CN102532815B - Method for recycling waste polyester textiles - Google Patents
Method for recycling waste polyester textiles Download PDFInfo
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- CN102532815B CN102532815B CN2011104015178A CN201110401517A CN102532815B CN 102532815 B CN102532815 B CN 102532815B CN 2011104015178 A CN2011104015178 A CN 2011104015178A CN 201110401517 A CN201110401517 A CN 201110401517A CN 102532815 B CN102532815 B CN 102532815B
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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
Abstract
The invention discloses a method for recycling waste polyester textiles, which comprises the following steps of (1) a polymerization system for recycling and (2) a purification system for collecting by-products and recycling solvent. The method for recycling the waste polyester textiles adopts a mode that the waste polyester textiles are treated continuously and enables polyester in the waste polyester textiles to be recycled, achieves recycling of massive waste polyester textiles, meets the requirements of users for additional textile fibers, reduces dependence level of the industry to petroleum, is energy-saving, emission-reducing, protects the environment, promotes sustainable development of the textile industry and develops recycling economy of the polyester industry.
Description
Technical field
The invention belongs to the resource recovery field, more specifically, the present invention relates to a kind of method of useless polyester-containing textiles recycling, this method is to handle useless polyester-containing textiles and make it obtain the industrialization recovery method of recycling for serialization.
Background technology
Along with improving constantly of people's living standard, demand to textiles constantly enlarges, natural fiber can not satisfy people's demand already, regenerated fiber has become the main body in the textile raw material, and terylene is as the maximum kind in China's chemical fibre industry, and its production capacity had reached more than 2,900 ten thousand tons in 2010, account for more than 2/3 of the world, and the trevira that the oil conversion is produced has accounted for great proportion in regenerated fiber, and the anxiety of oil has influenced the production of trevira again.Therefore, the space-pollution of terylene textiles will be more outstanding, thereby reclaim terylene textiles recycling on a large scale and have very urgent.Reclaim the Regenerated Polyester Fibres of producing with useless polyester product, both solved the direct dependence to oil, reduced white pollution again, become a main direction of green weaving future development.
The recycling of polyester is very important field during polymer is recycled.The waste polyester recovery technology is divided into physics recovery technology and chemical recovery technology two big classes.It is with the waste polyester heating and melting that physics reclaims, and the back of purifying is by the screw extruder extrusion moulding, and general process is: classification-fragmentation-cleaning-dehydration-drying-granulation (spinning).Chemical recovery method is by chemical reaction waste polyester to be depolymerized to low molecular compound such as terephthalic acid (TPA), dimethyl terephthalate (DMT) (DMT), ethylene glycol terephthalate (BHET), terephthalic acid two different new esters (DOTP), L--alcohol (EG) etc., can be again as polyester raw material after alcoholysis product is purified, or make other products.Chemical recovery method comprises that also chemistry improves, and adopts usually to increase chain modified, cross-linking modified, chlorination modified etc. to change chain length, the structure of polyester, thereby improves its some characteristic.
At present, also nearly all be to be confined to polyester bottles to reclaim the field in the useless polyester product field of reclaiming both at home and abroad, for example the U.S. utilizes useless PET bottle through the methyl alcohol alcoholysis, and production dimethyl terephthalate (DMT) and hexylene glycol directly carry out polycondensation again and prepare new polyester.These major parts all are that the Application Areas originally according to raw material reclaims degradation and uses.
Recently, carried out relevant report to reclaiming polyester-containing textiles abroad, namely from " fiber is to the regeneration technology ".This technology refers to trevira products such as used uniform, Sportswear are carried out chemical treatment, restores polyester raw material, produces the process of the trevira product that makes new advances then.At present, Japanese Supreme Being people company carries out this business in the Guia Hill of Japan Ehime Prefecture cause.Dupont is also studied this, and what it reclaimed employing is the methyl alcohol alcoholysis method, is DMT and EG with the polyester depolymerization.But the most serialization of these processing methodes, industrializing implementation degree are low, and the solvent toxicity of Cai Yonging is strong simultaneously, the cleaning manufacturing technique method that does not provide solvent cycle to utilize.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of useless polyester-containing textiles recycling method, this method can be recycled the useless pure textiles of washing, recovery obtains the trevira recycling of high viscosity, high added value, realize simultaneously reclaiming solvent recycling, guaranteed the cleaner production of this industrialization technology.
