CN114539454A - Preparation method of polyvinyl chloride paste resin - Google Patents
Preparation method of polyvinyl chloride paste resin Download PDFInfo
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- CN114539454A CN114539454A CN202011327377.XA CN202011327377A CN114539454A CN 114539454 A CN114539454 A CN 114539454A CN 202011327377 A CN202011327377 A CN 202011327377A CN 114539454 A CN114539454 A CN 114539454A
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- polymerization kettle
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- polyvinyl chloride
- emulsifier
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 45
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 45
- 239000011347 resin Substances 0.000 title claims abstract description 43
- 229920005989 resin Polymers 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 106
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 40
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007800 oxidant agent Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 24
- 230000032683 aging Effects 0.000 claims abstract description 23
- 230000001590 oxidative effect Effects 0.000 claims abstract description 23
- 239000000839 emulsion Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000003213 activating effect Effects 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- 239000006172 buffering agent Substances 0.000 claims abstract description 11
- 238000000889 atomisation Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000004816 latex Substances 0.000 claims abstract description 6
- 229920000126 latex Polymers 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 29
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 8
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical group [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 8
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 235000015424 sodium Nutrition 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- 239000000872 buffer Substances 0.000 claims description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 229940056585 ammonium laurate Drugs 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- VJCJAQSLASCYAW-UHFFFAOYSA-N azane;dodecanoic acid Chemical compound [NH4+].CCCCCCCCCCCC([O-])=O VJCJAQSLASCYAW-UHFFFAOYSA-N 0.000 claims description 4
- CJIAXHWXANNZPB-UHFFFAOYSA-N azanium;decanoate Chemical compound [NH4+].CCCCCCCCCC([O-])=O CJIAXHWXANNZPB-UHFFFAOYSA-N 0.000 claims description 4
- LRIHKZMLMWYPFS-UHFFFAOYSA-N azanium;hexadecanoate Chemical compound [NH4+].CCCCCCCCCCCCCCCC([O-])=O LRIHKZMLMWYPFS-UHFFFAOYSA-N 0.000 claims description 4
- BJOYVZZDDFVLPI-UHFFFAOYSA-N azanium;tetradecanoate Chemical compound [NH4+].CCCCCCCCCCCCCC([O-])=O BJOYVZZDDFVLPI-UHFFFAOYSA-N 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical group NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- QDIGBJJRWUZARS-UHFFFAOYSA-M potassium;decanoate Chemical compound [K+].CCCCCCCCCC([O-])=O QDIGBJJRWUZARS-UHFFFAOYSA-M 0.000 claims description 2
- MQOCIYICOGDBSG-UHFFFAOYSA-M potassium;hexadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCC([O-])=O MQOCIYICOGDBSG-UHFFFAOYSA-M 0.000 claims description 2
- PYJBVGYZXWPIKK-UHFFFAOYSA-M potassium;tetradecanoate Chemical compound [K+].CCCCCCCCCCCCCC([O-])=O PYJBVGYZXWPIKK-UHFFFAOYSA-M 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 claims description 2
- 229940082004 sodium laurate Drugs 0.000 claims description 2
- 229940045845 sodium myristate Drugs 0.000 claims description 2
- 229940045870 sodium palmitate Drugs 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- FIWQZURFGYXCEO-UHFFFAOYSA-M sodium;decanoate Chemical compound [Na+].CCCCCCCCCC([O-])=O FIWQZURFGYXCEO-UHFFFAOYSA-M 0.000 claims description 2
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 claims description 2
- JUQGWKYSEXPRGL-UHFFFAOYSA-M sodium;tetradecanoate Chemical compound [Na+].CCCCCCCCCCCCCC([O-])=O JUQGWKYSEXPRGL-UHFFFAOYSA-M 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 description 7
- 229940001584 sodium metabisulfite Drugs 0.000 description 6
- 230000002431 foraging effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004383 yellowing Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 239000002649 leather substitute Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 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
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a preparation method of polyvinyl chloride paste resin, which comprises the following steps: seed preparation: firstly, adding hot deionized water into a polymerization kettle, and then adding a buffering agent and an activating agent; then absorbing a first oxidant and a reducing agent into a polymerization kettle, then aging the solution in the polymerization kettle, adding a vinyl chloride monomer, a second oxidant, a first emulsifier, a second emulsifier and a third emulsifier into the polymerization kettle after aging, and obtaining and storing a seed emulsion after the reaction is finished; preparing a product: adding hot deionized water into a polymerization kettle, and then adding a buffering agent and an activating agent; then absorbing the reducing agent into a polymerization kettle, and adding the seed emulsion into the polymerization kettle; and then adding vinyl chloride into the polymerization kettle, then dropwise adding a second oxidant into the polymerization kettle, then adding a vinyl chloride monomer, a first emulsifier and a second emulsifier into the polymerization kettle, obtaining latex after the reaction is finished, and then carrying out atomization drying on the latex to finally obtain the polyvinyl chloride paste resin finished product.
