CN103694892B - A kind of fluorinated polysiloxane parting agent and preparation method thereof - Google Patents
A kind of fluorinated polysiloxane parting agent and preparation method thereof Download PDFInfo
- Publication number
- CN103694892B CN103694892B CN201310655164.3A CN201310655164A CN103694892B CN 103694892 B CN103694892 B CN 103694892B CN 201310655164 A CN201310655164 A CN 201310655164A CN 103694892 B CN103694892 B CN 103694892B
- Authority
- CN
- China
- Prior art keywords
- parting agent
- fluorinated polysiloxane
- silicone oil
- vinyl fluoride
- natural number
- 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.)
- Active
Links
- SEEYREPSKCQBBF-UHFFFAOYSA-N CN(C(C=C1)=O)C1=O Chemical compound CN(C(C=C1)=O)C1=O SEEYREPSKCQBBF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
- Paints Or Removers (AREA)
- Moulds For Moulding Plastics Or The Like (AREA)
Abstract
The invention discloses a kind of fluorinated polysiloxane parting agent and preparation method thereof.Wherein, fluorinated polysiloxane parting agent, to have the vinyl fluoride silicone oil of imide heterocycle for matrix, coordinates containing hydrogen silicone oil, inhibitor and catalyst mix to form.This fluorinated polysiloxane parting agent does not use any solvent, effectively avoids organic solvent to the injury of environment and human body, and makes the release film after solidifying have better anti-adhesion effects by introducing fluorine-containing long chain substituents.Meanwhile, the imide heterocyclic substituent added in vinyl fluoride silicone oil is conducive to the bonding intensity improving parting agent and polyester or Kapton base material.
Description
Technical field
The present invention relates to separated type material field, especially relate to a kind of fluorinated polysiloxane parting agent and preparation method thereof.
Background technology
Pressure sensitive adhesive (pressuresensitiveadhesive) is the abbreviation of pressure-sensitive adhesive, is that a class has tackiness agent pressure being had to susceptibility.Organic pressure-sensitive gel generally refers to the pressure sensitive adhesive based on organosilicon polymer, or by Organosiliconpolymermodified modified vinylformic acid-organic-silicon-modified rubber pressure-sensitive adhesive.Compared with traditional acrylate pressure-sensitive adhesive, rubber pressure-sensitive adhesive; vinylformic acid-organic-silicon-modified rubber pressure-sensitive adhesive has the performances such as excellent chemical-resistant resistance, waterproof oil resistant, solvent resistant and oxidative degradation; and can glued joint by the material sticky with multiple difficulty; be widely used in the products such as transformer, circuit card, mica pressure sensitive film, mobile TV machine screen protecting film, and be expected to be applied at other field.
Need to be coated with parting agent between silicone pressure sensitive glue-line and adhesive band base, to reduce adhesive power between the two, be convenient to uncoiling and the use of adhesive tape.Parting agent, also known as release agent, separant, be one of the critical material producing Pressuresensitive Tape, non-setting adhesive goods, its performance directly has influence on the quality of Pressuresensitive Tape, non-setting adhesive goods.Now relatively more conventional is the fluorine element parting agent that surface tension is low, and as existing disclosed a kind of fluorine silicon parting agent, its formula is fluorine-containing chain is C
nf
2n+1cH
2cH
2the vinyl fluoride silicone resin of-(n=4 ~ 8), containing hydrogen silicone oil and platinum catalyst; And it is existing disclosed another kind of containing F [CF (CF
3) CF
2o]
ncF (CF
3) CF
2the vinyl fluoride silicone resin of O-perfluoropolyether structures unit.But all need containing a large amount of organic solvent in the formula of this type of patent disclosure, and this kind solvent can volatilize in parting agent coating solidification process, thus contaminate environment, to be harmful to health.In addition, the solvent used in some formula is also for expensive contains fluorous solvent.Like this, the use of solvent, not only contaminate environment in above-mentioned formula, and the cost increasing fluorine silicon parting agent, thus the application and development of final restriction organic pressure-sensitive gel.
