CN105153796B - A kind of thermosetting property solder mask - Google Patents
A kind of thermosetting property solder mask Download PDFInfo
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- CN105153796B CN105153796B CN201510688215.1A CN201510688215A CN105153796B CN 105153796 B CN105153796 B CN 105153796B CN 201510688215 A CN201510688215 A CN 201510688215A CN 105153796 B CN105153796 B CN 105153796B
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Abstract
The present invention relates to ink areas, and in particular to a kind of thermosetting property solder mask.A kind of thermosetting property solder mask, is made of the component of following parts by weight：25 ~ 45 parts of hyperbranched resin；15 ~ 25 parts of reactive diluent；10 ~ 25 parts of inorganic filler；0 ~ 15 part of pigment；0 ~ 5 part of function additive；0 ~ 15 part of solvent；1 ~ 3 part of curing agent.The present invention provides a kind of thermosetting property solder mask, the solder mask is compared with traditional thermosetting property solder mask of domestic production, solder mask prepared by the present invention has the characteristics that low solidification temperature, excellent heat resistance, soldering resistance, yellowing resistance, and curing rate is fast, especially suitable for LED solder masks.
Description
Technical field
The present invention relates to ink areas, and in particular to a kind of thermosetting property solder mask.
Background technology
It is one of very crucial material to manufacture solder mask in the chemicals used in printed circuit board (PCB), it can prevent from leading
Line scratch and welding when lead short-circuit between conductors, meanwhile, also act as make conducting wire have moisture resistance, chemical proof, it is heat-resisting, insulation with
And beautiful effect, therefore, during printed-board technology progress, the research and development of solder mask is always in occupation of ten
Divide important position.But often solidification temperature is high for existing solder mask, poor heat resistance, be unfavorable for solder mask into one
Step uses.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of solidification temperature is low, heat-resist thermosetting property welding resistance oil
Ink.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
25 ~ 45 parts of hyperbranched resin；15 ~ 25 parts of reactive diluent；10 ~ 25 parts of inorganic filler；0 ~ 15 part of pigment；Function helps
0 ~ 5 part of agent；0 ~ 15 part of solvent；1 ~ 3 part of curing agent.
Further, the hyperbranched resin synthesizes in accordance with the following steps：
（1）Under the protection and stirring of inert atmosphere, in molar ratio, by 1 part of 3- methylpentanes -2,4- glycol and 2 parts
3,5- bis- (methylol) benzoic acid add in into closed container, then add in the concentrated sulfuric acid as catalyst, at 160 ~ 180 DEG C
The matrix G1 of hyperbranched resin is obtained after condensation reaction occurs when stirring 1 ~ 2 is small；
（2）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G1 of above-mentioned hyperbranched resin,
The matrix G2 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（3）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G2 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G3 of hyperbranched resin；
（4）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G3 of above-mentioned hyperbranched resin,
The matrix G4 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（5）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G4 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G5 of hyperbranched resin；
（6）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G5 of above-mentioned hyperbranched resin,
The matrix G6 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（7）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G6 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G7 of hyperbranched resin；
（8）Then by step（7）Reaction temperature be down to 80 DEG C, add in excessive epoxychloropropane and sodium hydroxide be water-soluble
Liquid, when reaction 3 is small after washing obtain the hyperbranched resin.
Further, the hyperbranched resin synthesis step（7）In the obtained matrix G7 of hyperbranched resin contain
100 ~ 118 terminal hydroxy groups.
Further, the reactive diluent is double ((3,4- epoxycyclohexyl) methyl) adipate esters, polypropylene glycol two
The mixture of glycidol ether and hexahydrophthalic acid bisglycidyl ester.
Wherein, No. CAS of double ((3,4- epoxycyclohexyl) methyl) adipate esters be 3130-19-6, hexahydro O-phthalic
No. CAS of sour bisglycidyl ester is 5493-45-8.
Further, the inorganic filler is at least one of calcium carbonate, aluminium hydroxide, barium sulfate, talcum powder.
Further, the function additive is at least one of antifoaming agent, levelling agent, antioxidant, dispersant.This hair
The present invention can be achieved for the commercial product of the art in bright function additive used.
Further, the solvent volume is at least one in alcohols solvent, esters solvent, ketones solvent, solvent of ether ester type
Kind.The present invention can be achieved for the common solvent of the art in solvent used in the present invention, such as ethylene glycol ethyl ether, acetone, third
The organic solvents such as glycol methyl ether acetate.
