CN107573735A - A kind of efficient and environment-friendly type UV dark curing three-proofing coatings - Google Patents
A kind of efficient and environment-friendly type UV dark curing three-proofing coatings Download PDFInfo
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- CN107573735A CN107573735A CN201710810762.1A CN201710810762A CN107573735A CN 107573735 A CN107573735 A CN 107573735A CN 201710810762 A CN201710810762 A CN 201710810762A CN 107573735 A CN107573735 A CN 107573735A
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- proofing
- dark curing
- proofing coatings
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- SWIPDARVKBUUKH-UHFFFAOYSA-N CC(C)(c(cc1CC=C)ccc1O)c(cc1CC=C)cc(CC=C)c1O Chemical compound CC(C)(c(cc1CC=C)ccc1O)c(cc1CC=C)cc(CC=C)c1O SWIPDARVKBUUKH-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention provides a kind of high-efficiency environment friendly UV dark curing three-proofing coatings, and the preparing raw material of the three-proofing coating includes：30 70 parts of acrylic resin；30 70 parts of reactive diluent；1 10 parts of light trigger；0.1 5 parts of leveling auxiliary agent；0.1 8 parts of defoamer；0.1 10 parts of wetting agent；0.1 3 parts of fire retardant.
Description
Technical field
The present invention relates to printed circuit board protection technology field, and in particular to a kind of wiring board anti-corrosion efficient and environment-friendly type UV-
Dark curing three-proofing coating.
Background technology
Three-proofing coating is widely used in electronic electric equipment wiring board anti-corrosion protection, such as intelligent appliance, automotive electronics, power supply/change
Frequently, intelligent industrial-control, military project ship, outdoor precision equipment etc..Three-proofing coating is coated in PCB surface, and one layer of densification is formed after solidification
Diaphragm, protection circuit plate from external environment (humidity, mould, salt fog, Gao Chen, vibrations, corrosive gas etc.) corrosion,
Product reliability is improved, increases coefficient safe to use.
Existing UV- moisture-curables mode, it solidifies based on photocuring and reacted with moisture in air, because of two kinds of curing modes
Be independent of each other, and the moisture in air is at all times, thus without illumination also can because with moisture reaction in air and caused by
Premature cure, cause viscosity to increase, and influence normal use, reduce service life.It is wet that UV- dark curings three-proofing coating is different from UV-
Curing mode, its principle of solidification are based on photocuring and dark reaction.During without illumination, autoreactivity will not occur；In addition, because not
Also do not reacted containing isocyano with moisture in air, extended storage stability can be kept, long shelf-life was up to 12 months.After by illumination
Can just solidify, illumination realize can irradiation area solidification, mercaptan and acrylate are triggered in shadow region after ultraviolet light
Group occurs dark reaction and realizes crosslinking curing.Shadow region occur dark reaction, solidification process is simple, quick solidifying, solidification process not by
Moisture content, coating accumulation and thickness effect；Solidification uniformity is good, and paint film cubical contraction is small, and adhesive force is strong；Stability is good,
It will not occur to cause product viscosity to increase because of affected by moisture, the problem of constructional difficulties.
Wiring board anti-corrosion material is usually used for solvent-borne type three-proofing coating at present, due to containing the organic solvents such as benzene class, tool
There are the danger such as combustion explosion, and be detrimental to health, Long Term Contact can induce occupational disease.With the raising of environmental requirement, and
The use limitation to volatile solvent, the solvent-free three-proofing coating of novel environment-friendly turn into an urgent demand in market both at home and abroad.
UV solidification three-proofing coatings are a kind of environment-friendly type solvent-free coating materials, have chemically active liquid by UV is light-initiated
Material rapid polymerization is crosslinked, instantaneous solidification film forming.There is rapid curing, low energy consumption, high efficiency, there is " 5E " characteristic：
Efficient is efficient, and Economical is economical, Energy Saving energy-conservations, Environmental Friendly environment friend
It is good, Enabling wide adaptabilities, it is with a wide range of applications.
Prior art discloses a kind of UV- moistures dual cure three-proofing coating, in the region that ultraviolet light is difficult to irradiate, by with
In air moisture react, crosslinking curing, so as to realize to various complicated type wiring boards (as shape, thickness, color have it is certain
Limitation) protective effect.
