CN109666402A - A kind of anti-static release lotion and preparation method thereof with good stability energy - Google Patents
A kind of anti-static release lotion and preparation method thereof with good stability energy Download PDFInfo
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- CN109666402A CN109666402A CN201811640608.5A CN201811640608A CN109666402A CN 109666402 A CN109666402 A CN 109666402A CN 201811640608 A CN201811640608 A CN 201811640608A CN 109666402 A CN109666402 A CN 109666402A
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Abstract
The present invention relates to release emulsion technology fields, disclose a kind of anti-static release lotion and preparation method thereof with good stability energy.The anti-static release lotion with good stability energy, by weight, consisting of: 5~20 parts of alkenyl polysiloxanes, 0.5~10 part of hydrogen containing siloxane, 0.05~1 part of the netted silicone resin of phenyl hydroxyl, 0.05~5 part of conducting polymer polythiophene, 0.05~2 part of single armed carbon nano-tube aqueous solutions, 60~85 parts of 1~10 part of 1~5 part of linear silane coupling agent, surfactant, the water containing epoxy group.Anti-static release emulsion applications of the invention had both had well stable antistatic property in film substrate, the release film of preparation, while having stable release performance, were suitble to online coating, can reduce process, reduce cost.
Description
Technical field
The present invention relates to release emulsion technology fields, more particularly to a kind of with the antistatic of good stability energy
Release lotion and preparation method thereof.
Background technique
In carrying or use process, surface is easy by contact staining the products such as glass, advanced plate, electronic product
Or scratch, thus plastic film, but plastics generally can be mostly used to avoid pollution or injure using protective film covering surface
The dielectric constant of film is small, belongs to non-conductor, and insulation performance is higher, thus can generate electrostatic.However build-up of static charges is in plastics
The surface of film easily causes adsorption dust, or even causes to discharge, and causes fire, therefore, to avoid Plastic film surface
Electrostatic accumulation, plastic film usually will do it antistatic treatment, enhance its electric conductivity.Conventional antistatic treatment is to plastics
Thin film coated antistatic agent, but with current technology, treated, and plastic film antistatic property is not sufficiently stable, and the retention time is short,
Especially after ambient humidity reduces, the antistatic property of plastic film can deteriorate, i.e., conductivity is reduced or even failed.
In addition, certain applications industry, the protective film as used in the product of electronics industry, except needing with antistatic property
Outside, it is also necessary to which there is release function.Due at present on the market most of antistatic agents or antistatic lotion do not have release function
Can, so conventional anti-static release membrane preparation method is after film base material is carried out antistatic treatment, then release processing is carried out, this
Sample just will increase process, cause the production cycle long, and when carrying out release processing, antistatic substance is easily led in film-forming process
The catalytic activity of catalyst system, which weakens, even to fail, thus need to increase catalyst amount, it could film-forming.By antistatic
Two-step method as processing and release processing prepares anti-static release film, not only increases cost, but also will lead to and store in the later period
The peeling force of release film is unstable in the process, or even influences the stability of antistatic property, and antistatic property is caused to fail.
In conclusion it is actually necessary to research and develop a kind of anti-static release lotion with good stability energy.
Summary of the invention
(deficiency) in order to overcome at least one of the drawbacks of the prior art described above, the present invention provide a kind of with good stable
The advantages of anti-static release lotion of performance and preparation method thereof, the anti-static release lotion, is, is applied to film
After substrate, substrate had both had well stable antistatic property, while having stable release function, is suitble to online coating, subtracts
Few process, reduces cost.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of anti-static release lotion with good stability energy, by weight, consisting of: alkenyl polysiloxanes
5~20 parts, 0.5~10 part of hydrogen containing siloxane, 0.05~1 part of the netted silicone resin of phenyl hydroxyl, conducting polymer polythiophene
0.05~5 part, 0.05~2 part of single armed carbon nano-tube aqueous solutions, 1~5 part of the linear silane coupling agent containing epoxy group, surface-active
1~10 part of agent, 60~85 parts of water.
As a preferred embodiment, the anti-static release lotion with good stability energy, by weight, group
Become: 20 parts of alkenyl polysiloxanes, 8.5 parts of hydrogen containing siloxane, 0.05 part of the netted silicone resin of phenyl hydroxyl, conductive polymer poly
0.05 part of thiophene, 2 parts of single armed carbon nano-tube aqueous solutions, 3.5 parts of linear silane coupling agent, surfactant 5.9 containing epoxy group
Part, 60 parts of water.
As a preferred embodiment, the anti-static release lotion with good stability energy, by weight, group
Become: 5 parts of alkenyl polysiloxanes, 4 parts of hydrogen containing siloxane, 1 part of the netted silicone resin of phenyl hydroxyl, conducting polymer polythiophene 5
Part, 0.05 part of single armed carbon nano-tube aqueous solutions, 10 parts of 5 parts of linear silane coupling agent, surfactant, water containing epoxy group
69.95 parts.
