CN101311390A - Production process of bamboo charcoal polyester fibres - Google Patents

Production process of bamboo charcoal polyester fibres Download PDF

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Publication number
CN101311390A
CN101311390A CNA200810062457XA CN200810062457A CN101311390A CN 101311390 A CN101311390 A CN 101311390A CN A200810062457X A CNA200810062457X A CN A200810062457XA CN 200810062457 A CN200810062457 A CN 200810062457A CN 101311390 A CN101311390 A CN 101311390A
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CN
China
Prior art keywords
bamboo charcoal
polyester
suspension
finishes
ethylene glycol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CNA200810062457XA
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Chinese (zh)
Inventor
王国德
崔恒海
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Hengyi Group Co., Ltd.
Zhejiang Hengyi Petrochemical Co., Ltd.
Zhejiang Hengyi Polymer Co., Ltd.
Original Assignee
ZHEJIANG HENGYI GROUP CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by ZHEJIANG HENGYI GROUP CO Ltd filed Critical ZHEJIANG HENGYI GROUP CO Ltd
Priority to CNA200810062457XA priority Critical patent/CN101311390A/en
Publication of CN101311390A publication Critical patent/CN101311390A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for producing bamboo charcoal polyester fiber. The technical problem which the method needs to solve is spreading the bamboo charcoal evenly in the polyester with a good performance of the fiber and a simple process. The method includes the steps of spreading super fine bamboo charcoal powders with particle diameters of 0.3 to 0.8 Mum into glycol solution to prepare bamboo charcoal/glycol suspension, adding the suspension in the production process of polyester to produce the polyester containing the superfine bamboo charcoal powder and producing the bamboo charcoal polyester fiber with a content of the super fine bamboo charcoal powder of 0.5 to 3 percent by the melt-spinning.