The present invention realizes by following technical scheme:
A kind of method of useless polyester-containing textiles recycling, it recycles useless polyester-containing textiles by following two big treatment systems:
(1) paradigmatic system of recycling;
(2) purification system that by product is collected and solvent cycle is utilized.
The paradigmatic system of described recycling comprises following three parts:
(1) the useless pure textile raw material fusion alcoholysis system of washing;
(2) polycondensation system;
(3) Masterbatch injected system;
The treating processes of the purification system of described by product collection and solvent cycle utilization comprises following six steps:
(1) ethylene glycol of extracting out from the alcoholysis still of the paradigmatic system of recycling enters an ethylene glycol lightness-removing column, removes the light constituent in the alcoholysis ethylene glycol, to light constituent, has obtained not containing the ethylene glycol of light constituent in overhead collection at the bottom of tower;
(2) ethylene glycol after the ethylene glycol lightness-removing column is handled enters an ethylene glycol weight-removing column and handles, and collection and treatment is carried out in the heavy constituent at the bottom of tower, obtains purity greater than 85% ethylene glycol at cat head;
(3) the high purity ethylene glycol that comes out from the ethylene glycol weight-removing column is divided into four parts: first part removes the alcoholysis still, for alcoholysis fusion operation provides alcoholysis ethylene glycol, second section removes the squirt pump of vacuum system through the ethylene glycol vaporizer of vacuum system, third part enters ethylene glycol squirt pump hot well, and last part is got back to fresh ethylene glycol storage tank;
(4) ethylene glycol of ethylene glycol squirt pump hot well is imported the ethylene glycol hot well of whole polycondensation vessel through pump, is used for the ethylene glycol spray of whole polycondensation vessel;
(5) the ethylene glycol hot well overflow of whole polycondensation vessel enters the ethylene glycol hot well of precondensation still, is used for the ethylene glycol spray of precondensation still, and other component concentration is higher in the ethylene glycol that this part produces, and returns the ethylene glycol lightness-removing column and carries out circular treatment;
(6) the spent glycol storage tank constantly replenishes the amount of the ethylene glycol of whole device consumption, partly is delivered to retrieving arrangement simultaneously and uses, and forms a system that circulation is airtight.
Described useless pure treating processes of washing textile raw material fusion alcoholysis system comprises the steps:
(1) uselessly purely wash the textiles fragmentation and enter the screw rod fusion by feed bin, add alcoholysis ethylene glycol toward screw rod simultaneously it is carried out partial alcoholysis, the amount of heated glycol is the useless pure 5%-1000% that washs quality of textile products, and the temperature of screw rod fusion alcoholysis is 150-250 ℃;
(2) material that comes out through the screw rod fusion enters the alcoholysis still, carry out further alcoholysis, guaranteed the abundant alcoholysis of useless polyester raw material, this stage alcoholysis is carried out under certain vacuum tightness, the vacuum tightness of this alcoholysis process is absolute pressure 1000Pa-10000Pa, and the ethylene glycol of extraction enters the ethylene glycol lightness-removing column and handles.
The treating processes of described polycondensation system comprises the steps:
(1) to enter three phases be precondensation stage to the material after the further alcoholysis of alcoholysis still, before entering precondensation stage, deviate from small molecules in the alcoholysate or/and add catalyzer, carry out partially polymerized to reduce the pressure that whole polycondensation vessel need increase substantially material viscosity simultaneously, this stage need carry out under certain negative pressure, the temperature control of this process is at 250-280 ℃, and vacuum tightness is absolute pressure 1000Pa-5000Pa;
(2) material after precondensation stage is handled enters the poly-stage of final minification, and the poly-tackify still that adopts of final minification is deviate from ethylene glycol and other small molecules, and the temperature control of this process is at 250-295 ℃, and its vacuum degree control is absolute pressure 50Pa-500Pa.
The melt-mixing of the treating processes of described Masterbatch injected system for described Masterbatch and polycondensation are come out.
Beneficial effect of the present invention is:
The method of waste spinning fabric disclosed by the invention recycling, the serialization recycling of extensive useless polyester-containing textiles will be realized, through engineering approaches is strong, and the solvent that adopts in the removal process can recycle, method successful implementation of the present invention will satisfied people to requiring under the prerequisite that textile fibres increases, can reduce the demand to oil, reduce industrial goods production discharge capacity.Reduced pollution simultaneously, the enabling environment protection promotes the weaving Sustainable development.The state of the art and the characteristics that meet textile industry, the recycling economy of realization PET industry.
