CN108841231A - A kind of rubber-type PE protection film parting agent and preparation method thereof - Google Patents
A kind of rubber-type PE protection film parting agent and preparation method thereof Download PDFInfo
- Publication number
- CN108841231A CN108841231A CN201810777974.9A CN201810777974A CN108841231A CN 108841231 A CN108841231 A CN 108841231A CN 201810777974 A CN201810777974 A CN 201810777974A CN 108841231 A CN108841231 A CN 108841231A
- Authority
- CN
- China
- Prior art keywords
- rubber
- type
- reflux
- flask
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- 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
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention discloses a kind of rubber-type PE protection film parting agents and preparation method thereof.Rubber-type PE prepared by the present invention protects film parting agent, and actually a kind of acrylate modified silicone release agent, it can realize crosslinking curing lower than 110 DEG C or under room temperature；Simultaneously as release effectiveness more special possessed by modified, especially to the release effect of rubber pressure sensitive glue, so that the uncoiling power of rubber-type PE protective film or other similar adhesive tape can control the range in needs.In addition, being greatly decreased due to easily shifting the opposite of composition in rubber-type PE protection film parting agent coating of the invention, so that the residual adhesion rate of pressure sensitive adhesive can be maintained at higher level.
Description
Technical field
The present invention relates to a kind of mould release and preparation method thereof, specifically a kind of rubber-type PE protects film parting agent
And preparation method thereof.The mould release can be coated on PE film or other substrates, to rubber pressure-sensitive adhesive have be suitable for
Release effect.
Background technique
Mould release is for preventing its stick to each other, or make the adhesion intensity control of both between two kinds of materials (medium)
The general name in a kind of material of required numerical value is made, there are many type.From material point, mould release is divided into inorganic type and organic
Type；There are internal lubrication type and external isolated form from usage mode point.Mould release commonly used in pressure sensitive adhesive product industry is mainly
Organic mould release, the major way of generation effect are external isolation --- as surface is coated with.
Organic mould release mainly includes organosilicon mould release, Organic fluoride mould release and other organic mould releases；Pressure-sensitive
Glue product industry, most widely used with silicone release agent, dosage is maximum, and using effect is best.
Silicone release agent can be divided into solvent type, emulsion-type and no-solvent type three categories.Use scope is most wide at home
It is solvent type and emulsion-type, no-solvent type is also in certain fields using more and more.Solvent type and no-solvent type are mainly used for thin
Film, emulsion-type are mainly used for paper.
Solvent type and no-solvent type silicone release agent, based on addition, using platinum as catalyst, at 140 DEG C or more, with
And heat cure is realized under~25 seconds time.It is for implementing coating waste water on the substrate for being resistant to such process conditions
Feasible.But if substrate is polyethylene (PE) film, such process conditions can make polyethylene (PE) deformation of thin membrane
Even melt.Therefore solvent type and no-solvent type silicone release agent are not suitable for PE film.It then, it is contemplated that should
Using the anti-adhesion performance that paper release silicone is excellent, the coating crosslinking condition of mould release is made to drop to what PE film was able to bear again
It is horizontal, it is necessary to silicone release agent is modified from molecular structure, i.e., should retain polysiloxanes in the molecular structure
Segment will also introduce group that can be crosslinked at 110 DEG C or less such as amino, hydroxyl, carboxyl etc..
Modified organic silicon mould release is prepared there are many method, the method according to the selection of purpose difference is different.The mesh of this modification
Object be for PE film, and should be guaranteed to be easy uncoiling, control again for the mould release to rubber pressure-sensitive adhesive
In uncoiling power range appropriate, so that the coating of protective film produces, cutting and use process are gone on smoothly.Also consider simultaneously
The adhesion strength of reduction pressure sensitive adhesive that all can be different degrees of to organosilicon anti-adhesive coating, and the main reason for causing such result, is
Caused by the small molecule organosilicon transfer not being crosslinked.Accordingly, it is considered to polyfunctionality siloxanes is introduced on acrylate molecule, then
By this polyfunctionality silicone acrylate and other (hydroxyl) acrylic ester copolymers, acrylate modified organosilicon is obtained
Mould release, then crosslinking method appropriate is used, by coating drying etc., can be formed on PE film release with release effect
Agent coating.