Description

A kind of production method of bamboo charcoal polyester fiber
Technical field
The invention belongs to chemical fiber field, specifically is a kind of production method of bamboo charcoal polyester fiber.
Background technology
Bamboo charcoal is that raw material forms through high-temperature firing with the mao bamboon.Its maximum feature is that molecular structure is hexagon, and quality is hard, fine and closely woven porous, the specific area of bamboo charcoal is big, has very strong absorption property, and bamboo charcoal contains abundant mineral matter simultaneously, can produce anion, releasing far infrared, also have the effect of conducting electricity and intercepting electromagenetic wave radiation.
Bamboo charcoal polyester fiber is to be the functional polyalkylene ester fiber that functional additive is made with super Fine bamboo charcoal powder, is a kind of release anion that has, emitting far-infrared outside, the health care fiber of antibiotic, adsorption function.
Chinese patent CN1807714 " bamboo-carbon fibre and preparation method thereof ", CN1939983 " a kind of functional bamboo-carbon powder process and use in synthetic fiber ", CN1590051 " a kind of processing method of bamboo charcoal superfine powder and the application in synthetic fiber thereof " have related to the production method of bamboo charcoal polyester fiber, method is: adopt ultra-fine bamboo-carbon powder, mix the back melt pelletization with synthetic fiber material (polyester), make the master batch that contains the high concentration bamboo charcoal powder, then bamboo charcoal master batch and synthetic fiber material (polyester) blend melt spinning production bamboo charcoal polyester fiber.There is following defective in this method: this technology is difficult to guarantee that bamboo-carbon powder is uniformly dispersed fully in fiber, causes the performance of fiber inhomogeneous; This technology melt spinnability is poor, difficulty in spinning; The Granulation Equipments that this arts demand is special, the production process complexity.
Summary of the invention
The technical issues that need to address of the present invention are at the deficiencies in the prior art, provide a kind of bamboo charcoal to be uniformly dispersed in polyester, spinning properties is good, the production method of the simple bamboo charcoal polyester fiber of production technology.
The production method of bamboo charcoal polyester fiber of the present invention, it is characterized in that, earlier grain through being that the ultra-fine bamboo charcoal powder of 0.3~0.8 μ m is dispersed in and makes bamboo charcoal/ethylene glycol (EG) suspension in the ethylene glycol solution, add above-mentioned suspension and directly produce the polyester that contains ultra-fine bamboo charcoal powder in polyester production process, to produce ultra-fine bamboo charcoal powder content be 0.5~3% bamboo charcoal polyester fiber to melt spinning again.
The preparation of above-mentioned bamboo charcoal/glycolic suspension: add ethylene glycol in material-compound tank, under agitation add ultra-fine bamboo charcoal powder and be made into slurries, pass through ball mill grinding then, be dispersed into uniform suspension, bamboo charcoal content is 10~40% in bamboo charcoal/glycolic suspension.
The grain of ultra-fine bamboo charcoal powder is through meticulous, and the manufacturing cost of bamboo-carbon powder increases; Grain is through big, and the polyester filament spinning component switching cycle that then contains bamboo charcoal is fast, is unfavorable for spinning, so the best grain of ultra-fine bamboo charcoal powder of the present invention is through being 0.3~0.8 μ m.When bamboo charcoal content in bamboo charcoal/glycolic suspension is low, need to consume a large amount of EG, the grinding effect of ball mill descends simultaneously; During the bamboo charcoal too high levels, then the stability decreases of bamboo charcoal suspension when esterification finishes the back interpolation, is unfavorable for that bamboo charcoal is uniformly dispersed, so bamboo charcoal content is 10~40% in bamboo charcoal/glycolic suspension of the present invention simultaneously in polyester.
The preparation of bamboo charcoal polyester can be adopted the device and the route of any production of polyester in the prior art.Can adopt DMT (dimethyl terephthalate (DMT)) route or PTA (terephthalic acid (TPA)) route; Can be batchwise polymerization flow process or continuous polymerization flow process.Polyester can be PET (poly terephthalic acid binaryglycol ester), PBT (poly terephthalic acid dibutylene glycol ester, PTT (poly terephthalic acid dipropylene glycol ester) or modified poly ester.
Bamboo charcoal/glycolic suspension can add in the preparation of raw material stage of polyester production process; Perhaps after esterification or ester exchange reaction end, join in the reaction system.
