CN110092850A - A kind of aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator and preparation method thereof - Google Patents
A kind of aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator and preparation method thereof Download PDFInfo
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- CN110092850A CN110092850A CN201910426851.5A CN201910426851A CN110092850A CN 110092850 A CN110092850 A CN 110092850A CN 201910426851 A CN201910426851 A CN 201910426851A CN 110092850 A CN110092850 A CN 110092850A
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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
- C08F14/00—Homopolymers and copolymers 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
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
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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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
- C08F2/42—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation using short-stopping agents
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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
- C08F214/00—Copolymers 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
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/06—Vinyl chloride
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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
- C08F218/00—Copolymers 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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses providing a kind of aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator, which terminates high-efficient, and resin ageing whiteness produced is high, up to 88 or more.Aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator of the invention, it is grouped as on the basis of 100 parts by the group of following mass parts: 4- hydroxyl -2,2,6,6- 3~20 parts of tetramethyl piperidine -1- oxygen radicals, 0.2~23 part of composite antioxidant, 1.5~24 parts of compound emulsifying agent, 0.2~5 part of dispersing agent, 1.1~23 parts of heat stabilizer, surplus are deionized water.
Description
Technical field
The present invention relates to a kind of terminator and preparation method thereof, more specifically to a kind of aqueous emulsion type polyvinyl chloride resin and
Vinyl chloride-vinyl acetate resin terminator and preparation method thereof.
Background technique
China is the first mass production state of world's polyvinyl chloride (PVC), and PVC production capacity suspends poly- per year over 20000000 t
Conjunction is most important production technology.In the later period of polymerization reaction, monomer concentration is low, and the probability for terminating reaction increases, and leads to low phase
Molecular mass and branched polymer are increased, the reduced performance of polymer.The method solved at present is down in reaction pressure
When 0.10~0.15MPa, terminator is added and terminates reaction immediately.The copolymer of vinyl chloride-vinyl acetate resin vinyl chloride and vinyl acetate, referred to as
Vinyl chloride-vinyl acetate resin.Vinyl chloride-vinyl acetate resin is most important chloroethylene copolymer resin, is mainly used for coating, flooring laminate, ink and adhesive etc.,
Suspension polymerisation is also most important production technology.It include coloration, thermostabilization to product quality as market competition is increasingly fierce
Property, the requirements such as residual monomer content be continuously improved, in the later period of polymerization reaction, also need that terminator is added.
Currently, polyvinyl chloride suspension polymerisation often includes bisphenol-A, acetone semicarbazone thiocarbamide (ATSC), diethyl with terminator
Azanol etc., dosage form include aqueous solution type, aqueous emulsion type, oil solution type and water slurry type.Such as Publication No. CN 107778395A
Chinese patent disclose a kind of nontoxic emulsion type terminator of polyvinyl chloride resin and preparation method thereof, the terminator is containing 5~10 parts of dispersions
Agent, 5~15 parts of phenolic antioxidants, 5~15 parts of stabilizers, 5~15 parts of polymerization inhibitors, 0.1~5 part of thickener, 1~5 part of rare-earth salts
Ethanol water, 2~10 parts of organic acids, 10~20 parts of emulsifiers, 100~200 parts of deionized waters.Publication No.
The Chinese patent of CN105801728B discloses molten terminator of a kind of polyvinyl chloride resin oil and preparation method thereof, including 5~50 parts of epoxies
Soybean oil, 10~30 parts of antioxidant, 10~40 parts of bisphenol-As, 1~20 part of solid terminator, 5~40 parts of stabilizers, 1~40 part of increasing
Mould agent, 5~45 parts of styrene, 5~25 parts of solvent naphthas, 5~40 parts of methanol.The China of Patent No. CN201110383453.3 is specially
Benefit discloses a kind of preparation method of polyvinyl chloride polymerization special emulsion type terminator, which contains 100 parts of one benzene of phosphorous acid
Di-isooctyl, 10~30 parts of acetone semicarbazone thiocarbamide bisphenol-As, 10~30 parts of α-methylstyrenes, 100~200 parts of pentaerythrites
Solution, 1~10 part of OP-4,3~20 parts of OP-10,20~100 parts of poly-vinyl alcohol solutions, 50~200 parts of deionized waters.Above-mentioned end
Although only agent is all using water as medium, have the characteristics that environmental-friendly, in the presence of terminating, inefficient, emulsion-stabilizing is poor etc. is asked
Topic, ageing whiteness generally can only achieve 81 or so, and there are also larger gaps for the requirement with ageing whiteness 88.Simultaneously there is storage in product
Phase is short, easy aggregation agglomeration, cohesion, precipitating etc..
