CN109021483A - A kind of AES-PET composite material and preparation method of low VOC - Google Patents

A kind of AES-PET composite material and preparation method of low VOC Download PDF

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Publication number
CN109021483A
CN109021483A CN201810638815.0A CN201810638815A CN109021483A CN 109021483 A CN109021483 A CN 109021483A CN 201810638815 A CN201810638815 A CN 201810638815A CN 109021483 A CN109021483 A CN 109021483A
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parts
aes
pet
temperature
area
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刘凯
徐志海
马建峰
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Anhui Jianghuai Automobile Group Corp
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Anhui Jianghuai Automobile Group Corp
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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
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L51/00Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L51/04Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
    • 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
    • C08J2351/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/04Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to rubbers
    • 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
    • C08J2467/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds

Abstract

The present invention relates to the AES-PET composite material and preparation methods of low VOC a kind of, 80 parts -100 parts of AES, 20 parts of -30 parts of PET, 10 parts of -20 parts of mica powders, 8 parts of -12 parts of POE, 4 parts of -8 parts of VOC is weighed to absorb master batch, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part of -0.5 part of antioxidant and be mixed and stirred for uniformly, obtaining mixture;Obtained mixture is arrived into AES-PET composite material by double screw extruder extruding pelletization.VOC in the application absorbs master batch in extrusion process, by the deionized water and calcium silicate mixture of removing volatile substance through being vaporizated into steam, volatile small molecule in AES-PET composite material can will be discharged by the vacuum in extruder, to achieve the purpose that promote AES-PET composite material VOC performance.