As a preferred embodiment, the anti-static release lotion with good stability energy, by weight, group
Become: 9 parts of alkenyl polysiloxanes, 0.5 part of hydrogen containing siloxane, 0.8 part of the netted silicone resin of phenyl hydroxyl, conductive polymer poly thiophene
2.5 parts of pheno, 1.2 parts of single armed carbon nano-tube aqueous solutions, 1 part of 1 part of linear silane coupling agent, surfactant, water containing epoxy group
85 parts.
As a preferred embodiment, the anti-static release lotion with good stability energy, by weight, group
Become: 12 parts of alkenyl polysiloxanes, 10 parts of hydrogen containing siloxane, 0.35 part of the netted silicone resin of phenyl hydroxyl, conductive polymer poly
3.55 parts of thiophene, 0.8 part of single armed carbon nano-tube aqueous solutions, 2.8 parts of linear silane coupling agent, surfactant 5 containing epoxy group
Part, 65.5 parts of water.
It is further preferred that the alkenyl polysiloxanes is straight-chain alkenyl organopolysiloxane or three dimensional network eye shape structure
One of the organopolysiloxane containing vinyl or several, the viscosity of the alkenyl polysiloxanes is 50~
10000mPas, preferably 100~1000mPas.
It is further preferred that end, side hanging or both can be located at the hydrogen atom of silicon bonding in the hydrogen containing siloxane
In end again in side hanging position, the structural formula of the hydrogen containing siloxane is as follows:
Wherein, R1、R4、R3For identical or different hydrogen-based, or the alkyl of the linear chain or branched chain for 1~6 carbon atom,
R1、R4、R3In at least one be hydrogen-based；R2For the alkyl of the linear chain or branched chain of 1~6 carbon atom；N, the value range of m be 5~
300。
It is further preferred that the structural formula of the netted silicone resin of phenyl hydroxyl are as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon of identical or different 6~20 carbon atoms
The aralkyl of atom, R' are hydroxyl.
The preparation method of the netted silicone resin of phenyl hydroxyl, comprising the following steps:
A. under an acid catalysis, under alcohol, water environment, the silane agent containing phenyl functional group is added dropwise and carries out polymerization reaction；
B. extractant is added, is based on the netted silicone resin of target hydroxyl containing phenyl, control reaction temperature is 50~90 DEG C, reaction
Time 1~7 hour；
C. product is stood, removes water layer, the netted silicone resin of phenyl hydroxyl is cleaned into neutrality with distilled water, obtains being dissolved in extraction
Take the netted silicon resin solution of phenyl hydroxyl of agent；
D. it by the neutral netted silicon resin solution of hydroxyl containing phenyl, after the membrane filtration for being 0.5~5 μm with aperture, depressurizes
Distillation removal low-boiling-point substance, obtains the netted silicone resin of phenyl hydroxyl.
In step a, the acid catalyst is lewis acid catalyst；Alcohol used is ethyl alcohol, one in isopropanol
Kind；The structural formula of the silane agent containing phenyl functional group is R1(R2O)3Si or R1(R2O)2SiR3, wherein R1、R3To be identical or
The aralkyl of the linear chain or branched chain aryl of different 6~20 carbon atoms either 7~20 carbon atoms, R2For 1~6 carbon
The linear or branched alkyl group of atom, acyloxy.The silane agent containing phenyl functional group can be but be not limited to as follows: phenyl three
Ethoxysilane, phenethyl (trimethoxy) silane, phenyltrimethoxysila,e, diphenyl diethoxy siloxanes.
In above-mentioned steps b, the extractant is one of isomeric alkane or methyl oligosiloxane.
In above-mentioned steps d, the operating condition of the vacuum distillation are as follows: pressure is -0.095MPa or more, and temperature is
120 DEG C~200 DEG C, the vacuum distillation time is 2~4hrs.
It is further preferred that the structural formula of the line style silane coupling agent containing epoxy group is as follows:
Wherein, R1、R4It for the linear or branched alkyl group of identical or different 1~6 carbon atom, or is 7~10 carbon originals
The arylmethylene alkyl or alkyl arylene of son, R1、R4It is preferred that methyl；R2、R3For identical or different hydrogen-based, or for containing 1~3 alkane
The silylation of the linear chain or branched chain of 1~6 carbon atom of oxygroup；R5For the straight chain or branch of 1~12 carbon atom containing epoxy group
The alkyl of chain；M, the value range of n is 1~12.
