CN101745999A - Clean production process for reclaiming nylon 66 from waste tire cords - Google Patents
Clean production process for reclaiming nylon 66 from waste tire cords Download PDFInfo
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- CN101745999A CN101745999A CN200910259922A CN200910259922A CN101745999A CN 101745999 A CN101745999 A CN 101745999A CN 200910259922 A CN200910259922 A CN 200910259922A CN 200910259922 A CN200910259922 A CN 200910259922A CN 101745999 A CN101745999 A CN 101745999A
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- nylon
- powder
- solvent
- waste tire
- cord fabric
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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
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
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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 clean production process for reclaiming nylon 66 from waste tire cords, which belongs to the technical field of harmful solid waste treatment of urban social sources, secondary pollution control and reclamation. The production process is characterized by comprising the following steps: 1) pre-treating the waste tire cords to form short fibers by crushing and screening; 2) mixing the short fibers and a solvent in a weight ratio of 1:5-15, stirring the mixture at the temperature of between 180 and 200 DEG C, and keeping the temperature for 10 to 50 minutes; and 3) cooling and filtering the mixture, and cooling the supernatant to separate out nylon 66 powder, wherein the solvent is one or a mixture of methanol, ethylene glycol, dimethyl sulfoxide and nitro-ethanol. The process creatively adopts a chemical method to reclaim the nylon 66 powder from the waste tire cords, can realize reclamation and utilization of waste tires and avoid secondary pollution brought by the current waste tire reclamation, and can effectively promote the development of nylon powder industry.
Description
Technical field
The invention belongs to the technical field of the harmful solid waste disposal in urban society source and prevention of secondary pollution and resource, be specifically related to a kind of damaged tire cord fabric thread and reclaim nylon 66 powder process for cleanly preparing.
Background technology
China's nylon powder development starts from the sixties in 20th century, is in batch process at present substantially.Along with national defense industry, mechanical industry, electronics industry and developing of automobile industry, to the demand of nylon powder with increasing.Though the most of nylon powder of annual import, kind is few, yield poorly, and far can not satisfy the needs of industry such as growing chemical industry, electronics, machinery, automobile, so market-oriented, the strength of depending on science and technology is developed the nylon powder of many kinds.
Nylon powder generally is to be raw material with pure nylon except that specific use, adopts the preparation of solvent precipitation method.The Yamamoto is dissolved in 2,2 through filial piety with nylon at a certain temperature, 2-trifluoroethanol or be in the solvent of main component with it adds under the normal temperature in whipping process and is insoluble to nylon, but the solvent that mixes fully with trifluoroethanol is (as water, acetone), thus nylon powder is separated out.The shortcoming of this technology is prepared powder diameter distribution very wide (1～250 micron), and grain size is wayward.Village Shan Mao uses 1 instead, and 4-oxygen azo-cycle hexane is a solvent, and nylon 12 powder diameters of preparation are 5～80 microns, and average grain diameter is 32 microns.But 1,4-oxygen azo-cycle hexane solution can corrode skin, and exciting eye and mucous membrane can cause when sucking steam that liver, ephrosis become, and diminish health, thereby its suitability for industrialized production are restricted.Li Kangcheng further utilizes the isopropyl alcohol of moisture mass fraction 20%～50% to be solvent, and nylon 6 powder diameters of preparation are the 2-6 micron, but it is not suitable for coating.People such as Cui Xiulan use diethylene glycol (DEG), diethylene glycol (DEG)-water, ethanol-calcium chloride and ethanol-hydrochloric acid-water mixed liquid solvent to prepare nylon 66, nylon 6, NYLON610, nylon 4 powder respectively.In order to widen the application of nylon powder, many scholars are devoted to the preparation of functionalization nylon powder.Crossing polyalcohol and the derivative thereof that border affair selects mass fraction 