CN105131707B - A kind of thermosetting solder mask ink composition - Google Patents
A kind of thermosetting solder mask ink composition Download PDFInfo
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- CN105131707B CN105131707B CN201510688219.XA CN201510688219A CN105131707B CN 105131707 B CN105131707 B CN 105131707B CN 201510688219 A CN201510688219 A CN 201510688219A CN 105131707 B CN105131707 B CN 105131707B
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- solder mask
- ink composition
- hyperbranched resin
- thermosetting solder
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 53
- 239000000203 mixture Substances 0.000 title claims abstract description 29
- 229920001187 thermosetting polymer Polymers 0.000 title claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 229920000728 polyester Polymers 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 239000003085 diluting agent Substances 0.000 claims abstract description 7
- 239000011256 inorganic filler Substances 0.000 claims abstract description 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 6
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 19
- 239000011159 matrix material Substances 0.000 claims description 15
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical group CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 8
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 8
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 8
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 8
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 7
- 229920001451 polypropylene glycol Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical group 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- MGMNPSAERQZUIM-UHFFFAOYSA-N 2-(hydroxymethyl)benzoic acid Chemical compound OCC1=CC=CC=C1C(O)=O MGMNPSAERQZUIM-UHFFFAOYSA-N 0.000 claims description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 3
- PFEOZHBOMNWTJB-UHFFFAOYSA-N 3-methylpentane Chemical class CCC(C)CC PFEOZHBOMNWTJB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000006482 condensation reaction Methods 0.000 claims description 3
- -1 ether ester Chemical class 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001802 infusion Methods 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- 238000007711 solidification Methods 0.000 abstract description 14
- 230000008023 solidification Effects 0.000 abstract description 14
- 238000004383 yellowing Methods 0.000 abstract description 8
- 238000005476 soldering Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000006229 carbon black Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000003466 welding Methods 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000011056 performance test Methods 0.000 description 7
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 6
- 229960001124 trientine Drugs 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013530 defoamer Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- DOHMTKLMXUAOPD-UHFFFAOYSA-N 3,5-bis(hydroxymethyl)benzoic acid Chemical compound OCC1=CC(CO)=CC(C(O)=O)=C1 DOHMTKLMXUAOPD-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical group CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- BLAKAEFIFWAFGH-UHFFFAOYSA-N acetyl acetate;pyridine Chemical compound C1=CC=NC=C1.CC(=O)OC(C)=O BLAKAEFIFWAFGH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002270 exclusion chromatography Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
Abstract
The present invention relates to ink area, and in particular to a kind of thermosetting solder mask ink composition.A kind of thermosetting solder mask ink composition, is made up of the component of following parts by weight：End group is 15 ~ 30 parts of the linear polyester of carboxyl；10 ~ 25 parts of hyperbranched resin；5 ~ 20 parts of reactive diluent；10 ~ 35 parts of inorganic filler；0 ~ 15 part of pigment；0 ~ 8 part of function additive；0 ~ 20 part of solvent；1 ~ 3 part of curing agent.The present invention provides a kind of thermosetting solder mask ink composition, the solder mask is compared with traditional thermosetting 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 area, and in particular to a kind of thermosetting solder mask ink composition.
Background technology
It is one of very crucial material to manufacture solder mask in the chemicals used in printed circuit board (PCB), and it can prevent from leading
Line scratch and welding when lead short-circuit between conductors, meanwhile, also act as make wire have moisture resistance, chemical proof, it is heat-resisting, insulation with
And effect attractive in appearance, therefore, during printed-board technology progress, the research and development of solder mask is all the time 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 enters 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 solder mask
Composition.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of thermosetting solder mask ink composition, is made up of the component of following parts by weight：
End group is 15 ~ 30 parts of the linear polyester of carboxyl；10 ~ 25 parts of hyperbranched resin；5 ~ 20 parts of reactive diluent；It is inorganic to fill out
10 ~ 35 parts of material；0 ~ 15 part of pigment；0 ~ 8 part of function additive；0 ~ 20 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 into closed container, then add the concentrated sulfuric acid as catalyst, at 160 ~ 180 DEG C
Stirring obtains the matrix G1 of hyperbranched resin after condensation reaction occurring within 1 ~ 2 hour；
（2）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G1 of above-mentioned hyperbranched resin
Acid, the matrix G2 of hyperbranched resin is obtained after stirring 1 ~ 2 hour at 160 ~ 180 DEG C, then this step is repeated 5 times, overspend
Change the matrix G7 of resin；；
（3）Then by step（2）Reaction temperature be down to 80 DEG C, add excessive epoxychloropropane and sodium hydroxide be water-soluble
Liquid, reaction are washed after 3 hours and obtain described hyperbranched resin.
Further, the hyperbranched resin synthesis step（2）In the obtained matrix G7 of hyperbranched resin contain
100 ~ 118 terminal hydroxy groups.
Further, the end group is that the hydroxyl value of the linear polyester of carboxyl is 120~180 mgKOH/g, Weight-average molecular
Measure as 10000~30000.
Further, the reactive diluent is ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether and different
The mixture of cyanuric acid three-glycidyl ester.
Further, the inorganic filler is at least one of calcium carbonate, aluminium hydroxide, barium sulfate, titanium dioxide.
Further, the function additive is at least one of defoamer, levelling agent, antioxidant.Used in the present invention
Function additive for the art commercial product can be achieved the present invention.
