CN107501575A - A kind of preparation technology of modified PVA mixed solution - Google Patents
A kind of preparation technology of modified PVA mixed solution Download PDFInfo
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- CN107501575A CN107501575A CN201710823851.XA CN201710823851A CN107501575A CN 107501575 A CN107501575 A CN 107501575A CN 201710823851 A CN201710823851 A CN 201710823851A CN 107501575 A CN107501575 A CN 107501575A
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- pva
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or 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 alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Graft Or Block Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation technology of modified PVA mixed solution, it is related to polyvinyl alcohol modification technical field.The preparation technology of the modified PVA mixed solution of the present invention comprises the following steps：(1) PVA is pre-processed：PVA powder is weighed, adds purified water, stirring obtains the PVA aqueous solution；(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, heating, add silane coupler and chain extender, insulation, add chain terminating agent, obtain the suspension solution of PVA surface graftings；(3) mechanical mixture：Comonomer is added into the suspension solution of PVA surface graftings, temperature reaction, demulsifier stirring demulsification is added, obtains the modified PVA mixed solution.The preparation technology of the present invention is reasonable in design, saves energy consumption, and mixed solution can obtain the PVC functional membranes of water resistance, temperature tolerance, good mechanical performance after post processing, expand the application of polyvinyl alcohol.
Description
Technical field：
The present invention relates to polyvinyl alcohol modification technical field, and in particular to a kind of preparation technology of modified PVA mixed solution.
Background technology：
Polyvinyl alcohol (PVA) is a kind of important high molecular weight water soluble polymer, and its purposes is broadly divided into fiber and non-fibre
Tie up two broad aspects.The initial purposes of polyvinyl alcohol is mainly used for synthetic fibers, and the effect of polyvinyl alcohol in recent years is gradually to non-
Machine direction develops.Due to the water resistance and less stable of polyvinyl alcohol, its application is have impact on to a certain extent.Pass through
Polyvinyl alcohol is modified, improves the performance of polyvinyl alcohol, develops high value added product, it is competing to the market of raising polyvinyl alcohol
Power is striven, promotes the development of polyvinyl alcohol industry significant.In the prior art, mainly by being etherified, being acidified to polyethylene
Alcohol is modified, but obtained materials water-resistant, gumminess, film forming is poor, it is necessary to further study.
The content of the invention：
The technical problems to be solved by the invention be to provide one kind can improve Water-Resistance of PVA, gumminess and into
The preparation technology of the modified PVA mixed solution of film.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, adds the purified water of 3~5 times of its quality, 60~80 DEG C of stirrings 30~
40min, it is standby to obtain the PVA aqueous solution；
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 40~50 DEG C is warming up to, adds appropriate acetic acid second
Ester, adds silane coupler and chain extender, after insulation 2~3 hours, adds chain terminating agent, 30~50min of normal-temperature reaction,
A small amount of glycerine increase stickiness is added, continues 20~30min of stirring, obtains the suspension solution of PVA surface graftings；Wherein, PVA water
Solution, silane coupler, chain extender, the mass ratio of chain terminating agent are 10~20：3~8：0.2~0.7：0.3~0.6；
(3) mechanical mixture：Comonomer is added into the suspension solution of PVA surface graftings, is warming up to 50~60 DEG C, is kept
800~1000r/min rotating speed, after being incubated 2~4 hours, demulsifier stirring demulsification is added, cooling and standings obtain the modified PVA
Mixed solution.
Preferably, the PVA aqueous solution 20~30min of vacuumize process, sealed storage is in 8~16 DEG C of antistaling cabinet.
Preferably, the silane coupler is selected from glycidyl ether oxygen propyl trimethoxy silicane, 3- aminopropyl trimethoxies
It is one or more in base silane, 3- aminopropyl triethoxysilanes, propyl trimethoxy silicane, propyl-triethoxysilicane
Combination.
Preferably, one kind in hydrogenated bisphenol A, resorcinol hydroxy ether, methyl diethanolamine of the chain extender or
A variety of combinations.
Preferably, the chain terminating agent is selected from SDD or phenyl-β-naphthylamine.
Preferably, step (3) comonomer is methyl methacrylate, methyl acrylate, butyl acrylate, propylene
One or more combinations in the different monooctyl ester of acid, lauryl methacrylate, n octyl methacrylate.
Preferably, step (3) demulsifier is sodium chloride or potassium chloride.
The beneficial effects of the invention are as follows：The preparation technology of the modified PVA mixed solution of the present invention, is made water by PVA first
Solution, then by silane coupler, chain extender, chain terminating agent carry out PVA surface graft modification, then add comonomer enter
One step is modified, and technological design is reasonable, saves energy consumption, and mixed solution can obtain water resistance, temperature tolerance, mechanics after post processing
The PVC functional membranes of function admirable, expand the application of polyvinyl alcohol.