If adopt the PTA process route: then
(1) bamboo charcoal/glycolic suspension in the production process of the preparation of raw material stage of polyester production process adding is:
PTA, ethylene glycol, catalyst, stabilizing agent are added the preparation of raw material still by conventional production process of the prior art, bamboo charcoal suspension together adds and stirs, move into the esterifying kettle esterification then, esterification finishes the back and moves into polymeric kettle, esterification and polymerization are undertaken by conventional production process of the prior art, and it is the polyester that contains bamboo charcoal that polymerization finishes the back product.
(2) bamboo charcoal/glycolic suspension finishes the back adding in the esterification of polyester production process, and production process is:
PTA, ethylene glycol, catalyst, stabilizing agent are added the making beating still by the production technology of prior art, after stirring, move into the production technology esterification of esterifying kettle by prior art; Esterification finishes the back and moves into polymeric kettle, adds bamboo charcoal/glycolic suspension then, fully dispersed with stirring, and be warmed up to polymeric reaction temperature, carry out polymerisation by the production technology of prior art then, it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning.
If adopt the DMT process route, then
1) bamboo charcoal/glycolic suspension in the concrete steps of the preparation of raw material stage of polyester production process adding is: by the prior art production technology, DMT, ethylene glycol are joined in the ester interchange vessel after the heating in DMT molten-bath, ethylene glycol still preheater respectively, add catalyst; Join in the ester interchange vessel after bamboo charcoal/glycolic suspension also is preheating to the temperature identical with preheating ethylene glycol earlier simultaneously; Carry out ester exchange reaction after stirring, ester exchange finishes back immigration polymeric kettle and carries out polymerization, and it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning;
Perhaps, 2) concrete steps of bamboo charcoal/glycolic suspension adding after the ester exchange reaction of polyester production process finishes are: by the prior art production technology, DMT, ethylene glycol are joined in the ester interchange vessel after the heating in DMT molten-bath, ethylene glycol still preheater respectively, add catalyst, carry out ester exchange reaction after stirring; Ester exchange finishes the back and moves into polymeric kettle, adds bamboo charcoal/glycolic suspension then, fully dispersed with stirring, and be warmed up to polymeric reaction temperature, carry out polymerisation by conventional production process of the prior art then, it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning.
The section of bamboo charcoal polyester or melt are transported to spinning equipment through melt pipe and carry out spinning, and the POY preliminary draft silk of spinning is produced bamboo charcoal behind the bullet and added stretch filament (DTY) or obtain draw textured yarn (DTY) DT through drawing-off through adding; Perhaps, bamboo charcoal polyester slice or melt are directly produced bamboo charcoal drafting (FDY) through the FDY device.
The thickness of finished fiber is 50D~300D, and the radical of finished fiber is from 36~144.
The production method of bamboo charcoal polyester fiber of the present invention has advantages such as bamboo charcoal is uniformly dispersed, spinning properties is good, production technology is simple in polyester.
The specific embodiment:
The present invention will be described below by specific embodiment.
Example 1
The preparation of 30% bamboo charcoal/glycolic suspension: add ethylene glycol 35kg in material-compound tank, under agitation add ultra-fine bamboo-carbon powder 15kg, dispersed with stirring was made into slurries in 3 hours, passed through ball mill grinding then 30 minutes, was dispersed into uniform suspension.
The preparation of 2% bamboo charcoal polyester---adopt the PTA process route, bamboo charcoal/glycolic suspension added in the preparation of raw material stage: terephthalic acid (TPA) (PTA) 200kg, ethylene glycol (EG) 95kg, The catalytic antimony trioxide 65g, stabilizing agent trimethyl phosphate 25g are together added the making beating still, add the above-mentioned suspension that contains bamboo charcoal 30% in making beating simultaneously in the still, make that bamboo charcoal content is 2% in the polyester.Move into esterifying kettle after stirring, by conventional production process esterification of the prior art, esterification finishes back immigration polymeric kettle, carries out polymerization by conventional production process of the prior art, and polymerization finishes the polyester slice that the back pelletizing obtains containing 2% bamboo charcoal.