Description
Technical Field
The invention relates to a preparation method of polyvinyl chloride paste resin.
Background
At present, the polyvinyl chloride paste resin is widely applied to various fields such as artificial leather, wallpaper, a conveying belt, disposable PVC gloves and the like. The polyvinyl chloride paste resins are mainly classified into foamed materials (wallpaper and the like), leather materials (artificial leather and the like), coating materials (conveyor belts and the like), and glove materials (disposable PVC gloves) according to their use characteristics. For the application of soft trademarks and the like, the polyvinyl chloride paste resin with good fluidity, high transparency and yellowing resistance after being formed into paste needs to be selected. At present, no special brand polyvinyl chloride paste resin for producing soft trademarks is available, and leather materials or coating materials are usually used for replacing the special brand polyvinyl chloride paste resin, so that the fluidity, the transparency and the yellowing resistance of the polyvinyl chloride paste resin are unstable, and the polyvinyl chloride paste resin cannot meet the production requirements of the soft trademarks.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of polyvinyl chloride paste resin which has the characteristics of good paste-forming fluidity, high product transparency, good yellowing resistance and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of polyvinyl chloride paste resin comprises the following steps:
(1) seed preparation: adding 100-140 parts by weight of hot deionized water into a polymerization kettle, wherein the temperature of the hot deionized water is 56-64 ℃, and then adding 0.05-0.2 part by weight of buffering agent and 0.005-0.02 part by weight of activating agent; then vacuumizing the polymerization kettle, wherein the vacuum degree is-0.09 to-0.095 MPa, sucking 0.1 to 0.3 weight part of first oxidant and 0.005 to 0.01 weight part of reducing agent into the polymerization kettle by utilizing negative pressure, and then aging the solution in the polymerization kettle at the aging temperature of 50 to 58 ℃ for 15 to 50 minutes; adding 20-30 parts by weight of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature in the polymerization kettle at 47-55 ℃, then adding 80-90 parts by weight of vinyl chloride monomer, 0.1-0.3 part by weight of second oxidant, and 0.5-1.5 parts by weight of first emulsifier, second emulsifier and third emulsifier into the polymerization kettle, carrying out polymerization reaction for 500-600 minutes, and obtaining and storing seed emulsion after the reaction is finished;
(2) preparing a product: extracting 1000-2500 Kg of seed emulsion, and pouring the seed emulsion into a seed metering tank; adding 90-120 parts by weight of hot deionized water into a polymerization kettle, wherein the temperature of the hot deionized water is 50-58 ℃, and then adding 0.05-0.02 part by weight of a buffering agent and 0.005-0.02 part by weight of an activating agent; then vacuumizing the polymerization kettle, wherein the vacuum degree is-0.09 to-0.095 MPa, sucking 0.005 to 0.01 weight part of reducing agent into the polymerization kettle by utilizing negative pressure, and adding the seed emulsion in the seed metering tank into the polymerization kettle; and adding 20-40 parts of vinyl chloride into the polymerization kettle, then dropwise adding 0.1-0.3 part by weight of a second oxidant into the polymerization kettle, keeping the reaction temperature in the polymerization kettle at 47-55 ℃, then adding 110-150 parts by weight of vinyl chloride monomer, 0.5-2.0 parts by weight of a first emulsifier and a second emulsifier into the polymerization kettle, continuing the polymerization reaction for 500-700 minutes, obtaining latex after the reaction is finished, and then carrying out atomization drying on the latex to finally obtain the polyvinyl chloride paste resin finished product.