Further, the curing agent is amine curing agent.The present invention uses the common amine curing agent of the art
The present invention, such as triethylamine, four ethylene triamine substances can be achieved.
The present invention can be achieved for the common pigment of the art in pigment used in the present invention, such as azo pigments, phthalocyanine
The organic pigments such as pigment, the inorganic pigments such as lead chromate yellow, lithopone, carbon black.
Further, the solder mask is made of the component of following parts by weight：
25 ~ 45 parts of hyperbranched resin；Double ((3,4- epoxycyclohexyls) methyl) 5 ~ 10 parts of adipate esters；Polypropylene glycol two contracts
5 ~ 8 parts of water glycerin ether；4 ~ 7 parts of hexahydrophthalic acid bisglycidyl ester；10 ~ 25 parts of inorganic filler；0 ~ 15 part of pigment；Function
0 ~ 5 part of auxiliary agent；0 ~ 15 part of solvent；1 ~ 3 part of curing agent.
The present invention is used as matrix resin by synthesizing specific asymmetric hyperbranched resin so that matrix resin of the invention
Not only there is good curing performance, solidification temperature is low, but also has extremely strong heat resistance, and excellent weatherability simultaneously should
Resin can also form fine and close polymer film, and the coating formed has excellent weatherability, heat-resisting quantity and splendid resistance to
Acid-base property.Further for asymmetric hyperbranched resin adhesive force is solved the problems, such as matrix adhesive force, the present invention passes through choosing
Select double ((3,4- epoxycyclohexyl) methyl) adipate esters, polypropylene glycol diglycidyl ether and the double shrinks of hexahydrophthalic acid
The mixture of glyceride can cleverly solve the problems, such as that asymmetric hyperbranched resin adhesive force is bad as reactive diluent,
And it can further reduce the solidification temperature of resin.
The present invention has the advantages that：
The present invention provides traditional thermosetting property welding resistance oil of a kind of thermosetting property solder mask, the solder mask and domestic production
Ink is compared, and solder mask prepared by the present invention has the spies such as low solidification temperature, excellent heat resistance, soldering resistance, yellowing resistance
Point, and curing rate is fast, especially suitable for LED solder masks.
Specific embodiment
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Hyperbranched resin used in the present invention synthesizes in accordance with the following steps：
（1）Under the protection and stirring of inert atmosphere, in molar ratio, by 1 part of 3- methylpentanes -2,4- glycol and 2 parts
3,5- bis- (methylol) benzoic acid add in into closed container, then add in the concentrated sulfuric acid as catalyst, at 160 ~ 180 DEG C
The matrix G1 of hyperbranched resin is obtained after condensation reaction occurs when stirring 1 ~ 2 is small；
（2）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G1 of above-mentioned hyperbranched resin,
The matrix G2 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（3）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G2 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G3 of hyperbranched resin；
（4）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G3 of above-mentioned hyperbranched resin,
The matrix G4 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（5）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G4 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G5 of hyperbranched resin；
（6）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G5 of above-mentioned hyperbranched resin,
The matrix G6 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（7）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G6 of above-mentioned hyperbranched resin
Acid, when stirring 1 ~ 2 is small at 160 ~ 180 DEG C after obtain the matrix G7 of hyperbranched resin；
（8）Then by step（7）Reaction temperature be down to 80 DEG C, add in excessive epoxychloropropane and sodium hydroxide be water-soluble
Liquid, when reaction 3 is small after washing obtain the hyperbranched resin.
The preparation method of the solder mask of the present invention is the common method of the art, is not described in detail herein.
Embodiment 1
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
35 parts of hyperbranched resin；Double ((3,4- epoxycyclohexyls) methyl) 6 parts of adipate esters；Polypropylene glycol diglycidyl
6 parts of ether；6 parts of hexahydrophthalic acid bisglycidyl ester；12 parts of calcium carbonate；10 parts of aluminium hydroxide；10 parts of carbon black；Antifoaming agent 1
Part；1 part of levelling agent；1 part of antioxidant；1 part of dispersant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 90 DEG C by test.
Quick-drying cures 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 100 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink non yellowing.
Adhesive force（GB/T 9286-1998）：1 grade.
Hardness（GB/T 6739-2006）：6H.
Glossiness（GB/T 1743-1979）：80.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Ink without xanthochromia, without explosion, without come off, non-soldering tin enter
Phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is more than 400 DEG C.
