CN106749795A - A kind of preparation method of Corvic - Google Patents
A kind of preparation method of Corvic Download PDFInfo
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- CN106749795A CN106749795A CN201610564409.5A CN201610564409A CN106749795A CN 106749795 A CN106749795 A CN 106749795A CN 201610564409 A CN201610564409 A CN 201610564409A CN 106749795 A CN106749795 A CN 106749795A
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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
- 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
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- Medicinal Chemistry (AREA)
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- Polymerisation Methods In General (AREA)
Abstract
A kind of preparation method of Corvic.It is characterized in that by water, VCM, compound dispersing agent, porosity controlling agent, chain-transferring agent, PH buffers and initiator addition polymeric kettle, under the pressure of 1.00 1.20MPa, it is provided with the polymerization reaction kettle of agitating device, polymerisation is carried out at 55 DEG C 70 DEG C, when keeping polymerization temperature to polymerization pressure 0.1 0.25MPa of decline, add reaction terminating agent, the remaining VCM of discharge that target product is then collected from product；Wherein described compound dispersing agent is the polyvinyl alcohol of two kinds of partial alcoholysis and the mixture of hydroxypropyl methyl cellulose.Using Corvic gas porosity is high obtained in the method that the present invention is announced, flake is few, epithelium coverage rate is low, and particle shape is regular, resin centralized particle diameter, easily removes residual monomer.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of preparation method of Corvic.
Background technology
Polyvinyl-chloride of low-polymerization degree (PVC) resin, generally refers to polyvinyl chloride (PVC) resin of the degree of polymerization below 800.
Because its molecular weight is low, apparent density is high, melt fluidity is good, fusion time is short, it is easy to the features such as processing, manufacture sheet material,
Extensively should have in terms of injection molding pipe part, blow molding and modified resin (chlorinated polyvinyl chloride resin is produced in such as depth chlorination)
With.
But, PVC resin with low degree of polymerization porosity is low, and resin particle is tightr, and dispersant is produced with chloride graft copolymerization
Raw particle epithelium is thicker, influences the processing characteristics of resin and is further modified.
Chlorination modified treatment, obtained chliorinated polyvinyl chloride (CPVC) resin tool are carried out to PVC resin with low degree of polymerization
Have excellent heat resistance, typically can at a high temperature of 95 DEG C long-term use, higher than 35 DEG C or so of PVC product.CPVC resins are made
For a kind of heat-resistant engineering plastic of function admirable is extruding the aspects such as heat-resisting pipes, sheet material or injection heat pipe connecting piece at home and abroad
Obtain extensive use.During chlorination PVC production CPVC resins, in order to improve the processing flowability of gained CPVC resins
And product properties, except chloridization process is improved, improve outside chlorination technique level, from the PVC resin with low degree of polymerization of suitable chlorination
It is critical that, in order that polyvinyl chloride resin is conducive to chlorination, it is desirable to which polyvinyl chloride resin is loose, internal void is more and uniform, and epithelium is most
(discontinuous, local exposed) may be lacked, granule regularizing degree is good.CPVC PVC resin speciallies have following spy in structure and performance
Point：(1) resin polymerization degree is relatively low.(2) resin apparent density is relatively low, and short texture, porosity is high.(3) epithelium of resin particle
It is thin as much as possible, or even few skin or without skin.
Loose porous, the resin that epithelium coverage rate the is low method of manufacture is matched somebody with somebody mainly around the adjustment to polymer dispersion system
With the change of power of agitator, PVC granulation process is controlled.
B.F.Goodrich chemical companies of the U.S. are proposed patent skill of many manufactures without skin or few skin porous PVC resin
Art, such as US4,711,908, US4,775,701, US4,775,702, US4,742,085 etc., the technology is in suspension polymerization of VC
Applied in system, the special dispersion for being used mainly constitutes as follows：A () a kind of can make that aqueous medium thickens it is unneutralized from
Sub- sensitiveness dispersant makees main dispersant；The polyvinyl alcohol of (b) certain alcoholysis degree；When VCM conversion ratios are 1-5%, foot is added
A kind of ionic compound of enough amounts, this ionic compound will account for the main dispersion of major amount of ion-sensitive in dispersion
Agent is got off from VCM droplet surface desorptions, to produce without skin or few skin, the polyvinyl chloride resin of high porosity.The technology uses dispersant
Kind is more special, complex operation, it is more difficult to control granulation process, situations such as coarse fodder easily occur, seize.