Description

A kind of AES-PET composite material and preparation method of low VOC
Technical field
The invention belongs to technical field of polymer materials, particularly relate to the AES-PET composite material and its system of a kind of low VOC Preparation Method.
Background technique
Since acrylonitrile-ethylene propylene diene rubber-styrene resin (AES) has excellent mechanical property, surface strength height, ruler Very little stabilization, chemical resistance and electrical property are good, processing easy to form, and price is low, are most widely used engineering plastics One of material.And PET has excellent organic solvent-resistant, self-lubrication, is such as able to achieve the two blending and modifying, performance complement has Critically important meaning.
A kind of low VOC AES-PET composite material has been made in the technical program innovation, it has good physical property With VOC performance, this material not yet sees report so far, this has the application of extension AES-PET composite material very heavy The realistic meaning wanted.
Summary of the invention
The object of the present invention is to provide the AES-PET composite material and preparation methods of low VOC a kind of, to improve AES material The performance of material.
The present invention is achieved by the following technical solutions:
A kind of AES-PET composite material of low VOC, composed of the following components by weight:
The mica powder mesh number is -3000 mesh of 2000 mesh, Al2O3Content be 30%-35%.
The toughener is POE.
The VOC absorbs master batch, is grouped as by the group of following parts by weight:
The foaming agent is Barium azodicarboxylate, and the blowing promotor is magnesia, and the antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
The VOC absorbs the preparation method of master batch, comprising the following steps:
(1) 60 parts of -80 parts of PET, 10 parts of -16 parts of Barium azodicarboxylates, 3 parts of -5 parts of magnesia, 0.1 part -0.3 part are weighed Irganox1010 is mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive the expandable pellet of PET;
(3) the expandable pellet of PET that (2) prepare is put into the mixture of excessive deionized water and calcium silicates and is carried out Sufficient physical absorption makes deionized water and the calcium silicates of adsorption saturation in the micropore of the expandable pellet of PET to get VOC suction Receive master batch.
The compatilizer is SEBS-g-MAH.
The antioxidant be three (2,4- di-t-butyl) phenyl-phosphites (, four [β-(3,5- di-t-butyl -4- hydroxy benzenes Base) propionic acid] pentaerythritol ester or 1,3,5- trimethyls -2,4, one of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene Or several mixing.
The preparation method of the low VOC AES-PET composite material of any of the above-described, comprising the following steps:
(1) 80 parts -100 parts of AES, 20 parts of -30 parts of PET, 10 parts of -20 parts of mica powders, 8 parts of -12 parts of POE, 4 part -8 are weighed Part VOC absorbs master batch, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part of -0.5 part of antioxidant and is mixed and stirred for uniformly, being mixed Close material;
(2) mixture obtained in step (1) is passed through into double screw extruder extruding pelletization to get compound to AES-PET Material.
The step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder and squeezed It being granulated out to get to AES-PET composite material, wherein the double screw extruder includes six humidity provinces sequentially arranged, and one 190~210 DEG C of area's temperature, two 230~250 DEG C of area's temperature, three 230~250 DEG C of area's temperature, four 230~250 DEG C of area's temperature, five 230~250 DEG C of area's temperature, six 230~250 DEG C of area's temperature, 230~250 DEG C of head temperature, 200~280r/min of screw speed.
The method have the benefit that:
1, the addition of SEBS-g-MAH improves the compatibility between AES and PET, improves AES-PET composite material Physical property.
2, the VOC in the application absorbs master batch in extrusion process, will remove the deionized water and silicic acid of volatile substance Volatile small molecule in AES-PET composite material can be passed through the vacuum in extruder through being vaporizated into steam by calcium compound It will be discharged, to achieve the purpose that promote AES-PET composite material VOC performance.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in the following embodiment of the application is as follows:
AES (model SK50), Japanese UMG;PET (model 008L), Canadian Aclo;Mica powder, Shijiazhuang horse jump mica Powder factory;POE (model 8150), Dow;SEBS-g-MAH, Suzhou Asia match plasticizing Co., Ltd;Antioxidant (model Irganox168, Irganox1010, Irganox1330), Switzerland's Ciba.
Test equipment used in the following embodiment of the application is as follows:
ZSK30 type double screw extruder, German W&P company;JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou The production of device company;HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd;XCJ-500 type shock-testing Machine, the production of Chengde testing machine factory;QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd;QD-GJS- B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
The application provides the AES-PET composite material of low VOC a kind of, composed of the following components by weight:
The mica powder mesh number is -3000 mesh of 2000 mesh, Al2O3Content be 30%-35%.
The toughener is POE.
The VOC absorbs master batch, is grouped as by the group of following parts by weight:
The foaming agent is Barium azodicarboxylate, and the blowing promotor is magnesia, and the antioxidant is BASF AG Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters (abbreviation Irganox1010).
The VOC absorbs the preparation method of master batch, comprising the following steps:
(1) 60 parts of -80 parts of PET, 10 parts of -16 parts of Barium azodicarboxylates, 3 parts of -5 parts of magnesia, 0.1 part -0.3 part are weighed Irganox1010 is mixed and stirred for uniformly, obtaining mixture;
(2) mixture obtained in step (1) is arrived into the expandable grain of PET by double screw extruder extruding pelletization Material;