Summary of the invention
In order to solve technical problem in the prior art, the present invention provides a kind of rubber-type PE to protect film parting agent,
Technical solution is as follows：
The preparation process of rubber-type PE protection film parting agent of the invention is divided into two steps, and the first step is polyfunctionality silicon oxygen
The synthesis of alkane acrylate monomer；Second step is the monomer for obtaining the first step and other esters of acrylic acid and other vinyl
Class monomer is copolymerized to obtain mould release of the present invention.
(1) preparation of polyfunctionality allyl acyloxy siloxanes (A)：By allyl acyloxy silane, alkylalkoxy silane,
Water and catalyst are reacted to obtain product polyfunctionality allyl acyloxy siloxanes (A) under polymerization inhibitor effect.Reaction temperature
Control is at 35--95 DEG C.
(2) rubber-type PE protects the preparation of film parting agent：By A, hydroxy acrylate, (methyl) acrylate, benzene second
Alkene, in organic solvent, copolymerization obtains rubber-type PE protection film parting agent under the action of initiator.
On the basis of above-mentioned principle technical solution, the present invention has also done following improvement.
Further, step (1) the allyl acyloxy silane, alkylalkoxy silane, water and acidic catalyst, inhibiting
The lower hydrolysis carried out between silane molecule of agent effect, reaction temperature control gradually steams low at 35--95 DEG C, in reaction process
The reaction product of boiling point.
Siloxane functionality number as needed, component design.Determine comparing for each key reaction material and catalyst
Example determines the volatile component that reaction generates, determines reaction temperature according to reactant used, determines and completes evaporation (reaction life
At) volatile component temperature and time.
Charging sequence, charging process will have a direct impact on the trend of hydrolysis product.The present invention this step the characteristics of
In：First allyl acyloxy silane is added in reaction kettle, is then added after polymerization inhibitor stirring and dissolving, alkyl alkoxy silicon is added
Alkane.Catalyst is first dissolved in water, the mode for taking side border ring to be added dropwise is added.
By the amount for steaming low boiling point reaction product of collection, the degree that reaction carries out is determined.
Further, the allyl acyloxy silane, can be：Methallyl monomethacryloxypropyl methyl dimethoxysilane, first
One of base allyl monomethacryloxypropyl ethyldimethoxysilane, methallyl monomethacryloxypropyl trimethoxy silane are a variety of mixed
Close object；
Further, the alkylalkoxy silane, can be：Methyltriethoxysilane, methyltrimethoxysilane, second
One of ethyl triethoxy silicane alkane, ethyl trimethoxy silane or a variety of mixtures；
Further, the water uses distilled water；
Further, the acidic catalyst, can be：Trifluoromethanesulfonic acid, p-methyl benzenesulfonic acid, trifluoroacetic acid, in hydrochloric acid
One kind；
Further, the polymerization inhibitor is one of hydroquinone, 1,4-benzoquinone, p-tert-Butylcatechol；
Further, the additional amount (water brought into including other raw materials) of the water is with silane all in reaction system point
For the percent hydrolysis of alkoxy grp come what is determined, the present invention controls percent hydrolysis within 80% in son；
Further, described that catalyst is first dissolved in water, the mode being gradually added dropwise during the reaction is taken, control exists
It completes to be added dropwise in 5-15 minutes；
Further, low-boiling reaction product is gradually steamed in the reaction process, in the present invention, this kind of product is exactly
Refer to alcohols, such as ethyl alcohol or methanol, just has for different alcohol and different finally steam temperature；
Further, the step (2) is that step (1) is reacted obtained polyfunctionality allyl acyloxy siloxanes, with (first
Base) acrylate, styrene etc., in organic solvent, copolymerization obtains acrylate modified organosilicon under the action of initiator
Mould release；
Further, the polyfunctionality allyl acyloxy siloxanes actually still contains a certain proportion of alkoxy,
These alkoxies still have the characteristic of hydrolyzable condensation；
Further, described (methyl) acrylate：It can be methyl methacrylate, methyl acrylate, methacrylic acid
Ethyl ester, methyl acrylate, two or more in butyl acrylate；
Further, the organic solvent refers to one or both of ethyl acetate, butyl acetate, toluene or three kinds
Mixture；
Further, the initiator is one of benzoyl peroxide (BPO), azodiisobutyronitrile (AIBN)；
Further, it is described copolymerization obtain rubber-type PE protection film parting agent, the main body of quality be esters of acrylic acid and
The copolymer of other a small amount of vinyl-containing monomers, and silicone portion is the smaller portions of quality, but finally generates release effect
Be still silicone portion, other polymers play synergistic effect.Therefore product is still known as by the present invention：Acrylate
Modified organic silicon mould release；
Further, the rubber-type PE protects film parting agent, wherein the acidic catalyst of step (1) is still remained,
This is beneficial to the wet cross-linking process of release coating, improves to the intensity of release coating advantageous；
Further, the rubber-type PE protects film parting agent, and in application test, needing to be diluted to solvent is needed
The solid content wanted, and using isocyanates as crosslinking agent, then be coated on PE film, at drying curing
Reason just will form the mould release coating with corresponding release effect, for rubber-type using the natural aging of certain time
Pressure sensitive adhesive plays the role of appropriate release；.