Embodiment 2
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
43 parts of hyperbranched resin；Double ((3,4- epoxycyclohexyls) methyl) 8 parts of adipate esters；Polypropylene glycol diglycidyl
5 parts of ether；5 parts of hexahydrophthalic acid bisglycidyl ester；20 parts of talcum powder；13 parts of carbon black；1 part of antifoaming agent；1 part of levelling agent；
1 part of antioxidant；1 part of dispersant；15 parts of propylene glycol methyl ether acetate；3 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 90 DEG C by test.
Quick-drying cures 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 100 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink non yellowing.
Adhesive force（GB/T 9286-1998）：1 grade.
Hardness（GB/T 6739-2006）：6H.
Glossiness（GB/T 1743-1979）：78.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Ink without xanthochromia, without explosion, without come off, non-soldering tin enter
Phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is more than 400 DEG C.
Embodiment 3
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
28 parts of hyperbranched resin；Double ((3,4- epoxycyclohexyls) methyl) 5 parts of adipate esters；Polypropylene glycol diglycidyl
8 parts of ether；6 parts of hexahydrophthalic acid bisglycidyl ester；8 parts of barium sulfate；15 parts of talcum powder；13 parts of carbon black；1 part of antifoaming agent；
1 part of levelling agent；1 part of antioxidant；1 part of dispersant；1.5 parts of ethylene glycol ethyl ether；1 part of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 90 DEG C by test.
Quick-drying cures 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 100 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink non yellowing.
Adhesive force（GB/T 9286-1998）：1 grade.
Hardness（GB/T 6739-2006）：6H.
Glossiness（GB/T 1743-1979）：76.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Ink without xanthochromia, without explosion, without come off, non-soldering tin enter
Phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is more than 400 DEG C.
Comparative example 1
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
35 parts of the epoxy resin that market can be sold；Double ((3,4- epoxycyclohexyls) methyl) 6 parts of adipate esters；Polypropylene glycol two
6 parts of glycidol ether；6 parts of hexahydrophthalic acid bisglycidyl ester；12 parts of calcium carbonate；10 parts of aluminium hydroxide；10 parts of carbon black；
1 part of antifoaming agent；1 part of levelling agent；1 part of antioxidant；1 part of dispersant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 140 DEG C by test.
Quick-drying cures 2 minutes in 140-160 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 150 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink starts xanthochromia.
Adhesive force（GB/T 9286-1998）：3 grades.
Hardness（GB/T 6739-2006）：3H.
Glossiness（GB/T 1743-1979）：56.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：It starts shedding off, find that scolding tin enters phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 270 DEG C.
Comparative example 2
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
35 parts of hyperbranched resin；6 parts of polypropylene glycol diglycidyl ether；12 parts of calcium carbonate；10 parts of aluminium hydroxide；Carbon black 10
Part；1 part of antifoaming agent；1 part of levelling agent；1 part of antioxidant；1 part of dispersant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 110 DEG C by test.
Quick-drying cures 2 minutes in 110-130 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 120 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink non yellowing.
Adhesive force（GB/T 9286-1998）：3 grades.
Hardness（GB/T 6739-2006）：5H.
Glossiness（GB/T 1743-1979）：68.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：It starts shedding off, find that scolding tin enters phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 350 DEG C.
Comparative example 3
A kind of thermosetting property solder mask, is made of the component of following parts by weight：
35 parts of hyperbranched resin；12 parts of calcium carbonate；10 parts of aluminium hydroxide；10 parts of carbon black；1 part of antifoaming agent；1 part of levelling agent；
1 part of antioxidant；1 part of dispersant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 120 DEG C by test.
Quick-drying cures 2 minutes in 120-140 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
It is cured 60 minutes for 130 DEG C in case.
Performance test methods and result are as follows：
Prebake conditions（75℃）：25 minutes.After prebake conditions, ink is tack-free.
After toast（180℃）：60 minutes.After toasting afterwards, ink non yellowing.
Adhesive force（GB/T 9286-1998）：4 grades.
Hardness（GB/T 6739-2006）：5H.
Glossiness（GB/T 1743-1979）：63.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：It starts shedding off, find that scolding tin enters phenomenon.
It is tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 340 DEG C.
By above-described embodiment and the test data of comparative example, solder mask of the invention is in hyperbranched resin and work
Property diluent synergistic effect under, into solder mask have curing rate is fast, solidification temperature is low, excellent heat resistance, soldering resistance,
The features such as yellowing resistance.