Further, in the above method for preparing a polyvinyl chloride paste resin, the particle size of the seeds is controlled to be 0.25 to 0.7 μm after the first oxidant is oxidized and the aging agent is aged.
Further, in the preparation method of the polyvinyl chloride paste resin, the buffer is one or more of sodium bicarbonate, ammonium bicarbonate, sodium carbonate, disodium hydrogen phosphate, sodium dihydrogen phosphate and ammonia water.
Further, in the preparation method of the polyvinyl chloride paste resin, the activating agent is a copper sulfate aqueous solution with a mass percentage concentration of 1-5% or a copper chloride aqueous solution with a mass percentage concentration of 1-5%; the first oxidant is potassium persulfate, and the second oxidant is sodium persulfate or ammonium persulfate; the reducing agent is sodium pyrosulfite or sodium bisulfite.
Further, in the preparation method of the polyvinyl chloride paste resin, the first emulsifier is one or more of ammonium decanoate, sodium decanoate, potassium decanoate, ammonium laurate, sodium laurate, potassium laurate, ammonium myristate, sodium myristate, potassium myristate, ammonium palmitate, sodium palmitate, and potassium palmitate; the second emulsifier is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and secondary alkyl sodium sulfonate.
Further, in the above method for preparing a polyvinyl chloride paste resin, the volume of the polymerization vessel is 24m3。
Further, in the preparation method of the polyvinyl chloride paste resin, the small particles with the particle size of 0.2-0.7 μm account for 5-25% of the prepared polyvinyl chloride paste resin, and the rest are large particles with the particle size of 1-1.3 μm.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts a system of composite emulsifiers, utilizes different characteristics of different emulsifiers to obtain a special product aiming at the production requirement of the soft trademark, adopts the same composite emulsifiers when preparing seeds and products, and can increase the stability of the product.
Detailed Description
The present invention is further illustrated by the following specific examples.
The principle of the invention is as follows: the same composite emulsifier system is adopted when the seeds and the products are prepared, and the seeds occupy a certain proportion in the products, so that the stability of the products can be improved. The properties of different emulsifiers are utilized and used in a compound way, so that the requirements of production and processing of soft trademarks are met.
The first embodiment is as follows: a preparation method of polyvinyl chloride paste resin comprises the following steps:
(1) seed preparation: adding 10 tons of hot deionized water with the temperature of 56 ℃ into a polymerization kettle, and then adding 8Kg of buffering agent, namely sodium bicarbonate, and 800g of activating agent, namely copper sulfate solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, and absorbing 850g of a first oxidizing agent, namely potassium persulfate and 8Kg of reducing agent, namely sodium metabisulfite into the polymerization kettle by utilizing negative pressure for aging, wherein the aging temperature is 50 ℃, and the aging time is 50 minutes; adding 2 tons of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature at 47 ℃, then adding 8.5 tons of vinyl chloride monomer, 1.2Kg of second oxidant, namely potassium persulfate, 40 Kg of first emulsifier, namely ammonium myristate and 40 Kg of second emulsifier, namely sodium dodecyl benzene sulfonate into the polymerization kettle, carrying out polymerization reaction for 550-600 minutes, and obtaining and storing seed emulsion with the particle size of 0.6-0.7 mu m after the reaction is finished;
(2) preparing a product: extracting 2000-2500 Kg of seed emulsion to a seed metering tank; adding 11 tons of hot deionized water with the temperature of 47 ℃ into a polymerization kettle, and then adding 10Kg of buffer agent, namely sodium bicarbonate, by weight and 1Kg of activating agent, namely copper sulfate solution with the mass percentage concentration of 1 percent; vacuumizing the polymerization kettle to a vacuum degree of-0.095 MPa, sucking 10Kg of reducing agent sodium metabisulfite into the polymerization kettle by utilizing negative pressure, and adding the seed emulsion in the seed metering tank into the polymerization kettle; adding 3 tons of vinyl chloride monomer into a polymerization kettle, then dropwise adding 1.5 kilograms of second oxidant, namely potassium persulfate, into the polymerization kettle, keeping the reaction temperature at 47 ℃, then adding 10 tons of vinyl chloride monomer, 50 kilograms of first emulsifier, namely ammonium myristate and 50 kilograms of second emulsifier, namely sodium dodecyl benzene sulfonate into the polymerization kettle, carrying out polymerization reaction for 650 plus materials for 700 minutes, and after the reaction is finished, carrying out atomization drying to obtain a polyvinyl chloride paste resin finished product. In the prepared polyvinyl chloride paste resin, small particles with the particle size of 0.2-0.7 mu m account for 5-25%, and the balance is large particles with the particle size of 1-1.3 mu m.