Specific embodiment
Below by way of specific preferred embodiment, invention is further described in detail, but the present invention be not limited in it is following
Embodiment.
Embodiment one
(1) preparation of polyfunctionality allyl acyloxy siloxanes (A)：
By weight into the four-hole boiling flask equipped with heating device, reflux condenser, thermometer, dropping funel and blender
It is added：7.7 parts of methallyl monomethacryloxypropyl trimethoxy silane, 82.3 parts of methyltrimethoxysilane, 0.2 part of hydroquinone,
8.0 parts of distilled water, and start blender.0.08 part of concentrated hydrochloric acid (C=37%Wt) is dissolved in 2 parts of distilled water, is then turned
It moves on to stand-by among dropping funel.At room temperature, the liquid in dropping funel is at the uniform velocity instilled in flask with 5 minutes time,
With the progress of dropwise addition, the temperature meeting nature of reaction mass rises, and starts to flow back at 68 DEG C, will be anti-after heat preservation reflux 30 minutes
It answers temperature of charge to be reduced to 65 DEG C, stops stirring, and reflux condenser is replaced with distillation condenser pipe, prepare collection reaction and generate
Lighter component.Restart to stir after ready and heat as light component constantly steams, the temperature of reaction mass also exists
Constantly rise, when temperature rises to 95 DEG C, without distillate, stops distillation procedure, cooling discharge obtains component A.
(2) rubber-type PE protects the preparation of film parting agent：
Get out the four-hole boiling flask polymerization reaction of heating device, reflux condenser, thermometer, dropping funel and blender
44 parts of ethyl acetate are added into flask for system.
Monomer and initiator solution are by weight：By 16 parts of component A, 7.4 parts of ethyl acrylate, methyl methacrylate
4.4 parts, 7.6 parts of butyl acrylate, 3.4 parts of styrene, 1.2 parts of 2-hydroxypropyl acrylate are uniformly mixed, and by AIBN 0.6
Part is dissolved in mix monomer.
Start blender, 10 parts of mix monomer liquid is added into flask, and start to warm up；Remaining monomer mixed solution is complete
Portion is transferred to spare in dropping funel.
Reflux is begun with when temperature of charge rises to about 77 DEG C in flask, heat preservation reflux after forty minutes, will with 1.5 hours
Remaining monomer mixed solution is at the uniform velocity added drop-wise in flask, during which reaction mass is kept to be in reflux state.Monomer mixed solution is added dropwise
After the completion, continue to maintain the reflux for state 50 minutes, by 0.1 part and 16 parts of ethyl acetate of solution of AIBN, be added to dropping funel
In, and instilled in flask in 10 minutes, continue to maintain the reflux for reaction 2 hours, cooling discharge obtains rubber-type PE protective film use
Mould release.
Embodiment two
(1) preparation of polyfunctionality allyl acyloxy siloxanes (A)：
Directly adopt component A obtained in embodiment one
(2) rubber-type PE protects the preparation of film parting agent：
Get out the four-hole boiling flask polymerization reaction of heating device, reflux condenser, thermometer, dropping funel and blender
53.6 parts of ethyl acetate are added into flask for system.