(3) the expandable pellet of PET that (2) prepare is put into the mixture of excessive deionized water and calcium silicates and is carried out Sufficient physical absorption makes deionized water and the calcium silicates of adsorption saturation in the micropore of the expandable pellet of PET to get VOC suction Receive master batch.
The double screw extruder includes six humidity provinces, 240~260 DEG C of area's temperature, two area's temperature 280~300 DEG C, three 280~300 DEG C of area's temperature, four 280~300 DEG C of area's temperature, five 280~300 DEG C of area's temperature, six area's temperature 280~300 DEG C, 280~300 DEG C of head temperature, 200~280r/min of screw speed.
The compatilizer is SEBS-g-MAH.
The antioxidant is three (2,4- di-t-butyl) phenyl-phosphites (abbreviation of BASF AG
Irganox168), four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters (abbreviation Irganox1010) or 1,3,5- trimethyls -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene is (referred to as One or more of) Irganox1330 mixing.
The preparation method of the low VOC AES-PET composite material of any of the above-described, comprising the following steps:
(1) 80 parts -100 parts of AES, 20 parts of -30 parts of PET, 10 parts of -20 parts of mica powders, 8 parts of -12 parts of POE, 4 part -8 are weighed Part VOC absorbs master batch, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part of -0.5 part of antioxidant and is mixed and stirred for uniformly, being mixed Close material;
(2) mixture obtained in step (1) is passed through into double screw extruder extruding pelletization to get compound to AES-PET Material.
The step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder and squeezed It being granulated out to get to AES-PET composite material, wherein the double screw extruder includes six humidity provinces sequentially arranged, and one 190~210 DEG C of area's temperature, two 230~250 DEG C of area's temperature, three 230~250 DEG C of area's temperature, four 230~250 DEG C of area's temperature, five 230~250 DEG C of area's temperature, six 230~250 DEG C of area's temperature, 230~250 DEG C of head temperature, 200~280r/min of screw speed.
Embodiment 1
(1) it weighs 80 parts of AES, 20 parts of PET, 10 parts of mica powders, 8 parts of part POE, 4 parts of VOC and absorbs master batches, 0.1 part SEBS-g-MAH, 0.1 part of Irganox168 are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 190 DEG C of area's temperature, two 230 DEG C of area's temperature, Three 230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 230 DEG C of area's temperature, 230 DEG C of head temperature, screw rod turns Fast 200r/min.
Embodiment 2
(1) it weighs 100 parts of AES, 30 parts of PET, 20 parts of mica powders, 12 parts of POE, 8 parts of VOC and absorbs master batches, 0.3 part SEBS-g-MAH, 0.1 part of Irganox168,0.2 part of Irganox1010,0.2 part of Irganox1330 are mixed and stirred for uniformly, obtaining To mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 210 DEG C of area's temperature, two 250 DEG C of area's temperature, Three 250 DEG C of area's temperature, four 250 DEG C of area's temperature, five 250 DEG C of area's temperature, six 250 DEG C of area's temperature, 250 DEG C of head temperature, screw rod turns Fast 280r/min.
Embodiment 3
(1) 90 parts of AES, 25 parts of PET, 15 parts of mica powders, 10 parts of POE, 6 parts of VOC absorption master batches, 0.2 part of SEBS- are weighed G-MAH, 0.1 part of Irganox168,0.2 part of Irganox1010 are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 200 DEG C of area's temperature, two 240 DEG C of area's temperature, Three 240 DEG C of area's temperature, four 240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 240 DEG C of area's temperature, 240 DEG C of head temperature, screw rod turns Fast 240r/min.
Embodiment 4
(1) 85 parts of AES, 24 parts of PET, 14 parts of mica powders, 8 parts of POE, 8 parts of VOC absorption master batches, 0.1 part of SEBS- are weighed G-MAH, 0.1 part of Irganox1010,0.2 part of Irganox1330 are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material P4.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 195 DEG C of area's temperature, two 235 DEG C of area's temperature, Three 235 DEG C of area's temperature, four 235 DEG C of area's temperature, five 235 DEG C of area's temperature, six 235 DEG C of area's temperature, 235 DEG C of head temperature, screw rod turns Fast 225r/min.
Embodiment 5
(1) it weighs 95 parts of AES, 28 parts of PET, 18 parts of mica powders, 12 parts of POE, 4 parts of VOC and absorbs master batches, 0.3 part SEBS-g-MAH, 0.1 part of Irganox1010,0.1 part of Irganox168 are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material P5.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 195 DEG C of area's temperature, two 245 DEG C of area's temperature, Three 245 DEG C of area's temperature, four 245 DEG C of area's temperature, five 245 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, screw rod turns Fast 245r/min.
Comparative example 1
(1) 80 parts of AES, 20 parts of PET, 16 parts of mica powders, 12 parts of POE, 0.1 part of Irganox1010,0.2 part are weighed Irganox168 is mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES-PET composite material D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 195 DEG C of area's temperature, two 245 DEG C of area's temperature, Three 245 DEG C of area's temperature, four 245 DEG C of area's temperature, five 245 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, screw rod turns Fast 245r/min.
Performance test:
Batten test is made with injection molding machine in AES-PET composite material prepared by above-described embodiment 1-5 and comparative example 1, is surveyed Examination data are as follows:
It can also be seen that physical property, the VOC performance of embodiment 1-5 will be better than comparative example 1 from table.This is for extension The application field of AES-PET composite material, has very important significance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And deformation, the scope of the present invention are extremely equally limited by appended claims.