Based on the requirement of environmental protection and cost, prior art discloses a kind of fluorine silicon parting agent formula of no-solvent type, there is good anti-adhesion effects, but the firmness of this fluorine silicon parting agent and base material need further raising, this is because the long fluorine chain in fluorine silicon parting agent formula provides lower surface tension, but also bring the shortcoming such as not enough with base material bonding intensity simultaneously.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of fluorinated polysiloxane parting agent and preparation method thereof is provided, contain hazardous solvent and the technical problem with base material bonding intensity deficiency to solve fluorine element parting agent in prior art.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of fluorinated polysiloxane parting agent, comprises the vinyl fluoride silicone oil of 100 weight parts, the containing hydrogen silicone oil of 1 ~ 30 weight part, also comprises and account for 100 ~ 2000ppm inhibitor of fluorinated polysiloxane parting agent gross weight and the platinum-type catalyzer of 1 ~ 800ppm; And the general formula of molecular structure of described vinyl fluoride silicone oil is:
Wherein, R is the linear of carbon number 1 ~ 3 or branched alkyl groups;
R
1for the substituting group containing phthalic imidine;
R
2for the substituting group containing maleimide heterocycle;
R
vfor the substituting group of end alkene structure;
R
f1for taking Propylene oxide hexafluoride as the PFPE substituting group of structural unit;
R
f2for perfluoroalkyl;
X and Y is the bivalent hydrocarbon radical of carbon number 2 ~ 8;
A, b, c, d, e, f are all natural number, and 200 ﹥ a ﹥ b ﹥ 0,50 ﹥ d ﹥ e >=0, f ﹥ 2 (a+b+c+d+e), 400 ﹥ f ﹥ 10,0.02 ﹥ c/ (a+b+c+d+e) >=0.
And a kind of preparation method of fluorinated polysiloxane parting agent, comprises the steps:
Each component is taken respectively according to the formula of above-mentioned fluorinated polysiloxane parting agent;
Described each component is mixed, obtains mixture.
Above-mentioned fluorinated polysiloxane parting agent is the vinyl fluoride silicone oil with imide heterocycle is matrix, coordinates containing hydrogen silicone oil, inhibitor and catalyst mix to form.This fluorinated polysiloxane parting agent does not use any solvent, effectively avoids organic solvent to the injury of environment and human body, and makes the release film after solidifying have better anti-adhesion effects by introducing fluorine-containing long chain substituents.Meanwhile, the imide heterocyclic substituent added in vinyl fluoride silicone oil is conducive to the bonding intensity improving parting agent and polyester or Kapton base material.
Each component only need mix by step interpolation according to formula by above-mentioned fluorinated polysiloxane parting agent preparation method, also without the need to special equipment, therefore, the method technique is simple, be applicable to suitability for industrialized production, and effectively prevent the pollution to environment, reduce cost.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of fluorinated polysiloxane parting agent, comprise the vinyl fluoride silicone oil of 100 weight parts, the containing hydrogen silicone oil of 1 ~ 30 weight part, also comprise and account for 100 ~ 2000ppm inhibitor of fluorinated polysiloxane parting agent gross weight and the platinum-type catalyzer of 1 ~ 800ppm; And the general formula of molecular structure of above-mentioned vinyl fluoride silicone oil is:
Wherein, R is the linear of carbon number 1 ~ 3 or branched alkyl groups;
R
1for the substituting group containing phthalic imidine;
R
2for the substituting group containing maleimide;
R
vfor the substituting group of end alkene structure;
R
f1for taking Propylene oxide hexafluoride as the PFPE substituting group of structural unit;
R
f2for perfluoroalkyl;
X and Y is the bivalent hydrocarbon radical of carbon number 2 ~ 8;
A, b, c, d, e, f are all natural number, and 200 ﹥ a ﹥ b ﹥ 0,50 ﹥ d ﹥ e >=0, f ﹥ 2 (a+b+c+d+e), 400 ﹥ f ﹥ 10,0.02 ﹥ c/ (a+b+c+d+e) >=0.
Matrix composition vinyl fluoride silicone oil in above-mentioned fluorinated polysiloxane parting agent contains multiple Si-O bond structure, and it gives the release film after coating excellent flexibility, thermotolerance, oxygen resistence, weather-resistant property.And due to the very low surface energy of fluorine atom, when introducing the fluorine-containing chain alkyl of higher fluorine content at vinyl fluoride silicone oil side chain, the molecular structure of its uniqueness makes fluorinated polysiloxane polymkeric substance have excellent anti-adhesion performance.In addition, carbon number is the tridimensional network adding this parting agent of expansion further of bivalent hydrocarbon radical X and the Y of 2 ~ 8, increases the toughness that parting agent forms release film.