Description of drawings
Fig. 1 is the process flow sheet of useless polyester-containing textiles recycling;
Fig. 2 is the recycle process for cleanly preparing schema of solvent for use.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
As shown in Figure 1, take by weighing the useless pure textiles 100kg/h that washs, enter the screw rod fusion, adding ethylene glycol 10kg/h toward screw rod simultaneously, is 190 ℃ of following alcoholysis 30min in normal pressure, temperature, and the material that comes out through the screw rod fusion enters the alcoholysis still, under little negative pressure, carry out further alcoholysis, temperature is 200 ℃ of following alcoholysis 10min, has guaranteed the abundant alcoholysis of useless polyester raw material, and the ethylene glycol that this stage extracts out enters the ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, before entering precondensation stage, add catalyzer 0.1g, the catalyst glycol concentration that is made into is 20%, be 2000Pa in vacuum tightness, temperature of reaction is 275 ℃, be 60min between reaction is seasonable, deviate from the small molecules in the alcoholysate, simultaneously partially polymerized, it is poly-that the material after precondensation is handled enters final minification, at vacuum tightness＜300Pa, temperature of reaction is 285 ℃, be 90min between reaction is seasonable, deviate from small molecules such as ethylene glycol, the limiting viscosity＞0.67dl/g of the polyester that obtains regenerating.
Embodiment 1
As shown in Figure 1, take by weighing the useless pure textiles 100kg/h that washs, enter the screw rod fusion, adding ethylene glycol 10kg/h toward screw rod simultaneously, is 190 ℃ of following alcoholysis 30min in normal pressure, temperature, and the material that comes out through the screw rod fusion enters the alcoholysis still, under little negative pressure, carry out further alcoholysis, temperature is 200 ℃ of following alcoholysis 10min, has guaranteed the abundant alcoholysis of useless polyester raw material, and the ethylene glycol that this stage extracts out enters the ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, before entering precondensation stage, add catalyzer 0.1g, the catalyst glycol concentration that is made into is 20%, be 2000Pa in vacuum tightness, temperature of reaction is 275 ℃, reaction times is 60min, deviate from the small molecules in the alcoholysate, simultaneously partially polymerized, it is poly-that the material after precondensation is handled enters final minification, at vacuum tightness＜300Pa, temperature of reaction is 285 ℃, be 90min between reaction is seasonable, deviate from small molecules such as ethylene glycol, the limiting viscosity＞0.67dl/g of the polyester that obtains regenerating.
Embodiment 2
As shown in Figure 1, take by weighing the useless pure textiles 100kg/h that washs, enter the screw rod fusion, adding ethylene glycol 20kg/h toward screw rod simultaneously, is 200 ℃ of following alcoholysis 30min in normal pressure, temperature, and the material that comes out through the screw rod fusion enters the alcoholysis still, under little negative pressure, carry out further alcoholysis, temperature is 200 ℃ of following alcoholysis 10min, has guaranteed the abundant alcoholysis of useless polyester raw material, and the ethylene glycol that this stage extracts out enters the ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, before entering precondensation stage, add catalyzer 0.1g, the catalyst glycol concentration that is made into is 20%, be 5000Pa in vacuum tightness, temperature of reaction is 270 ℃, reaction times is 60min, deviate from the small molecules in the alcoholysate, simultaneously partially polymerized, it is poly-that the material after precondensation is handled enters final minification, at vacuum tightness＜300Pa, temperature of reaction is 290 ℃, be 90min between reaction is seasonable, deviate from small molecules such as ethylene glycol, the limiting viscosity＞0.70dl/g of the polyester that obtains regenerating.