Existing UV- moisture-curables mode, it solidifies based on photocuring and reacted with moisture in air, because of two kinds of curing modes
Be independent of each other, and the moisture in air is at all times, thus without illumination also can because with moisture reaction in air and caused by shift to an earlier date
Solidification, causes viscosity to increase, and influences normal use, reduces service life.
UV- moisture dual cure three-proofing coatings can occur anti-because containing isocyano (- NCO) in formula with moisture in air
Should, and then realize the solidification in shadow region.But problems be present：
1) without illumination also can because with air moisture reaction and caused by premature cure, cause viscosity to increase, and influence just
Often use, reduce service life；
2) to moisture-sensitive, viscosity increases during causing construction storage, increases difficulty of construction；
3) shadow region curing rate depends on moisture content in air, and humidity is low, hardening time length, has objectivity；
4) cubical contraction is big, poor adhesive force, and the insulating properties of paint film and antiseptic property have decline after the solidification of shadow region.
The UV- dark curing three-proofing coatings of the present invention, are mainly used in wiring board corrosion-resistant field, have environmentally friendly, the advantage such as efficient.
It can just solidify after illumination, not reacted with moisture in air, stable storing, long shelf-life.After ultraviolet light, trigger
Mercaptan occurs dark reaction with acrylate group and realizes crosslinking curing.A variety of construction technologies can be met：Spraying, brush, dipping, point
Glue etc. is semi-automatic and full-automatic coating processes.
The content of the invention
In view of the above-mentioned problems, the present invention provides a kind of high-efficiency environment friendly UV- dark curing three-proofing coatings, in parts by weight, institute
The preparing raw material for stating three-proofing coating includes：
As one embodiment of the present invention, in parts by weight, the preparing raw material of the three-proofing coating includes：
As one embodiment of the present invention, in parts by weight, the preparing raw material of the three-proofing coating includes：
As one embodiment of the present invention, the monomer for preparing of the acrylic resin includes acrylic acid, non-functional
Alkyl acrylate, the alkyl acrylate containing function monomer.
As one embodiment of the present invention, the light trigger is selected from 2,4,6- trimethylbenzoy-diphenies
Phosphine oxide, 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-phenyl ketone, 2- methyl isophthalic acids-[4- methyl mercaptos
Phenyl] -2- morpholinyl -1- acetone, 2- isopropyl thioxanthones, 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyls-ring
It is one or more in base-phenyl ketone.
As one embodiment of the present invention, the leveling auxiliary agent is selected from silicon-type leveling auxiliary agent.
As one embodiment of the present invention, the defoamer is selected from saturated alcohols, fatty alcohol, fatty acid alcohol, advanced fat
Mixture more than one or both of fat acid metallic soap, sulfonated oil or organic silicone oil.
As one embodiment of the present invention, the reactive diluent is selected from the reactive diluent containing epoxide group.
As one embodiment of the present invention, the fire retardant is organic fire-retardant.
The second aspect of the present invention provides a kind of method for preparing above-mentioned high-efficiency environment friendly UV- dark curing three-proofing coatings, and it is special
Sign is, as follows the step of methods described：
1) acrylic resin, reactive diluent, light trigger is taken to pour into reactor by weight, with 300r/min rotating speed
Mix 60 minutes；
2) leveling auxiliary agent, defoamer, wetting agent, fire retardant are added by weight percentage in step 1), with 300r/min
Rotating speed mix what can be made within 60 minutes.
Beneficial effect：
1) principle of solidification is based on photocuring and dark reaction.
2) when without illumination, autoreactivity will not occur；Because also not reacted without isocyano with moisture in air, can protect
Extended storage stability is held, long shelf-life was up to 12 months.
3) composition in being formulated, can react with key, realize dark curing.
The present invention can just solidify after by illumination, illumination realize can irradiation area solidification, shadow region is through ultraviolet lighting
After penetrating, trigger mercaptan that dark reaction occurs with acrylate group and realize crosslinking curing.
4) three-proofing coating of the invention, shadow region can carry out dark reaction at room temperature, without heating operation.
5) quick solidifying (under normal temperature, shadow region 24H can completion of cure), solidification process is not influenceed by moisture content.In addition,
Heating can accelerate the solidification in shadow region, be greatly improved efficiency.