U.S. US 7683144 discloses a kind of excellent chloroethylene polymerization terminator, 1. technical solution specifically includes that
Stable NO free radical is added into reaction system；2. phenolic antioxidant is added.This terminator can be used for the cream of vinyl chloride
Liquid polymerization, suspension polymerisation, though it is most effective to suspension polymerisation, it is inconvenient for use.NO free radical (nitroxyl radicals) includes morpholine
Ketone, piperazine, imidazolone or their derivative (piperazine that such as tetramethyl piperazine, senior alkyl replace).Therefore it needs to grind
System develops a kind of aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator, of the existing technology to solve the problems, such as, is especially used for
The terminator of vinyl chloride-vinyl acetate resin production.
Summary of the invention
The present invention solves problems of the prior art and insufficient, provides a kind of aqueous emulsion type polyvinyl chloride resin and chlorine vinegar
Resin terminator, the terminator good emulsion stability terminate high-efficient, resin ageing whiteness height produced, up to 88 or more.
The present invention also provides the preparation method of the aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator, preparation methods simultaneously
It is simple and easy, it is at low cost.
The present invention is achieved by the following technical solutions:
Aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator of the invention, by the group of following mass parts on the basis of 100 parts
It is grouped as:
The above-mentioned terminator of the present invention, further technical solution is the composite antioxidant by antioxidant 1010
{ i.e. four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters } and irgasfos 168 { i.e. three (2,4- of phosphorous acid
Di-tert-butyl-phenyl) ester or antioxidant 1010 and antioxidant 264 (i.e. 2,6- is to di-tert-butyl p-cresol) form, wherein with end
Only on the basis of 100 parts of agent mass parts, the dosage of antioxidant 1010 is 0.1~15 part, and irgasfos 168 dosage is 0.1~6 part, is resisted
264 dosage of oxygen agent is 0.1~8 part.
The above-mentioned terminator of the present invention, further technical solution can also be the compound emulsifying agent by sorbierite
Acid anhydride stearate, fatty alcohol polyoxyethylene ether and polyoxyethylene sorbitan carboxylic ester composition, wherein with terminator mass parts
On the basis of 100 parts, sorbitan tristearate dosage is 0.5~8 part, and fatty alcohol polyoxyethylene ether dosage is 0.5~7 part, is gathered
Ethylene oxide sorbitan carboxylic esters dosage is 0.5~9 part.
The above-mentioned terminator of the present invention, further technical solution can also be the heat stabilizer by stearate
It is formed with methyl tin, wherein stearate dosage is 1~20 part on the basis of 100 parts of terminator mass parts, methyl tin dosage is
0.1~3 part.Further technical solution is that the stearate is zinc stearate, calcium stearate, magnesium stearate, tristearin
One of sour aluminium, barium stearate or combinations thereof.
The above-mentioned terminator of the present invention, further technical solution can also be the dispersing agent by extraordinary silicone oil with
Diisooctyl phthalate or extraordinary silicone oil and diisooctyl phenyl phosphite form, wherein with 100 parts of terminator mass parts
On the basis of, extraordinary silicon oil dosage is 2~10 parts, and the dosage of diisooctyl phthalate or diisooctyl phenyl phosphite is
0.2~5 part.Further technical solution is the polyether modified silicon oil that the extraordinary silicone oil is 20~80mgKOH/g of hydroxyl value.
The terminator preparation method of the present invention above-mentioned aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator comprising following
Step:
Composite antioxidant, heat stabilizer stearate, dispersing agent are added in reaction kettle by composition amounts first, slowly heated up
To 50~80 DEG C, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyl piperidine -1- oxygen are then added
Free radical forms homogeneous solution, adds heat stabilizer methyl tin, compound emulsifying agent continues to stir 5min~10min, more than addition
The deionized water of amount, then quickly 0.5~1h of stirring；It is most emulsified afterwards through emulsification pump, aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin is made
Terminator.