Embodiment described above only expresses embodiments of the present invention, and description is more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (7)
1. a kind of thermosetting property solder mask, which is characterized in that be made of the component of following parts by weight：
25 ~ 45 parts of hyperbranched resin；
15 ~ 25 parts of reactive diluent；
10 ~ 25 parts of inorganic filler；
0 ~ 15 part of pigment；
0 ~ 5 part of function additive；
0 ~ 15 part of solvent；
1 ~ 3 part of curing agent；
The hyperbranched resin synthesizes in accordance with the following steps：
（1）Under the protection and stirring of inert atmosphere, in molar ratio, by 1 part of 3- methylpentanes -2,4- glycol and the 3 of 2 parts,
5- bis- (methylol) benzoic acid is added in into closed container, is then added in the concentrated sulfuric acid as catalyst, is stirred at 160 ~ 180 DEG C
1 ~ 2 it is small when occur condensation reaction after obtain the matrix G1 of hyperbranched resin；
（2）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G1 of above-mentioned hyperbranched resin, 160 ~
The matrix G2 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 180 DEG C；
（3）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and the concentrated sulfuric acid are continuously added in the matrix G2 of above-mentioned hyperbranched resin,
The matrix G3 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（4）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G3 of above-mentioned hyperbranched resin, 160 ~
The matrix G4 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 180 DEG C；
（5）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and the concentrated sulfuric acid are continuously added in the matrix G4 of above-mentioned hyperbranched resin,
The matrix G5 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（6）Then 2 parts of 3,5- dihydroxy-benzoic acids and the concentrated sulfuric acid are continuously added in the matrix G5 of above-mentioned hyperbranched resin, 160 ~
The matrix G6 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 180 DEG C；
（7）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and the concentrated sulfuric acid are continuously added in the matrix G6 of above-mentioned hyperbranched resin,
The matrix G7 of hyperbranched resin is obtained after when stirring 1 ~ 2 is small at 160 ~ 180 DEG C；
（8）Then by step（7）Reaction temperature be down to 80 DEG C, add in excessive epoxychloropropane and sodium hydrate aqueous solution,
React 3 it is small when after washing obtain the hyperbranched resin；
The reactive diluent is double ((3,4- epoxycyclohexyl) methyl) adipate esters, polypropylene glycol diglycidyl ether and six
The mixture of hydrogen phthalic acid bisglycidyl ester.
A kind of 2. thermosetting property solder mask according to claim 1, which is characterized in that the hyperbranched resin synthesis step
（7）In the obtained matrix G7 of hyperbranched resin contain 100 ~ 118 terminal hydroxy groups.
3. a kind of thermosetting property solder mask according to claim 1, which is characterized in that the inorganic filler for calcium carbonate,
At least one of aluminium hydroxide, barium sulfate, talcum powder.
4. a kind of thermosetting property solder mask according to claim 1, which is characterized in that the function additive for antifoaming agent,
At least one of levelling agent, antioxidant, dispersant.
5. a kind of thermosetting property solder mask according to claim 1, which is characterized in that the solvent is alcohols solvent, ester
At least one of class solvent, ketones solvent, solvent of ether ester type.
6. a kind of thermosetting property solder mask according to claim 1, which is characterized in that the curing agent is amine-type cure
Agent.
7. a kind of thermosetting property solder mask according to claim 1 ~ 6 any one, which is characterized in that by following parts by weight
Several component compositions：
25 ~ 45 parts of hyperbranched resin；
Double ((3,4- epoxycyclohexyls) methyl) 5 ~ 10 parts of adipate esters；
5 ~ 8 parts of polypropylene glycol diglycidyl ether；
5 ~ 7 parts of hexahydrophthalic acid bisglycidyl ester；
10 ~ 25 parts of inorganic filler；
0 ~ 15 part of pigment；
0 ~ 5 part of function additive；
0 ~ 15 part of solvent；
1 ~ 3 part of curing agent.
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Effective date of registration: 20180424 Address after: 528400 No. 260, No. 260 Jie Fu Road, people's town of Zhongshan City, Guangdong province. (1 additional establishments are designated as 28 Ping Ping Road, Sha Tsai administrative village, people's town). Applicant after: Zhongshan Fu day printing materials Co., Ltd. Address before: 246523 Anhui city of Anqing province Susong County Xu Zhen Luo Wu Cun Baiyun Group No. 6 Applicant before: Xu Weipeng |
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