Monomer and initiator solution are by weight：By 17.8 parts of component A, 3.6 parts of ethyl acrylate, methyl methacrylate
2.2 parts of ester, 3.8 parts of butyl acrylate, 1.7 parts of styrene, 1.3 parts of 2-hydroxypropyl acrylate are uniformly mixed, and by AIBN
0.32 part is dissolved in mix monomer.
Start blender, 10.0 parts of mix monomer liquid is added into flask, and start to warm up；By remaining monomer mixed solution
It is transferred completely into spare in dropping funel.
Reflux is begun with when temperature of charge rises to about 77 DEG C in flask, heat preservation reflux after forty minutes, will with 1.5 hours
Remaining monomer mixed solution is at the uniform velocity added drop-wise in flask, during which reaction mass is kept to be in reflux state.Monomer mixed solution is added dropwise
After the completion, continue to maintain the reflux for state 50 minutes, by 0.1 part and 16 parts of ethyl acetate of solution of AIBN, be added to dropping funel
In, and instilled in flask in 10 points, continue to maintain the reflux for reaction 2 hours, cooling discharge obtain rubber-type PE protective film with from
Type agent.
Embodiment three
(1) preparation of polyfunctionality allyl acyloxy siloxanes (A)：
By weight into the four-hole boiling flask equipped with heating device, reflux condenser, thermometer, dropping funel and blender
It is added：8.4 parts of methallyl monomethacryloxypropyl trimethoxy silane, 80.6 parts of methyltrimethoxysilane, 0.18 part of hydroquinone,
9.0 parts of distilled water, and start blender.0.03 part of concentrated hydrochloric acid (C=37%Wt) is dissolved in 2.0 parts of distilled water, then
It is transferred among dropping funel stand-by.At room temperature, the liquid in dropping funel is at the uniform velocity instilled into flask with 10 minutes time
In, with the progress of dropwise addition, the temperature meeting nature of reaction mass rises, and starts to flow back at 68 DEG C, heat preservation reflux after sixty minutes, will
Reaction mass temperature is reduced to 65 DEG C, stops stirring, and reflux condenser is replaced with distillation condenser pipe, prepares to collect reaction life
At lighter component.Restart to stir after ready and heat, as light component constantly steams, the temperature of reaction mass
Constantly rising, when temperature rises to 95 DEG C, without distillate, is stopping distillation procedure, cooling discharge obtains component A.
(2) preparation of acrylate modified silicone release agent：
Get out the four-hole boiling flask polymerization reaction of heating device, reflux condenser, thermometer, dropping funel and blender
54 parts of ethyl acetate are added into flask for system.
Monomer and initiator solution are by weight：By 17.9 parts of component A, 2.6 parts of ethyl acrylate, methyl methacrylate
2.3 parts of ester, 3.1 parts of butyl acrylate, 2.6 parts of styrene, 1.5 parts of 2-hydroxypropyl acrylate are uniformly mixed, and by AIBN
0.3 part is dissolved in mix monomer.
Start blender, 7.5 parts of mix monomer liquid is added into flask, and start to warm up；By remaining monomer mixed solution
It is transferred completely into spare in dropping funel.
Reflux is begun with when temperature of charge rises to about 77 DEG C in flask, heat preservation reflux after forty minutes, will with 2.0 hours
Remaining monomer mixed solution is at the uniform velocity added drop-wise in flask, during which reaction mass is kept to be in reflux state.Monomer mixed solution is added dropwise
After the completion, continue after maintaining the reflux for state 45 minutes, add AIBN for the first time：By the molten of 0.05 part of AIBN and 8 parts of ethyl acetate
Liquid is added in dropping funel, and is instilled in flask in 5 minutes, continues to maintain the reflux for reaction 1 hour；It adds for the second time
AIBN：With add same amount and operating process for the first time, equally continue to maintain the reflux for reaction 1 hour, cooling discharge obtains one kind
Rubber-type PE protects film parting agent.