The line style silane coupling agent containing epoxy group passes through silicon by oligosiloxane containing hydrogen-based and the alkene containing epoxy group
Addition reaction of hydrogen synthesis, or added by oligosiloxane containing hydrogen-based, the alkene containing alkenyl siloxane and containing epoxy group by silicon hydrogen
It is synthesized at reaction.The line style silane coupling agent containing epoxy group the preparation method comprises the following steps: being added in oligosiloxane containing hydrogen-based
Then catalyst is added dropwise to hydrogeneous by the alkene containing epoxy group or by the alkene containing epoxy group and mixed liquor containing alkenyl siloxane
In base oligosiloxane, synthesized by hydrosilylation addition reaction；The catalyst uses platinum metal catalysts, can promote
The addition reaction of Si-H and Si-C=C.
It is further preferred that the surfactant is quaternary cationics or band containing chain alkyl
There is one or more of the nonionic surfactant of polyoxyethylene segment.Surfactant is for emulsifying above-mentioned material
Into water, the surfactant can be but be not limited to as follows: octadecyltrimethylammonium chloride, octadecyl trimethyl bromine
Change ammonium, polyoxyethylene (23) lauryl ether, polyoxyethylene tridecyl ether, nonylphenol polyoxyethylene ether etc..
It is further preferred that the conducting polymer polythiophene be poly- (3,4- ethylenedioxythiophene) and its derivative,
It is preferred that poly- (3,4- ethylenedioxythiophene) is poly- (styrene sulfonic acid), conductivity > 100s/cm.
It is further preferred that the single armed carbon nano-tube aqueous solutions, main component is single armed carbon nanotube, hydroxylating list
One of arm carbon nanotube or carboxylated single armed carbon nanotube, conductivity > 150s/ of the single armed carbon nano-tube aqueous solutions
cm。
Another object of the present invention is to also disclose a kind of system of anti-static release lotion with good stability energy
Preparation Method, comprising the following steps:
1. is weighed the alkenyl polysiloxanes, hydrogen containing siloxane, phenyl hydroxyl web-like silicon tree of corresponding parts by weight by formula
Rouge, conducting polymer polythiophene, single armed carbon nano-tube aqueous solutions, the linear silane coupling agent containing epoxy group, surfactant,
Water；
2. is by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conductive polymer poly
Thiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying
In equipment, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the anti-of good stability energy by
The release lotion of electrostatic.
Compared with prior art, the beneficial effect of technical solution of the present invention is:
1. conducting polymer polythiophene and single armed carbon nanotube are added in anti-static release lotion of the invention, both have
It has conductivity, but conductivity principle is different, is used in mixed way, can play synergistic effect, mutual tonifying for the deficiency, so as to so that quiet using resisting
The release film of ionization type lotion preparation has well stable antistatic property；
2. the linear silane coupling agent containing epoxy group is introduced in anti-static release lotion of the invention, to conductive polymer poly
Thiophene plays inducing action, enhances its electric conductivity, and stability is good, meanwhile, can reduce conducting polymer polythiophene to from
The negatively influencing of catalyst system during type film preparation can achieve the desired results without increasing catalyst amount；
3. the netted silicone resin of phenyl hydroxyl is introduced in anti-static release lotion of the invention, due to phenyl hydroxyl web-like silicon tree
Rouge structure is special, and active group, thus after being applied to film substrate, it can be ensured that release film peeling force obtained is steady
It is fixed；
4. emulsifying by the way that surfactant and high speed is added, it is sufficiently mixed each component, anti-static release lotion obtained
For water-based system, it is applicable to online or offline coating solidification, primary coating can reach antistatic and release effect, and
With good storage stability.
Specific embodiment
Further illustrate that the present invention, following embodiment are the preferable embodiment party of the present invention below by specific embodiment
Formula, but embodiments of the present invention are not limited by following embodiments, therefore the scope of protection of present invention is not limited to
In described.
Embodiment 1:
A kind of anti-static release lotion with good stability energy, by weight, consisting of: alkenyl polysiloxanes
20 parts, 8.5 parts of hydrogen containing siloxane, 0.05 part of the netted silicone resin of phenyl hydroxyl, 0.05 part of conducting polymer polythiophene, single armed carbon
2 parts of nanotube aqueous solution, 60 parts of 5.9 parts of 3.5 parts of linear silane coupling agent, surfactant, the water containing epoxy group.
The alkenyl polysiloxanes is by the polysiloxane and 15 that 5 parts of viscosity are that 100mPas straight-chain ethylene base blocks
Part viscosity is that the MQ resin of 700mPas ethenyl blocking forms.
The hydrogen containing siloxane is that (hydrogen content is methyl hydrogen siloxane-dimethyl siloxane cyclocopolymer
0.8mmol/g)。
The structural formula of the netted silicone resin of phenyl hydroxyl is as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon of identical or different 6~20 carbon atoms
The aralkyl of atom, R' are hydroxyl.