Embodiment 3
As shown in Figure 1, take by weighing the useless pure textiles 120kg/h that washs, enter the screw rod fusion, adding ethylene glycol 30kg/h toward screw rod simultaneously, is 200 ℃ of following alcoholysis 30min in normal pressure, temperature, and the material that comes out through the screw rod fusion enters the alcoholysis still, under little negative pressure, carry out further alcoholysis, temperature is 200 ℃ of following alcoholysis 10min, has guaranteed the abundant alcoholysis of useless polyester raw material, and the ethylene glycol that this stage extracts out enters the ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, before entering precondensation stage, add catalyzer 0.1g, the catalyst glycol concentration that is made into is 20%, be 5000Pa in vacuum tightness, temperature of reaction is 270 ℃, reaction times is 60min, deviate from the small molecules in the alcoholysate, simultaneously partially polymerized, it is poly-that the material after precondensation is handled enters final minification, at vacuum tightness＜300Pa, temperature of reaction is 290 ℃, be 90min between reaction is seasonable, deviate from small molecules such as ethylene glycol, the limiting viscosity＞0.70dl/g of the polyester that obtains regenerating.
Embodiment 4
Come the ethylene glycol 80kg/h of the alcoholysis still extraction of autonomous technology retrieving arrangement, entering an ethylene glycol lightness-removing column handles, remove the light constituent in the alcoholysis ethylene glycol, carry out the export trade processing in overhead collection to light constituent and with this part light constituent collection, at the bottom of tower, obtained the ethylene glycol 78kg/h of light constituent, entered an ethylene glycol weight-removing column and handle, export trade has been collected in the heavy constituent at the bottom of tower handle, obtain highly purified ethylene glycol 74kg/h at cat head, purity is＞85%.
Should be appreciated that above narration only is example and illustrative for the present invention who sets forth as claim, is limited it.The of the present invention content disclosed according to this paper, other embodiment of the present invention is apparent for a person skilled in the art.Should be noted that this specification sheets and embodiment only should be regarded as is example, and actual range of the present invention should be determined by claim.
Claims (1)
1. the method for a useless polyester-containing textiles recycling is characterized in that: by following two big treatment systems useless polyester-containing textiles is recycled:
(1) paradigmatic system of recycling;
(2) purification system that by product is collected and solvent cycle is utilized;
The paradigmatic system of described recycling comprises following three parts:
(1) the useless pure textile raw material fusion alcoholysis system of washing;
(2) polycondensation system;
(3) Masterbatch injected system;
The treating processes of the purification system of described by product collection and solvent cycle utilization comprises following six steps: the ethylene glycol that extract out from the alcoholysis still of the paradigmatic system of recycling (1) enters an ethylene glycol lightness-removing column, remove the light constituent in the alcoholysis ethylene glycol, to light constituent, at the bottom of tower, obtained not containing the ethylene glycol of light constituent in overhead collection;
(2) ethylene glycol after the ethylene glycol lightness-removing column is handled enters an ethylene glycol weight-removing column and handles, and collection and treatment is carried out in the heavy constituent at the bottom of tower, obtains purity greater than 85% ethylene glycol at cat head;
(3) the high purity ethylene glycol that comes out from the ethylene glycol weight-removing column is divided into four parts: first part removes the alcoholysis still, for alcoholysis fusion operation provides alcoholysis ethylene glycol, second section removes the squirt pump of vacuum system through the ethylene glycol vaporizer of vacuum system, third part enters ethylene glycol squirt pump hot well, and last part is got back to fresh ethylene glycol storage tank;
(4) ethylene glycol of ethylene glycol squirt pump hot well is imported the ethylene glycol hot well of whole polycondensation vessel through pump, is used for the ethylene glycol spray of whole polycondensation vessel;
(5) the ethylene glycol hot well overflow of whole polycondensation vessel enters the ethylene glycol hot well of precondensation still, is used for the ethylene glycol spray of precondensation still, and other component concentration is higher in the ethylene glycol that this part produces, and returns the ethylene glycol lightness-removing column and carries out circular treatment;
(6) the spent glycol storage tank constantly replenishes the amount of the ethylene glycol of whole device consumption, partly is delivered to retrieving arrangement simultaneously and uses, and forms a system that circulation is airtight;
Described useless pure treating processes of washing textile raw material fusion alcoholysis system comprises the steps:
(1) uselessly purely wash the textiles fragmentation and enter the screw rod fusion by feed bin, add alcoholysis ethylene glycol toward screw rod simultaneously it is carried out partial alcoholysis, the amount of heated glycol is the useless pure 5%-1000% that washs quality of textile products, and the temperature of screw rod fusion alcoholysis is 150-250 ℃;
(2) material that comes out through the screw rod fusion enters the alcoholysis still, carry out further alcoholysis, guaranteed the abundant alcoholysis of useless polyester raw material, this stage alcoholysis is carried out under certain vacuum tightness, the vacuum tightness of this alcoholysis process is absolute pressure 1000Pa-10000Pa, and the ethylene glycol of extraction enters the ethylene glycol lightness-removing column and handles;
The treating processes of described polycondensation system comprises the steps:
(1) to enter three phases be precondensation stage to the material after the further alcoholysis of alcoholysis still, before entering precondensation stage, deviate from small molecules in the alcoholysate or/and add catalyzer, carry out partially polymerized to reduce the pressure that whole polycondensation vessel need increase substantially material viscosity simultaneously, this stage need carry out under certain negative pressure, the temperature control of this process is at 250-280 ℃, and vacuum tightness is absolute pressure 1000Pa-5000Pa;
(2) material after precondensation stage is handled enters the poly-stage of final minification, and the poly-tackify still that adopts of final minification is deviate from ethylene glycol and other small molecules, and the temperature control of this process is at 250-295 ℃, and its vacuum degree control is absolute pressure 50Pa-500Pa;
The treating processes of described Masterbatch injected system is with the melt-mixing after described Masterbatch and the polycondensation.