The preparation of fiber: the bamboo charcoal polyester slice is joined after super-dry in the spinning equipment, 288~292 ℃ of spinning temperatures, spinning speed 3000m/min obtains preliminary draft silk POY, is reprocessed into DTY, obtains containing the bamboo charcoal polyester fiber of bamboo charcoal 2%.Fiber dimensious 150dtex/72f, fibre strength 3.0CN/dtex, extension at break 15%.Pressure did not have obviously rising in 48 hours before the spinning filter, and spinning process is normal.
Example 2
The preparation of 25% bamboo charcoal/EG suspension: add ethylene glycol 37.5kg in material-compound tank, under agitation add ultra-fine bamboo-carbon powder 12.5kg, dispersed with stirring was made into slurries in 3 hours, passed through ball mill grinding then 30 minutes, was dispersed into uniform suspension.
The preparation of 1% bamboo charcoal polyester---adopt the PTA process route, bamboo charcoal/glycolic suspension finishes the back in esterification and adds: with terephthalic acid (TPA) (PTA) 200kg, ethylene glycol (EG) 95kg, The catalytic antimony trioxide 65g, stabilizing agent trimethyl phosphate 25g together adds the making beating still, back immigration esterifying kettle stirs, by conventional production process esterification of the prior art, esterification finishes the back and moves into polymeric kettle, add the above-mentioned suspension that contains bamboo charcoal 25%, make that bamboo charcoal content is 1% in the polyester, dispersed with stirring 30 minutes, and be warmed up to 260 ℃, carry out polymerization by conventional production process of the prior art then, polymerization finishes the polyester slice that the back pelletizing obtains containing 1% bamboo charcoal.
The preparation of fiber: the bamboo charcoal polyester slice is joined after super-dry in the FDY equipment, 288~292 ℃ of spinning temperatures, spinning speed 3500m/min obtains containing the bamboo charcoal FDY fiber of bamboo charcoal 1%.Fiber dimensious 150dtex/72f, fibre strength 3.1CN/dtex, extension at break 12%.Pressure did not have obviously rising in 48 hours before the spinning filter, and spinning is normal.
Example 3: adopt the preparation of DMT technology bamboo charcoal polyester fiber
The preparation of 25% bamboo charcoal/EG suspension: with example 2.
The preparation of 1% bamboo charcoal polyester: with DMT 200kg, EG 150kg is respectively at the DMT molten-bath, be heated to 150 ℃ in the EG still preheater, add manganese acetate 65g then, the back intensification stirs, carry out ester exchange reaction, ester exchange finishes the back and moves into polymeric kettle, add The catalytic antimony trioxide 65g, stabilizing agent trimethyl phosphate 25g, add the above-mentioned suspension that contains bamboo charcoal 25%, make that bamboo charcoal content is 1% in the polyester, dispersed with stirring 30 minutes, and be warmed up to 260 ℃, and carry out polymerization by conventional production process of the prior art then, polymerization finishes the polyester slice that the back pelletizing obtains containing 1% bamboo charcoal.
The preparation of fiber: with reference to example 2, spinning bamboo charcoal FDY fiber.Fiber dimensious 75dtex/72f, fibre strength 3.06CN/dtex, extension at break 13%.Pressure did not have obviously rising in 48 hours before the spinning filter, and spinning is normal.
Comparative Examples 1:
The preparation of 50% bamboo charcoal/EG suspension: add ethylene glycol 25kg in material-compound tank, under agitation add ultra-fine bamboo-carbon powder 25kg, dispersed with stirring was made into slurries in 3 hours, passed through ball mill grinding then 30 minutes, was dispersed into uniform suspension.
The preparation of 1% bamboo charcoal polyester: terephthalic acid (TPA) (PTA) 200kg, ethylene glycol (EG) 95kg The catalytic antimony trioxide 65g, stabilizing agent trimethyl phosphate 25g are together added the making beating still, the esterification of back immigration esterifying kettle stirs, esterification finishes the back and moves into polymeric kettle, add the above-mentioned suspension that contains bamboo charcoal 50%, make that bamboo charcoal content is 1% in the polyester, dispersed with stirring 30 minutes, and be warmed up to 260 ℃, carry out polymerization by conventional production process of the prior art then, polymerization finishes the polyester that the back pelletizing obtains containing 1% bamboo charcoal.
The preparation of fiber: the bamboo charcoal polyester slice is joined after super-dry in the spinning equipment, 288~292 ℃ of spinning temperatures, spinning speed 3000m/min is involved silk in advance, is reprocessed into DTY, obtains containing the bamboo charcoal polyester fiber of bamboo charcoal 1%.Fiber dimensious 150dtex/72f, fibre strength 3.3CN/dtex, extension at break 21.5%.Pressure obviously rose in 20 hours before the spinning filter, and a phenomenon of wafing is arranged in the spinning process.