Particularly, difference due to the polymerization degree of polymkeric substance can cause its character also to change, for strengthening over-all properties and the anti-adhesion effects of above-mentioned fluorinated polysiloxane parting agent, polymerization degree a, b, c, d, e, f of above-mentioned fluorinated polysiloxane parting agent are all natural number, and 200 ﹥ a ﹥ b ﹥ 0,50 ﹥ d ﹥ e >=0, f ﹥ 2 (a+b+c+d+e), 400 ﹥ f ﹥ 10,0.02 ﹥ c/ (a+b+c+d+e) >=0.Certainly, above-mentioned part link configuration unit can be selected flexibly according to actual needs, such as, can not be included in above-mentioned vinyl fluoride silicone oil with the link structure unit that polymerization degree c and e is corresponding.
Above-mentioned fluorinated polysiloxane parting agent is a kind of stable mixture under low temperature or normal temperature, but this parting agent its component in hot setting film-forming process addition reaction of silicon with hydrogen can occur.CH particularly in vinyl fluoride silicone oil
2=CH
2under the katalysis of platinum-type catalyzer, there is addition reaction of silicon with hydrogen with the Si-H key in containing hydrogen silicone oil, thus make crosslinked polymer be tridimensional network.
Particularly, the viscosity of above-mentioned ethene fluorosilicon oil at 25 DEG C is 10 ~ 1500mPas, the viscosity of containing hydrogen silicone oil at 25 DEG C is 1 ~ 1000mPas, like this by selecting the vinyl fluoride silicone oil of proper viscosity to be conducive to mixing of each composition with containing hydrogen silicone oil, be conducive to the carrying out of addition reaction of silicon with hydrogen in high temperature cure process further.
The fluorine-containing side base of above-mentioned vinyl fluoride silicone oil is hydrophobicity, and cause itself and hydrophilic substrate adhesion poor, such as polyester or Kapton etc., reduce further the firmness between itself and base material.Therefore, by introducing with polyester or Kapton structural similitude and the larger imide heterocycle of polarity, the bonding firmness between fluorinated polysiloxane parting agent and base material can significantly be improved.As preferred embodiment, above-mentioned R
1general structure be
Wherein, r is the natural number of 3 ~ 10.
Above-mentioned containing in the substituting group of phthalic imidine, lone-pair electron on nitrogen can with two carbonyl generation conjugation, thus part transfer on oxygen, make negative ion form more stable, be connected with phenyl ring again and expand the electron-conjugated system of imide heterocycle, strengthen imido stability further.
For promoting the bonding firmness between fluorinated polysiloxane parting agent and base material further, in above-mentioned fluorine-containing vinyl fluoride silicone oil, introduce the substituent R containing maleimide again
2.As preferred embodiment, above-mentioned R
2general structure be
Wherein, t is the natural number of 3 ~ 10.
As preferred embodiment, above-mentioned R
1and R
2the mol ratio of middle imide heterocyclic monomer and described vinyl fluoride silicone oil is 0.001 ~ 0.05:1.This is because molar ratio is too large, vinyl fluoride silicon oil viscosity can be caused excessive, and addition reaction of silicon with hydrogen is obstructed, and curing speed is slack-off, and solidified nature is poor; And molar ratio is too little, the adhesiving effect of imide heterocycle to base material is not obvious.
Particularly, for improving the reaction efficiency of high temperature cure process medium vinyl fluorosilicon oil and containing hydrogen silicone oil generation crosslinking reaction, expand the tridimensional network of parting agent, improve its over-all properties, the substituent R of the present invention's leading-in end alkene structure again on the basis of existing end-blocking vinyl
v.Preferably, R
vgeneral structure is C
mh
2mcH=CH
2, m is the natural number of 1 ~ 8.
As mentioned above, when the fluorine-containing side base of higher fluorine content introduced by vinyl fluoride silicone oil side chain, significantly can reduce the surfactivity of vinyl fluoride silicone oil, be conducive to the anti-adhesion performance improving fluorinated polysiloxane polymkeric substance.When above-mentioned fluorine-containing side base is PFPE substituting group, not only improve the fluorine content of vinyl fluoride silicone oil, strengthening anti-adhesion effects, and owing to PFPE substituting group existing soft ether segment, make the side chain of vinyl fluoride silicone molecule also become submissive, effectively reduce the viscosity of fluorosilicon oil.
As preferred embodiment, above-mentioned to take Propylene oxide hexafluoride as the general structure of the PFPE substituent R f1 of structural unit be:
Or
Wherein, n is the natural number of 2 ~ 15
The polymerization degree above by regulation and control Propylene oxide hexafluoride structural unit is 2 ~ 15 thus controls the fluorine content in fluorinated polysiloxane parting agent, the final off-type force regulating release film; In addition, the molecular structure unit of PFPE not only can provide higher fluorine content, and there is splendid molecular flexibility, effectively can reduce the viscosity of fluorosilicon oil, final and imide heterocyclic substituent works in coordination with the defect improving fluorine-containing parting agent and base material bonding intensity deficiency.
