CN112457437A - Preparation method of low-viscosity polyvinyl chloride paste resin - Google Patents

Preparation method of low-viscosity polyvinyl chloride paste resin Download PDF

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Publication number
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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China
Prior art keywords
polyvinyl chloride
micro
paste resin
chloride paste
emulsifier
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CN202011355174.1A
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Chinese (zh)
Inventor
孟永华
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Jiangsu Kangning Chemical Co ltd
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Jiangsu Kangning Chemical Co ltd
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Priority to CN202011355174.1A priority Critical patent/CN112457437A/en
Publication of CN112457437A publication Critical patent/CN112457437A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F114/00Homopolymers 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
    • C08F114/02Monomers containing chlorine
    • C08F114/04Monomers containing two carbon atoms
    • C08F114/06Vinyl 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

Preparation method of low-viscosity polyvinyl chloride paste resin
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.
CN202011355174.1A 2020-11-27 2020-11-27 Preparation method of low-viscosity polyvinyl chloride paste resin Pending CN112457437A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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