Shanghai chlor-alkali delivers patent and produces high porosity resin, CN1927898A, a kind of low alcoholysis level, low viscous PVA
A kind of compound dispersing agent constituted with HPMC, porosity controlling agent is auxiliary agent, carries out suspension polymerization of VC, is produced high loose
Degree resin, but resin surface epithelium exposed part is less, and internal void is less and skewness.
The patent CN87 of domestic Zhejiang University, 1,01663A with magnesium hydroxide as main dispersant, of different nature with two classes
Dispersant supplemented by porosity controlling agent, with water-soluble inorganic salt as auxiliary agent, carries out suspension polymerization of VC, prepares loose, nothing and connects
Epithelium and apparent density polyvinyl chloride particles high that graft copolymer is formed, and the method for reducing kettle pasting matter, but resin particle is very
Slightly, technology there is no method application.
The content of the invention
The technical problem to be solved in the invention is to provide a kind of preparation method of Corvic, obtained polychlorostyrene second
Olefine resin gas porosity is high, flake is few, and epithelium coverage rate is low, and particle shape is regular, resin centralized particle diameter, and easily removing residual is single
Body.
A kind of preparation method of Corvic of the present invention, is by water, VCM, composite dispersing agent, porosity
Conditioning agent, chain-transferring agent, PH buffers and initiator are added in polymeric kettle, under the pressure of 1.00-1.20MPa, are provided with stirring
In the polymerization reaction kettle of device, carry out polymerisation at 55 DEG C-70 DEG C, keep polymerization temperature to polymerization pressure decline 0.1-
During 0.25MPa, reaction terminating agent is added, discharge remnants VCM monomers, target product is then collected from product.
Described compound dispersing agent is the polyvinyl alcohol and hydroxypropyl methyl cellulose of two kinds of partial alcoholysis（HPMC）'s
Mixture；
Two kinds of described polyvinyl alcohol of partial alcoholysis include that a kind of alcoholysis degree high, the polyvinyl alcohol (I) of middle viscosity and one kind are low
Alcoholysis degree, high-viscosity polyvinyl alcohol (II)；
Described alcoholysis degree high, the alcoholysis degree of the PVAC polyvinylalcohol (I) of middle viscosity are 70-90% (molar fraction), preferably
78-82%, viscosity is preferably 40-55 mPa.s (at 20 DEG C, being determined during 4% concentration).This dispersant can make the surface of system
Power reduction, plays a part of the colloid protection ability and dispersibility of coordination system, polymerization system is being kept certain protection drop
While power, dispersibility is taken into account, prevent viscous kettle, hang oar.
Described low alcoholysis level, the alcoholysis degree of high-viscosity PVAC polyvinylalcohol (II) are 40-50% (molar fraction), most
It is well 42-46%, viscosity is preferably 60-120mPa.s (at 25 DEG C, being determined during 35% concentration).This dispersant is in oil-soluble,
Influence can be produced on the primary particle in polyvinyl chloride particles and its aggregation, improve resin particle during chloroethylene polymerization
Porousness, improve resin internal void uniformity, reduce resin particle surfaces epithelium fold situation.
The methoxyl content of described HPMC is 20-40%, preferably 25-35%；Hydroxypropyl content 5-15%, preferably
5—10%.Viscosity is 30-70mPa.s (20 DEG C, determined during 2% concentration), best 40-60 mPa.s；HPMC is played in system
Dispersion VCM drop effects, while having certain protective role to VCM drops, being attached to VCM droplet surfaces can preferably coordinate drop point
- coalescence is dissipated, coarse fodder is prevented out.
Alcoholysis degree high, the consumption of middle viscosity PVA (I) are 0.001-the 0.10% of VCM weight, preferably
0.01—0.03%；
Low alcoholysis level, the consumption of high-viscosity PVAC polyvinylalcohol (II) are 0.001-the 0.15% of VCM weight, best
For 0.04-0.14%；
The consumption of HPMC is 0.001-the 0.10% of VCM weight, preferably 0.02-0.06%.