Equally, for significantly reducing vinyl fluoride silicone oil surface energy, promote the bonding between organic pressure-sensitive gel and parting agent further, as preferred embodiment, perfluoroalkyl R introduced by above-mentioned vinyl fluoride silicone oil
f2, its general expression is :-C
qf
2q+1, wherein, q is the natural number of 4 ~ 10.
Because PFPE both can provide higher fluorine content, significantly can reduce vinyl fluoride silicon oil viscosity again, simultaneously also for improving release performance and the mechanical property of release film, the molar content that the PFPE in above-mentioned vinyl fluoride silicone molecule replaces fiduciary point vinyl fluoride silicone oil should be greater than the molar content that perfluoroalkyl accounts for fluorosilicon oil.
In the formula of above-mentioned fluorinated polysiloxane parting agent, the general structure of containing hydrogen silicone oil is preferably:
Wherein, g, h, i are all natural number, and 10<g<100,0<h<11,1<i<100.For improving the consistency with vinyl fluoride silicone oil, in this containing hydrogen silicone oil, add above-mentioned fluorine-containing chain alkyl R
f3.
As preferred embodiment, the hydrogen content of above-mentioned containing hydrogen silicone oil is preferably 0.l% ~ 1.6%.This is because when hydrogen content is less than 0.l%, the reactive behavior of containing hydrogen silicone oil is lower, affects mechanical property and the surface property of the release film that it is formed.Further, for preventing Si-H key from losing, guarantee that material sulfuration is complete, Si-H key should be appropriate excessive, the CH namely in vinyl fluoride silicone oil
2=CH
2be 1:1.5 ~ 2.5 with the mol ratio of the Si-H key of containing hydrogen silicone oil.
Because the catalyst activity of the vinyl fluoride silicone oil of add-on type is high, just can react under room temperature after vinyl fluoride silicone oil, containing hydrogen silicone oil, catalyst mix.When adding inhibitor in reaction system, inhibitor at room temperature can postpone hydrosilylation addition reaction, and under high temperature, inhibitor inefficacy makes hydrosilylation addition reaction speed increase sharply.Therefore, add inhibitor in above-mentioned fluorinated polysiloxane, and this inhibitor accounts for 100 ~ 2000ppm of fluorinated polysiloxane parting agent gross weight, its general structure is preferably:
Wherein, n is the natural number of 2 ~ 8.
Select the inhibitor with above-mentioned general formula be because its not only comprised imide group but also containing above-mentioned take Propylene oxide hexafluoride as the PFPE substituting group of structural unit, so not only make inhibitor, vinyl fluoride silicone oil and containing hydrogen silicone oil better compatible, the anti-adhesion effects of more collaborative raising fluorinated polysiloxane and the bonding firmness between itself and base material.
In the addition reaction of silicon with hydrogen of above-mentioned high temperature cure process, to have before cross moulding except wanting guarantee system and except the highly efficient depressor of safe storage, also can will have the highly active platinum catalyst that vinyl fluoride silicone oil matrix and containing hydrogen silicone oil can be made to be cross-linked completely.In a particular embodiment, above-mentioned platinum-type catalyzer is Karstedt platinum catalyst, and its consumption in formula system is 1 ~ 800ppm.
In addition, compared with prior art, in the composition of above-mentioned fluorinated polysiloxane parting agent, do not comprise organic solvent, thus avoid parting agent volatilize in coating process produce toxic and harmful contaminate environment, be harmful to health.
Above-mentioned fluorinated polysiloxane parting agent is the vinyl fluoride silicone oil with imide heterocycle is matrix, coordinates containing hydrogen silicone oil, inhibitor and catalyst mix to form.This fluorinated polysiloxane parting agent does not use any solvent, effectively avoids organic solvent to the injury of environment and human body, and makes the release film after solidifying have better anti-adhesion effects by introducing fluorine-containing long chain substituents.Meanwhile, the imide heterocyclic substituent added in vinyl fluoride silicone oil is conducive to the bonding intensity improving parting agent and polyester or Kapton base material.In addition, the stable performance under normal temperature or low temperature of above-mentioned fluorinated polysiloxane parting agent, each composition can steady in a long-termly exist, at high temperature each composition generation addition reaction of silicon with hydrogen, and is solidified into the release film high with base material bonding intensity.
