CN112142912B - Preparation method of ultra-high molecular weight anionic polyacrylamide - Google Patents
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 36
- 125000000129 anionic group Chemical group 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- KZJPVUDYAMEDRM-UHFFFAOYSA-M silver;2,2,2-trifluoroacetate Chemical group [Ag+].[O-]C(=O)C(F)(F)F KZJPVUDYAMEDRM-UHFFFAOYSA-M 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 6
- 230000005587 bubbling Effects 0.000 claims description 5
- 238000006392 deoxygenation reaction Methods 0.000 claims description 5
- CZKMPDNXOGQMFW-UHFFFAOYSA-N chloro(triethyl)germane Chemical compound CC[Ge](Cl)(CC)CC CZKMPDNXOGQMFW-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- XSHKVZDGAVXGCC-UHFFFAOYSA-N 4,5-dihydro-1h-imidazol-1-ium;dichloride Chemical compound [Cl-].[Cl-].C1CN=C[NH2+]1.C1CN=C[NH2+]1 XSHKVZDGAVXGCC-UHFFFAOYSA-N 0.000 claims 1
- 238000010526 radical polymerization reaction Methods 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- -1 silver ions Chemical class 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 description 14
- 229920000642 polymer Polymers 0.000 description 13
- 238000004090 dissolution Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- NISQVXMPIWWGOO-UHFFFAOYSA-N 4,5-dihydro-1h-imidazole;dihydrochloride Chemical compound Cl.Cl.C1CN=CN1 NISQVXMPIWWGOO-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- WAKFRZBXTKUFIW-UHFFFAOYSA-N 2-bromo-2-phenylacetic acid Chemical compound OC(=O)C(Br)C1=CC=CC=C1 WAKFRZBXTKUFIW-UHFFFAOYSA-N 0.000 description 5
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- MONMFXREYOKQTI-UHFFFAOYSA-N 2-bromopropanoic acid Chemical compound CC(Br)C(O)=O MONMFXREYOKQTI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulphite Substances [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/06—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen
- C08F4/10—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen of alkaline earth metals, zinc, cadmium, mercury, copper or silver
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a preparation method for synthesizing ultra-high molecular weight anionic polyacrylamide by catalysis of trace silver ions through organic bromide, which is different from the traditional free radical polymerization.
Description
Technical Field
The invention relates to a preparation method of ultra-high molecular weight anionic polyacrylamide, belonging to the technical field of high molecular materials.
Background
The copolymer of acrylamide and acrylic acid is a multifunctional high molecular compound with wide application, has excellent physicochemical properties such as thickening, flocculation sedimentation, filtration, resistance reduction, purification and the like, is the most important variety in water-soluble high molecular polyelectrolytes, is widely applied to the industrial and agricultural fields such as oil field development, mining industry, printing and dyeing, water treatment, soil improvement and the like and departments such as medicines, sanitary foods and the like, can also be used as intelligent hydrogel, and has the reputation of 'a hundred industry auxiliary agent'. With the environmental protection concept of China being deepened into people continuously, the application requirement of polyacrylamide in the field of water treatment is more and more.
At present, the free radical solution polymerization method is generally adopted for synthesizing polyacrylamide in a laboratory and industrially producing the polyacrylamide. For example, rabiee et al (Iranian Polymer Journal,2005,14 (7): 603-608) initiate aqueous solution polymerization of acrylamide monomers using potassium persulfate-sodium sulfite as a radical polymerization initiator to produce polyacrylamide having a molecular weight of 1200 ten thousand. Wang Hongping (academic thesis: synthesis and performance research of ultra-high molecular weight polyacrylamide, northeast oil university, 2014) adopts a self-developed bifunctional radical initiator to perform redox reaction to initiate aqueous solution polymerization of acrylamide monomers, and the average molecular weight is 3.0 × 10 7 The polyacrylamide of (1). Although the methods can prepare the polyacrylamide with ultrahigh molecular weight, the methods have the problems of low monomer conversion rate, complex polymerization reaction process, unstable quality, uneven molecular weight distribution of the obtained polyacrylamide polymer, slow polymer dissolution rate, poor dissolution performance and the like.
Disclosure of Invention
The invention aims to: provides a preparation method which is different from the traditional free radical polymerization and utilizes the catalysis of trace silver ions to synthesize the anionic polyacrylamide with the ultra-high molecular weight through the promotion of organic bromides.
The technical scheme of the invention is as follows:
a preparation method of ultra-high molecular weight anionic polyacrylamide comprises the following steps (in parts by weight):
at the temperature of 0-10 ℃, 1000000 parts of acrylamide, 240000 parts of acrylic acid, 130000 parts of sodium hydroxide and 1800000 parts of deionized water are uniformly mixed, nitrogen is introduced for bubbling and deoxygenation (20 min), 0.5-2 parts of silver salt (catalyst), 50-250 parts of organic bromide (accelerant) and 100-250 parts of 2,2-azabicyclo (2-imidazoline) dihydrochloride are added, after the bubbling and deoxygenation is continued for 10min, the temperature is raised to 45 ℃ at the speed of 4 ℃/h, the temperature is preserved for 3 h to obtain anionic polyacrylamide gel blocks, the gel blocks are taken out and sheared, vacuum drying (60 ℃) is carried out, and grinding is carried out to obtain finished products;
the silver salt is silver trifluoroacetate or silver trifluoromethanesulfonate, and preferably, the silver salt is fed in the form of 1.0mg/mL aqueous solution;
the organic bromide is alpha-bromobenzene acetic acid or 2-bromine propionic acid.
The viscosity average molecular weight of the prepared anionic polyacrylamide is more than 1000 ten thousand.
The invention has the beneficial effects that:
aiming at the defects of the existing polyacrylamide free radical polymerization technology, the invention provides a novel method for synthesizing the anionic polyacrylamide with the ultra-high molecular weight by using trace silver ions as a catalyst and organic bromide as an accelerant.
Detailed Description
The invention is further described below by means of specific examples, without the scope of protection of the invention being limited thereto.
Characterization test method:
(1) Determination of the monomer residue ratio (Mono.%) in the Polymer
Monomer residual rate the content of unreacted acrylamide monomer in the polymer was determined with reference to GB 12005.3, monomer residual rate:
Mono.％＝m 1 /(m 1 +m 2 )×100％，
in the formula is m 1 Mass (g) of unreacted acrylamide monomer, m 2 Mass (g) of the polyacrylamide polymer.
(2) Reaction conversion (Conv.%) determination
Conv.％＝100％-Mono.％
(3) Determination of Polyacrylamide molecular weight
The molecular weight of polyacrylamide is measured by an Ubbelohde viscometer with the capillary inner diameter of 0.55mm (+ -2%) according to the national standard GB 175124-2008.
(4) Method for measuring dissolution rate of polyacrylamide
The determination of the dissolution rate of polyacrylamide in water was carried out according to the method described in GB 12005.8.
Example 1
The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoroacetate: 0.02mg (prepared as a 1.0mg/ml aqueous solution, 20. Mu.L added); α -bromophenylacetic acid: 3.0mg;2,2-azabicyclo (2-imidazoline) dihydrochloride: 4.0mg.
The preparation method comprises the following steps:
(1) 20.0g of acrylamide, 4.8g of acrylic acid, 2.6g of sodium hydroxide and 36.0g of deionized water are taken, stirred, dissolved and mixed uniformly, and nitrogen is introduced into the aqueous solution at the temperature of 0 ℃ for bubbling and deoxygenation for 20min.
(2) 0.02mg of silver trifluoroacetate catalyst, 3.0mg of alpha-bromophenylacetic acid promoter and 4.0mg of 2,2-azabicyclo (2-imidazoline) dihydrochloride are added to the aqueous solution, and oxygen is continuously bubbled at 0 ℃ for 10min.
(3) Introducing nitrogen into a reaction bottle to remove oxygen for 20min, adding the aqueous solution into the reaction bottle, and then placing the reaction bottle in a water bath for temperature programming: the temperature is raised from 10 ℃ to 45 ℃ at the heating rate of 4 ℃/h, and the anionic polyacrylamide gel block is obtained after heat preservation is carried out for 3 hours at 45 ℃.
(4) Taking out the rubber block, shearing the rubber block into pieces, drying the rubber block in vacuum at the temperature of 60 ℃ to obtain anionic polyacrylamide particles, and grinding the particles to obtain the ultra-high molecular weight anionic polyacrylamide powder.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1430 ten thousand, the monomer conversion rate is 99.0 percent, and the polymer dissolution rate is less than 20min.
Example 2
The preparation method is the same as example 1. The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoromethanesulfonate: 0.02mg (prepared as a 1.0mg/ml aqueous solution to which 20. Mu.L of the solution was added); 2-bromopropionic acid: 5.0mg;2,2-azabicyclo (2-imidazoline) dihydrochloride: 5.0mg.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1370 ten thousand, the monomer conversion rate is 98.6%, and the polymer dissolution rate is less than 15min.
Example 3
The preparation method is the same as example 1. The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoroacetate: 0.04mg (prepared as a 1.0mg/ml aqueous solution, 40. Mu.L added); α -bromophenylacetic acid: 4.0mg;2,2-azabicyclo (2-imidazoline) dihydrochloride: 2.0mg.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1123 thousands, the monomer conversion rate is 97.4%, and the polymer dissolution rate is less than 15min.
Example 4
The preparation method is the same as example 1. The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoromethanesulfonate: 0.01mg (prepared as a 1.0mg/ml aqueous solution to which 10. Mu.L of the suspension was added); α -bromophenylacetic acid: 1.0mg;2,2-azabicyclo (2-imidazoline dihydrochloride): 4.0mg.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1060 ten thousand, the monomer conversion rate is 97.1%, and the polymer dissolution rate is less than 15min.
Example 5
The preparation method is the same as example 1. The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoroacetate: 0.02mg (prepared as a 1.0mg/ml aqueous solution, 40. Mu.L added); α -bromophenylacetic acid: 3.0mg;2,2-azabicyclo (2-imidazoline) dihydrochloride: 3.0mg.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1228 ten thousand, the monomer conversion rate is 98.9%, and the polymer dissolution rate is less than 15min.
Example 6
The preparation method is the same as example 1. The raw material composition formula of the polymerization reaction is as follows: acrylamide: 20.0g; acrylic acid: 4.8g; sodium hydroxide: 2.6g; deionized water: 36.0g; silver trifluoroacetate: 0.03mg (prepared as a 1.0mg/ml aqueous solution, 30. Mu.L added); 2-bromopropionic acid: 5.0mg;2,2-azabis (2-imidazoline) dihydrochloride: 4.0mg.
The characterization test results show that: the molecular weight of the anionic polyacrylamide is 1648 thousands, the monomer conversion rate is 99.6 percent, and the polymer dissolution rate is less than 20min.
Comparative example
Sun Xiangdong (Liaoning chemical, 2003,032 (006): 233-235) uses acrylamide as monomer, potassium persulfate-sodium bisulfite as redox initiator, and sodium carbonate, EDTA, ammonia water, etc. are added into the monomer solution to prepare anionic polyacrylamide by aqueous solution polymerization. The polymerization temperature is 30-70 ℃, the molecular weight of the obtained polyacrylamide ranges from 700 to 1142 ten thousand, the polymer dissolution speed is 240 minutes, and the screen residue is 10%.
Claims (2)
1. A preparation method of ultra-high molecular weight anionic polyacrylamide is characterized by comprising the following steps:
at the temperature of 0-10 ℃, 1000000 parts of acrylamide, 240000 parts of acrylic acid, 130000 parts of sodium hydroxide and 1800000 parts of deionized water are uniformly mixed, nitrogen is introduced for bubbling and deoxygenation, 0.5-2 parts of silver salt, 50-250 parts of organic bromide and 100-250 parts of 2,2-aza bis (2-imidazoline) dihydrochloride are added, after the bubbling and the deoxygenation are continued, the temperature is raised to 45 ℃ at the speed of 4 ℃/hour, the temperature is kept for 3 hours, anionic polyacrylamide gel blocks are obtained, the gel blocks are taken out and sheared, dried in vacuum and ground, and finished products are obtained;
the silver salt is silver trifluoroacetate or silver trifluoromethanesulfonate;
the organic bromide is alpha-bromobenzene acetic acid or 2-bromine propionic acid.
2. The method of claim 1, wherein the silver salt is dosed as a 1.0mg/mL aqueous solution.
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Effective date of registration: 20240304 Address after: No. 1 South 1st Street, High tech Industrial Park, Chuhou Township, Linyi County, Yuncheng City, Shanxi Province 044100 Patentee after: Shanxi Xianghua Chemical Co.,Ltd. Country or region after: China Address before: 030610 Room 102, Taiheng Technology, No.1 Road, Xiuwen Base, Xiaohe Industrial Park, Jinzhong Development Zone, Shanxi Comprehensive Reform Demonstration Zone, Jinzhong City, Shanxi Province Patentee before: SHANXI XINDEHUI TECHNOLOGY Co.,Ltd. Country or region before: China |
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