The netted silicone resin of phenyl hydroxyl the preparation method comprises the following steps: have stirring, reflux condensing tube, thermometer and dropping liquid
It is separately added into 140g distilled water in the four-hole boiling flask of funnel, the hydrochloric acid that 1.0g concentration is 1mol/L, after being stirred, is added dropwise
360.56g phenyl triethoxysilane, 180.11g dimethyldimethoxysil,ne add 100g dehydrated alcohol, 10g 37%
Hydrochloric acid and 170g isohexadecane extractant carry out cohydrolysis-polycondensation reaction, and reaction temperature is 85 DEG C, after the control reaction time is 2h
Stratification removes water phase, is washed organic phase to neutrality with distilled water, with aperture be 0.5 μm membrane filtration after will in
Property organic phase, be evaporated under reduced pressure (110~130 DEG C/- 0.096Mpa) removal low-boiling-point substances to get clear phenyl hydroxyl net
Shape silicone resin.
The structural formula of the linear silane coupling agent containing epoxy group is as follows:
The surfactant is Cetyltrimethylammonium bromide.
The conducting polymer polythiophene is commercially available poly- (3,4- ethylenedioxythiophene) poly- (styrene sulfonic acid) solution,
Wherein active constituent content is 3-5%, conductivity > 100s/cm.
The single armed carbon nano-tube aqueous solutions are commercially available carboxylated single armed carbon nano-tube solution, purity > 90%, conductivity
> 150s/cm, caliber 1-2nm, length 0.5-2um, specific surface area > 450m2/g。
A kind of preparation method of above-mentioned anti-static release lotion with good stability energy, comprising the following steps:
1. is weighed the alkenyl polysiloxanes, hydrogen containing siloxane, phenyl hydroxyl web-like silicon tree of corresponding parts by weight by formula
Rouge, conducting polymer polythiophene, single armed carbon nano-tube aqueous solutions, the linear silane coupling agent containing epoxy group, surfactant,
Water；
2. is by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conductive polymer poly
Thiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying
In equipment, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the anti-of good stability energy by
The release lotion of electrostatic.
Embodiment 2:
A kind of anti-static release lotion with good stability energy, by weight, consisting of: alkenyl polysiloxanes
5 parts, 4 parts of hydrogen containing siloxane, 1 part of the netted silicone resin of phenyl hydroxyl, 5 parts of conducting polymer polythiophene, single armed carbon nanotube water
0.05 part of solution, 69.95 parts of 10 parts of 5 parts of linear silane coupling agent, surfactant, the water containing epoxy group.
The alkenyl polysiloxanes is the MT resin that viscosity is 100mPas ethenyl blocking.
The hydrogen containing siloxane is that (hydrogen content is methyl hydrogen siloxane-dimethyl siloxane cyclocopolymer
0.45mmol/g)。
The structural formula of the netted silicone resin of phenyl hydroxyl is as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon of identical or different 6~20 carbon atoms
The aralkyl of atom, R' are hydroxyl；
The netted silicone resin of phenyl hydroxyl the preparation method comprises the following steps: have stirring, reflux condensing tube, thermometer and dropping liquid
It is separately added into 200g distilled water in the four-hole boiling flask of funnel, the hydrochloric acid that 1.2g concentration is 1mol/L, after being stirred, is added dropwise
339.51g phenethyl (trimethoxy) silane, 272g diphenyl diethoxy silane, add 100g dehydrated alcohol, 10g
37% hydrochloric acid and 380g isohexadecane extractant carry out cohydrolysis-polycondensation, and reaction temperature is 90 DEG C, after the control reaction time is 1h
Stratification removes water phase, is washed organic phase to neutrality with distilled water, with aperture be 0.5 μm membrane filtration after will in
Property organic phase, be evaporated under reduced pressure (110~130 DEG C/- 0.096Mpa) removal low-boiling-point substances to get clear phenyl hydroxyl net
The silicone resin of shape structure.
The structural formula of the linear silane coupling agent containing epoxy group is as follows:
The surfactant is polyoxyethylene (23) lauryl ether.
The conducting polymer polythiophene is commercially available poly- (3,4- ethylenedioxythiophene) poly- (styrene sulfonic acid) solution,
Wherein active constituent content is 1-1.5%, conductivity > 100s/cm.
The single armed carbon nano-tube aqueous solutions are commercially available hydroxylating single armed carbon nano-tube solution, purity > 90%, conductivity
> 150s/cm, caliber 1-2nm, length 5-30um, specific surface area > 450m2/g。
A kind of preparation method of above-mentioned anti-static release lotion with good stability energy, comprising the following steps:
1. is weighed the alkenyl polysiloxanes, hydrogen containing siloxane, phenyl hydroxyl web-like silicon tree of corresponding parts by weight by formula
Rouge, conducting polymer polythiophene, single armed carbon nano-tube aqueous solutions, the linear silane coupling agent containing epoxy group, surfactant,
Water；
2. is by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conductive polymer poly
Thiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying
In equipment, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the anti-of good stability energy by
The release lotion of electrostatic.