Example IV
(1) preparation of polyfunctionality allyl acyloxy siloxanes (A)：
By weight into the four-hole boiling flask equipped with heating device, reflux condenser, thermometer, dropping funel and blender
It is added：9.1 parts of methallyl monomethacryloxypropyl trimethoxy silane, 80.9 parts of methyltrimethoxysilane, 0.1 part of hydroquinone,
8.0 parts of distilled water, and start blender.0.06 part of concentrated hydrochloric acid (C=37%Wt) is dissolved in 2 distilled water, is then shifted
To stand-by among dropping funel.At room temperature, the liquid in dropping funel is at the uniform velocity instilled in flask with 15 minutes time, with
The progress being added dropwise, the temperature of reaction mass can nature rise, start to flow back at 65 DEG C, heat preservation reflux after sixty minutes, will react
Temperature of charge is reduced to 65 DEG C, stops stirring, and reflux condenser is replaced with distillation condenser pipe, prepares to collect what reaction generated
Lighter component.Restart to stir after ready and heat as light component constantly steams, the temperature of reaction mass is not yet
It is disconnected to rise, when temperature rises to 95 DEG C, without distillate, stop distillation procedure, cooling discharge obtains component A.
(2) rubber-type PE protects the preparation of film parting agent：
Get out the four-hole boiling flask polymerization reaction of heating device, reflux condenser, thermometer, dropping funel and blender
54 parts of ethyl acetate are added into flask for system.
Monomer and initiator solution are by weight：By 21.1 parts of component A, 1.6 parts of methyl methacrylate, acrylic acid fourth
3.5 parts of ester, 2.6 parts of styrene, 1.2 parts of 2-hydroxypropyl acrylate are uniformly mixed, and are dissolved in mixing for 0.26 part of AIBN
In monomer.
Start blender, 7.5 parts of mix monomer liquid is added into flask, and start to warm up；By remaining monomer mixed solution
It is transferred completely into spare in dropping funel.
Reflux is begun with when temperature of charge rises to about 77 DEG C in flask, heat preservation reflux after forty minutes, will with 2.0 hours
Remaining monomer mixed solution is at the uniform velocity added drop-wise in flask, during which reaction mass is kept to be in reflux state.Monomer mixed solution is added dropwise
After the completion, continue to maintain the reflux for state after sixty minutes, add AIBN for the first time：By 0.05 part and 8 parts of ethyl acetate of cream of AIBN
Liquid is added in dropping funel, and is instilled in flask in 5 points, continues to maintain the reflux for reaction 1 hour；AIBN is added for the second time：
With add same amount and operating process for the first time, continue to maintain the reflux for reaction 2 hours, cooling discharge obtains a kind of rubber-type PE and protects
Protect film parting agent.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, therefore
Without departing from the technical solutions of the present invention, to the above embodiments according to the technical essence of the invention any simply to repair
Change, equivalent variations and modification, all of which are still within the scope of the technical scheme of the invention.
Claims (3)
1. a kind of rubber-type PE protects film parting agent, it is polymerize in a kettle by following each component and is prepared, forms
Match as follows according to parts by weight, ingredient A：16~21.1, ethyl acrylate：0~7.4, methyl methacrylate：1.6~
4.4, butyl acrylate：3.1~7.6, styrene：1.7~3.4,2-hydroxypropyl acrylate：1.2~1.5, ethyl acetate：
59.6~70, azodiisobutyronitrile：0.36~0.72；
The ingredient A by weight, is prepared in a kettle by following each component, methacryloxypropyl front three
Oxysilane：7.7~8.4, methyltrimethoxysilane：80.6~82.3, water：10~11, concentrated hydrochloric acid (37%)：0.03~
0.08, hydroquinone：0.1~0.2.