1%～8% hydroxyethylcellulose (hydroxyethylcellulose plays anti-cementation in reaction) for use is solvent, making particle diameter is the spherical nylon powder of 3～50nm, is mainly used in the application of cosmetics, lubricant powder.Paddy clear two and virtuous two utilize the water of sodium chloride-containing, aluminum sulfate, acetate brill, calcium chloride or potassium chloride or ethanol to be solvent makes powder with low water absorption (as nylon 12 etc.) safely.Plant a people greatly and utilize calcium nitrate-ethanol to be solvent, make porous nylon 6 powder, this powder can be used as absorbent to reduce the impurity polyphenol content in the beer.Surplus beautiful people such as grade also develops porous nylon powder, earlier inorganic salts is dissolved in the lower alcohol, then nylon is continued the backflow stirring and dissolving.After treating that nylon dissolves fully, under high-speed stirred, drip alcohol excess-water mixed solvent, nylon crystalline deposit from solution is come out, filter with Buchner funnel, again with 40～50 warm water washings, in case of necessity with the acetone washing, wet-milling in 60-80 ℃ of hot blast dry 2-3 hour, remove redundant moisture and alcohol, make dry porous polyamide powder.Ding Shuzhen, Li Yunfei are added to nylon 6 waste silks and a certain proportion of alcoholic solution in the autoclave heated sealed for reducing environmental pollution, make nylon 6 waste silks be dissolved into saturated alcohols solution, be cooled to 70～80 ℃, nylon 6 powder precipitation are separated out, the dry powder particle diameter that obtains is 53～75 microns.Isolated alcoholic solution can replenish fresh alcoholic solution to be continued to use, and washing lotion can recycle through distillation.
The preparation method of nylon powder has 3 kinds usually, be direct polymerization, mechanical crushing method and chemical method, directly polymerization generally is the method acquisition nylon powder of application class like precipitation polymerization, emulsion polymerisation, suspension polymerisation now, the nylon powder almost spherical that this method obtains, powder generally exists with micron order, and particle diameter is less, can adapt to specific (special) requirements, but the technological requirement strictness is difficult to large-scale industrial production.Reported in recent years in addition that utilizing polyamide and water-soluble polymer to carry out melt blending was distributed in the water-soluble polymer nylon resin, obtained spherical particle, then water-soluble polymer water dissolving was finally obtained nylon powder.The nylon powder that this method obtains is that spherical powder is better mobile substantially.But can only make product than small particle diameter with this method, and the aqueous solution recycling that is dissolved with water soluble polymer is difficult, be in other auxiliary agent in the polyamide and be distributed in the water-soluble polymer easily and go and the ratio of wayward other auxiliary agent and polyamide, thereby limited its range of application.
At present, about 1,000,000 tons of the annual in the world reinforcing material that is used for tire production, tire cord is a key factor of determining tyre performance.In China, tire cord market Fypro cord fabric thread still accounts for more than 70%, and domestic owing to rapid economic development and current situation of traffic, and the Fypro cord fabric thread will be occupied an leading position in the long term.Along with the development of Domestic Automotive Industry, damaged tire quantity sharply increases, and a large amount of useless cord fabric thread that thereupon produces uses or landfill through simple the pulverizing as filler usually, not only causes the serious waste of resource, and forms secondary pollution.Damaged tire Fypro cord fabric thread main component is a nylon 66, and nylon 66 powder are mainly used in production plastic-blasting coating, aspects such as ferrite magnetic material.
Summary of the invention
The invention provides a kind of method that from the damaged tire cord fabric thread, reclaims nylon 66 powder, not only can make damaged tire fully realize the secondary pollution that resource recycles, avoids present damaged tire recovery to bring, more can effectively drive the development of nylon powder industry.The employing chemical method of novelty of the present invention reclaims nylon 66 powder from the damaged tire cord fabric thread, still do not have report at home and abroad.