Embodiment 3:
A kind of anti-static release lotion with good stability energy, by weight, consisting of: alkenyl polysiloxanes
9 parts, 0.5 part of hydrogen containing siloxane, 0.8 part of the netted silicone resin of phenyl hydroxyl, 2.5 parts of conducting polymer polythiophene, single armed carbon receives
1.2 parts of mitron aqueous solution, 85 parts of 1 part of 1 part of linear silane coupling agent, surfactant, the water containing epoxy group.
The alkenyl polysiloxanes is the polysiloxane that viscosity is 500mPas straight-chain ethylene base sealing end.
The hydrogen containing siloxane is that the dimethyl polysiloxane that two ends are blocked through dimethylhydrogensiloxy is (hydrogeneous
Amount is 1.7mmol/g).
The structural formula of the netted silicone resin of phenyl hydroxyl is as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon of identical or different 6~20 carbon atoms
The aralkyl of atom, R' are hydroxyl；
The netted silicone resin of phenyl hydroxyl the preparation method comprises the following steps: have stirring, reflux condensing tube, thermometer and dropping liquid
It is separately added into 200g distilled water in the four-hole boiling flask of funnel, the hydrochloric acid that 1.2g concentration is 1mol/L, after being stirred, is added dropwise
339.51g phenethyl (trimethoxy) silane, 272g diphenyl diethoxy silane, add 100g dehydrated alcohol, 10g
37% hydrochloric acid and 380g isohexadecane extractant carry out cohydrolysis-polycondensation, and reaction temperature is 90 DEG C, after the control reaction time is 1h
Stratification removes water phase, is washed organic phase to neutrality with distilled water, with aperture be 0.5 μm membrane filtration after will in
Property organic phase, be evaporated under reduced pressure (110~130 DEG C/- 0.096Mpa) removal low-boiling-point substances to get clear phenyl hydroxyl net
The silicone resin of shape structure.
The structural formula of the linear silane coupling agent containing epoxy group is as follows:
The surfactant is polyoxyethylene (23) lauryl ether.
The conducting polymer polythiophene is commercially available poly- (3,4- ethylenedioxythiophene) poly- (styrene sulfonic acid) solution,
Wherein active constituent content is 2-3%, conductivity > 100s/cm.
The single armed carbon nano-tube aqueous solutions are commercially available single armed carbon nano-tube solution, purity > 90%, conductivity > 150s/
Cm, caliber 1-2nm, length 0.5-2um, specific surface area > 450m2/g。
A kind of preparation method of above-mentioned anti-static release lotion with good stability energy, comprising the following steps:
1. is weighed the alkenyl polysiloxanes, hydrogen containing siloxane, phenyl hydroxyl web-like silicon tree of corresponding parts by weight by formula
Rouge, conducting polymer polythiophene, single armed carbon nano-tube aqueous solutions, the linear silane coupling agent containing epoxy group, surfactant,
Water；
2. is by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conductive polymer poly
Thiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying
In equipment, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the anti-of good stability energy by
The release lotion of electrostatic.
Embodiment 4:
A kind of anti-static release lotion with good stability energy, by weight, consisting of: alkenyl polysiloxanes
12 parts, 10 parts of hydrogen containing siloxane, 0.35 part of the netted silicone resin of phenyl hydroxyl, 3.55 parts of conducting polymer polythiophene, single armed carbon
0.8 part of nanotube aqueous solution, 65.5 parts of 5 parts of 2.8 parts of linear silane coupling agent, surfactant, the water containing epoxy group.
The alkenyl polysiloxanes is that viscosity is MT resin of the 750mPas branch containing vinyl.
The hydrogen containing siloxane is the methylhydrogenpolysi,oxane (hydrogen content that two ends are blocked through trimethylsiloxy
For 0.25mmol/g).
The structural formula of the netted silicone resin of phenyl hydroxyl is as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon of identical or different 6~20 carbon atoms
The aralkyl of atom, R' are hydroxyl；
The netted silicone resin of phenyl hydroxyl the preparation method comprises the following steps: have stirring, reflux condensing tube, thermometer and dropping liquid
It is separately added into 140g distilled water in the four-hole boiling flask of funnel, the hydrochloric acid that 1.g concentration is 1mol/L, after being stirred, 408g is added dropwise
Diphenyl diethoxy silane, 180.11g dimethyldimethoxysil,ne, 360.56g phenyl triethoxysilane, add
50g dehydrated alcohol, 10g37% hydrochloric acid and 250g decamethyl tetrasiloxane extractant carry out cohydrolysis-polycondensation, reaction temperature 85
DEG C, the control reaction time is stratification after 2h, and water phase is removed, and is washed organic phase to neutrality with distilled water, is with aperture
By neutral organic phase after 0.5 μm of membrane filtration, be evaporated under reduced pressure (110~130 DEG C/- 0.096Mpa) removal low-boiling-point substances to get
The silicone resin of the phenyl hydroxyl reticular structure of clear.
The structural formula of the linear silane coupling agent containing epoxy group is as follows:
The surfactant is Cetyltrimethylammonium bromide.
The conducting polymer polythiophene is commercially available poly- (3,4- ethylenedioxythiophene) poly- (styrene sulfonic acid) solution,
Wherein active constituent content is 1-1.5%, conductivity > 100s/cm.
The single armed carbon nano-tube aqueous solutions are commercially available carboxylated single armed carbon nano-tube solution, purity > 90%, conductivity
> 150s/cm, caliber 1-2nm, length 5-30um, specific surface area > 450m2/g。
A kind of preparation method of above-mentioned anti-static release lotion with good stability energy, comprising the following steps:
1. is weighed the alkenyl polysiloxanes, hydrogen containing siloxane, phenyl hydroxyl web-like silicon tree of corresponding parts by weight by formula
Rouge, conducting polymer polythiophene, single armed carbon nano-tube aqueous solutions, the linear silane coupling agent containing epoxy group, surfactant,
Water；
2. is by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conductive polymer poly
Thiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying
In equipment, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the anti-of good stability energy by
The release lotion of electrostatic.
A kind of beneficial effect of anti-static release lotion with good stability energy to illustrate the invention, will be of the invention
Examples 1 to 4 made from anti-static release lotion be used to prepare anti-static release film, while adding comparative example 1, comparative example 1
For the anti-static release film of conventional method preparation, and to anti-static release film made from the embodiment of the present invention 1~4 and comparative example
1 anti-static release film carries out performance detection.
1. the anti-static release film formulation of embodiment 1-4:
Table 1
In the anti-static release film formulation of table 1, it is described self-control catalyst system lotion component and the preparation method is as follows:
1. component: diacetyl acetate ester closes the poly organo of 8 parts of platinum (platinum content 100ppm), straight-chain ethylene base sealing end
27 parts of alkane (viscosity 100mPas), 10 parts, 55 parts of water of polyoxyethylene (23) lauryl ether；
2. preparation method: the diacetyl acetate ester of above-mentioned parts by weight is closed to the poly organo of platinum, straight-chain ethylene base sealing end
Alkane, polyoxyethylene (23) lauryl ether and water are added in emulsifying equipment, are emulsified to get the catalyst system is arrived
Lotion.
2. the anti-static release membrane preparation method of embodiment 1-4:
A. substrate: 25umPET film is selected；
B. Meyer stick is coated with: by the release film formulation of table 1, by anti-static release lotion, catalyst system lotion and distillation
Water is mixed and made into coating fluid, and coating fluid is applied to respectively on corresponding substrate using 5# standardization Meyer stick；
C. curing process: under the conditions of the substrate for being coated with coating fluid is placed in 160 DEG C of temperature, dry solidification 1min is to get anti-
Electrostatic release film.
3. the anti-static release membrane preparation method of comparative example 1:
A. substrate: 25umPET film is selected；
B. antistatic film is prepared: molten using poly- (3,4- ethylenedioxythiophene) poly- (styrene sulfonic acid) bought on the market
Liquid is coating fluid, and coating fluid is applied on substrate using 5# standardization Meyer stick, is placed under the conditions of 170 DEG C of temperature, dry solid
Change 1min to get antistatic film；
C. it prepares anti-static release film: coating is made with 25 parts of silicone release lotion, 5 parts of catalytic emulsion and 73 parts of water
Coating fluid is applied in step b on antistatic film obtained using 5# standardization Meyer stick, is placed in 160 DEG C of temperature conditions by liquid
Under, dry solidification 1min is to get anti-static release film.
In the preparation method step c of the anti-static release film of above-mentioned comparative example 1, the component of the catalytic emulsion and preparation side
Method:
1. component: diacetyl acetate ester closes the poly organo of 8 parts of platinum (platinum content 100ppm), straight-chain ethylene base sealing end
27 parts of alkane (viscosity 100mPas), 10 parts, 55 parts of water of polyoxyethylene (23) lauryl ether；
2. preparation method: the diacetyl acetate ester of above-mentioned parts by weight is closed to the poly organo of platinum, straight-chain ethylene base sealing end
Alkane, polyoxyethylene (23) lauryl ether and water are added in emulsifying equipment, are emulsified to get the catalyst system is arrived
Lotion.
