CN114471407B - Production system and method for producing EVA (ethylene vinyl acetate) by multi-kettle-tubular series-parallel continuous polymerization - Google Patents
Production system and method for producing EVA (ethylene vinyl acetate) by multi-kettle-tubular series-parallel continuous polymerization Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 55
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 33
- 239000005038 ethylene vinyl acetate Substances 0.000 title abstract description 43
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 title abstract description 43
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 title description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 177
- 239000000178 monomer Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims description 25
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 23
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 21
- 239000005977 Ethylene Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims description 5
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 4
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- -1 acrylic ester Chemical class 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 2
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 2
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 claims description 2
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 2
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims description 2
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 2
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 2
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 claims description 2
- FWLDHHJLVGRRHD-UHFFFAOYSA-N decyl prop-2-enoate Chemical compound CCCCCCCCCCOC(=O)C=C FWLDHHJLVGRRHD-UHFFFAOYSA-N 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 2
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 150000002734 metacrylic acid derivatives Chemical class 0.000 claims description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 claims description 2
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 27
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 19
- 230000000087 stabilizing effect Effects 0.000 description 5
- 238000012662 bulk polymerization Methods 0.000 description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical group C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/2425—Tubular reactors in parallel
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- 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
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/02—Ethene
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00065—Pressure measurement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
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Abstract
The invention discloses a production system and a method for producing EVA (ethylene-vinyl acetate copolymer) by multi-kettle-tubular series-parallel continuous polymerization, belonging to the technical field of production of EVA resin, and comprising a first pipeline, a pre-reaction kettle, a first tubular reaction component, a second tubular reaction component, a buffer tank and an online detection component; the first tubular reaction component is connected with the pre-reaction kettle in series, the second tubular reaction component is connected with the pre-reaction kettle in a circulating manner, the first tubular reaction component and the second tubular reaction component are connected in parallel, and the conversion rate of the material is detected through the online detection component; the feeding speed of the materials is controlled in a combined manner, so that the feeding speed and the proportion are more accurate; by utilizing the design modes of kettle-type and tube-type pre-reaction and tube-type main reaction, a multiple kettle-tube type serial-parallel continuous polymerization production technology is formed, the conversion rate of materials is effectively improved to be more than 80%, the recovery amount of unreacted raw material monomers is less, and the energy consumption of the whole production system is lower; the controllability of the EVA melt polymerization temperature is realized.
Description
Technical Field
The invention belongs to the technical field of EVA resin production, and particularly relates to a production system and a production method for producing EVA by multi-kettle-tube type series-parallel continuous polymerization.
Background
Ethylene-vinyl acetate copolymer resin (EVA) is formed by copolymerization of nonpolar ethylene monomer and strong polar vinyl acetate monomer (VAc). Compared with Polyethylene (PE), due to the introduction of the VAc monomer into the molecular chain segment, the crystallinity of the polymer is greatly reduced, and the aging resistance, the impact resistance, the compatibility and the flexibility of the polymer are obviously enhanced. The EVA products have larger performance difference due to different VAc composition contents in the copolymer, and the VAc content of common EVA products is lower than 40%.
At present, the common production processes of domestic and foreign EVA products include high-pressure continuous bulk polymerization, medium-pressure suspension polymerization, solution polymerization, emulsion polymerization and the like. As for EVA resin products with 5-40% of VAc content, most enterprises adopt a high-pressure continuous bulk polymerization process for production, and the method has high yield and high process continuity. The medium-pressure suspension polymerization, solution polymerization and emulsion polymerization processes are less applicable in recent years due to the low purity of the EVA resin finished product, the low content of ethylene in the finished product and the limited production capacity of the reactor.
The high-pressure continuous bulk polymerization process adopts a high-pressure tubular reactor, the pressure is 160-230MPa, but the following two main problems exist: (1) The reaction is violent, the reaction temperature is uncontrollable, the reaction process is not controlled by the temperature, and the reaction device has explosion danger; if the structural mode that the high-pressure tubular reactor is coated by the super-strong explosion-proof concrete is adopted, the investment of a production device is huge; (2) The conversion rate is less than or equal to 30 percent, and the unreacted monomer which is more than 70 percent needs to be decompressed, cooled and recovered, then compressed and heated, and the process has huge energy consumption.