The following technical scheme of the concrete employing of the present invention:
A kind of damaged tire cord fabric thread reclaims nylon 66 powder process for cleanly preparing, it is characterized in that, comprises the steps:
1) waste and old cord fabric thread is a short fiber through pulverizing, screening preliminary treatment, and its length is generally 1-5mm;
2) short fiber and solvent are mixed stirring under temperature is 180～200 ℃, constant temperature 10～50 minutes according to weight ratio 1: 5～15;
3) nylon 66 powder are separated out in cooling, the upper strata stillness of night cooling of filtration back;
Described solvent is a kind of in methyl alcohol, ethylene glycol, dimethyl sulfoxide (DMSO), the nitroethyl alcohol or its mixture arbitrarily.
The average grain diameter that makes nylon 66 powder is 70～130 μ m.
Principle of the present invention be select certain solvent (nylon in this solvent under the high temperature dissolubility good, and almost insoluble at low temperatures), under high temperature, make the nylon dissolving, high degree of agitation, cooling obtain Powdered precipitation.This legal system is equipped with the nylon powder construction equipment that only need routinize, and production process is easy to control, the recyclable utilization of solvent; And can select different solvents according to different requirements, prepare the nylon powder of different grain size scope, different structure performance, gained powder particle shape subglobular, narrow particle size distribution, resin etc. do not have degraded substantially.Solvent for use is methyl alcohol, ethylene glycol, dimethyl sulfoxide (DMSO), nitroethyl alcohol and their mixture etc. preferably.
Compared with prior art, the beneficial effect that the present invention had is:
It is feedstock production nylon 66 powder that the present invention selects useless cord fabric thread for use, compares with existing nylon powder manufacturing process, and raw material sources are extensive, and are cheap, and cost is the 1/4-1/3 of existing technology; Effectively solve simultaneously damaged tire and handled the secondary pollution problem of being brought.
The specific embodiment
Embodiment 1
Waste and old cord fabric thread becomes the short fiber that length is 1-5mm after pulverizing, sieving preliminary treatment, contain scrap rubber 10%-13%.Handling back fiber and methyl alcohol weight ratio is 1: 5, and reaction temperature is 180 ℃, and constant temperature is 20 minutes under the stirring.Nylon powder is separated out in cooling, the upper strata stillness of night cooling of filtration back, and average grain diameter is 75 μ m.
Embodiment 2
Waste and old cord fabric thread becomes the short fiber that length is 1-5mm after pulverizing, sieving preliminary treatment, contain scrap rubber 10%-13%.Handling back fiber and ethanol weight ratio is 1: 8, and reaction temperature is 190 ℃, and constant temperature is 30 minutes under the stirring.Nylon powder is separated out in cooling, the upper strata stillness of night cooling of filtration back, and average grain diameter is 95 μ m.
Embodiment 3
Waste and old cord fabric thread becomes the short fiber that length is 1-5mm after pulverizing, sieving preliminary treatment, contain scrap rubber 10%-13%.Handling back fiber and ethylene glycol weight ratio is 1: 12, and reaction temperature is 180 ℃, and constant temperature is 20 minutes under the stirring.Nylon powder is separated out in cooling, the upper strata stillness of night cooling of filtration back, and average grain diameter is 125 μ m.
Embodiment 4
Waste and old cord fabric thread becomes the short fiber that length is 1-5mm after pulverizing, sieving preliminary treatment, contain scrap rubber 10%-13%.Handling back fiber and diethylene glycol weight ratio is 1: 12, and reaction temperature is 220 ℃, and constant temperature is 35 minutes under the stirring.Nylon powder is separated out in cooling, the upper strata stillness of night cooling of filtration back, and average grain diameter is 100 μ m.
Embodiment 5
Waste and old cord fabric thread becomes the short fiber that length is 1-5mm after pulverizing, sieving preliminary treatment, contain scrap rubber 10%-13%.Handling back fiber and mixed alcohol volume ratio is 1: 10, and mixed alcohol consists of methyl alcohol and the ethanol volume ratio is 1: 1, and reaction temperature is 190 ℃, and constant temperature is 20 minutes under the stirring.Nylon powder is separated out in cooling, the upper strata stillness of night cooling of filtration back, and average grain diameter is 85 μ m.