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| CN2011104015178A CN102532815B (en) | 2011-12-06 | 2011-12-06 | Method for recycling waste polyester textiles |
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| CN2011104015178A CN102532815B (en) | 2011-12-06 | 2011-12-06 | Method for recycling waste polyester textiles |
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| CN102532815B true CN102532815B (en) | 2013-09-25 |
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| CN106609405A (en) * | 2015-10-23 | 2017-05-03 | 南通金康弘纺织品有限公司 | Method for recovery and reutilization of waste cotton textile |
| CN106353216A (en) * | 2016-08-15 | 2017-01-25 | 宁波大发化纤有限公司 | Inorganic or mechanical impurity test method in waste polyester textiles |
| CN106279656A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | The method that 1.4 butanediol alcoholysis Waste Polyester textile preparation height join quality melt |
| CN106279758A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt |
| CN106279757A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | The method that glycolysis alcoholysis Waste Polyester textile preparation height joins quality melt |
| CN108754674A (en) * | 2018-05-27 | 2018-11-06 | 上海锦湾实业有限公司 | A kind of regenerated silk processing and treating method |
| TWI694064B (en) | 2018-09-26 | 2020-05-21 | 遠東新世紀股份有限公司 | Method for manufacturing terephthalic acid and system thereof |
| CN110527138B (en) * | 2019-07-10 | 2020-07-03 | 艾凡佳德(上海)环保科技有限公司 | Continuous alcoholysis recovery method of waste polyester |
| CN110511137B (en) * | 2019-07-10 | 2020-06-26 | 艾凡佳德(上海)环保科技有限公司 | Continuous alcoholysis and ester exchange recovery method for waste polyester material |
| CN110483279B (en) * | 2019-07-10 | 2020-08-14 | 艾凡佳德(上海)环保科技有限公司 | Method for recovering waste polyester material |
| CN110777445A (en) * | 2019-11-22 | 2020-02-11 | 浙江海利环保科技股份有限公司 | Preparation method of regenerated polyester fiber |
| CN114425173B (en) * | 2020-10-10 | 2023-07-04 | 中国石油化工股份有限公司 | Device and method for recycling crude ethylene glycol in polyester production process |
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| US6410607B1 (en) * | 1999-02-10 | 2002-06-25 | Eastman Chemical Company | Glycolysis process for recycling of post-consumer pet |
| WO2001030729A1 (en) * | 1999-10-22 | 2001-05-03 | Teijin Limited | Method for separating and recovering dimethyl terephthalate and ethylene glycol from polyester waste |
| CN1292014C (en) * | 2004-11-18 | 2006-12-27 | 华东理工大学华昌聚合物有限公司 | Synthesis of p-phenyl unsaturated polyester resin by using waste polyester material |
| CN101805445B (en) * | 2010-01-29 | 2012-01-25 | 成强 | Chemical treating method for melt polycondensation high polymer old material regeneration |
| CN102153734B (en) * | 2010-12-30 | 2013-09-11 | 金发科技股份有限公司 | Method for preparing biodegradable polyester from consumed polyester |
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