Described porosity controlling agent is selected from sorbitan fatty acid fat, to use Span60 effect
Preferably, wherein sorbitan fatty acid fat hydrophilic and oleophilic value HLB is 2.0-9.0, and best 3.0-6.0.Above-mentioned porosity is adjusted
After in section agent addition system, because its lipophile is stronger, molecular radical is penetrated into inside monomer droplet, between can preventing primary particle
Frequent coalescence, eliminates agglomerate, while polymerization system lipophile can be increased, promotes the hydrophilic segment in dispersant to VCM liquid
Drop diffusion inside, and then the epithelium coverage rate of resin surface is reduced, porosity controlling agent consumption is VCM weight
0.005-0.50%, preferably 0.01-0.20%;
Chain-transferring agent is selected from mercaptan compound, trichloro ethylene, carbon tetrachloride and the chloro- 1- iodoethane of 1- etc., wherein to use mercaptan
Preferably, mercaptan compound can be 2 mercapto ethanol, thioglycollic acid-2-ethyl hexyl ester, isooctyl thioglycolate, second two to compound
The mercaptan type chain transfer agents such as alcohol dimercapto acetic acid esters, wherein again with 2 mercapto ethanol as best.Chain-transferring agent consumption is about chloroethene
0.001-the 0.20% of alkene monomer weight, preferably 0.005-0.15%.Chain-transferring agent can once be added before polymerization,
Can be that a part is added before polymerization starts, another part starts certain hour and adds in polymerization, such as first adds gross weight
10-50%, when polymerisation conversion reaches 15-30%, add the chain-transferring agent of surplus；
PH buffers are selected from NaOH, sodium acid carbonate, ammonium hydrogen carbonate etc., maximum still for improving the contribution of resin gas porosity
Ammonium salt class PH buffers, preferably ammonium hydrogen carbonate, it can improve resin particle form, prevent the generation of resin involucra, improve tree
The regularity of fat particle, its addition are so that the PH controls of reaction system are advisable 5-8；
The water of addition and monomer weight ratio are 1.2/1 to 1.8/1, preferably 1.3/1 to 1.5/1, water-oil factor is too small, and polymerization is anti-
Should occur unstable, resin particle distribution broadens, and a large amount of bulky grains and " flake " occurs.The excessive then production efficiency drop of water-oil factor
It is low.
Initiator can select organic peroxide initiator or azo-initiator, can be the peroxidating tertiary fourth of new enanthic acid
Ester, peroxidating pivalic acid spy pentyl ester, peroxide tert pivalate ester, peroxy dicarbonate pair-(2- Octyl Nitrites), azo two are different
One or more in the initiators such as heptonitrile are combined, and its addition is 0.01-the 0.1% of VCM weight；
Reaction terminating agent is selected from acetone semicarbazone thiocarbamide, bisphenol-A, diethyl hydroxylamine or natrium nitrosum, and its addition is vinyl chloride
0.005-the 0.03% of monomer weight；
At 55 DEG C -70 DEG C, polymerization temperature determines PVC molecular weight for polymeric reaction temperature control, while polymerization temperature corresponds to VCM
Saturated vapor pressure, polymerization temperature is higher, and polymerization pressure is higher, and too high polymerization temperature has higher wanting to the pressure-resistant energy level of polymeric kettle
Ask.
The present invention uses compound dispersing agent, is coordinated with certain proportion, in addition the porosity of addition regulation resin voids rate
Conditioning agent, so that it is few (discontinuous, local without skin) to be obtained surface epithelium, loose and porous inner surface and even pore distribution, particle rule
It is whole, plasticizer absorption polyvinyl chloride resin high.
In suspension polymerization of VC, vinyl chloride (VCM) drop under stirring, is dispersed in water drawing through initiator
Send out and polymerisation occurs, generate polyvinyl chloride resin.Dispersant adsorption plays dispersion and protects the double of drop in monomer droplet top layer
Recast use, with stirring together with influence vinyl chloride drop dispersion and merging process, and to final resin surface epithelium, gas porosity,
The performances such as particle diameter produce influence.By converting dispersion, suitable dispersant proportioning is selected, to adjust dividing between water-liquid phase
- colloid protection ability is dissipated, being obtained has good particle characteristics, low epithelium coverage rate, the resin of high porosity.