Correspondingly, the embodiment of the present invention also provides a kind of method preparing above-mentioned fluorinated polysiloxane parting agent, comprises the steps:
S01. each component is taken respectively according to the formula of above-mentioned fluorinated polysiloxane parting agent;
S02. each component is mixed, obtain mixture.
Particularly, above-mentioned preparation method all can carry out under normal temperature or low temperature.In addition, vinyl fluoride silicone oil and Silicon Containing Hydrogen oil viscosity should be selected according to actual needs, to obtain the fluorinated polysiloxane parting agent of proper viscosity, thus ensure the solidification rate of the solidification process of follow-up acquisition release film.
Each component only need mix by step interpolation according to formula by above-mentioned fluorinated polysiloxane parting agent preparation method, also without the need to special equipment, therefore, the method technique is simple, be applicable to suitability for industrialized production, and effectively prevent the pollution to environment, reduce cost.
Above-mentioned fluorinated polysiloxane parting agent at high temperature solidifies and can form release film, and its concrete die-manufacturing method is as follows:
Above-mentioned fluorinated polysiloxane parting agent is coated rapidly on certain thickness polyester or thin polyurethane film base material, control glue spread, and solidify 30s ~ 3min under warm air, obtain fluorinated polysiloxane release film.
Now for concrete fluorinated polysiloxane parting agent and preparation method thereof, the present invention is further elaborated.
Embodiment 1
A kind of fluorinated polysiloxane parting agent, comprises the composition of following weight part:
100g viscosity is the vinyl fluoride silicone oil (its structural formula is as shown in the formula (1) Suo Shi) of 390mPas;
3.25g containing hydrogen silicone oil (its structure is as shown in the formula (2) Suo Shi);
The fluorine-containing acetylenic alcohol inhibitor of 0.1g (its structure is as shown in the formula (3) Suo Shi);
The Karstedt platinum catalyst of 500ppm.
The preparation method of this fluorinated polysiloxane parting agent is:
Each component is taken respectively according to the formula of above-mentioned fluorinated polysiloxane parting agent;
Each component is mixed, obtains mixture.
Embodiment 2
Prepare fluorinated polysiloxane parting agent according to the recipe ingredient of above-described embodiment 1 and step, wherein, the structure of containing hydrogen silicone oil is constant, and the consumption of fluorine-containing alkynol and platinum catalyst is constant.Compare with embodiment 1, difference is that the polymerization degree of the link units of the present embodiment vinyl fluoride silicone oil changes, i.e. a=60, b=10, d=8, f=180, and with this, b, d, f numerical value and Si-H and CH=CH
2mol ratio be 2:1 be foundation, add the containing hydrogen silicone oil of respective quality.
Embodiment 3
Fluorinated polysiloxane parting agent is prepared according to the recipe ingredient of above-described embodiment 2 and step.Compare with embodiment 2, difference is that the polymerization degree of the link units of the present embodiment vinyl fluoride silicone oil changes, i.e. a=90, b=11, d=5, f=220, and with this, b, d, f numerical value and Si-H and CH=CH
2mol ratio be 2:1 be foundation, add the containing hydrogen silicone oil of respective quality.
Comparative example 1
Fluorinated polysiloxane parting agent is prepared according to the recipe ingredient of above-described embodiment 2 and step.Compare with embodiment 1, difference is that the polymerization degree of the link units of the present embodiment vinyl fluoride silicone oil changes, i.e. a=50, b=11, d=0, f=152, and with this, b, d, f numerical value and Si-H and CH=CH
2mol ratio be 2:1 be foundation, add the containing hydrogen silicone oil of respective quality.
Comparative example 2
Fluorinated polysiloxane parting agent is prepared according to the recipe ingredient of above-described embodiment 2 and step.Compare with embodiment 2, difference is that the polymerization degree of the link units of the present embodiment vinyl fluoride silicone oil changes, i.e. a=50, b=10, d=30, f=200, and with this, b, d, f numerical value and Si-H and CH=CH
2mol ratio be 2:1 be foundation, add the containing hydrogen silicone oil of respective quality.
Comparative example 3
Fluorinated polysiloxane parting agent is prepared according to the recipe ingredient of above-described embodiment 2 and step.Compare with embodiment 2, difference is that the polymerization degree of the link units of the present embodiment vinyl fluoride silicone oil changes, i.e. a=30, b=60, d=10, f=160, and with this, b, d, f numerical value and Si-H and CH=CH
2mol ratio be 2:1 be foundation, add the containing hydrogen silicone oil of respective quality.