Claims (3)
1. a damaged tire cord fabric thread reclaims nylon 66 powder process for cleanly preparing, it is characterized in that, comprises the steps:
1) waste and old cord fabric thread is a short fiber through pulverizing, screening preliminary treatment;
2) short fiber and solvent are mixed stirring under temperature is 180～200 ℃, constant temperature 10～50 minutes according to weight ratio 1: 5～15;
3) nylon 66 powder are separated out in cooling, the upper strata stillness of night cooling of filtration back;
Described solvent is a kind of in methyl alcohol, ethylene glycol, dimethyl sulfoxide (DMSO), the nitroethyl alcohol or its mixture arbitrarily.
2. damaged tire cord fabric thread according to claim 1 reclaims nylon 66 powder process for cleanly preparing, it is characterized in that the average grain diameter that makes nylon 66 powder is 70～130 μ m.
3. damaged tire cord fabric thread according to claim 1 reclaims nylon 66 powder process for cleanly preparing, it is characterized in that described staple length is 1-5mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910259922A CN101745999A (en) | 2009-12-23 | 2009-12-23 | Clean production process for reclaiming nylon 66 from waste tire cords |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910259922A CN101745999A (en) | 2009-12-23 | 2009-12-23 | Clean production process for reclaiming nylon 66 from waste tire cords |
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| Publication Number | Publication Date |
|---|---|
| CN101745999A true CN101745999A (en) | 2010-06-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910259922A Pending CN101745999A (en) | 2009-12-23 | 2009-12-23 | Clean production process for reclaiming nylon 66 from waste tire cords |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642065A (en) * | 2013-12-10 | 2014-03-19 | 江南大学 | Process of regenerating nylon 6 and nylon 66 from waste carpet by selective dissolving-precipitating method |
| CN105566894A (en) * | 2014-10-15 | 2016-05-11 | 中国石油化工股份有限公司 | Method for using recycled nylon for preparation of polyamide powder |
| CN105713229A (en) * | 2016-03-31 | 2016-06-29 | 武汉纺织大学 | Method for separating nylon 66 and nylon 6 in polyamide thermal barrier strips |
| CN115197468A (en) * | 2022-03-21 | 2022-10-18 | 福建华峰新材料有限公司 | Process for extracting chinlon from waste blended fabric by using selective solvent and product |
-
2009
- 2009-12-23 CN CN200910259922A patent/CN101745999A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642065A (en) * | 2013-12-10 | 2014-03-19 | 江南大学 | Process of regenerating nylon 6 and nylon 66 from waste carpet by selective dissolving-precipitating method |
| CN105566894A (en) * | 2014-10-15 | 2016-05-11 | 中国石油化工股份有限公司 | Method for using recycled nylon for preparation of polyamide powder |
| CN105566894B (en) * | 2014-10-15 | 2018-01-23 | 中国石油化工股份有限公司 | A kind of method for reclaiming nylon and preparing polyamide powder |
| CN105713229A (en) * | 2016-03-31 | 2016-06-29 | 武汉纺织大学 | Method for separating nylon 66 and nylon 6 in polyamide thermal barrier strips |
| CN105713229B (en) * | 2016-03-31 | 2018-08-14 | 武汉纺织大学 | A kind of method of nylon66 fiber and nylon 6 in separation polyamide thermal barrier strip |
| CN115197468A (en) * | 2022-03-21 | 2022-10-18 | 福建华峰新材料有限公司 | Process for extracting chinlon from waste blended fabric by using selective solvent and product |
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| C06 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Yin Jinhua Inventor after: Du Lei Inventor after: Li Zhaoshun Inventor after: Chen Xuexi Inventor before: Yin Jinhua Inventor before: Du Lei Inventor before: Chen Xuexi |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: YIN JINHUA DU LEI CHEN XUEXI TO: YIN JINHUA DU LEI LI ZHAOSHUN CHEN XUEXI |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Open date: 20100623 |