High porosity, the resin of low epithelium coverage rate prepared using the above-mentioned method of the present invention, resin particle size are held
Easy to control, it is not easy to go out coarse fodder, industrial operation is strong, and resin melting is easily, few to plasticizer absorption very good, flake, tool
There is larger industrializing implementation prospect.
Embodiment 1
Polymerisation is two layers of flat paddle in stirring, and bottom insert canal and thermowell are baffle plate, and volume in the kettle of 5L to carry out.Technique bar
Part and process are summarized as follows：First 2.1Kg desalted waters, PVA (I) 0.19g, PVA (II) 0.68g, HPMC 0.68g, 0.7g are lost
Water sorbitan monostearate (HLB 4.7), 0.10g 2 mercapto ethanols, 0.5g ABVNs, 0.5g NH4HCO3Throw
Enter in kettle, stirring is started after pressure testing, VCM 1.4Kg are added after being evacuated to -0.90MPa, be warming up to 62 DEG C and start polymerization, keep
Polymerization temperature declines 0.15MPa to polymerization pressure, adds 0.3g diethyl hydroxylamine terminating reactions, is discharged after receipts monomer is pushed back certainly,
Polyvinyl chloride resin is obtained after centrifugal drying.
Above dispersant PVA (I) is alcoholysis degree 80% (molar fraction), the mPa.s of viscosity 48 (20 DEG C, determined under 4% concentration)
Polyvinyl alcohol；Dispersant PVA (II) is alcoholysis degree 45% (molar fraction), and viscosity is that (25 DEG C, survey 90 mPa.s under 35% concentration
Polyvinyl alcohol calmly)；Dispersant HPMC is methoxyl substitution 25%, hydroxypropyl substitution value 6%, viscosity 50 mPa.s (20 DEG C, 2%
Under concentration determine) HPMC.
Test result is as follows：K values 57, apparent density 0.48 (g/ml), 100g resin plasticizers absorb 28g, average grain diameter
115.0 (μm), the dispersion of distribution is 1.15.
Embodiment 2
The addition of dispersant PVA (I) is changed to 0.26g, dispersant PVA (II) addition is changed to 1.60g, and dispersant HPMC adds
Enter amount and be changed to 0.40g, other process conditions are with embodiment 1, and its test result is as follows：K values 58, apparent density 0.42 (g/ml),
100g resin plasticizers absorb 33g, and average grain diameter 110.0 (μm), the dispersion of distribution is 1.20.
Embodiment 3
The addition of dispersant PVA (I) is changed to 0.22g, dispersant PVA (II) addition is changed to 1.10g, and dispersant HPMC adds
Enter amount and be changed to 0.40g, other process conditions are with embodiment 1, and its test result is as follows：K values 57, apparent density 0.46 (g/ml),
100g resin plasticizers absorb 30g, and average grain diameter 113.0 (μm), the dispersion of distribution is 1.20.
Embodiment 4
The addition of dispersant PVA (I) is changed to 0.23g, dispersant PVA (II) addition is changed to 0.88g, and dispersant HPMC adds
Enter amount and be changed to 0.41g, 0.7g sorbitan monostearates, with embodiment 1, its test result is such as other process conditions
Under：K values 57, apparent density 0.49 (g/ml), 100g resin plasticizers absorb 24g, average grain diameter 125.0 (μm), the dispersion of distribution
It is 1.25.
Comparative example 1
It is alcoholysis degree 80% (molar fraction) to use dispersant PVA (I), and viscosity is 48 mPa.s (20 DEG C, 4% solution concentration condition
Under) polyvinyl alcohol, be not added with PVA (II), and be not added with porosity controlling agent；, with embodiment 1, test result is such as other process conditions
Under：K values 57, apparent density 0.53 (g/ml), 100g resin plasticizers absorb 20g, average grain diameter 120.0 (μm), the dispersion of distribution
It is 1.15, particle surface has compared with pachydermia film, and primary particle is invisible, and particle internal void is few, and agglomerate is more.