Example two: a preparation method of polyvinyl chloride paste resin comprises the following steps:
(1) seed preparation: adding 10 tons of hot deionized water with the temperature of 59 ℃ into a polymerization kettle, and then adding 7Kg of buffering agent, namely sodium carbonate, and 800g of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, sucking 900g of a first oxidizing agent, namely potassium persulfate, and 8Kg of a reducing agent, namely sodium metabisulfite into the polymerization kettle by utilizing negative pressure for aging, wherein the aging temperature is 53 ℃, and the aging time is 40 minutes; adding 2 tons of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature at 50 ℃, then adding 8.5 tons of vinyl chloride monomer, 1.1Kg of second oxidant, namely potassium persulfate, 60 Kg of first emulsifier, namely ammonium laurate, and 20 Kg of second emulsifier, namely sodium dodecyl sulfate into the polymerization kettle, carrying out polymerization reaction for 550-600 minutes, and obtaining and storing seed emulsion with the particle size of 0.5-0.6 mu m after the reaction is finished;
(2) preparing a product: extracting 1700-2000 Kg of seed emulsion to a seed metering tank; adding 11 tons of hot deionized water at 50 ℃ into a polymerization kettle, and then adding 10Kg of buffer, namely sodium carbonate, by weight and 1Kg of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, sucking 10Kg of reducing agent, namely sodium metabisulfite into the polymerization kettle by utilizing negative pressure, and adding seed emulsion in a seed metering tank into the polymerization kettle; adding 3 tons of vinyl chloride monomer into a polymerization kettle, then dropwise adding 1.3 kilograms of second oxidant, namely potassium persulfate, into the polymerization kettle, keeping the reaction temperature at 50 ℃, then adding 10.5 tons of vinyl chloride monomer, 75 kilograms of first emulsifier, namely ammonium laurate, and 25 kilograms of second emulsifier, namely sodium dodecyl sulfate into the polymerization kettle, carrying out polymerization reaction for 600-700 minutes, and after the reaction is finished, carrying out atomization drying to obtain a polyvinyl chloride paste resin finished product. In the prepared polyvinyl chloride paste resin, small particles with the particle size of 0.2-0.7 mu m account for 5-25%, and the balance is large particles with the particle size of 1-1.3 mu m.
Example three: a preparation method of polyvinyl chloride paste resin comprises the following steps:
(1) seed preparation: adding 10 tons of hot deionized water with the temperature of 61 ℃ into a polymerization kettle, and then adding 4Kg of buffering agent, namely disodium hydrogen phosphate and 800g of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, and sucking 1000g of a first oxidizing agent, namely potassium persulfate, and 8Kg of a reducing agent, namely sodium metabisulfite into the polymerization kettle by utilizing negative pressure for aging, wherein the aging temperature is 55 ℃, and the aging time is 30 minutes; adding 2 tons of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature at 52 ℃, then adding 8 tons of vinyl chloride monomer, 1Kg of second oxidant, namely potassium persulfate, 40 Kg of first emulsifier, namely ammonium palmitate and 40 Kg of second emulsifier, namely secondary alkyl sodium sulfonate into the polymerization kettle, carrying out polymerization for 550-600 minutes, and obtaining and storing seed emulsion with the particle size of 0.4-0.5 mu m after the reaction is finished;
(2) preparing a product: extracting 1400-1700 Kg of seed emulsion to a seed metering tank; adding 11.5 tons of hot deionized water with the temperature of 52 ℃ into a polymerization kettle, and then adding 5Kg of buffering agent, namely disodium hydrogen phosphate, and 1Kg of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing the polymerization kettle to a vacuum degree of-0.095 MPa, sucking 9.5Kg of reducing agent, namely sodium metabisulfite, into the polymerization kettle by utilizing negative pressure, and adding the seed emulsion in the seed metering tank into the polymerization kettle; adding 3 tons of vinyl chloride monomer into a polymerization kettle, then dropwise adding 1.2 kilograms of second oxidant, namely potassium persulfate, into the polymerization kettle, keeping the reaction temperature at 52 ℃, then adding 10.5 tons of vinyl chloride monomer, 50 kilograms of first emulsifier, namely ammonium palmitate, and 50 kilograms of second emulsifier, namely secondary alkyl sodium sulfonate, into the polymerization kettle, carrying out polymerization reaction for 600-700 minutes, and after the reaction is finished, carrying out atomization drying to obtain a polyvinyl chloride paste resin finished product. In the prepared polyvinyl chloride paste resin, small particles with the particle size of 0.2-0.7 mu m account for 5-25%, and the balance is large particles with the particle size of 1-1.3 mu m.