Embodiment：
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 3 times of its quality is added, 66 DEG C of stirring 35min, obtains PVA
The aqueous solution, vacuumize process 25min, sealed storage are standby in 10 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 46 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler 3- aminopropyl trimethoxysilanes and chain extender hydrogenated bisphenol A are added, after being incubated 2.5 hours, adds chain end
Only agent phenyl-β-naphthylamine, normal-temperature reaction 38min, a small amount of glycerine increase stickiness is added, continues to stir 27min, obtains PVA tables
The suspension solution of face grafting；Wherein, the PVA aqueous solution, silane coupler, chain extender, the mass ratio of chain terminating agent are 12：5：
0.4：0.5.
(3) mechanical mixture：Comonomer methacrylic acid lauryl is added into the suspension solution of PVA surface graftings, is risen
Temperature keeps 800~1000r/min rotating speed to 50 DEG C, after insulation 2.5, adds the stirring demulsification of demulsifier potassium chloride, cooling and standings
Obtain the modified PVA mixed solution.
Embodiment 2
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 3.6 times of its quality is added, 70 DEG C of stirring 35min, obtains
The PVA aqueous solution, vacuumize process 25min, sealed storage are standby in 12 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 48 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler 3- aminopropyl triethoxysilanes and chain extender methyl diethanolamine are added, after being incubated 2.6 hours, adds chain
Terminator SDD, normal-temperature reaction 40min, a small amount of glycerine increase stickiness is added, continues to stir
28min, obtain the suspension solution of PVA surface graftings；Wherein, the matter of the PVA aqueous solution, silane coupler, chain extender, chain terminating agent
Amount ratio is 15：6：0.6：0.5.
(3) mechanical mixture：Comonomer methacrylic acid n-octyl is added into the suspension solution of PVA surface graftings, is risen
Temperature keeps 800~1000r/min rotating speed to 58 DEG C, after being incubated 3 hours, adds the stirring demulsification of demulsifier sodium chloride, cooling is quiet
Put to obtain the modified PVA mixed solution.
Embodiment 3
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 5 times of its quality is added, 72 DEG C of stirring 40min, obtains PVA
The aqueous solution, vacuumize process 27min, sealed storage are standby in 15 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 50 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler glycidyl ether oxygen propyl trimethoxy silicane and chain extender resorcinol hydroxy ether are added, is incubated 2.8 hours
Afterwards, chain terminating agent phenyl-β-naphthylamine is added, normal-temperature reaction 50min, a small amount of glycerine increase stickiness is added, continues to stir
30min, obtain the suspension solution of PVA surface graftings；Wherein, the matter of the PVA aqueous solution, silane coupler, chain extender, chain terminating agent
Amount ratio is 17：7：0.6：0.6.
(3) mechanical mixture：Comonomer methacrylic acid methyl esters, heating are added into the suspension solution of PVA surface graftings
To 60 DEG C, 800~1000r/min rotating speed is kept, after being incubated 4 hours, adds the stirring demulsification of demulsifier sodium chloride, cooling and standings
Obtain the modified PVA mixed solution.
Embodiment 4
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 5 times of its quality is added, 72 DEG C of stirring 40min, obtains PVA
The aqueous solution, vacuumize process 27min, sealed storage are standby in 15 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 50 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler 3- aminopropyl triethoxysilanes and chain extender methyl diethanolamine are added, after being incubated 2.8 hours, adds chain
Terminator SDD, normal-temperature reaction 50min, a small amount of glycerine increase stickiness is added, continues to stir
30min, obtain the suspension solution of PVA surface graftings；Wherein, the matter of the PVA aqueous solution, silane coupler, chain extender, chain terminating agent
Amount ratio is 18：5：0.3：0.4.
(3) mechanical mixture：Comonomer butyl acrylate is added into the suspension solution of PVA surface graftings, is warming up to 60
DEG C, 800~1000r/min rotating speed is kept, after being incubated 4 hours, adds the stirring demulsification of demulsifier sodium chloride, cooling and standings obtain
The modified PVA mixed solution.
Embodiment 5
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 5 times of its quality is added, 72 DEG C of stirring 40min, obtains PVA
The aqueous solution, vacuumize process 27min, sealed storage are standby in 15 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 50 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler propyl-triethoxysilicane and chain extender hydrogenated bisphenol A are added, after being incubated 2.8 hours, adds chain terminating agent
Phenyl-β-naphthylamine, normal-temperature reaction 50min, a small amount of glycerine increase stickiness is added, continues to stir 30min, obtains PVA surfaces and connect
The suspension solution of branch；Wherein, the PVA aqueous solution, silane coupler, chain extender, the mass ratio of chain terminating agent are 20：6：0.4：
0.5。
(3) mechanical mixture：Comonomer methacrylic acid n-octyl is added into the suspension solution of PVA surface graftings, is risen
Temperature keeps 800~1000r/min rotating speed to 60 DEG C, after being incubated 4 hours, adds demulsifier stirring demulsification, cooling and standings obtain
The modified PVA mixed solution.