6) dark reaction occurs for shadow region, and solidification is simple, quick solidifying, and solidification process is not by moisture content, coating accumulation and thickness
Degree influences；Solidification uniformity is good, and paint film cubical contraction is small, and adhesive force is strong；Stability is good, will not occur because of affected by moisture and
Product viscosity is caused to increase, the problem of constructional difficulties.
Embodiment
Participate in the election of the detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention
The identical implication that technical staff is generally understood that.When contradiction be present, the definition in this specification is defined.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or
Such a composition, step, method, product or the intrinsic key element of device.
Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this
Phrase will make claim be closed, it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme,
It is only limited to the key element described in the clause；Other key elements are not excluded outside the claim as entirety.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value limits, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope
All scopes that any pairing of lower limit or preferred value is formed, regardless of whether the scope separately discloses.For example, when open
During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end
Value and all integers and fraction within the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any
It is a kind of " refer to that the item that describes thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to represent that the present invention is not limited to this
Quantity, include the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase
Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.It is approximate in some examples
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope limits can be with
Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article " one kind " before key element of the present invention or component and "one" to key element or the quantitative requirement of component
(i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number
The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.
The present invention provides a kind of high-efficiency environment friendly UV- dark curing three-proofing coatings, in parts by weight, the preparation of the three-proofing coating
Raw material includes：
Acrylic resin
Acrylic resin refers to the resin synthesized by acrylic compounds and methyl acrylic ester and other vinyl monomer copolymerizations.
Conventional acrylic resin is prepared by three class monomers：Hard monomer, soft monomer and function monomer.The vitrifying of the hard monomer
Temperature is high, assigns hardness of film, tensile strength, cohesive force and wearability；Soft monomer gives the certain pliability of film, extensibility
And durability.The introducing of function monomer is to introduce functional group, assigns polymer certain crosslinking reactivity, plays crosslinked action.
In the present invention, prepare the acrylic resin monomer comprise at least acrylic acid, non-functional alkyl acrylate,
Alkyl acrylate containing function monomer, and a length of C1-C8 of carbochain of the alkyl acrylate.
In the present invention, the non-functional alkyl acrylate can enumerate methyl acrylate, ethyl acrylate, acrylic acid
Propyl ester, butyl acrylate, 2-EHA, n-octyl.
In the present invention, the non-functional alkyl acrylate is propyl acrylate.
In the present invention, the alkyl acrylate containing function monomer can enumerate hydroxy-ethyl acrylate, acrylic acid -4-
Hydroxy butyl ester, methacrylic acid -4- hydroxy butyl esters, the own ester of acrylic acid -6- hydroxyls, the own ester of methacrylic acid -6- hydroxyls, acrylic acid -8- hydroxyls are pungent
Ester, methacrylic acid -8- hydroxyls monooctyl ester, acrylic acid -10- hydroxyls last of the ten Heavenly stems ester, methacrylic acid -10- hydroxyls last of the ten Heavenly stems ester, acrylic acid sulphur propyl ester, first
One or more combination in base acrylic acid sulphur propyl ester, dimethylaminoethyl acrylate and dimethylaminoethyl methacrylate.
In the present invention, the alkyl acrylate containing function monomer is acrylic acid -8- hydroxyl monooctyl esters.
In the present invention, the monomer for preparing of the acrylic resin is acrylic acid, propyl acrylate and acrylic acid -8- hydroxyl monooctyl esters
It is 1 according to weight part ratio：0.1：0.1 ratio is mixed with to obtain.
Reactive diluent：Heretofore described reactive diluent is made up of two kinds of reactive diluents.
Reactive diluent 1：The preparation method of heretofore described reactive diluent 1 is as follows：
1、
Wherein, the mol ratio of allyl bromide, bromoallylene and bisphenol-A is 3：1.1.
2、
Wherein, the mol ratio of step 1 is prepared product, epoxychloropropane and 4 bromide is 1：8：0.05.