Example four: a preparation method of polyvinyl chloride paste resin comprises the following steps:
(1) seed preparation: adding 10 tons of hot deionized water with the temperature of 64 ℃ into a polymerization kettle, and then adding 4Kg of buffering agent, namely disodium hydrogen phosphate and 800g of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, sucking 1200g of a first oxidizing agent, namely potassium persulfate, and 10Kg of a reducing agent, namely sodium bisulfite into the polymerization kettle by utilizing negative pressure for aging, wherein the aging temperature is 58 ℃, and the aging time is 20 minutes; and adding 2 tons of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature at 55 ℃, then adding 8 tons of vinyl chloride monomer, 1Kg of second oxidant, namely ammonium persulfate, 60 Kg of first emulsifier, namely ammonium decanoate, and 40 Kg of second emulsifier, namely secondary alkyl sodium sulfonate into the polymerization kettle, carrying out polymerization for 550-600 minutes, and obtaining and storing seed emulsion with the particle size of 0.3-0.4 mu m after the reaction is finished.
(2) Preparing a product: extracting 1000-1500 Kg of seed emulsion to a seed metering tank; adding 11.5 tons of hot deionized water with the temperature of 55 ℃ into a polymerization kettle, and then adding 5Kg of buffer agent, namely sodium dihydrogen phosphate, and 1Kg of activating agent, namely copper chloride solution with the mass percentage concentration of 1 percent; vacuumizing a polymerization kettle, wherein the vacuum degree is-0.095 MPa, sucking 11Kg of reducing agent, namely sodium bisulfite, into the polymerization kettle by utilizing negative pressure, and adding the seed emulsion in a seed metering tank into the polymerization kettle; adding 3 tons of vinyl chloride monomer into a polymerization kettle, then dropwise adding 1.1kg of a second oxidant, namely ammonium persulfate, into the polymerization kettle, keeping the reaction temperature at 55 ℃, then adding 10 tons of vinyl chloride monomer, 75 kg of a first emulsifier, namely ammonium decanoate, and 50 kg of a second emulsifier, namely secondary alkyl sodium sulfonate, into the polymerization kettle, carrying out polymerization reaction for 500-600 minutes, and after the reaction is finished, carrying out atomization drying to obtain a polyvinyl chloride paste resin finished product. In the prepared polyvinyl chloride paste resin, small particles with the particle size of 0.2-0.7 mu m account for 5-25%, and the balance is large particles with the particle size of 1-1.3 mu m.
The polymerization vessel used in each of the above examples had a volume of 24m3The polymerization kettle with the volume can improve the heat exchange effect of the polymerization kettle, and can effectively control the stable operation of polymerization reaction.