Compared with prior art the invention has the following advantages:
(1) preparation process is simple.Preparation process is not related to chemically reacting, it is only necessary to simply be mixed, be emulsified；
(2) good emulsion stability terminates high-efficient, resin ageing whiteness height produced, up to 90 or more；
(3) applied widely, it can be not only used for polyvinyl chloride system, it can also be used to vinyl chloride-vinyl acetate resin system.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the scope of the present invention is not limited to the following examples.
Embodiment 1
By 12 parts of antioxidant 1010,4 parts of irgasfos 168,12 parts of zinc stearate, 20~80mgKOH/g of hydroxyl value polyethers
In 3 parts of 8 parts of modified silicon oil, diisooctyl phthalate or diisooctyl phenyl phosphite addition reaction kettles, it is to slowly warm up to
50 DEG C, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyl piperidine -1- oxygen radicals are then added
15 parts, continues stirring and form homogeneous solution, add 1.5 parts of methyl tin, 5 parts of sorbitan tristearate, fatty alcohol polyoxy second
4 parts of alkene ether, 5 parts of polyoxyethylene sorbitan carboxylic ester continue stir 10min, the deionized water of surplus is added, then quickly stir
Mix 1h.It is most emulsified afterwards through emulsification pump, obtains product 1#.
Embodiment 2
By 12 parts of antioxidant 1010,4 parts of antioxidant 264,8 parts of zinc stearate, 5 parts of barium stearate, hydroxyl value 20~
4 parts of 10 parts of the polyether modified silicon oil of 80mgKOH/g, diisooctyl phthalate or diisooctyl phenyl phosphite addition reactions
In kettle, 80 DEG C are to slowly warm up to, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyls are then added
12 parts of piperidines -1- oxygen radical, continue stirring form homogeneous solution, add 2 parts of methyl tin, 3 parts of sorbitan tristearate,
5 parts and 3 parts of polyoxyethylene sorbitan carboxylic ester of fatty alcohol polyoxyethylene ether are continued to stir 5min, and the deionization of surplus is added
Water, then quickly stirring 0.5h.It is most emulsified afterwards through emulsification pump, obtains product 2#.
Embodiment 3
By 15 parts of antioxidant 1010,2 parts of irgasfos 168,16 parts of calcium stearate, 20~80mgKOH/g of hydroxyl value polyethers
In 5 parts of 4 parts of modified silicon oil, diisooctyl phthalate or diisooctyl phenyl phosphite addition reaction kettles, it is to slowly warm up to
80 DEG C, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyl piperidine -1- oxygen radicals are then added
18 parts, continues stirring and form homogeneous solution, add 0.5 part of methyl tin, 1 part of sorbitan tristearate, fatty alcohol polyoxy second
7 parts of alkene ether, 1 part of polyoxyethylene sorbitan carboxylic ester continue stir 10min, the deionized water of surplus is added, then quickly stir
Mix 1h.It is most emulsified afterwards through emulsification pump, obtains product 3#.
Embodiment 4
By 10 parts of antioxidant 1010,6 parts of irgasfos 168,8 parts of magnesium stearate, 3 parts of aluminum stearate, hydroxyl value 20~
3 parts of 8 parts of the polyether modified silicon oil of 80mgKOH/g, diisooctyl phthalate or diisooctyl phenyl phosphite addition reactions
In kettle, 60 DEG C are to slowly warm up to, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyls are then added
15 parts of piperidines -1- oxygen radical, continue stirring form homogeneous solution, add 3 parts of methyl tin, 2 parts of sorbitan tristearate,
5 parts of fatty alcohol polyoxyethylene ether, 8 parts of polyoxyethylene sorbitan carboxylic ester continue stir 10min, the deionization of surplus is added
Water, then quickly stirring 1h.It is most emulsified afterwards through emulsification pump, obtains product 4#.
Embodiment 5
By 8 parts of antioxidant 1010,8 parts of antioxidant 264,12 parts of zinc stearate, 3 parts of calcium stearate, hydroxyl value 20~
3 parts of 8 parts of the polyether modified silicon oil of 80mgKOH/g, diisooctyl phthalate or diisooctyl phenyl phosphite addition reactions
In kettle, 50 DEG C are to slowly warm up to, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2,6,6- tetramethyls are then added
15 parts of piperidines -1- oxygen radical, continue stirring form homogeneous solution, add 3 parts of methyl tin, 1 part of sorbitan tristearate,
2 parts of fatty alcohol polyoxyethylene ether, 8 parts of polyoxyethylene sorbitan carboxylic ester continue stir 10min, the deionization of surplus is added
Water, then quickly stirring 1h.It is most emulsified afterwards through emulsification pump, obtains product 5#.