Reactive diluent 2：The preparation method of heretofore described reactive diluent 2 is as follows：
5- sulfydryl Benadon HPPMP (1mol), epoxychloropropane (10mol) and 4 bromide (0.06mol) are put
Put in four neck round-bottom flasks equipped with magnetic stirring apparatus, thermometer and reflux condensing tube, reactant is stirred at room temperature
After 15 minutes, then under nitrogen atmosphere, be heated to 95 DEG C maintain 2 hours, then be added dropwise sodium hydroxide solution (2mol,
48wt%) into four neck round-bottom flasks, reaction temperature is then maintained 95 DEG C, reacted 2 hours.By the chlorination in course of reaction
Sodium is filtered out, and remaining epoxychloropropane is evaporated in vacuo and separated.Then the NaOH aqueous solution (1mol, mass fraction are used：5%) and
Toluene adds crude product and further reacted, and after reaction is kept for 85 DEG C, 2 hours, uses NaH2PO4PH is adjusted to 7 with deionized water, then is used
Anhydrous sodium sulfate drying, residual ECH and solvent are removed with rotary evaporator.
In the present invention, the weight ratio of the reactive diluent 1 and reactive diluent 2 is 2：1.
Light trigger：Heretofore described light trigger is selected from 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2-
Hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-phenyl ketone, 2- methyl isophthalic acids-[4- methyl mercaptos phenyl] -2-
Quinoline base -1- acetone, 2- isopropyl thioxanthones, 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyl-cyclohexyl-phenyl first
It is one or more in ketone.
As one embodiment of the present invention, the light trigger is 2- hydroxy-2-methyl -1- phenyl -1- acetone.
Leveling auxiliary agent：Leveling auxiliary agent is a kind of conventional coating additive, and it can promote coating shape during drying and forming-film
Into a smooth, smooth, uniform film.It can effectively reduce and cover with paint, lacquer, colour wash, etc. liquid surface tension, improve the one of its levelability and uniformity
Class material.The permeability for covering with paint, lacquer, colour wash, etc. liquid can be improved, the possibility that spot and spot are produced when brushing can be reduced, increase spreadability, make
Film forming is uniform, natural.Mainly surfactant, organic solvent etc..Levelling agent species is a lot, the levelling agent used in different coating
Species is also not quite similar.
Heretofore described leveling auxiliary agent is selected from silicon-type leveling auxiliary agent.
The preparation method of heretofore described silicon-type leveling auxiliary agent is as follows：
1st, allyl bromide, bromoallylene (0.9mol), bisphenol-A (0.3mol) and potassium carbonate (0.1mol) are dissolved in acetone (50mL),
80 DEG C are heated to after stirring 30 minutes at room temperature, isothermal reaction 12 hours, product is alternately washed 3 times through second alcohol and water, then true
(80 DEG C) are dried in vacuo in empty drying box, obtain product 1；
2nd, product 1 (1mol), epoxychloropropane (10mol) and 4 bromide (0.06mol) are stirred at room temperature
After 20 minutes, then under nitrogen atmosphere, be heated to 95 DEG C maintain 2 hours, then be added dropwise sodium hydroxide solution (2mol,
48wt%) into four neck round-bottom flasks, reaction temperature is then maintained 95 DEG C, reacts 4 hours, obtains product 2；
3rd, it is that (allyl double bonds and SiH mol ratio are 1 to preparing raw material by product 2 and 1,1,2,2- tetramethyls disilane：
1) Pt catalyst (concentration 15ppm), is added, is dissolved in toluene, above-mentioned preparing raw material is added in four-neck flask in the lump,
90 DEG C are reacted 2 hours under nitrogen atmosphere, are then removed excess of solvent with rotary evaporator, are obtained organosilicon leveling auxiliary agent.
Defoamer：Heretofore described defoamer be selected from saturated alcohols, fatty alcohol, fatty acid alcohol, higher fatty acid metal soap,
Mixture more than one or both of sulfonated oil or organic silicone oil.
As one embodiment of the present invention, heretofore described defoamer is dimethyl silicone polymer.
Wetting agent：Ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propane diols, DPG, tripropylene glycol, 1,
Ammediol, isopropylidene glycol, isobutylene-glycol, BDO, 1,3-BDO, 1,2- pentanediols, 1,5- penta 2
Any one or a few in alcohol, 1,2- hexylene glycols, 1,6- hexylene glycols, 1,2,6- hexanetriols, 1,8- ethohexadiols, 1,2- ethohexadiols
Mixing.