Claims (9)

1. a kind of AES-PET composite material of low VOC, which is characterized in that composed of the following components by weight:
2. the AES-PET composite material of low VOC according to claim 1, which is characterized in that the mica powder mesh number is - 3000 mesh of 2000 mesh, Al2O3Content be 30%-35%.
3. the AES-PET composite material of low VOC according to claim 1, which is characterized in that the toughener is POE.
4. the AES-PET composite material of low VOC according to claim 1, which is characterized in that the VOC absorbs master batch, by The group of following parts by weight is grouped as:
The foaming agent is Barium azodicarboxylate, and the blowing promotor is magnesia, and the antioxidant is four [β-(3,5- bis- uncles Butyl -4- hydroxy phenyl) propionic acid] pentaerythritol ester.
5. the AES-PET composite material of low VOC according to claim 4, which is characterized in that the VOC absorbs master batch Preparation method, comprising the following steps:
(1) 60 parts of -80 parts of PET, 10 parts of -16 parts of Barium azodicarboxylates, 3 parts of -5 parts of magnesia, 0.1 part -0.3 part are weighed Irganox1010 is mixed and stirred for uniformly, obtaining mixture;
(2) by mixture extruding pelletization obtained in step (1) to get arrive the expandable pellet of PET;
(3) the expandable pellet of PET that (2) prepare is put into the mixture of excessive deionized water and calcium silicates and is carried out sufficiently Physical absorption, absorb deionized water and the calcium silicates of adsorption saturation in the micropore of the expandable pellet of PET to get VOC female Grain.
6. the AES-PET composite material of low VOC according to claim 4, which is characterized in that the compatilizer is SEBS- g-MAH。
7. the AES-PET composite material of low VOC according to claim 4, which is characterized in that the antioxidant be three (2, 4- di-t-butyl) phenyl-phosphite (, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 1,3,5- Trimethyl -2,4, the mixing of one or more of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene.
8. the preparation method of the low VOC AES-PET composite material of any one of the claims 1 to 7, which is characterized in that including Following steps:
(1) 80 parts -100 parts of AES, 20 parts of -30 parts of PET, 10 parts of -20 parts of mica powders, 8 parts of -12 parts of POE, 4 parts -8 parts are weighed VOC absorbs master batch, 0.1 part -0.3 part of SEBS-g-MAH, 0.1 part of -0.5 part of antioxidant and is mixed and stirred for uniformly, being mixed Material;
(2) mixture obtained in step (1) is arrived into AES-PET composite material by double screw extruder extruding pelletization.
9. the preparation method of low VOC AES-PET composite material according to claim 8, which is characterized in that the step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder extruding pelletization to get arriving AES-PET composite material, wherein the double screw extruder includes six humidity provinces sequentially arranged, area's temperature 190~ 210 DEG C, two 230~250 DEG C of area's temperature, three 230~250 DEG C of area's temperature, four 230~250 DEG C of area's temperature, five area's temperature 230~ 250 DEG C, six 230~250 DEG C of area's temperature, 230~250 DEG C of head temperature, 200~280r/min of screw speed.
CN201810638815.0A 2018-06-20 2018-06-20 A kind of AES-PET composite material and preparation method of low VOC Pending CN109021483A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845831A (en) * 2019-11-27 2020-02-28 安徽江淮汽车集团股份有限公司 VOC (volatile organic compound) improved master batch, preparation method thereof and preparation method of polyolefin composite material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101418111A (en) * 2008-11-14 2009-04-29 上海金发科技发展有限公司 Weather resistant halogen-free flame retardant ABS resin and preparation process thereof
CN106479166A (en) * 2016-10-21 2017-03-08 安徽江淮汽车集团股份有限公司 Low VOC polyamide 6 composite material of a kind of antistatic and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101418111A (en) * 2008-11-14 2009-04-29 上海金发科技发展有限公司 Weather resistant halogen-free flame retardant ABS resin and preparation process thereof
CN106479166A (en) * 2016-10-21 2017-03-08 安徽江淮汽车集团股份有限公司 Low VOC polyamide 6 composite material of a kind of antistatic and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845831A (en) * 2019-11-27 2020-02-28 安徽江淮汽车集团股份有限公司 VOC (volatile organic compound) improved master batch, preparation method thereof and preparation method of polyolefin composite material

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Address after: 230601 No. 99 Ziyun Road, Hefei Economic and Technological Development Zone, Anhui Province

Applicant after: Anhui Jianghuai Automobile Group Limited by Share Ltd

Address before: 230601 No. 669 Shixin Road, Taohua Industrial Park, Hefei City, Anhui Province

Applicant before: Anhui Jianghuai Automobile Group Limited by Share Ltd

Address after: 230601 No. 99 Ziyun Road, Hefei Economic and Technological Development Zone, Anhui Province

Applicant after: Anhui Jianghuai Automobile Group Limited by Share Ltd

Address before: 230601 No. 669 Shixin Road, Taohua Industrial Park, Hefei City, Anhui Province

Applicant before: Anhui Jianghuai Automobile Group Limited by Share Ltd

WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20181218