Performance test
The preparation of release film: coat rapidly on the thick Kapton of 0.125mm by the fluorinated polysiloxane parting agent that embodiment 1 ~ 3 and comparative example 1 ~ 3 obtain, glue spread is 0.2 ~ 0.3g/m
2, and solidify 2 minutes in 150 DEG C of warm airs, obtain release film.
Performance test: carry out performance test according to following appraisal procedure to the release film in above-mentioned each example, test gained property indices sees the following form 1.
(1) release film curing performance test
With the release film of finger friction after solidification treatment, observe film and whether tarnish or scratch.
Judgement criteria is as follows:
Release film is not scratched and do not tarnish completely (√) completely;
Release film has local scratch or stain (⊙);
Release film has most of area to occur scratching or staining (×).
(2) release film bonding intensity test
Testing method: by solidification after release film temperature be 50 DEG C, relative humidity be 70% climatic chamber in place for some time after, with finger rub tightly on the stripping release film of completion of cure 10 back and forth observe release film whether damaged, solidify if continue to put back in climatic chamber without breakage, until observe breakage, when record release film is damaged, be placed in the number of days in climatic chamber.
(3) release film peeling force performance test
Testing method: be that the NITOFLON923S Pressuresensitive Tape of 19mm adheres to release film surface by width, at 25 DEG C and load 20g/cm
2lower aging 12 hours; Utilize the fluorinated polysiloxane release film of peel test force instrument to each embodiment and comparative example to test with reference to GB GB/T2790-1995, the adhesive tape on each release film surface is peeled off with the detachment rate of the angle of 180 ° and 0.3m/min to test peeling force in opposite direction.
(4) the remaining adhesive performance test of release film
Testing method: the tape stripping on above-mentioned sealing coat is adhered on stainless steel plate, and use peel test force instrument, adopt peeling force performance test methods in (3) to test the peeling force being adhered to the adhesive tape on stainless steel plate and peeling off from stainless steel plate, the ratio of this peeling force and the initial peeling force of adhesive tape is defined as remaining stripping rate.
Above-mentioned each the performance test results sees the following form 1.
Table 1
From upper table 1, the curing performance of each embodiment and comparative example is good, and in ratio 1, imide heterocyclic monomer accounts for the molar fraction of vinyl fluoride silicone oil is 0, cause the adhesion between its release film and base material poor, in comparative example 2 and 3, fluorine content is less, cause release film anti-adhesion effects poor, peeling force is larger.In summary, fluorinated polysiloxane parting agent makes the release film after solidifying have better anti-adhesion effects to organic pressure-sensitive gel by introducing fluorine-containing long chain substituents.Meanwhile, the imide heterocyclic substituent added in vinyl fluoride silicone oil is conducive to the bonding intensity improving parting agent and polyester or Kapton base material.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a fluorinated polysiloxane parting agent, comprises the vinyl fluoride silicone oil of 100 weight parts, the containing hydrogen silicone oil of 1 ~ 30 weight part, also comprises and accounts for 100 ~ 2000ppm inhibitor of fluorinated polysiloxane parting agent gross weight and the platinum-type catalyzer of 1 ~ 800ppm; And the general formula of molecular structure of described vinyl fluoride silicone oil is:
Wherein, R is the straight or branched alkyl of carbon number 1 ~ 3;
R
1for the substituting group containing phthalic imidine;
R
2for the substituting group containing maleimide;
R
vfor the substituting group of end alkene structure;
R
f1for taking Propylene oxide hexafluoride as the PFPE substituting group of structural unit;
R
f2for perfluoroalkyl;
X and Y is the bivalent hydrocarbon radical of carbon number 2 ~ 8;
A, b, c, d, e, f are all natural number, and 200 ﹥ a ﹥ b ﹥ 0,50 ﹥ d ﹥ e >=0, f ﹥ 2 (a+b+c+d+e), 400 ﹥ f ﹥ 10,0.02 ﹥ c/ (a+b+c+d+e) >=0.
2. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, described R
1general structure be
Wherein, r is the natural number of 3 ~ 10.
3. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, described R
2general structure be
Wherein, t is the natural number of 3 ~ 10.
4. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, described R
vgeneral structure be C
mh
2mcH=CH
2, m is the natural number of 1 ~ 8.
5. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, described R
f1general structure be:
Wherein, n is the natural number of 2 ~ 15.
6. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, described R
f2general structure be :-C
qf
2q+1, wherein, q is the natural number of 4 ~ 10.
7., according to the arbitrary described fluorinated polysiloxane parting agent of claim 1 ~ 6, it is characterized in that, described R
1and R
2the mol ratio of middle dant monomer and described vinyl fluoride silicone oil is 0.001 ~ 0.05:1.