Claims (7)

1, a kind of production method of bamboo charcoal polyester fiber, it is characterized in that, earlier grain through being that the ultra-fine bamboo charcoal powder of 0.3~0.8 μ m is dispersed in and makes bamboo charcoal/glycolic suspension in the ethylene glycol solution, add above-mentioned suspension and directly produce the polyester that contains ultra-fine bamboo charcoal powder in polyester production process, to produce ultra-fine bamboo charcoal powder content be 0.5~3% bamboo charcoal polyester fiber to melt spinning again.
2, the production method of bamboo charcoal polyester fiber according to claim 1, it is characterized in that, the preparation of described bamboo charcoal/glycolic suspension: in material-compound tank, add ethylene glycol, under agitation add ultra-fine bamboo charcoal powder and be made into slurries, pass through ball mill grinding then, be dispersed into uniform suspension, bamboo charcoal content is 10~40% in bamboo charcoal/glycolic suspension.
3, the production method of bamboo charcoal polyester fiber according to claim 1 and 2 is characterized in that, bamboo charcoal/glycolic suspension can add in the preparation of raw material stage of polyester production process; Perhaps after esterification or ester exchange reaction end, join in the reaction system.
4, the production method of bamboo charcoal polyester fiber according to claim 3 is characterized in that, for the PTA process route,
1) bamboo charcoal/glycolic suspension in the concrete steps of the preparation of raw material stage of polyester production process adding is: by the technology of prior art, PTA, ethylene glycol, catalyst, stabilizing agent are added the making beating still, bamboo charcoal suspension together adds and stirs, move into the esterifying kettle esterification then, esterification finishes back immigration polymeric kettle and carries out polymerisation, it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning;
Perhaps, 2) concrete steps of bamboo charcoal/glycolic suspension adding after the esterification of polyester production process finishes are: PTA, ethylene glycol, catalyst, stabilizing agent are added the making beating still by the production technology of prior art, after stirring, move into the production technology esterification of esterifying kettle by prior art; Esterification finishes the back and moves into polymeric kettle, adds bamboo charcoal/glycolic suspension then, fully dispersed with stirring, and be warmed up to polymeric reaction temperature, carry out polymerisation by the production technology of prior art then, it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning.
5, the production method of bamboo charcoal polyester fiber according to claim 3 is characterized in that, for the DMT process route,
1) bamboo charcoal/glycolic suspension in the concrete steps of the preparation of raw material stage of polyester production process adding is: by the prior art production technology, DMT, ethylene glycol are joined in the ester interchange vessel after the heating in DMT molten-bath, ethylene glycol still preheater respectively, add catalyst; Join in the ester interchange vessel after bamboo charcoal/glycolic suspension also is preheating to the temperature identical with preheating ethylene glycol earlier simultaneously; Carry out ester exchange reaction after stirring, ester exchange finishes back immigration polymeric kettle and carries out polymerization, and it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning;
Perhaps, 2) concrete steps of bamboo charcoal/glycolic suspension adding after the ester exchange reaction of polyester production process finishes are: by the prior art production technology, DMT, ethylene glycol are joined in the ester interchange vessel after the heating in DMT molten-bath, ethylene glycol still preheater respectively, add catalyst, carry out ester exchange reaction after stirring; Ester exchange finishes the back and moves into polymeric kettle, adds bamboo charcoal/glycolic suspension then, fully dispersed with stirring, and be warmed up to polymeric reaction temperature, carry out polymerisation by conventional production process of the prior art then, it is the polyester that contains bamboo charcoal that polymerization finishes the back product, gets product through melt spinning.
6, the production method of bamboo charcoal polyester fiber according to claim 4 is characterized in that bamboo charcoal polyester slice or melt can be processed into preliminary draft silk POY earlier, adds bullet again and produces and add elater DTY or drawing-off obtains draw textured yarn (DTY) DT; Perhaps, bamboo charcoal polyester slice or melt are directly produced bamboo charcoal drafting FDY with the FDY device.
7, the production method of bamboo charcoal polyester fiber according to claim 5 is characterized in that bamboo charcoal polyester slice or melt can be processed into preliminary draft silk POY earlier, adds bullet again and produces and add elater DTY or drawing-off obtains draw textured yarn (DTY) DT; Perhaps, bamboo charcoal polyester slice or melt are directly produced bamboo charcoal drafting FDY with the FDY device.
CNA200810062457XA 2008-06-11 2008-06-11 Production process of bamboo charcoal polyester fibres Pending CN101311390A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857981A (en) * 2010-04-20 2010-10-13 安徽省和胜新材料科技有限公司 Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group
CN101921428A (en) * 2010-08-17 2010-12-22 丁宏广 Monofilament applied to bamboo charcoal air strainer and preparation process and application thereof
CN102197892A (en) * 2011-06-29 2011-09-28 常熟市众望经纬编织造有限公司 Mask
CN103014891A (en) * 2012-11-30 2013-04-03 吴江市超维纺织有限公司 Process for producing bamboo charcoal viscose fibers
CN103014908A (en) * 2012-11-30 2013-04-03 吴江市超维纺织有限公司 Process for producing bamboo charcoal polyester composite fibers
CN103243426A (en) * 2013-05-22 2013-08-14 常州新力纤维科技有限公司 High-absorption deodorant drafted twisted polyester filament and production method thereof
TWI458683B (en) * 2014-07-08 2014-11-01 Fengyang Production Co Ltd Sodalite-containing composition and polyester composite
CN105463588A (en) * 2016-01-11 2016-04-06 河南省龙都生物科技有限公司 Bamboo charcoal polylactic acid melt direct spinning technology
CN105504236A (en) * 2016-01-11 2016-04-20 河南省龙都生物科技有限公司 Production process for polylactic acid bamboo charcoal slices
CN105603551A (en) * 2016-01-30 2016-05-25 河南省龙都生物科技有限公司 Production system for bamboo charcoal and polylactic acid chips