2. a kind of rubber-type PE protection film parting agent of claim 1 and preparation method thereof, it is characterised in that：
(1) preparation of composition A
A) it is added into the four-hole boiling flask equipped with heating device, reflux condenser, thermometer, dropping funel and blender：Methyl
Acrylyl oxygen propyl trimethoxy silicane 7.7g, methyltrimethoxysilane 82.3g, hydroquinone 0.2g, distilled water 8.0g, and
Start blender；
B) 0.08g concentrated hydrochloric acid (37%Wt) is dissolved in the distilled water of 2g, is then transferred among dropping funel stand-by；
C) at room temperature, the liquid in dropping funel is at the uniform velocity instilled in flask with 5~15 minutes time；
D) with the progress of dropwise addition, the temperature meeting nature of reaction mass rises, starts to flow back at 68 DEG C, 30~60 points of heat preservation reflux
Clock；
E) during distillating light component, the method for being gradually warmed up and steaming is taken, as light component constantly steams, reaction mass
Temperature also constantly rising, when temperature rises to 95 DEG C, stop distillation procedure, cooling discharge obtains component A；
(2) rubber-type PE protects the preparation of film parting agent
A) the four-hole boiling flask polymerization reaction system of heating device, reflux condenser, thermometer, dropping funel and blender is got out
44~54 parts by weight of ethyl acetate are added into flask for system；
B) component ratio by weight is mixed, wherein component A 16~21.1, ethyl acrylate 0~7.4, methyl methacrylate
Ester 1.6~4.4, butyl acrylate 3.1~7.6, styrene 1.7~3.4,2-hydroxypropyl acrylate 1.2~1.5, mixing are equal
It is even, and 0.6 part of AIBN is dissolved in mix monomer；
C) start blender, 7.5~10 parts by weight of mix monomer liquid are added into flask, and start to warm up；By remaining monomer
Mixed liquor is transferred completely into spare in dropping funel；
D) reflux is begun with when temperature of charge rises to about 77 DEG C in flask, heat preservation flows back after forty minutes, with 1.5~2 hours
Remaining monomer mixed solution is at the uniform velocity added drop-wise in flask, during which reaction mass is kept to be in reflux state；
E) after monomer mixed solution is added dropwise to complete, continue to maintain the reflux for state 45~60 minutes, by 0.1 part of AIBN and ethyl acetate
16 points of solution, is added in dropping funel, and instills in flask in 10 minutes, continues to maintain the reflux for reaction 2 hours, cooling
Discharging obtains acrylate modified silicone release agent；Or：Initiator is added in two times, i.e., adds AIBN for the first time：It will
The solution of AIBN 0.05 and ethyl acetate 8, are added in dropping funel, and instill in flask in 5 points, continue to maintain the reflux for
Reaction 1 hour；AIBN is added for the second time：With add same amount and operating process for the first time, it is small equally to continue to maintain the reflux for reaction 1
When, cooling discharge obtains rubber-type PE protection film parting agent.
3. claim 1 and a kind of rubber-type PE as claimed in claim 2 protect film parting agent, application range includes coating
Play the role of release in PE substrate or other substrates or play unmentioned function in other present invention, belongs to the present invention,
I.e. a kind of application range of rubber-type PE protection film parting agent, regardless of the allotment before being coated with which kind of formula.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810777974.9A CN108841231B (en) | 2018-07-16 | 2018-07-16 | Release agent for rubber type PE protective film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810777974.9A CN108841231B (en) | 2018-07-16 | 2018-07-16 | Release agent for rubber type PE protective film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108841231A true CN108841231A (en) | 2018-11-20 |
| CN108841231B CN108841231B (en) | 2022-09-27 |
Family
ID=64197585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810777974.9A Active CN108841231B (en) | 2018-07-16 | 2018-07-16 | Release agent for rubber type PE protective film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108841231B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090171010A1 (en) * | 2007-12-31 | 2009-07-02 | John Kilgour | Low temperature cure silicone release coatings containing branched silylhydrides |
| CN104530875A (en) * | 2014-12-05 | 2015-04-22 | 佛山市南海高拓包装材料有限公司 | Release agent and preparation method thereof |
| CN106220881A (en) * | 2016-08-11 | 2016-12-14 | 苏州柯创电子材料有限公司 | Modified organic silicon mould release membrance |
| CN107075341A (en) * | 2014-10-17 | 2017-08-18 | 信越化学工业株式会社 | Stripping film re-release additive and stripping film organopolysiloxane composition and stripping film |