8. fluorinated polysiloxane parting agent according to claim 1, is characterized in that, the general structure of described inhibitor is:
Wherein, n is the natural number of 2 ~ 8.
9. a preparation method for fluorinated polysiloxane parting agent, comprises the steps:
Each component is taken respectively according to the formula of the fluorinated polysiloxane parting agent described in any one of claim 1 ~ 8;
Described each component is mixed, obtains mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310655164.3A CN103694892B (en) | 2013-12-05 | 2013-12-05 | A kind of fluorinated polysiloxane parting agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310655164.3A CN103694892B (en) | 2013-12-05 | 2013-12-05 | A kind of fluorinated polysiloxane parting agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103694892A CN103694892A (en) | 2014-04-02 |
| CN103694892B true CN103694892B (en) | 2015-12-02 |
Family
ID=50356565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310655164.3A Active CN103694892B (en) | 2013-12-05 | 2013-12-05 | A kind of fluorinated polysiloxane parting agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103694892B (en) |
Families Citing this family (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923334B (en) * | 2014-04-09 | 2016-04-06 | 东南大学 | A kind of fluorine silicon release film and preparation method thereof |
| CN104789167B (en) * | 2015-04-24 | 2017-01-11 | 苏州市新广益电子有限公司 | High-temperature-resistant adhesive tape as well as high-temperature-resistant release film and high-temperature-resistant adhesive used by high-temperature-resistant adhesive tape |
| CN105131833A (en) * | 2015-09-02 | 2015-12-09 | 上海应用技术学院 | Paraffin sliding feel organic silicon release agent |
| CN105295723B (en) * | 2015-11-27 | 2017-07-07 | 怀化学院 | A kind of curing type coating composition and its application |
| CN105860082B (en) * | 2016-03-22 | 2019-03-22 | 中科院广州化学有限公司南雄材料生产基地 | A kind of fluorine-containing alkene based polysiloxane and the preparation method and application thereof |
| CN106349717B (en) * | 2016-08-29 | 2019-04-26 | 太仓中化环保化工有限公司 | A kind of high intensity perfluoropolyether fluorosilicon oil curable compositions and preparation method thereof |
| CN106832538B (en) * | 2016-12-08 | 2021-04-02 | 福建恒安集团有限公司 | Disposable moisture absorption article |
| CN106827746A (en) * | 2016-12-08 | 2017-06-13 | 福建恒安集团有限公司 | A kind of multi-layer co-extruded compound mould release membrance |
| CN106832539B (en) * | 2016-12-08 | 2021-05-04 | 福建恒安集团有限公司 | Disposable absorption article |
| CN106832537A (en) * | 2016-12-08 | 2017-06-13 | 福建恒安集团有限公司 | One inter-species advises mould release membrance |
| TW201905139A (en) * | 2017-06-23 | 2019-02-01 | 日商道康寧東麗股份有限公司 | 剥离Adhesive stripper composition and release film |
| CN107619479B (en) * | 2017-08-23 | 2021-01-12 | 无锡龙驰氟硅新材料有限公司 | Fluorosilicone release agent and preparation method thereof |
| CN108326229A (en) * | 2018-04-17 | 2018-07-27 | 苏州捷德瑞精密机械有限公司 | A kind of high intensity releasing agent and preparation method thereof |
| CN109016278B (en) * | 2018-08-16 | 2020-10-23 | 怀化学院 | Release agent and spray type release agent |
| CN109294374B (en) * | 2018-08-22 | 2021-01-01 | 四川羽玺新材料股份有限公司 | Fluorosilicone modified acrylate release agent and preparation method thereof |
| CN109385207B (en) * | 2018-10-10 | 2021-06-29 | 杭州崇耀科技发展有限公司 | Smooth and elastic organic silicon release agent |
| CN111405751B (en) * | 2020-04-22 | 2021-04-27 | 上海科谷纳新材料科技有限公司 | Structure for improving performance of MPI (Multi-layer printed Circuit) base material FPC (Flexible printed Circuit) antenna and preparation method |
| CN112646188B (en) * | 2020-12-17 | 2022-08-30 | 山东东岳高分子材料有限公司 | Linear organic fluorine-containing polysiloxane and preparation method and application thereof |
| CN112608477A (en) * | 2020-12-17 | 2021-04-06 | 山东东岳高分子材料有限公司 | Linear organic fluorine-containing polysiloxane and preparation method and application thereof |
| CN113249033B (en) * | 2021-04-15 | 2022-02-11 | 南昌大学 | Condensed fluorine-containing release agent and preparation method of main component |
| CN114350260B (en) * | 2022-01-18 | 2023-03-28 | 美氟新材料科技(常州)有限公司 | Fluorine release coating with wear resistance and high stability and preparation method thereof |