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857981A (en) * 2010-04-20 2010-10-13 安徽省和胜新材料科技有限公司 Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group
CN101857981B (en) * 2010-04-20 2012-10-03 安徽省和胜新材料科技有限公司 Process for producing nanometer bamboo carbon fiber by adopting polylactic acid group
CN101921428A (en) * 2010-08-17 2010-12-22 丁宏广 Monofilament applied to bamboo charcoal air strainer and preparation process and application thereof
CN101921428B (en) * 2010-08-17 2012-11-14 浙江金海环境技术股份有限公司 Monofilament applied to bamboo charcoal air strainer and preparation process and application thereof
CN102197892A (en) * 2011-06-29 2011-09-28 常熟市众望经纬编织造有限公司 Mask
CN103014908A (en) * 2012-11-30 2013-04-03 吴江市超维纺织有限公司 Process for producing bamboo charcoal polyester composite fibers
CN103014891A (en) * 2012-11-30 2013-04-03 吴江市超维纺织有限公司 Process for producing bamboo charcoal viscose fibers
CN103243426A (en) * 2013-05-22 2013-08-14 常州新力纤维科技有限公司 High-absorption deodorant drafted twisted polyester filament and production method thereof
TWI458683B (en) * 2014-07-08 2014-11-01 Fengyang Production Co Ltd Sodalite-containing composition and polyester composite
CN105463588A (en) * 2016-01-11 2016-04-06 河南省龙都生物科技有限公司 Bamboo charcoal polylactic acid melt direct spinning technology
CN105504236A (en) * 2016-01-11 2016-04-20 河南省龙都生物科技有限公司 Production process for polylactic acid bamboo charcoal slices
CN105463588B (en) * 2016-01-11 2018-02-16 河南省龙都生物科技有限公司 Bamboo charcoal polylactic acid melt direct spinning
CN105603551A (en) * 2016-01-30 2016-05-25 河南省龙都生物科技有限公司 Production system for bamboo charcoal and polylactic acid chips
CN105603551B (en) * 2016-01-30 2017-11-14 河南省龙都生物科技有限公司 Bamboo charcoal polylactic acid slice manufacturing system

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Effective date of registration: 20081212

Address after: Hangzhou City, Zhejiang province Xiaoshan Yaqian

Applicant after: Zhejiang Hengyi Group Co., Ltd.

Co-applicant after: Zhejiang Hengyi Petrochemical Co., Ltd.

Co-applicant after: Zhejiang Hengyi Polymer Co., Ltd.

Address before: Hangzhou City, Zhejiang province Xiaoshan Yaqian

Applicant before: Zhejiang Hengyi Group Co., Ltd.

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Open date: 20081126