Claims (7)
1. A preparation method of polyvinyl chloride paste resin is characterized by comprising the following steps: the method comprises the following steps:
(1) seed preparation: adding 100-140 parts by weight of hot deionized water into a polymerization kettle, wherein the temperature of the hot deionized water is 56-64 ℃, and then adding 0.05-0.2 part by weight of buffering agent and 0.005-0.02 part by weight of activating agent; then vacuumizing the polymerization kettle, wherein the vacuum degree is-0.09 to-0.095 MPa, sucking 0.1 to 0.3 weight part of first oxidant and 0.005 to 0.01 weight part of reducing agent into the polymerization kettle by utilizing negative pressure, and then aging the solution in the polymerization kettle at the aging temperature of 50 to 58 ℃ for 15 to 50 minutes; adding 20-30 parts by weight of vinyl chloride monomer into a polymerization kettle after aging, keeping the reaction temperature in the polymerization kettle at 47-55 ℃, then adding 80-90 parts by weight of vinyl chloride monomer, 0.1-0.3 part by weight of second oxidant, and 0.5-1.5 parts by weight of first emulsifier, second emulsifier and third emulsifier into the polymerization kettle, continuing the polymerization reaction for 500-600 minutes, and obtaining and storing seed emulsion after the reaction is finished;
(2) preparing a product: extracting 1000-2500 Kg of seed emulsion, and pouring the seed emulsion into a seed metering tank; adding 90-120 parts by weight of hot deionized water into a polymerization kettle, wherein the temperature of the hot deionized water is 50-58 ℃, and then adding 0.05-0.02 part by weight of a buffering agent and 0.005-0.02 part by weight of an activating agent; then vacuumizing the polymerization kettle, wherein the vacuum degree is-0.09 to-0.095 MPa, sucking 0.005 to 0.01 weight part of reducing agent into the polymerization kettle by utilizing negative pressure, and adding the seed emulsion in the seed metering tank into the polymerization kettle; and adding 20-40 parts of vinyl chloride into the polymerization kettle, then dropwise adding 0.1-0.3 part by weight of a second oxidant into the polymerization kettle, keeping the reaction temperature in the polymerization kettle at 47-55 ℃, then adding 110-150 parts by weight of vinyl chloride monomer, 0.5-2.0 parts by weight of a first emulsifier and a second emulsifier into the polymerization kettle, continuing the polymerization reaction for 500-700 minutes, obtaining latex after the reaction is finished, and then carrying out atomization drying on the latex to finally obtain the polyvinyl chloride paste resin finished product.
2. The method for preparing a polyvinyl chloride paste resin according to claim 1, wherein: the grain diameter of the seed is controlled to be 0.25-0.7 mu m after the oxidation of the first oxidant and the aging of the aging agent.
3. The method for preparing a polyvinyl chloride paste resin according to claim 1, wherein: the buffer is one or more of sodium bicarbonate, ammonium bicarbonate, sodium carbonate, disodium hydrogen phosphate, sodium dihydrogen phosphate and ammonia water.
4. The method for preparing a polyvinyl chloride paste resin according to claim 1, wherein: the activating agent is a copper sulfate aqueous solution with the mass percentage concentration of 1-5% or a copper chloride aqueous solution with the mass percentage concentration of 1-5%; the first oxidant is potassium persulfate, and the second oxidant is sodium persulfate or ammonium persulfate; the reducing agent is sodium pyrosulfite or sodium bisulfite.
5. The method for preparing a polyvinyl chloride paste resin according to claim 1, wherein: the first emulsifier is one or more of ammonium decanoate, sodium decanoate, potassium decanoate, ammonium laurate, sodium laurate, potassium laurate, ammonium myristate, sodium myristate, potassium myristate, ammonium palmitate, sodium palmitate and potassium palmitate; the second emulsifier is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and secondary alkyl sodium sulfonate.
6. The method for preparing a polyvinyl chloride paste resin according to any one of claims 1 to 5, wherein: the volume of the polymerization kettle is 24m3。
7. The method for preparing a polyvinyl chloride paste resin according to any one of claims 1 to 5, wherein: in the prepared polyvinyl chloride paste resin, small particles with the particle size of 0.2-0.7 mu m account for 5-25%, and the balance is large particles with the particle size of 1-1.3 mu m.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105884945A (en) * | 2016-06-29 | 2016-08-24 | 唐山三友氯碱有限责任公司 | Method for improving production efficiency of micro-suspension polyvinyl chloride paste resin |
| CN110862474A (en) * | 2019-11-08 | 2020-03-06 | 上海氯碱化工股份有限公司 | Low-atomization-value polyvinyl chloride paste resin and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105884945A (en) * | 2016-06-29 | 2016-08-24 | 唐山三友氯碱有限责任公司 | Method for improving production efficiency of micro-suspension polyvinyl chloride paste resin |
| CN110862474A (en) * | 2019-11-08 | 2020-03-06 | 上海氯碱化工股份有限公司 | Low-atomization-value polyvinyl chloride paste resin and production method thereof |
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