In the prior art, a Chinese granted patent CN106543337A discloses a method for preparing EVA by ethylene sectional pressurization, the method uses a single reaction kettle for polymerization, an emulsion polymerization process is used, a method of ethylene four-section pressure holding is adopted for staged copolymerization, the highest reaction pressure is 11MPa, but the highest value of the vinyl acetate content is only 40%, the reaction time exceeds 10h, the time consumption is long, the conversion rate is not high, and the operation is complicated.
U.S. granted patent US4921898A provides a process for preparing vinyl acetate-ethylene copolymer emulsions in the presence of a stabilizing system of a low molecular weight polyvinyl alcohol and a surfactant. The method records that ethylene and vinyl acetate are polymerized under the condition of free radical initiation, a water phase system is adopted, the polymerization reaction process adopts one-step pressurization to 1.4-3.4MPa, the polymerization is initiated at 45-80 ℃, and the glass transition temperature Tg is-30-20 ℃. However, the method is a single-kettle reaction, equipment needs to be cleaned among batches, and the use efficiency of the equipment is low.
The Chinese granted patent CN102695725A provides a method for continuous emulsion polymerization initiated by a water-containing free radical, which adopts a multi-kettle series connection process and initiates copolymerization reaction at 50-90 ℃; the pressure of reaction ethylene is 1.0-9.0MPa, the pressure of the multi-kettle series connection is gradually reduced, the polymerization time is 24h, and the solid content of the product is 50%. However, the method also has the problems of complex multi-kettle process operation, high polymerization control difficulty, high device cost and energy consumption and the like. The final product had a Tg of about 6 ℃ and a Tg too high, indicating a low vinyl acetate content.
Chinese patent application CN108239207A provides a production device of ethylene-vinyl acetate copolymer, wherein ethylene serving as a raw material of the production device is subjected to primary compression and secondary compression, then enters a tubular reactor together with other raw materials, and is subjected to polymerization reaction at 205 ℃ and 140MPa to obtain a crude product containing the vinyl acetate copolymer. Separating the crude product and unreacted gas by a 22MPa high-pressure separator, and adding the unreacted gas into the tubular reactor again by a high-pressure circulating cooler to participate in the reaction. However, the process operation of the production device is also complicated, and the content of the finally obtained product vinyl acetate is only 17 percent.
Disclosure of Invention
Aiming at the problems of low material conversion rate, huge monomer recovery amount, high energy consumption and the like caused by adopting a mode of continuously pressurizing to react, separating products, relieving pressure and recovering unreacted monomers, and pressurizing to enter circulation in the existing high-pressure tubular polymerization production technology of the EVA resin, the invention provides a production system for producing the EVA by multi-kettle-tubular serial-parallel continuous polymerization, which is realized by the following technology.
The production system for producing EVA (ethylene vinyl acetate) by multi-kettle-tubular series-parallel continuous polymerization comprises a first pipeline, a pre-reaction kettle, a first tubular reaction component, a second tubular reaction component, a buffer tank and an online detection component; the number of the first pipelines is multiple, and each first pipeline is connected with the feeding port of the pre-reaction kettle; the feed inlets of the first tubular reaction component and the second tubular reaction component are respectively connected with the discharge outlet of the pre-reaction kettle through a second pipeline and a third pipeline; the discharge hole of the first tubular reaction component is connected with the feed inlet of the buffer tank through a fourth pipeline, and the discharge hole of the second tubular reaction component is connected with the feed inlet of the pre-reaction kettle through a fifth pipeline;
the first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline are all provided with a temperature sensor, a pressure sensor and a regulating valve, and the regulating valve on the fourth pipeline is arranged close to one end of the buffer tank; the first pipeline, the second pipeline and the third pipeline are provided with pumps, and the online detection assembly is communicated with the third pipeline and the fourth pipeline through a sixth pipeline respectively; and the sixth pipeline is provided with a regulating valve.