Fire retardant：
Existing fire retardant has halogenated flame retardant, phosphorus flame retardant, nitrogenated flame retardant, silicon-series five-retardant, expansion type flame-retarding
Agent, boron flame retardant, magnalium flame retardant, Sb system fire retardant, molybdenum system fire retardant.
Heretofore described fire retardant is organic fire-retardant.
Heretofore described fire retardant is various organic fire-retardants well known by persons skilled in the art, can be specifically ten bromines
Double (the 2,3- dioxanes propyl group) ether of diphenyl ether, tetrabromobisphenol A, octabromodiphenyl ether, tetrabromobisphenol A, 2,4,6- tribromphenols, red phosphorus and
Microencapsulated powder oil halogenated phosphate, non-halogenated phosphate, ammonium phosphate, APP, microcosmic salt etc..
As one embodiment of the present invention, heretofore described fire retardant is to contain morpholinyl thiocarbamide, specially 1-
Cyclohexyl -3- (2- morpholinyl ethyls) thiocarbamide.
As one embodiment of the present invention, in parts by weight, the preparing raw material of the three-proofing coating includes：
As one embodiment of the present invention, in parts by weight, the preparing raw material of the three-proofing coating includes：
The second aspect of the present invention provides the method for preparing the high-efficiency environment friendly UV- dark curing three-proofing coatings, specific steps
It is as follows：
1) acrylic resin, reactive diluent, light trigger is taken to pour into reactor by weight, with 300r/min rotating speed
Mix 60 minutes；
2) leveling auxiliary agent, defoamer, wetting agent, fire retardant are added by weight percentage in step 1), with 300r/min
Rotating speed mix what can be made within 60 minutes.
Mechanism is explained：High-efficiency environment friendly UV- dark curing three-proofing coatings provided by the invention can just solidify after by illumination, Gu
Abbreviation list, quick solidifying, solidification process is not by moisture content, coating accumulation and thickness effect；It is good to solidify uniformity, paint film volume is received
Shrinkage is small, and adhesive force is strong；Stability is good, will not occur to cause product viscosity to increase because of affected by moisture, constructional difficulties are asked
Topic.The reason for its is possible is not to be easy in reactive diluent and light trigger provided by the invention containing isocyano etc. and air
In moisture react, therefore can be steady in a long-term presence, secondly in the present invention, the reactive diluent be two kinds it is dilute
The combination product of agent is released, synergy is produced between the two and promotes the UV- dark curings of product, stable and NBC protective performance.
Embodiment 1：Present embodiment provides a kind of high-efficiency environment friendly UV- dark curing three-proofing coatings, in parts by weight, institute
The preparing raw material for stating three-proofing coating includes：
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 2., it is in parts by weight, described
The preparing raw material of three-proofing coating includes：
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 3., it is in parts by weight, described
The preparing raw material of three-proofing coating includes：
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 4., the system of the acrylic resin
Standby monomer includes acrylic acid, non-functional alkyl acrylate, the alkyl acrylate containing function monomer.
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 5., the light trigger are selected from 2,
4,6- trimethylbenzoy-dipheny phosphine oxides, 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-benzene
Base ketone, 2- methyl isophthalic acids-[4- methyl mercaptos phenyl] -2- morpholinyl -1- acetone, 2- isopropyl thioxanthones, 2- hydroxyl -2- first
It is one or more in base -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-phenyl ketone.
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 6., the leveling auxiliary agent, which is selected from, to be had
Machine silicon systems leveling auxiliary agent.
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 7., the defoamer are selected from saturation
Mixing more than one or both of alcohol, fatty alcohol, fatty acid alcohol, higher fatty acid metal soap, sulfonated oil or organic silicone oil
Thing.
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 8., the reactive diluent are selected from
Reactive diluent containing epoxide group.
High-efficiency environment friendly UV- dark curing three-proofing coatings described in the embodiment 1 of embodiment 9., the fire retardant are organic resistance
Fire agent.
