fabric separation and recovery reuse method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09309956A (en) * 1996-05-22 1997-12-02 Asahi Chem Ind Co Ltd Agglomerate of polyamide particles and its production
WO2000029463A1 (en) * 1998-11-13 2000-05-25 Stefandl Roland E Improved process for recycling and recovery of purified nylon polymer
JP2009286867A (en) * 2008-05-28 2009-12-10 Univ Kansai Method for recovering aliphatic polyamide from composite of aliphatic polyamide fiber base fabric
CN101745999A (en) * 2009-12-23 2010-06-23 陈学玺 Clean production process for reclaiming nylon 66 from waste tire cords
CN105367818A (en) * 2015-11-08 2016-03-02 韶关市连邦环保新材料股份有限公司 Method for preparing pure product nylon 6 by taking nylon 6 waste material as raw material
CN109881306A (en) * 2019-01-21 2019-06-14 五邑大学 A kind of blended fabric separation and recovery reuse method

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