Embodiment 6
A kind of preparation technology of modified PVA mixed solution, comprises the following steps：
(1) PVA is pre-processed：PVA powder is weighed, the purified water of 5 times of its quality is added, 72 DEG C of stirring 40min, obtains PVA
The aqueous solution, vacuumize process 27min, sealed storage are standby in 15 DEG C of antistaling cabinet.
(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 50 DEG C is warming up to, adds appropriate ethyl acetate, then
Silane coupler glycidyl ether oxygen propyl trimethoxy silicane and chain extender methyl diethanolamine are added, after being incubated 2.8 hours,
Chain terminating agent phenyl-β-naphthylamine is added, normal-temperature reaction 50min, a small amount of glycerine increase stickiness is added, continues to stir 30min,
Obtain the suspension solution of PVA surface graftings；Wherein, the mass ratio of the PVA aqueous solution, silane coupler, chain extender, chain terminating agent
For 20：8：0.7：0.5.
(3) mechanical mixture：Comonomer Isooctyl acrylate monomer is added into the suspension solution of PVA surface graftings, is warming up to
60 DEG C, 800~1000r/min rotating speed is kept, after being incubated 4 hours, adds demulsifier stirring demulsification, cooling and standings obtain this and changed
Property PVA mixed solutions.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
- A kind of 1. preparation technology of modified PVA mixed solution, it is characterised in that：Comprise the following steps：(1) PVA is pre-processed：PVA powder is weighed, adds the purified water of 3~5 times of its quality, 60~80 DEG C are stirred 30~40min, It is standby to obtain the PVA aqueous solution；(2) PVA surface graftings：The PVA aqueous solution is added in reaction bulb, 40~50 DEG C is warming up to, adds appropriate ethyl acetate, then Silane coupler and chain extender are added, after being incubated 2~3 hours, chain terminating agent is added, 30~50min of normal-temperature reaction, adds few Glycerine increase stickiness is measured, continues 20~30min of stirring, obtains the suspension solution of PVA surface graftings；Wherein, the PVA aqueous solution, Silane coupler, chain extender, the mass ratio of chain terminating agent are 10~20：3~8：0.2~0.7：0.3~0.6；(3) mechanical mixture：Comonomer is added into the suspension solution of PVA surface graftings, is warming up to 50~60 DEG C, keeps 800 ~1000r/min rotating speed, after being incubated 2~4 hours, demulsifier stirring demulsification is added, cooling and standings obtain modified PVA mixing Solution.
- 2. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：The PVA aqueous solution is taken out 20~30min of application of vacuum, sealed storage is in 8~16 DEG C of antistaling cabinet.
- 3. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：The silane coupler Selected from glycidyl ether oxygen propyl trimethoxy silicane, 3- aminopropyl trimethoxysilanes, 3- aminopropyl triethoxysilanes, third One or more combinations in base trimethoxy silane, propyl-triethoxysilicane.
- 4. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：The chain extender is selected from One or more combinations in hydrogenated bisphenol A, resorcinol hydroxy ether, methyl diethanolamine.
- 5. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：The chain terminating agent choosing From SDD or phenyl-β-naphthylamine.
- 6. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：Step (3) copolymerization Monomer is methyl methacrylate, methyl acrylate, butyl acrylate, Isooctyl acrylate monomer, lauryl methacrylate, methyl One or more combinations in n-octyl.
- 7. the preparation technology of modified PVA mixed solution according to claim 1, it is characterised in that：Step (3) demulsification Agent is sodium chloride or potassium chloride.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710823851.XA CN107501575A (en) | 2017-09-13 | 2017-09-13 | A kind of preparation technology of modified PVA mixed solution |
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| CN201710823851.XA CN107501575A (en) | 2017-09-13 | 2017-09-13 | A kind of preparation technology of modified PVA mixed solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558227A (en) * | 2022-09-13 | 2023-01-03 | 安徽瑞鸿新材料科技有限公司 | Thermoplastic processing method of polyvinyl alcohol composite material |
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2017
- 2017-09-13 CN CN201710823851.XA patent/CN107501575A/en not_active Withdrawn
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|---|---|---|---|---|
| JP2003171600A (en) * | 2001-09-27 | 2003-06-20 | Kyodo Printing Co Ltd | Gas-barrier coating composition and gas-barrier film |
| CN1847334A (en) * | 2005-04-11 | 2006-10-18 | 刘建林 | Modified PVA paint and its prepn process |
| CN101033355A (en) * | 2007-04-01 | 2007-09-12 | 浙江比例包装股份有限公司 | Polyvinyl alcohol coating liquid capable of holding strong oxygen obstruction at high humidity and producing process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115558227A (en) * | 2022-09-13 | 2023-01-03 | 安徽瑞鸿新材料科技有限公司 | Thermoplastic processing method of polyvinyl alcohol composite material |
| CN115558227B (en) * | 2022-09-13 | 2024-01-12 | 安徽瑞鸿新材料科技有限公司 | Thermoplastic processing method of polyvinyl alcohol composite material |
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