| CN114672028B (en) * | 2022-03-22 | 2023-07-18 | 山东灵晓新材料有限公司 | Ultraviolet light cured epoxy modified organosilicon release agent and preparation method thereof |
| CN114907772B (en) * | 2022-05-26 | 2023-05-23 | 山东北方现代化学工业有限公司 | Special polyfluorosiloxane release coating for precast concrete members and preparation method thereof |
| KR20240144465A (en) * | 2022-05-30 | 2024-10-02 | 도요보 가부시키가이샤 | Silicone-release polyester film and method for producing the same |
| CN115894931B (en) * | 2022-09-01 | 2023-10-10 | 江立鼎 | Fluorine-containing hydrogen silicone oil and preparation method thereof |
| CN117286740B (en) * | 2023-09-05 | 2024-08-16 | 广东杰果新材料有限公司 | Solvent-free paper release agent |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880396B (en) * | 2010-06-03 | 2011-11-23 | 杭州师范大学 | Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation |
| CN102174262B (en) * | 2011-01-30 | 2012-12-19 | 东莞市贝特利新材料有限公司 | Environmental-friendly synthetic organosilicon leather and method for producing same |
| CN103059575A (en) * | 2012-12-16 | 2013-04-24 | 青岛研博电子有限公司 | Macromolecule heat conduction material |
| CN103342896A (en) * | 2013-06-26 | 2013-10-09 | 苏州天脉导热科技有限公司 | High temperature resistant heat-conducting silica gel sheet and preparation method thereof |
-
2013
- 2013-12-05 CN CN201310655164.3A patent/CN103694892B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103694892A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103694892B (en) | A kind of fluorinated polysiloxane parting agent and preparation method thereof | |
| TWI754630B (en) | Two-sided differential release paper or two-sided differential release film | |
| US4565714A (en) | Low surface energy material | |
| US5578381A (en) | Release coating compositions | |
| US20030139287A1 (en) | Use of a boron derivative as heat-activated catalyst for polymerisation and/or crosslinking of silicone by dehydrogenative condensation | |
| US4764576A (en) | Silicone-based coating composition for surface-releasing film | |
| JP4524549B2 (en) | Release agent composition for silicone adhesive and release sheet using the same | |
| CN115052945B (en) | Silicone-based coating composition and silicone-based release film comprising same | |
| CN115975503B (en) | Anchoring agent for fluorine-silicon release agent and application thereof | |
| CN108728023A (en) | Pressure-sensitive adhesive composition and the film formed using the composition | |
| KR20170096881A (en) | Anti-static silicone tight-release coating film | |
| JPS60228561A (en) | Curable organopolysiloxane composition and use | |
| CN106189904A (en) | Anti-acid acrylate pressure-sensitive adhesive protecting film | |
| CN104817702A (en) | Spherical dendritic organic silicon macromolecule, preparation method thereof and application | |
| JP3024445B2 (en) | Silicone composition for release agent and release paper | |
| CN108976454A (en) | A kind of optics shows the preparation method with fluorine silicon release film | |
| CN111423843A (en) | Organic silicon pressure-sensitive adhesive and preparation method and application thereof | |
| US5166294A (en) | Curable silicone composition | |
| CN115386309B (en) | Organic silicon protective film for electronic product and preparation method thereof | |
| JPH01215857A (en) | Organopolysiloxane composition for release paper | |
| WO2003029375A1 (en) | Organohydrogenpolysiloxane mixture and silicone release coating composition | |
| JPH09176491A (en) | Releasable silicone composition | |
| KR20180012966A (en) | Pressure Sensitive Adhesive composition using foldable display | |
| CN111454431A (en) | High-temperature yellowing resistant epoxy resin curing agent and preparation method thereof | |
| CN116875128B (en) | Release film and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 518000 Zhongliang (Fuan) Robot Intelligence Industrial Park, 90 Dayang Road, Fuyong Street, Baoan District, Shenzhen City, Guangdong Province Patentee after: SHENZHEN GUANHENG NEW MATERIALS TECHNOLOGY CO., LTD. Address before: 518000 East partition of the second building, first floor, second floor, East partition of Baokun Investment Co., Ltd., Xinling Road, Dalang Street, Baoan District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN GUANHENG NEW MATERIALS TECHNOLOGY CO., LTD. |