In the scheme, the feed inlet of the first tubular reaction component is connected with the discharge outlet of the pre-reaction kettle through a second pipeline, so that a kettle-tubular series connection mode is formed; the feed inlet and the discharge outlet of the second tubular reaction component are respectively connected with the feed inlet and the discharge outlet of the pre-reaction kettle, so that the first tubular reaction component and the second tubular reaction component form a parallel connection mode, and a circulating reaction structure is formed between the pre-reaction kettle and the second tubular reaction component. Governing valve and pump on the first pipeline are allied oneself with accuse and are carried out the input speed control, realize various materials according to setting for the accurate feeding of input speed. Not only can set up a plurality of first pipelines on the preliminary reaction cauldron and be used for reinforced, also can add other filling tube on the buffer tank and be used for adding other raw materials that current production EVA material often needs such as antioxidant, terminating agent.
The temperature sensors and the pressure sensors are used for monitoring the temperature and the pressure on the corresponding first/second/third/fourth/fifth pipelines. The on-line detection component is used for detecting the conversion rate of the materials flowing out of the first tubular reaction component and the second tubular reaction component, so that the flow rate proportion of the materials flowing into the first tubular reaction component and the second tubular reaction component is controlled.
The existing high-pressure continuous bulk polymerization technology mostly adopts a simple series or circulation reaction mode, continuous pressurization reaction is needed in the process, unreacted monomers are decompressed and recovered for recycling reaction again, the material conversion rate is very low and can only reach 20-30 percent generally and not exceed 50 percent at most; the monomer raw materials which do not complete the reaction are compressed and liquefied by a compressor and then recycled, so that the monomer recovery amount is huge and the energy consumption is high. According to the production system for producing EVA, provided by the invention, the pre-reaction kettle and the first tubular reaction component are connected in series, the first tubular reaction component and the second tubular reaction component are connected in parallel, and the pre-reaction kettle and the second tubular reaction component are connected in a circulating manner, so that the continuous production of ethylene-vinyl acetate copolymer resin (EVA) is realized, and the reaction process can be controlled more accurately according to the reaction state (such as reaction temperature, prepolymerization melting state, prepolymerization concentration and the like); through the cooperation of the on-line detection component, the regulating valves and the pumps on various pipelines, the flow velocity of materials in the first tubular reaction component and the second tubular reaction component reaches more than 1m/s, the first tubular reaction component and the second tubular reaction component can independently or jointly control the flow velocity and the residence time of raw materials participating in the reaction, the conversion rate of the final raw materials can be improved to more than 80%, the monomer recovery amount is reduced to more than 60%, and the energy consumption is reduced. In the prior patent, literature technology and commercial products, no one is found, or two groups of tubular reaction components are connected in series in practical use, one group of the tubular reaction components is circularly connected with a pre-reaction kettle, the other group of the tubular reaction components is connected in series with the pre-reaction kettle, and the raw material conversion rate which can be achieved by the system is achieved through the cooperative matching of a regulating valve and a pump.
Preferably, the first tubular reaction component and the second tubular reaction component respectively comprise a temperature control groove and a tubular reactor positioned in the temperature control groove, and the tubular reactor is formed by connecting a plurality of reaction tubes in series. The length of the tubular reactor can be increased or decreased according to the requirement, and the tubular reactor is immersed in the temperature control tank, so that the temperature in the tubular reactor is stable, and the materials in the tubular reactor can be quickly and efficiently reacted.
Preferably, the vacant end of the first pipeline is connected with a raw material tank, and a metering pump or a flowmeter is arranged on the first pipeline. The raw material tank is used for storing corresponding reaction materials, and raw material ethylene monomers can be stored by the raw material tank and also can be directly introduced without being stored by the raw material tank. The flow rate of the solid/liquid raw materials and the flow rate of the ethylene can be controlled by a metering pump or a flowmeter, so that the feeding amount of the reaction raw materials can be accurately controlled.
Preferably, the pump on the first pipeline is a metering pump.
Preferably, the regulating valves on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the fifth pipeline and the sixth pipeline are self-operated regulating valves.
Preferably, the number of the first tubular reaction modules is not less than 2, and the adjacent first tubular reaction modules are connected in series.
The invention also provides a method for producing EVA by adopting any one of the production systems through continuous polymerization, which comprises the following steps:
s1, checking the air tightness of a device, cleaning and drying a first pipeline, a pre-reaction kettle, a first tubular reaction component, a second tubular reaction component and a buffer tank, vacuumizing, and introducing nitrogen for replacing for a plurality of times;
s2, closing pumps on the second pipeline and the third pipeline, inputting ethylene, vinyl acetate and a third monomer into the pre-reaction kettle through the first pipelines according to a set dosage, and starting a temperature and pressure raising program;
s3, after the temperature and the pressure in the pre-reaction kettle reach preset values, inputting an initiator into the pre-reaction kettle through the first pipeline according to a set dosage; starting pumps and regulating valves on the third pipeline and the fifth pipeline at the same time, starting a regulating valve on the sixth pipeline, and starting detection by the online detection assembly;
s4, when the conversion rate of the raw materials detected in the third pipeline is larger than or equal to 20%, opening pumps and regulating valves on the second pipeline and the fourth pipeline; controlling the flow proportion on the second pipeline and the third pipeline through an adjusting valve according to the liquid level in the pre-reaction kettle;
s5, opening a regulating valve on the fourth pipeline, and controlling the pressure entering the buffer tank according to the preset system pressure maintaining pressure; discharging the reacted product after pressure relief and temperature reduction in the buffer tank, and introducing the residual ethylene monomer into tail gas for recovery.
In the method for producing EVA, the most core technology is to complete the cooperative matching of the pre-reaction kettle, the first tubular reaction component and the second tubular reaction component according to the material conversion rate detected by the online detection component. Generally, when the on-line detection component detects that the conversion rate of the material in the third pipeline is more than or equal to 20%, the pump (continuous reaction pump) on the second pipeline is started to make part of the circulating material enter the first tubular reaction component for continuous reaction. According to the liquid level in the pre-reaction kettle, the flow of a pump (prepolymer circulating pump) on the third pipeline and the flow of a pump (continuous reaction pump) on the second pipeline are adjusted, and then the material flow distribution control in the pre-reaction kettle is completed.
The materials enter a discharging buffer tank for stabilizing pressure after passing through the main reaction tubular reactor, and the discharging buffer tank for stabilizing pressure is provided with a self-operated regulating valve which can set the pressure condition of the materials entering the discharging buffer tank for stabilizing pressure according to the pressure maintaining pressure of the system; the material can be discharged after being subjected to pressure relief and temperature reduction by a discharge buffer tank for stabilizing pressure, and the residual monomer is connected into tail gas for recycling
Preferably, in step S2, the third monomer input by the first pipeline is one or more selected from olefins, acrylates, methacrylates, unsaturated acids, and acrylonitrile.
More preferably, the olefins are one or more of propylene, n-butene, 1-hexene, 1,5-dihexene, 1-octene, 1,7-dihexene and vinyl chloride;
the acrylic ester is one or more of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-propyl acrylate, 2-ethylhexyl acrylate, n-octyl acrylate, isooctyl acrylate, decyl acrylate, 2-hydroxyethyl acrylate and 2-hydroxypropyl acrylate;
the methacrylate is one or more of methyl methacrylate, ethyl methacrylate, isobutyl methacrylate, n-butyl methacrylate, tert-butyl methacrylate, isopropyl methacrylate, hexyl methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, glycidyl methacrylate, cyclohexyl methacrylate and dimethylaminoethyl methacrylate;
the unsaturated acid is one or more of acrylic acid, methacrylic acid, itaconic acid, crotonic acid and maleic acid.
Compared with the prior art, the invention has the advantages that:
1. a brand-new production system for producing EVA is provided, the feeding speed of materials is controlled in a combined manner, and the feeding speed and the proportioning are more accurate; by utilizing the design modes of kettle type and tube type pre-reaction and tube type main reaction, a multiple kettle type-tube type series-parallel connection continuous polymerization production technology is formed, the conversion rate of materials is effectively improved to be more than 80%, the recovery amount of unreacted raw material monomers is less, and the energy consumption of the whole production system is lower;
2. the tubular reactor can increase the series stages according to the heat removal requirement of the reaction, increase the heat exchange area and realize the controllability of the EVA melting polymerization temperature.
Drawings
FIG. 1 is a schematic structural diagram of a production system for producing EVA by multi-kettle-tubular series-parallel continuous polymerization provided in example 1;
in the figure: 1. a first conduit; 2. a pre-reaction kettle; 3. a first tubular reaction assembly; 4. a second tubular reaction assembly; 5. a buffer tank; 6. an online detection component; 7. a second conduit; 8. a third pipeline; 9. a fourth conduit; 10. a fifth pipeline; 11. a temperature control tank; 12. a tubular reactor; 13. a temperature sensor; 14. a pressure sensor; 15. adjusting a valve; 16. a raw material tank; 17. a metering pump; 18. a flow meter; 19. a continuous reaction pump; 20. a circulation pump; 21. and a sixth pipeline.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first tubular reaction module and the second tubular reaction module used in the following examples were purchased from FITOK corporation as model numbersT60 (maximum working pressure 4137 bar); the pre-reaction kettle and the buffer tank are both provided with a temperature sensor and a pressure sensor conventionally, and are also provided with one or a plurality of necessary feed inlets according to the conventional production requirements; the self-operated regulating valve is purchased from Shanghai company, self-lubricating gelatin valve, inc., and has the model number of SP3211-16-15. The continuous reaction pump and the circulating pump are purchased from ProMinent company and have the model of
MHSH 600, with parameters of 35L/h,3000bar. The on-line detection component is purchased from BRUKER company and is of the type MATRIX-MF.
Example 1
The production system for producing EVA by multiple kettle-tube type serial-parallel continuous polymerization provided by this embodiment is, as shown in fig. 1, structurally comprising a first pipeline 1, a pre-reaction kettle 2, a first tube type reaction component 3, a second tube type reaction component 4, a buffer tank 5, and an online detection component 6; 5 first pipelines 1 are arranged, and each first pipeline 1 is connected with a feed inlet of the pre-reaction kettle 2; the feed inlets of the first tubular reaction component 3 and the second tubular reaction component 4 are respectively connected with the discharge outlet of the pre-reaction kettle 2 through a second pipeline 7 and a third pipeline 8; the discharge hole of the first tubular reaction component 3 is connected with the feed inlet of the buffer tank 5 through a fourth pipeline 9, and the discharge hole of the second tubular reaction component 4 is connected with the feed inlet of the pre-reaction kettle 2 through a fifth pipeline 10; the first tubular reaction component 3 and the second tubular reaction component 4 respectively comprise a temperature control groove 11 and a tubular reactor 12 positioned in the temperature control groove 11, and the tubular reactor 12 is formed by connecting a plurality of reaction tubes in series.
A temperature sensor 13, a pressure sensor 14 and an adjusting valve 15 are arranged on the first pipeline 1, the second pipeline 7, the third pipeline 8, the fourth pipeline 9 and the fifth pipeline 10, and the adjusting valve 15 (self-operated adjusting valve) on the fourth pipeline 9 is arranged close to one end of the buffer tank 5; the vacant ends of 4 first pipelines 1 are connected with a raw material tank 16, and a metering pump 17 is arranged on the corresponding first pipeline 1; the rest 1 first pipelines 1 are used for introducing ethylene monomers, flow meters 18 are correspondingly arranged on the first pipelines 1, continuous reaction pumps 19 are arranged on the second pipelines 7, circulating pumps 20 are arranged on the third pipelines 8, and the online detection assembly 6 is respectively communicated with the third pipelines 8 and the fourth pipelines 9 through sixth pipelines 21; the sixth pipeline 21 is provided with an adjusting valve 15 (self-operated adjusting valve).
The method for producing EVA by using the production system comprises the following steps:
s1, checking the air tightness of a device, cleaning and drying a first pipeline, a pre-reaction kettle, a first tubular reaction component, a second tubular reaction component and a buffer tank, vacuumizing, introducing nitrogen for replacing for a plurality of times, and removing oxygen and moisture; respectively adding vinyl acetate monomer, initiator and ethylene monomer into each raw material tank; other redundant material tanks are temporarily left empty;
s2, closing a circulating pump on the third pipeline and a continuous reaction pump on the second pipeline, inputting ethylene and vinyl acetate into the pre-reaction kettle through the first pipelines according to a predetermined dosage (ethylene: vinyl acetate mass ratio of 85);
s3, after the temperature and the pressure in the pre-reaction kettle reach preset values (120 ℃,150 MPa), recording the liquid level in the pre-reaction kettle, starting a pump (a circulating pump) and an adjusting valve on a third pipeline and a fifth pipeline at the same time, starting the adjusting valve on the fifth pipeline to enable materials in the pre-reaction kettle to enter a second tubular reaction assembly, simultaneously inputting an initiator into the pre-reaction kettle through the first pipeline, wherein the initiator accounts for 0.05 percent of the total amount of all monomers, and the online detection assembly starts to detect; continuously adding ethylene to keep the pressure of the whole system constant at 150MPa;
s4, when the on-line monitoring assembly detects that the conversion rate of the raw materials in the third pipeline is more than or equal to 20%, opening a pump (a continuous reaction pump) on the second pipeline and a regulating valve (a self-operated pressure regulating valve) on the fourth pipeline to enable part of the pre-polymerization materials to enter the first tubular reaction assembly for continuous reaction;
continuously adding vinyl acetate monomer and initiator in proportion during the operation of the system to restore the liquid level in the pre-reaction kettle and maintain the initial liquid level all the time, and controlling the flow proportion on the second pipeline and the third pipeline through regulating valves according to the liquid level in the pre-reaction kettle; the materials in the pre-reaction kettle and the second tubular reaction component are always in a circulating flow state, so that continuous production is achieved;
s5, when the materials are subjected to polymerization reaction through the first tubular reaction component, and an online monitoring system detects that the conversion rate reaches 80%, a regulating valve on the fourth pipeline is opened, and the pressure entering the buffer tank is controlled according to preset system pressure maintaining pressure; discharging the reacted product after pressure relief and temperature reduction (about 40 ℃ and 1.0 MPA) in the buffer tank, and introducing the residual ethylene monomer into tail gas for recycling.
Finally, the monomer conversion of the EVA product obtained in the surge tank was 80.62%. The product has a vinyl acetate content of 22% and a melt index of 35g/10min (190 ℃/2.16 kg) as determined by FTIR methods (Infrared Spectroscopy/molecular rotation Spectroscopy).
Example 2
The production system for producing EVA by multiple kettle-tube type serial-parallel continuous polymerization provided in this example has the same structure as that in example 1, and the method for producing EVA is basically the same, except that the raw material contains a methacrylic acid monomer (third monomer) in addition to an ethylene monomer and a vinyl acetate monomer, and the usage ratio of the ethylene monomer, the vinyl acetate monomer and the methacrylic acid monomer is 70
In step S1 of the production method, methacrylic acid monomers are also stored in an empty raw material tank and added to the pre-reaction tank in a proportion along with vinyl acetate monomers in step S2.
Finally, the monomer conversion of the resulting EVA product in the surge tank was 82%. The product has a vinyl acetate content of 22% and a melt index of 13g/10min (190 ℃/2.16 kg) as determined by FTIR methods (Infrared Spectroscopy/molecular rotation Spectroscopy).
Example 3
The production system for producing EVA by multiple kettle-tube type serial-parallel continuous polymerization provided in this example has the same structure as in example 1, and the raw materials and proportions used, and the method for producing EVA are also substantially the same as in example 1, except that in the production method, the temperature of step S3 is raised to a maximum temperature of 120 ℃ and a pressure of 150MPa, and then the temperature and pressure are continuously maintained.
Finally, the monomer conversion of the EVA product obtained in the surge tank was 80.5%. The product has a vinyl acetate content of 32% and a melt index of 13g/10min (190 ℃/2.16 kg) as determined by FTIR methods (Infrared Spectroscopy/molecular rotation Spectroscopy).
The above examples 1-3 prove that when the production system and the corresponding production method of the present invention are used to produce the EVA material, the monomer conversion rate of the EVA product is all over 80%, and the vinyl acetate content is significantly increased.
Claims (8)
1. A method for continuous polymerization production of EVA by a multiple kettle-tube type series-parallel production system is characterized in that the production system comprises a first pipeline, a pre-reaction kettle, a first tube type reaction component, a second tube type reaction component, a buffer tank and an online detection component; the number of the first pipelines is multiple, and each first pipeline is connected with the feeding port of the pre-reaction kettle; the feed inlets of the first tubular reaction component and the second tubular reaction component are respectively connected with the discharge outlet of the pre-reaction kettle through a second pipeline and a third pipeline; the discharge hole of the first tubular reaction component is connected with the feed inlet of the buffer tank through a fourth pipeline, and the discharge hole of the second tubular reaction component is connected with the feed inlet of the pre-reaction kettle through a fifth pipeline;
the first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline are all provided with a temperature sensor, a pressure sensor and a regulating valve, and the regulating valve on the fourth pipeline is arranged close to one end of the buffer tank; the first pipeline, the second pipeline and the third pipeline are provided with pumps, and the online detection assembly is respectively communicated with the third pipeline and the fourth pipeline through a sixth pipeline; the sixth pipeline is provided with an adjusting valve;
the method for producing EVA by the continuous polymerization of the production system comprises the following steps:
s1, checking the air tightness of a device, cleaning and drying a first pipeline, a pre-reaction kettle, a first tubular reaction component, a second tubular reaction component and a buffer tank, vacuumizing, and introducing nitrogen for replacing for a plurality of times;
s2, closing pumps on the second pipeline and the third pipeline, inputting ethylene, vinyl acetate and a third monomer into the pre-reaction kettle through the first pipelines according to a set dosage, and starting a temperature and pressure raising program;
s3, after the temperature and the pressure in the pre-reaction kettle reach preset values, inputting an initiator into the pre-reaction kettle through the first pipeline according to a set dosage; simultaneously opening the pumps and the regulating valves on the third pipeline and the fifth pipeline, starting the regulating valve on the sixth pipeline, and starting the detection of the online detection assembly;
s4, when the conversion rate of the raw materials detected in the third pipeline is larger than or equal to 20%, opening pumps and regulating valves on the second pipeline and the fourth pipeline; controlling the flow proportion on the second pipeline and the third pipeline through an adjusting valve according to the liquid level in the pre-reaction kettle;
s5, opening a regulating valve on the fourth pipeline, and controlling the pressure entering the buffer tank according to the preset system pressure maintaining pressure; discharging the reacted product after pressure relief and temperature reduction in the buffer tank, and introducing the residual ethylene monomer into tail gas for recovery.
2. The continuous polymerization production method of EVA of claim 1, wherein the first tubular reaction module and the second tubular reaction module each comprise a temperature control tank and a tubular reactor in the temperature control tank, and the tubular reactor is composed of a plurality of reaction tubes connected in series.
3. The continuous polymerization EVA production method of claim 1, wherein the empty end of the first pipeline is connected with a raw material tank, and a metering pump or a flow meter is arranged on the first pipeline.
4. The continuous polymerization process for producing EVA according to claim 1, characterized in that the pump on the first pipe is a metering pump.
5. The continuous polymerization production EVA method of claim 1, wherein the regulating valves on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the fifth pipeline and the sixth pipeline are self-operated regulating valves.
6. The continuous polymerization production method for EVA according to claim 1, wherein the number of the first tubular reaction modules is not less than 2, and the adjacent first tubular reaction modules are connected in series.
7. The continuous polymerization production method of EVA according to claim 1, wherein in step S2, the third monomer input by the first pipeline is one or more selected from olefins, acrylates, methacrylates, unsaturated acids, and acrylonitrile.
8. The continuous polymerization production EVA method of claim 7, wherein the olefins are one or more of propylene, n-butene, 1-hexene, 1,5-dihexene, 1-octene, 1,7-dioctene, and vinyl chloride;
the acrylic ester is one or more of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-propyl acrylate, 2-ethylhexyl acrylate, n-octyl acrylate, isooctyl acrylate, decyl acrylate, 2-hydroxyethyl acrylate and 2-hydroxypropyl acrylate;
the methacrylate is one or more of methyl methacrylate, ethyl methacrylate, isobutyl methacrylate, n-butyl methacrylate, tert-butyl methacrylate, isopropyl methacrylate, hexyl methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, glycidyl methacrylate, cyclohexyl methacrylate and dimethylaminoethyl methacrylate;
the unsaturated acid is one or more of acrylic acid, methacrylic acid, itaconic acid, crotonic acid and maleic acid.
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Denomination of invention: A Production System and Method for EVA Production through Series Parallel Continuous Polymerization of Multiple Kettles and Pipes Granted publication date: 20221220 Pledgee: Kunming Branch of China Minsheng Bank Co.,Ltd. Pledgor: YUNNAN ZHENGBANG TECHNOLOGY CO.,LTD. Registration number: Y2023530000069 |