Claims (7)
1. a kind of preparation method of Corvic, it is characterised in that by water, VCM, compound dispersing agent, hole
Rate conditioning agent, chain-transferring agent, PH buffers and initiator are added in polymeric kettle, under the pressure of 1.00-1.20MPa, are provided with and are stirred
Mix in the polymerization reaction kettle of device, polymerisation is carried out at 55 DEG C -70 DEG C, keep polymerization temperature to decline 0.1- to polymerization pressure
During 0.25MPa, add reaction terminating agent, the remaining VCM of discharge that target product is then collected from product；Wherein
Described compound dispersing agent is the polyvinyl alcohol of two kinds of partial alcoholysis and the mixture of hydroxypropyl methyl cellulose, two kinds of portions
The polyvinyl alcohol of point alcoholysis include a kind of alcoholysis degree for 70-90% alcoholysis degree high, the poly- second of the middle viscosity of 40-55 mPa.s
Enol I and low alcoholysis level, the high-viscosity polyvinyl alcohol II of 60-120mPa.s, alcoholysis high that a kind of alcoholysis degree is 40-50%
Degree, the consumption of the polyvinyl alcohol I of middle viscosity are 0.001-the 0.10% of VCM weight, low alcoholysis level, high-viscosity poly-
The consumption of vinyl alcohol PVA II is 0.001-the 0.15% of VCM weight, and the consumption of hydroxypropyl methyl cellulose is chloroethene
0.001-the 0.10% of alkene monomer weight.
2. the preparation method of Corvic according to claim 1, it is characterised in that alcoholysis degree high, middle viscosity it is poly-
The consumption of vinyl alcohol I is 0.01-the 0.03% of VCM weight, low alcoholysis level, the use of high-viscosity PVAC polyvinylalcohol II
It is 0.04-the 0.14% of VCM weight to measure, and the consumption of hydroxypropyl methyl cellulose is VCM weight
0.02—0.06%。
3. the preparation method of Corvic according to claim 1, it is characterised in that described hydroxypropyl methyl is fine
The methoxyl content for tieing up element is 20-40%, hydroxypropyl content 5-15%, and viscosity is 30-70mPa.s.
4. the preparation method of Corvic according to claim 1, it is characterised in that described hydroxypropyl methyl is fine
The methoxyl content for tieing up element is 25-35%, hydroxypropyl content 5-10%, and viscosity is 40-60mPa.s.
5. the preparation method of Corvic according to claim 1, it is characterised in that described porosity controlling agent
Selected from sorbitan fatty acid fat, fat hydrophilic and oleophilic value HLB is in 2.0-9.0, porosity controlling agent for sorbitan fatty acid
Consumption is 0.005-the 0.50% of VCM weight.
6. the preparation method of Corvic according to claim 1, it is characterised in that chain-transferring agent is selected from Thiolation
Compound, trichloro ethylene, carbon tetrachloride or the chloro- 1- iodoethane of 1-, chain-transferring agent consumption for VCM weight 0.001-
0.20%。
7. the preparation method of Corvic according to claim 6, it is characterised in that chain-transferring agent is using Thiolation
Compound, mercaptan compound can be 2 mercapto ethanol, thioglycollic acid-2-ethyl hexyl ester, isooctyl thioglycolate or ethylene glycol two
Mercaptoacetate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236065A (en) * | 2017-06-06 | 2017-10-10 | 滁州市宏源喷涂有限公司 | One kind avoids the method that " flake " is produced in PVC Production Process |
| CN108192001A (en) * | 2017-12-26 | 2018-06-22 | 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) | A kind of preparation method of polyvinyl chloride resin used for chlorination |
| CN114716594A (en) * | 2022-04-12 | 2022-07-08 | 新疆圣雄氯碱有限公司 | Process for producing polyvinyl chloride resin |
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| CN1389483A (en) * | 2002-06-25 | 2003-01-08 | 上海氯碱化工股份有限公司 | Suspension polymerization process of preparing polyvinyl chloride resin with high molecular weight |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107236065A (en) * | 2017-06-06 | 2017-10-10 | 滁州市宏源喷涂有限公司 | One kind avoids the method that " flake " is produced in PVC Production Process |
| CN108192001A (en) * | 2017-12-26 | 2018-06-22 | 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) | A kind of preparation method of polyvinyl chloride resin used for chlorination |
| CN114716594A (en) * | 2022-04-12 | 2022-07-08 | 新疆圣雄氯碱有限公司 | Process for producing polyvinyl chloride resin |
| CN114716594B (en) * | 2022-04-12 | 2023-09-19 | 新疆圣雄氯碱有限公司 | Production method of polyvinyl chloride resin |
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Application publication date: 20170531 |