Embodiment 10. is a kind of to prepare high-efficiency environment friendly UV- dark curing three-proofing coatings any one of embodiment 1-9
Method is as follows the step of methods described：
1) acrylic resin, reactive diluent, light trigger is taken to pour into reactor by weight, with 300r/min rotating speed
Mix 60 minutes；
2) leveling auxiliary agent, defoamer, wetting agent, fire retardant are added by weight percentage in step 1), with 300r/min
Rotating speed mix what can be made within 60 minutes.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following examples are only used
In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
In addition, if without other explanations, raw materials used is all commercially available.
Embodiment 1：The present embodiment provides a kind of high-efficiency environment friendly UV- dark curing three-proofing coatings, in parts by weight, described three
The preparing raw material of anti-paint includes：
In the present embodiment, the monomer for preparing of the acrylic resin is that acrylic acid, propyl acrylate and acrylic acid -8- hydroxyls are pungent
Ester is 1 according to weight part ratio：0.1：0.1 ratio is mixed with to obtain.
Reactive diluent：Reactive diluent described in the present embodiment is made up of two kinds of reactive diluents.
Reactive diluent 1：The preparation method of reactive diluent 1 described in the present embodiment is as follows：
1、
Wherein, the mol ratio of allyl bromide, bromoallylene and bisphenol-A is 3：1.1.
2、
Wherein, the mol ratio of step 1 is prepared product, epoxychloropropane and 4 bromide is 1：8：0.05.
Reactive diluent 2：The preparation method of reactive diluent 2 described in the present embodiment is as follows：
5- sulfydryl Benadon HPPMP (1mol), epoxychloropropane (10mol) and 4 bromide (0.06mol) are put
Put in four neck round-bottom flasks equipped with magnetic stirring apparatus, thermometer and reflux condensing tube, reactant is stirred at room temperature
After 15 minutes, then under nitrogen atmosphere, be heated to 95 DEG C maintain 2 hours, then be added dropwise sodium hydroxide solution (2mol,
48wt%) into four neck round-bottom flasks, reaction temperature is then maintained 95 DEG C, reacted 2 hours.By the chlorination in course of reaction
Sodium is filtered out, and remaining epoxychloropropane is evaporated in vacuo and separated.Then the NaOH aqueous solution (1mol, mass fraction are used：5%) and
Toluene adds crude product and further reacted, and after reaction is kept for 85 DEG C, 2 hours, uses NaH2PO4PH is adjusted to 7 with deionized water, then is used
Anhydrous sodium sulfate drying, residual ECH and solvent are removed with rotary evaporator.
In the present embodiment, the weight ratio of the reactive diluent 1 and reactive diluent 2 is 2：1.
The light trigger is 2- hydroxy-2-methyl -1- phenyl -1- acetone.
The preparation method of silicon-type leveling auxiliary agent described in the present embodiment is as follows：
1st, allyl bromide, bromoallylene (0.9mol), bisphenol-A (0.3mol) and potassium carbonate (0.1mol) are dissolved in acetone (50mL),
80 DEG C are heated to after stirring 30 minutes at room temperature, isothermal reaction 12 hours, product is alternately washed 3 times through second alcohol and water, then true
(80 DEG C) are dried in vacuo in empty drying box, obtain product 1；
2nd, product 1 (1mol), epoxychloropropane (10mol) and 4 bromide (0.06mol) are stirred at room temperature
After 20 minutes, then under nitrogen atmosphere, be heated to 95 DEG C maintain 2 hours, then be added dropwise sodium hydroxide solution (2mol,
48wt%) into four neck round-bottom flasks, reaction temperature is then maintained 95 DEG C, reacts 4 hours, obtains product 2；
3rd, it is that (allyl double bonds and SiH mol ratio are 1 to preparing raw material by product 2 and 1,1,2,2- tetramethyls disilane：
1) Pt catalyst (concentration 15ppm), is added, is dissolved in toluene, above-mentioned preparing raw material is added in four-neck flask in the lump,
90 DEG C are reacted 2 hours under nitrogen atmosphere, are then removed excess of solvent with rotary evaporator, are obtained organosilicon leveling auxiliary agent.
Defoamer described in the present embodiment is dimethyl silicone polymer.
Wetting agent described in the present embodiment is 1,3-BDO.
Fire retardant described in the present embodiment is 1- cyclohexyl -3- (2- morpholinyl ethyls) thiocarbamide.