In the preparation method step c of the anti-static release film of above-mentioned comparative example 1, the component of the silicone release lotion and
The preparation method is as follows:
1. component: 15 parts of the polysiloxane (viscosity 500mPas) of straight-chain ethylene base sealing end, two ends are through diformazan
5 parts of dimethyl polysiloxane (hydrogen content 0.85mmol/g), the netted silicone resin 1 of phenyl hydroxyl of base hydrogen siloxy sealing end
Part, 10 parts of polyoxyethylene (23) lauryl ether, 69 parts of water, be added in emulsifying equipment, emulsified, obtain organosilicon from
Type system lotion；
2. preparation method: by the polysiloxane of the straight-chain ethylene base sealing end of above-mentioned parts by weight, two ends through dimethyl
Hydrogen siloxy sealing end dimethyl polysiloxane, the netted silicone resin of phenyl hydroxyl, polyoxyethylene (23) lauryl ether and
Water is added in emulsifying equipment, is emulsified to get silicone release system lotion is arrived.
4. anti-static release film performance detection index and method:
1. appearance: range estimation, and test haze value changes delta H (ASTM D1003)；
2. anchor performance (20min): being placed at room temperature for 20min after solidification, rubbed back and forth with finger 10 times, observation release layer is
No to occur fuzzy or be rubbed off, anchor the performance test results is indicated with zero, △, X, and zero is no significant change；△ is that appearance becomes dim,
But do not reveal substrate；X is rubbed off for release layer, exposes substrate.
3. anchor performance (rs for 24 hours): being placed at room temperature for rs for 24 hours after solidification, rubbed back and forth with finger 10 times, observation release layer is
No to occur fuzzy or be rubbed off, anchor the performance test results is indicated with zero, △, X, and zero is no significant change；△ is that appearance becomes dim,
But do not reveal substrate；X is rubbed off for release layer, exposes substrate.
4. surface resistivity: using the surface resistivity of electrostatic tester SIMCO ST-4 test layer upper surface.
5. peel test force: standard testing adhesive tape (TESA7475) longitudinally gently being covered in layer upper surface, sample is greater than
175mm*25mm, roller reciprocal each roll-in 3 times, is fixed sample on stainless steel with double-sided adhesive with 300mm/min, stainless
Steel square is pressed on sample (pressure 20g/cm2), 23 ± 2 DEG C &20min after square takes out, are tested using pulling force or release machine
Peeling force, speed 300mm/min.Each sample parallel testing 3 times takes 3 test result average values；
6. aging peel test force: standard testing adhesive tape (TESA7475) longitudinally gently being covered in layer upper surface, sample is big
In 175mm*25mm, roller reciprocal each roll-in 3 times, is fixed sample on stainless steel with double-sided adhesive, no with 300mm/min
Rust steel square is pressed on sample (pressure 20g/cm2), 70 DEG C &20hrs, after square takes out, at 23 ± 2 DEG C of temperature, 55 ± 5%
R.H. 4hrs is placed under (relative humidity), tests peeling force, speed 300mm/min using pulling force or release machine.Each sample is flat
Row test 3 times, takes 3 test result average values.
7. remaining adhesion: standard testing adhesive tape (TESA7475) gently being covered in film layer upper surface, sample is greater than
175mm*25mm, roller is with 300mm/min, and reciprocal each roll-in 3 times, stainless steel square is pressed on sample (pressure 20g/cm2),
70℃&20hrs；Briquetting is taken out, sample is placed in 23 ± 2 DEG C, places 4hrs under 50 ± 5%R.H. (relative humidity)；It will test
Adhesive tape is torn, and is gently covered on clean dustless stainless steel plate (smooth surface), and roller is with 300mm/min, reciprocal each roll-in three
It is secondary, peeling force, 180 ° of removings, speed 300mm/min test are tested using puller system.Blank sample is that test tape overlays on Teflon
On imperial plate, remaining step is consistent with the above.Remaining adhesion is connect rate and is indicated with residual, residual to connect rate=test peeling force/blank stripping
From power * 100%.Each sample parallel testing 3 times takes 3 test result average values.
Anti-static release film made from the anti-static release lotion of the embodiment of the present invention 1~4 and comparative example 1 it is antistatic from
Each performance test results of type film are as follows:
Table 2
From table 2 it can be seen that anti-static release film made from anti-static release lotion using the embodiment of the present invention 1~4
Compared with the anti-static release film of comparative example 1, clear property is presented in appearance indifference；The embodiment of the present invention 1~4 it is antistatic
The haze value changes delta H of release film is lower than the anti-static release film of comparative example 1；The anti-static release film of the embodiment of the present invention 1~4
Anchor performance (rs for 24 hours) be better than comparative example 1 anti-static release film；Anti-static release film made from the embodiment of the present invention 1~4
Surface resistivity be below the anti-static release film of comparative example 1, i.e. anti-static release film made from the embodiment of the present invention 1~4
Antistatic property be superior to comparative example 1；In terms of peeling force, by comparing peeling force (0hrs) and 70 DEG C of aging peeling forces,
It was found that the anti-static release film of the embodiment of the present invention 1~4 aging before and after peeling force changing value lower than comparative example 1 it is antistatic from
Type film；In addition, the remaining adhesion of the anti-static release film of the embodiment of the present invention 1~4 be also above made from comparative example 1 resist it is quiet
Ionization type film.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also be made on the basis of the above description
Its various forms of variation or variation, there is no need and unable to be exhaustive to all embodiments.It is all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., the protection scope of the claims in the present invention should be included in
Within.