The terminator the performance test results and commercially available similar terminator that embodiment 1-5 is obtained (contain diethyl hydroxylamine, bisphenol-A
Water and milk terminator) test comparison is as follows:
* according to the actual measurement solid content of embodiment and commercially available similar terminator, identical solid content is diluted to water ion water.
Claims (8)
1. a kind of aqueous emulsion type polyvinyl chloride resin and vinyl chloride-vinyl acetate resin terminator, it is characterised in that by following mass parts on the basis of 100 parts
Group be grouped as:
Surplus is deionized water.
2. terminator according to claim 1, it is characterised in that the composite antioxidant is by antioxidant 1010 and antioxygen
Agent 168 or antioxidant 1010 and antioxidant 264 form, wherein on the basis of 100 parts of terminator mass parts, the use of antioxidant 1010
Amount is 0.1~15 part, and irgasfos 168 dosage is 0.1~6 part, and antioxidant 264 dosage is 0.1~8 part.
3. terminator according to claim 1, it is characterised in that the compound emulsifying agent by sorbitan tristearate,
Fatty alcohol polyoxyethylene ether and polyoxyethylene sorbitan carboxylic ester composition, wherein on the basis of 100 parts of terminator mass parts,
Sorbitan tristearate dosage is 0.5~8 part, and fatty alcohol polyoxyethylene ether dosage is 0.5~7 part, polyoxyethylene sorbitol
Acid anhydride aliphatic ester dosage is 0.5~9 part.
4. terminator according to claim 1, it is characterised in that the heat stabilizer is by stearate and methyl tin group
At wherein stearate dosage is 1~20 part on the basis of 100 parts of terminator mass parts, methyl tin dosage is 0.1~3 part.
5. terminator according to claim 4, it is characterised in that the stearate be zinc stearate, calcium stearate,
One of magnesium stearate, aluminum stearate, barium stearate or combinations thereof.
6. terminator according to claim 1, it is characterised in that the dispersing agent is by extraordinary silicone oil and phthalic acid
Di-isooctyl or extraordinary silicone oil and diisooctyl phenyl phosphite form, wherein on the basis of 100 parts of terminator mass parts, it is extraordinary
Silicon oil dosage is 2~10 parts, and the dosage of diisooctyl phthalate or diisooctyl phenyl phosphite is 0.2~5 part.
7. terminator according to claim 1, it is characterised in that the extraordinary silicone oil is 20~80mgKOH/g's of hydroxyl value
Polyether modified silicon oil.
8. a kind of terminator preparation method as claimed in claim 1, it is characterised in that the following steps are included:
Composite antioxidant, heat stabilizer stearate, dispersing agent are added in reaction kettle by composition amounts first, are to slowly warm up to 50
~80 DEG C, insulated and stirred dissolves solid component all, and 4- hydroxyl -2,2 is then added, and 6,6- tetramethyl piperidine -1- oxygen are free
Base, formed homogeneous solution, add heat stabilizer methyl tin, compound emulsifying agent continue stir 5min~10min, surplus is added
Deionized water, then quickly 0.5~1h of stirring；It is most emulsified afterwards through emulsification pump, aqueous emulsion type polyvinyl chloride resin is made and vinyl chloride-vinyl acetate resin terminates
Agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910426851.5A CN110092850B (en) | 2019-05-22 | 2019-05-22 | Aqueous emulsion type PVC resin and vinyl chloride-vinyl acetate terminator and preparation method thereof |
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| CN201910426851.5A CN110092850B (en) | 2019-05-22 | 2019-05-22 | Aqueous emulsion type PVC resin and vinyl chloride-vinyl acetate terminator and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830986A (en) * | 2020-12-27 | 2021-05-25 | 新沂市星辰新材料科技有限公司 | PVC (polyvinyl chloride) terminator capable of improving whiteness and aged whiteness and preparation method thereof |
| CN115246986A (en) * | 2021-04-26 | 2022-10-28 | 中国石油化工股份有限公司 | Heat stabilizer, transparent PVC resin and preparation method |
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| CN112830986A (en) * | 2020-12-27 | 2021-05-25 | 新沂市星辰新材料科技有限公司 | PVC (polyvinyl chloride) terminator capable of improving whiteness and aged whiteness and preparation method thereof |
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