The second aspect of the present embodiment provides the method for preparing the high-efficiency environment friendly UV- dark curing three-proofing coatings, specific step
It is rapid as follows：
1) acrylic resin, reactive diluent, light trigger is taken to pour into reactor by weight, with 300r/min rotating speed
Mix 60 minutes；
2) leveling auxiliary agent, defoamer, wetting agent, fire retardant are added by weight percentage in step 1), with 300r/min
Rotating speed mix what can be made within 60 minutes.
Embodiment 2：Difference with embodiment 1 is that the reactive diluent only has reactive diluent 1.
Embodiment 3：Difference with embodiment 1 is that the reactive diluent only has reactive diluent 2.
Embodiment 4：Difference with embodiment 1 is that the reactive diluent replaces with the double contractings of ethylene glycol of bicyclic epoxide
Water glycerin ether.
Embodiment 5：Difference with embodiment 1 is that the leveling auxiliary agent is dimethyl silicone polymer.
Embodiment 6：Difference with embodiment 1 is that the acrylic resin is pure acrylic resin.
Embodiment 7：Difference with embodiment 1 is that the reactive diluent is sweet for the double shrinks of ethylene glycol of bicyclic epoxide
Oily ether, the leveling auxiliary agent are dimethyl silicone polymer.
Test：
Test result：
Foregoing example is merely illustrative, some features of the feature for explaining the disclosure.Appended claim
It is intended to require the scope as wide as possible being contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the explanation present invention
Feature example selectional restriction.And the progress in science and technology will not formed due to the inaccuracy of language performance and not
The possible equivalent or son being presently considered are replaced, and these changes should also be interpreted by appended in the conceived case
Claim covers.
Claims (10)
- A kind of 1. high-efficiency environment friendly UV- dark curing three-proofing coatings, it is characterised in that in parts by weight, the preparation of the three-proofing coating Raw material includes：
- 2. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that in parts by weight, described three The preparing raw material of anti-paint includes：
- 3. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that in parts by weight, described three The preparing raw material of anti-paint includes：
- 4. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the system of the acrylic resin Standby monomer includes acrylic acid, non-functional alkyl acrylate, the alkyl acrylate containing function monomer.
- 5. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the light trigger is selected from 2, 4,6- trimethylbenzoy-dipheny phosphine oxides, 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-benzene Base ketone, 2- methyl isophthalic acids-[4- methyl mercaptos phenyl] -2- morpholinyl -1- acetone, 2- isopropyl thioxanthones, 2- hydroxyl -2- first It is one or more in base -1- phenyl -1- acetone, 1- hydroxyls-cyclohexyl-phenyl ketone.
- 6. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the leveling auxiliary agent, which is selected from, to be had Machine silicon systems leveling auxiliary agent.
- 7. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the defoamer is selected from saturation Mixing more than one or both of alcohol, fatty alcohol, fatty acid alcohol, higher fatty acid metal soap, sulfonated oil or organic silicone oil Thing.
- 8. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the reactive diluent is selected from Reactive diluent containing epoxide group.
- 9. the high-efficiency environment friendly UV- dark curing three-proofing coatings described in claim 1, it is characterised in that the fire retardant is organic resistance Fire agent.
- 10. a kind of method for preparing high-efficiency environment friendly UV- dark curing three-proofing coatings any one of claim 1-9, its feature It is, it is as follows the step of methods described：1) take acrylic resin, reactive diluent, light trigger to pour into reactor by weight, mixed with 300r/min rotating speed Stirring 60 minutes；2) leveling auxiliary agent, defoamer, wetting agent, fire retardant are added by weight percentage in step 1), with turning for 300r/min Speed mixes what can be made within 60 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778962A (en) * | 2021-01-12 | 2021-05-11 | 亿铖达（深圳）新材料有限公司 | Efficient environment-friendly black UV adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589320A (en) * | 2012-08-13 | 2014-02-19 | 深圳市微步电子有限责任公司 | Conformal coating for protection of printed circuit board, and preparation method and usage method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103589320A (en) * | 2012-08-13 | 2014-02-19 | 深圳市微步电子有限责任公司 | Conformal coating for protection of printed circuit board, and preparation method and usage method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778962A (en) * | 2021-01-12 | 2021-05-11 | 亿铖达（深圳）新材料有限公司 | Efficient environment-friendly black UV adhesive |
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