Claims (10)
1. it is a kind of with good stability can anti-static release lotion, which is characterized in that by weight, it is described it is antistatic from
The composition of type lotion are as follows: 5~20 parts of alkenyl polysiloxanes, 0.5~10 part of hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl
0.05~1 part, 0.05~5 part of conducting polymer polythiophene, 0.05~2 part of single armed carbon nano-tube aqueous solutions, the line containing epoxy group
Property 1~5 part of silane coupling agent, 1~10 part of surfactant, 60~85 parts of water.
2. the anti-static release lotion according to claim 1 with good stability energy, which is characterized in that the alkenyl
Polysiloxanes is in straight-chain alkenyl organopolysiloxane or the organopolysiloxane containing vinyl of three dimensional network eye shape structure
One or more, the viscosity of the alkenyl polysiloxanes are 50~10000mPas.
3. the anti-static release lotion according to claim 2 with good stability energy, which is characterized in that described hydrogeneous
End, side hanging can be located at the hydrogen atom of silicon bonding in polysiloxanes or not only in end again in side hanging position, it is described hydrogeneous to gather
The structural formula of siloxanes is as follows:
Wherein, R1、R4、R3For identical or different hydrogen-based, or the alkyl of the linear chain or branched chain for 1~6 carbon atom, R1、R4、
R3At least one is hydrogen-based；R2For the alkyl of the linear chain or branched chain of 1~6 carbon atom；N, the value range of m is 5~300.
4. the anti-static release lotion according to claim 3 with good stability energy, which is characterized in that the phenyl
The structural formula of the netted silicone resin of hydroxyl are as follows:
Wherein, R, R ", R " ' for the linear chain or branched chain aryl or 7~20 carbon atoms of identical or different 6~20 carbon atoms
Aralkyl, R' is hydroxyl.
5. the anti-static release lotion according to claim 4 with good stability energy, which is characterized in that the surface
Activating agent is that the quaternary cationics containing chain alkyl or the non-ionic surface with polyoxyethylene segment are living
One or more of property agent.
6. the anti-static release lotion according to claim 5 with good stability energy, which is characterized in that described to contain ring
The structural formula of the line style silane coupling agent of oxygroup is as follows:
Wherein, R1、R4It for the linear or branched alkyl group of identical or different 1~6 carbon atom, or is 7~10 carbon atoms
Arylmethylene alkyl or alkyl arylene；R2、R3It for identical or different hydrogen-based, or is 1~6 carbon atom containing 1~3 alkoxy
Linear chain or branched chain silylation；R5For the alkyl of the linear chain or branched chain of 1~12 carbon atom containing epoxy group；M, the range of n
Value is 1~12.
7. the anti-static release lotion according to claim 6 with good stability energy, which is characterized in that described to contain ring
The line style silane coupling agent of oxygroup synthesized by oligosiloxane containing hydrogen-based and the alkene containing epoxy group by hydrosilylation or
Person is synthesized by oligosiloxane containing hydrogen-based, the alkene containing alkenyl siloxane and containing epoxy group by hydrosilylation.
8. the anti-static release lotion according to claim 1-7 with good stability energy, which is characterized in that
The conducting polymer polythiophene is poly- (3,4- ethylenedioxythiophene) and its derivative.
9. the anti-static release lotion according to claim 8 with good stability energy, which is characterized in that the list
Arm carbon nano-tube aqueous solutions are one in single armed carbon nanotube, hydroxylating single armed carbon nanotube or carboxylated single armed carbon nanotube
Kind.
10. a kind of preparation method of the anti-static release lotion with good stability energy, which is characterized in that including following step
It is rapid:
1. is weighed the alkenyl polysiloxanes of corresponding parts by weight by formula, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, led
Electric polymer polythiophene, single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group；
2. by weighed alkenyl polysiloxanes, hydrogen containing siloxane, the netted silicone resin of phenyl hydroxyl, conducting polymer polythiophene,
Single armed carbon nano-tube aqueous solutions, linear silane coupling agent, surfactant, water containing epoxy group are added to emulsifying equipment
In, high speed emulsification is carried out, lotion is obtained；
3. the step lotion that 2. middle emulsification obtains is filtered with 1um filter core to get with the antistatic of good stability energy by
Release lotion.
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