-
2018
- 2018-07-16 CN CN201810777974.9A patent/CN108841231B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090171010A1 (en) * | 2007-12-31 | 2009-07-02 | John Kilgour | Low temperature cure silicone release coatings containing branched silylhydrides |
| CN107075341A (en) * | 2014-10-17 | 2017-08-18 | 信越化学工业株式会社 | Stripping film re-release additive and stripping film organopolysiloxane composition and stripping film |
| CN104530875A (en) * | 2014-12-05 | 2015-04-22 | 佛山市南海高拓包装材料有限公司 | Release agent and preparation method thereof |
| CN106220881A (en) * | 2016-08-11 | 2016-12-14 | 苏州柯创电子材料有限公司 | Modified organic silicon mould release membrance |
Non-Patent Citations (3)
| Title |
|---|
| 穆锐等: "有机硅改性丙烯酸酯乳液隔离剂的研究", 《化学与黏合》 * |
| 魏赛琦: "丙烯酸（酯）改性有机硅提高离型膜表面张力的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 黄文润: "《硅烷偶联剂及硅树脂》", 31 August 2010, 四川科学技术出版社 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108841231B (en) | 2022-09-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107075341B (en) | Stripping film is with re-releasing additive and stripping film organopolysiloxane composition and stripping film | |
| CN102639663B (en) | Adhesive agent | |
| Marcu et al. | Incorporation of alkoxysilanes into model latex systems: vinyl copolymerization of vinyltriethoxysilane and n-butyl acrylate | |
| US8945815B2 (en) | Alkaline soluble resin and light sensible resin composition comprising same and use thereof | |
| CN104342073A (en) | Organic silicon modified phenyl emulsion pressure-sensitive adhesive with high release force and low residue as well as preparation method thereof and application | |
| CN109111878A (en) | A kind of no-solvent ultraviolet dual cure hot-fusible pressure-sensitive adhesive | |
| CN107201180A (en) | Ultraviolet curing acrylic ester hot-fusible pressure-sensitive adhesive and preparation method thereof | |
| CN104497332B (en) | A kind of mould release membrance and preparation method thereof | |
| CN104530875B (en) | Release agent and preparation method thereof | |
| CN104817986A (en) | Preparation method of single-component solvent-type high-stripping acrylic acid pressure-sensitive adhesive | |
| EP3480223A1 (en) | Low temperature curable addition polymers from vinyl arylcyclobutene-containing monomers and methods for making the same | |
| CN108219702B (en) | Acrylic acid pressure-sensitive adhesive protection film | |
| CN105907340A (en) | Low-toxicity and low-odor single-component acrylate pressure sensitive adhesive and preparation method thereof | |
| CN108728023A (en) | Pressure-sensitive adhesive composition and the film formed using the composition | |
| CN106256840A (en) | Adhesive composition | |
| CN109997080A (en) | Photoinitiator and shading photosensitive resin composition comprising it | |
| KR101250492B1 (en) | Shelf-stable silane-modified aqueous dispersion polymers | |
| JP2007238853A (en) | Adhesive composition and adhesive film produced by using the adhesive composition | |
| CN106752623B (en) | A kind of preparation method of heat curing type polyacrylate hydrophilic antifogging coating | |
| CN106054532B (en) | Negative photosensitive polysiloxane composition | |
| CN106046912A (en) | Waterproof slipping auxiliary for leather and method for preparing waterproof slipping auxiliary | |
| CN104592848B (en) | BOPET release film and preparation method thereof | |
| CN108841231A (en) | A kind of rubber-type PE protection film parting agent and preparation method thereof | |
| CN106146754A (en) | 3D prints by the preparation method and applications of silicon-containing nano gel light-cured resin | |
| CN110452490B (en) | Dual POSS polyether hybrid water-based acrylic resin dispersion, preparation method and composition for preparing resin coating film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220713 Address after: 528325 No. 3, Yunxian street, Maicun Central Avenue, Xingtan town, Shunde District, Foshan City, Guangdong Province Applicant after: Mai Guangming Address before: 528325 Chong Chong Industrial Zone, new town, Shunde District, Guangdong, Foshan Applicant before: GUANGDONG TAMAY NEW MATERIALS Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220907 Address after: 528325 No. 3, Building 7, Cuihui Science and Technology Industrial Park, No. 3, Keji 8th Road, Wanmu Industrial Park, Xingtan Town, Shunde District, Foshan City, Guangdong Province (domicile declaration) Applicant after: Guangdong Chuangyang New Material Technology Co.,Ltd. Address before: 528325 No. 3, Yunxian street, Maicun Central Avenue, Xingtan town, Shunde District, Foshan City, Guangdong Province Applicant before: Mai Guangming |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |