CN112457437A - Preparation method of low-viscosity polyvinyl chloride paste resin - Google Patents
Preparation method of low-viscosity polyvinyl chloride paste resin Download PDFInfo
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- CN112457437A CN112457437A CN202011355174.1A CN202011355174A CN112457437A CN 112457437 A CN112457437 A CN 112457437A CN 202011355174 A CN202011355174 A CN 202011355174A CN 112457437 A CN112457437 A CN 112457437A
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- Prior art keywords
- polyvinyl chloride
- micro
- paste resin
- chloride paste
- emulsifier
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 48
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 48
- 239000011347 resin Substances 0.000 title claims abstract description 47
- 229920005989 resin Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 26
- 238000010557 suspension polymerization reaction Methods 0.000 claims abstract description 24
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000004816 latex Substances 0.000 claims abstract description 12
- 229920000126 latex Polymers 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 11
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000889 atomisation Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- STXKJYSBNDTAGK-UHFFFAOYSA-N (2-propan-2-ylphenyl) 7,7-dimethyloctaneperoxoate Chemical compound CC(C)C1=CC=CC=C1OOC(=O)CCCCCC(C)(C)C STXKJYSBNDTAGK-UHFFFAOYSA-N 0.000 claims description 2
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 claims description 2
- ZACVGCNKGYYQHA-UHFFFAOYSA-N 2-ethylhexoxycarbonyloxy 2-ethylhexyl carbonate Chemical compound CCCCC(CC)COC(=O)OOC(=O)OCC(CC)CCCC ZACVGCNKGYYQHA-UHFFFAOYSA-N 0.000 claims description 2
- KFGFVPMRLOQXNB-UHFFFAOYSA-N 3,5,5-trimethylhexanoyl 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOC(=O)CC(C)CC(C)(C)C KFGFVPMRLOQXNB-UHFFFAOYSA-N 0.000 claims description 2
- 235000021360 Myristic acid Nutrition 0.000 claims description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000005187 foaming Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 5
- 239000010985 leather Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229940082500 cetostearyl alcohol Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002649 leather substitute Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000203 mixture Substances 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
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/02—Monomers containing chlorine
- C08F114/04—Monomers containing two carbon atoms
- C08F114/06—Vinyl chloride
Abstract
The invention relates to a preparation method of low-viscosity polyvinyl chloride paste resin, which comprises the following steps: (1) vacuumizing the polymerization kettle by the micro-suspension method; (2) uniformly dispersing deionized water, vinyl chloride, an initiator and an emulsifier in a micro-suspension method dispersion tank, and pumping into a vacuumized micro-suspension polymerization kettle by a pump; (3) and carrying out polymerization reaction in a micro-suspension polymerization kettle to obtain latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product. The invention adopts the compound emulsifier, combines the characteristics of different emulsifiers, ensures that the paste viscosity of the product is lower, and meets the requirement of low-viscosity processing.
Description
Technical Field
The invention relates to a preparation method of paste resin, in particular to a preparation method of low-viscosity polyvinyl chloride paste resin.
Background
The polyvinyl chloride paste resin is widely applied to various fields such as artificial leather, wallpaper, conveyer belts, disposable PVC gloves and the like. Depending on the use characteristics, polyvinyl chloride paste resins are mainly classified into several types, namely, foamed material-based polyvinyl chloride paste resins (used in the field of wallpaper and the like), leather material-based polyvinyl chloride paste resins (used in the field of artificial leather and the like), coating material-based polyvinyl chloride paste resins (used in the field of conveyor belts and the like), and glove material-based polyvinyl chloride paste resins (used in the field of disposable PVC gloves). When producing products such as foaming wallpaper, drop molding and the like, the polyvinyl chloride paste resin of foaming materials with low viscosity after being pasted needs to be selected. At present, leather material polyvinyl chloride paste resin or glove material polyvinyl chloride paste resin is mostly adopted to replace the existing polyvinyl chloride paste resin, but the two polyvinyl chloride paste resins have higher viscosity, and cannot well meet the production requirements of products such as foaming wallpaper, drop molding and the like, and particularly, the viscosity of the leather material polyvinyl chloride paste resin or the glove material polyvinyl chloride paste resin is higher in a low-temperature environment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of low-viscosity polyvinyl chloride paste resin.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of low-viscosity polyvinyl chloride paste resin comprises the following steps:
(1) vacuumizing a polymerization kettle: vacuumizing the micro-suspension polymerization kettle, wherein the vacuum degree is-0.09 MPa to-0.095 MPa, and reducing the temperature of a jacket of the micro-suspension polymerization kettle to 7-9 ℃; after negative pressure is formed in the micro-suspension polymerization kettle, the speed of the materials entering the micro-suspension polymerization kettle can be improved through pressure difference;
(2) and (3) product ingredients: adding 13-15 tons of normal-temperature deionized water, 2.5-5 Kg of initiator A, 2.2-4.4 Kg of initiator B, 19-20 tons of vinyl chloride monomer, 100-220 Kg of emulsifier A, 40-160 Kg of emulsifier B and 160-200 Kg of emulsifier C into a micro-suspension method dispersion tank for premixing, then adding the mixed material in the micro-suspension method dispersion tank into a micro-suspension polymerization kettle through a dispersion pump, and controlling the whole feeding time to be 40-90 minutes;
(3) and (3) product polymerization: and carrying out polymerization reaction on the mixed materials in a micro-suspension polymerization kettle, controlling the reaction temperature at 45-60 ℃ and the reaction time at 750-1400 minutes, obtaining latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product.
Further, in the preparation method of the low-viscosity polyvinyl chloride paste resin, the initiator a is one or two of azobisisoheptonitrile or azobisisobutyronitrile; the initiator B is one or more of di- (3,5, 5-trimethyl hexanoyl) peroxide, isopropylphenyl peroxyneodecanoate, tert-butyl peroxyneodecanoate or di (2-ethylhexyl) peroxydicarbonate.
Further, in the preparation method of the low-viscosity polyvinyl chloride paste resin, the emulsifier A is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or ammonium dodecyl sulfate; the emulsifier B is one or two of myristic acid or palmitic acid; the emulsifier C is one or more of dodecanol, hexadecanol, tetradecanol, hexadecanol or stearic acid.
Further, the preparation method of the low-viscosity polyvinyl chloride paste resin is characterized in that the reaction volume is 48m3In the polymerization vessel.
Further, the preparation method of the low-viscosity polyvinyl chloride paste resin is characterized in that the particle size of the particles in the polyvinyl chloride paste resin is 0.2-1.4 μm, and the particles are in monomodal distribution.
Compared with the prior art, the invention has the beneficial effects that: the particle size of the particles in the polyvinyl chloride paste resin produced by adopting a system of the composite emulsifier and utilizing different characteristics of different emulsifiers is 0.2-1.4 mu m, and the particles are distributed in a single peak, so that the particles are widely distributed, and compared with the conventional polyvinyl chloride paste resin with large particles and dense distribution, the polyvinyl chloride paste resin has lower viscosity and higher foaming effect, and is beneficial to producing foaming wallpaper and drop plastics. And because the viscosity of the polyvinyl chloride paste resin is low, the use of a viscosity reducer is reduced in the production process of the foaming wallpaper and the plastic drop, so that the produced foaming wallpaper and plastic drop products meet the environmental protection requirement.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples.
The first embodiment is as follows: a preparation method of low-viscosity polyvinyl chloride paste resin comprises the following steps:
(1) vacuumizing a polymerization kettle: vacuumizing the micro-suspension polymerization kettle, wherein the vacuum degree is-0.09 MPa to-0.095 MPa, and reducing the temperature of a jacket of the micro-suspension polymerization kettle to 7-9 ℃;
(2) and (3) product ingredients: adding 14 tons of normal-temperature deionized water, 19.5 tons of vinyl chloride monomer, 3Kg of initiator A-azodiisoheptanonitrile, 3Kg of initiator B-bis (2-ethylhexyl) peroxydicarbonate, 140Kg of emulsifier A-sodium dodecyl sulfate, 60Kg of emulsifier B-myristic acid and 160Kg of emulsifier C-cetostearyl alcohol into a microsuspension method dispersion tank for premixing, and then adding the mixed material in the microsuspension method dispersion tank into a microsuspension polymerization kettle by a dispersion pump, wherein the whole feeding time is 60 minutes;
(3) and (3) product polymerization: and carrying out polymerization reaction on the mixed material in a micro-suspension polymerization kettle at the reaction temperature of 50 +/-0.5 ℃ for 750-900 minutes, obtaining latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product, wherein the particle size of particles in the polyvinyl chloride paste resin is 0.2-1.4 mu m, and the particles are in unimodal distribution.
Example two: a preparation method of low-viscosity polyvinyl chloride paste resin comprises the following steps:
(1) vacuumizing a polymerization kettle: vacuumizing the micro-suspension polymerization kettle, wherein the vacuum degree is-0.09 MPa to-0.095 MPa, and reducing the temperature of a jacket of the micro-suspension polymerization kettle to 7-9 ℃;
(2) and (3) product ingredients: adding 15 tons of normal-temperature deionized water, 19 tons of vinyl chloride monomer, 2.5Kg of initiator A-azobisisobutyronitrile, 2.8Kg of initiator B-isopropylphenyl peroxyneodecanoate, 200Kg of emulsifier A-ammonium lauryl sulfate, 40Kg of emulsifier B-palmitic acid and 80Kg of emulsifier C-hexadecanol into a micro-suspension method dispersion tank for premixing, and then adding the mixture in the micro-suspension method dispersion tank into a micro-suspension polymerization kettle by a dispersion pump, wherein the whole feeding time is 70 minutes;
(3) and (3) product polymerization: and carrying out polymerization reaction on the mixed material in a micro-suspension polymerization kettle at the reaction temperature of 57 +/-0.5 ℃ for 750-850 minutes, obtaining latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product, wherein the particle size of particles in the polyvinyl chloride paste resin is 0.2-1.4 mu m, and the particles are in unimodal distribution.
Example three: a preparation method of low-viscosity polyvinyl chloride paste resin comprises the following steps:
(1) vacuumizing a polymerization kettle: vacuumizing the micro-suspension polymerization kettle, wherein the vacuum degree is-0.09 MPa to-0.095 MPa, and reducing the temperature of a jacket of the micro-suspension polymerization kettle to 7-9 ℃;
(2) and (3) product ingredients: 13 tons of normal-temperature deionized water, 20 tons of vinyl chloride monomer, 3Kg of initiator A-azobisisoheptonitrile, 4Kg of initiator B-bis (2-ethylhexyl) peroxydicarbonate, 220Kg of emulsifier A-sodium dodecyl benzene sulfonate, 30Kg of emulsifier B-myristic acid and 200Kg of emulsifier C-cetostearyl alcohol are added into a micro-suspension method dispersion tank for premixing, and then the mixed material in the micro-suspension method dispersion tank is added into a micro-suspension polymerization kettle through a dispersion pump, wherein the whole feeding time is 50 minutes;
(3) and (3) product polymerization: and carrying out polymerization reaction on the mixed material in a micro-suspension polymerization kettle at the reaction temperature of 46 +/-0.5 ℃ for 1000-1300 minutes, obtaining latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product, wherein the particle size of particles in the polyvinyl chloride paste resin is 0.2-1.4 mu m, and the particles are in unimodal distribution.
The volume of the micro suspension polymerizer used in each of the above examples was 48m3The micro-suspension polymerization kettle with the volume can improve the heat exchange effect and effectively control the stable operation of polymerization reaction.
Claims (5)
1. A preparation method of low-viscosity polyvinyl chloride paste resin is characterized by comprising the following steps: the method comprises the following steps:
(1) vacuumizing a polymerization kettle: vacuumizing the micro-suspension polymerization kettle, wherein the vacuum degree is-0.09 MPa to-0.095 MPa, and reducing the temperature of a jacket of the micro-suspension polymerization kettle to 7-9 ℃;
(2) and (3) product ingredients: adding 13-15 tons of normal-temperature deionized water, 2.5-5 Kg of initiator A, 2.2-4.4 Kg of initiator B, 19-20 tons of vinyl chloride monomer, 100-220 Kg of emulsifier A, 40-160 Kg of emulsifier B and 160-200 Kg of emulsifier C into a micro-suspension method dispersion tank for premixing, then adding the mixed material in the micro-suspension method dispersion tank into a micro-suspension polymerization kettle through a dispersion pump, and controlling the whole feeding time to be 40-90 minutes;
(3) and (3) product polymerization: and carrying out polymerization reaction on the mixed materials in a micro-suspension polymerization kettle, controlling the reaction temperature at 45-60 ℃ and the reaction time at 750-1400 minutes, obtaining latex after the reaction is finished, and carrying out atomization drying on the latex to obtain a polyvinyl chloride paste resin finished product.
2. The method for preparing a low-viscosity polyvinyl chloride paste resin according to claim 1, wherein the method comprises the steps of: the initiator A is one or two of azobisisoheptonitrile or azobisisobutyronitrile; the initiator B is one or more of di- (3,5, 5-trimethyl hexanoyl) peroxide, isopropylphenyl peroxyneodecanoate, tert-butyl peroxyneodecanoate or di (2-ethylhexyl) peroxydicarbonate.
3. The method for preparing a low-viscosity polyvinyl chloride paste resin according to claim 1, wherein the method comprises the steps of: the emulsifier A is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or ammonium dodecyl sulfate; the emulsifier B is one or two of myristic acid or palmitic acid; the emulsifier C is one or more of dodecanol, hexadecanol, tetradecanol, hexadecanol or stearic acid.
4. A method for preparing a low viscosity polyvinyl chloride paste resin according to claim 1, 2 or 3, wherein: the reaction is carried out in a volume of 48m3In the polymerization vessel.
5. A method for preparing a low viscosity polyvinyl chloride paste resin according to claim 1, 2 or 3, wherein: the particle diameter of the particles in the polyvinyl chloride paste resin is 0.2-1.4 mu m, and the particles are distributed in a single peak.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114230699A (en) * | 2022-01-06 | 2022-03-25 | 江苏康宁化学有限公司 | High-viscosity low-fluidity polyvinyl chloride paste resin and preparation method thereof |
CN114437265A (en) * | 2022-01-04 | 2022-05-06 | 江苏康宁化学有限公司 | Ultra-low viscosity polyvinyl chloride paste resin and preparation method thereof |
CN114437266A (en) * | 2022-01-13 | 2022-05-06 | 江苏康宁化学有限公司 | Low-foaming-agent high-foaming polyvinyl chloride paste resin and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102952229A (en) * | 2011-08-26 | 2013-03-06 | 沈阳化工股份有限公司 | PVC (Polyvinyl Chloride) paste resin and preparation method thereof |
CN105440219A (en) * | 2015-12-30 | 2016-03-30 | 江苏康宁化学有限公司 | PVC (polyvinyl chloride) paste resin and preparation method thereof |
-
2020
- 2020-11-27 CN CN202011355174.1A patent/CN112457437A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102952229A (en) * | 2011-08-26 | 2013-03-06 | 沈阳化工股份有限公司 | PVC (Polyvinyl Chloride) paste resin and preparation method thereof |
CN105440219A (en) * | 2015-12-30 | 2016-03-30 | 江苏康宁化学有限公司 | PVC (polyvinyl chloride) paste resin and preparation method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114437265A (en) * | 2022-01-04 | 2022-05-06 | 江苏康宁化学有限公司 | Ultra-low viscosity polyvinyl chloride paste resin and preparation method thereof |
CN114230699A (en) * | 2022-01-06 | 2022-03-25 | 江苏康宁化学有限公司 | High-viscosity low-fluidity polyvinyl chloride paste resin and preparation method thereof |
CN114437266A (en) * | 2022-01-13 | 2022-05-06 | 江苏康宁化学有限公司 | Low-foaming-agent high-foaming polyvinyl chloride paste resin and preparation method thereof |
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Application publication date: 20210309 |