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 solvent that the art is commonly used 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 amine curing agent that the present invention is commonly used using the art
The present invention, such as triethylamine, four ethene triamine materials can be achieved.
The present invention can be achieved for the pigment that the art is commonly used in pigment used in the present invention, such as AZOpigments, phthalocyanine
The inorganic pigment such as the organic pigments such as pigment, lead chromate yellow, lithopone, carbon black.
Further, the solder mask ink composition is made up of the component of following parts by weight：
End group is 15 ~ 30 parts of the linear polyester of carboxyl；10 ~ 25 parts of hyperbranched resin；Ethylene glycol diglycidylether 1 ~ 5
Part；2 ~ 4 parts of polypropylene glycol diglycidyl ether；3 ~ 7 parts of isocyanuric acid three-glycidyl ester；10 ~ 35 parts of inorganic filler；Pigment 0 ~
15 parts；0 ~ 8 part of function additive；0 ~ 20 part of solvent；1 ~ 3 part of curing agent.
Then the present invention coordinates specific linear polyester as main body tree by synthesizing specific asymmetric hyperbranched resin
Fat so that matrix resin of the invention not only has good curing performance, and solidification temperature is low, and has to most of grounds
Excellent adhesive force, but also the polymerization that there is extremely strong heat resistance, excellent weatherability, while the resin can also form densification
Thing film, its coating formed have excellent weatherability, heat-resisting quantity and splendid resistance to acids and bases.Further for solution never
It is the problem of symmetrical hyperbranched resin and specific linear polyester compatibility, of the invention by selecting ethylene glycol diglycidylether,
The mixture of polypropylene glycol diglycidyl ether and isocyanuric acid three-glycidyl ester can be solved cleverly as reactive diluent
The problem of certainly 2 compatibilities are bad, further reduce the solidification temperature of resin.
The present invention has the advantages that：
The present invention provides traditional thermosetting of a kind of thermosetting solder mask ink composition, the solder mask and domestic production
Solder mask is compared, and solder mask prepared by the present invention has low solidification temperature, excellent heat resistance, soldering resistance, color inhibition
The features such as property, and curing rate is fast, especially suitable for LED solder masks.
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 into closed container, then add the concentrated sulfuric acid as catalyst, stirred at 170 DEG C
The matrix G1 of hyperbranched resin is obtained after condensation reaction occurring within 2 hours；
（2）Then 2 parts of (methylol) benzoic acid of 3,5- bis- and dense sulphur are continuously added in the matrix G1 of above-mentioned hyperbranched resin
Acid, the matrix G2 of hyperbranched resin is obtained after stirring 1 ~ 2 hour at 160 ~ 180 DEG C, then this step is repeated 5 times, overspend
Change the matrix G7 of resin；
（3）Then by step（2）Reaction temperature be down to 80 DEG C, add excessive epoxychloropropane and sodium hydroxide be water-soluble
Liquid, reaction are washed after 3 hours and obtain described hyperbranched resin.
End group used in the present invention is that the hydroxyl value of the linear polyester of carboxyl is 120~180 mgKOH/g, weight average molecular weight
For 10000~30000.
Wherein hydroxyl value is measured by acetic anhydride pyridine method；Weight average molecular weight is surveyed by exclusion chromatography
It is fixed.
The preparation method of the solder mask ink composition of the present invention is the common method of the art, is no longer retouched in detail herein
State.
Embodiment 1
A kind of thermosetting solder mask ink composition, is made up of the component of following parts by weight：
End group is 18 parts of the linear polyester of carboxyl；20 parts of hyperbranched resin；3 parts of ethylene glycol diglycidylether；Poly- the third two
3 parts of alcohol diglycidyl ether；4 parts of isocyanuric acid three-glycidyl ester；12 parts of calcium carbonate；15 parts of aluminium hydroxide；10 parts of carbon black；Disappear
1 part of infusion；1 part of levelling agent；1 part of antioxidant；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 solidifies 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
100 DEG C cure 60 minutes 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）：79.
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.
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 solder mask ink composition, is made up of the component of following parts by weight：
End group is 28 parts of the linear polyester of carboxyl；12 parts of hyperbranched resin；2 parts of ethylene glycol diglycidylether；Poly- the third two
4 parts of alcohol diglycidyl ether；6 parts of isocyanuric acid three-glycidyl ester；20 parts of barium sulfate；10 parts of aluminium hydroxide；13 parts of carbon black；Disappear
1 part of infusion；1 part of levelling agent；1 part of antioxidant；18 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 solidifies 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
100 DEG C cure 60 minutes 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）：77.
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.
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 solder mask ink composition, is made up of the component of following parts by weight：
End group is 16 parts of the linear polyester of carboxyl；23 parts of hyperbranched resin；4 parts of ethylene glycol diglycidylether；Poly- the third two
2 parts of alcohol diglycidyl ether；3 parts of isocyanuric acid three-glycidyl ester；15 parts of barium sulfate；15 parts of calcium carbonate；13 parts of carbon black；Defoaming
1 part of agent；1 part of levelling agent；1 part of antioxidant；2 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 solidifies 2 minutes in 90-100 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
100 DEG C cure 60 minutes 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）：81.
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.
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 solder mask ink composition, is made up of the component of following parts by weight：
End group is 18 parts of the linear polyester of carboxyl；3 parts of ethylene glycol diglycidylether；Polypropylene glycol diglycidyl ether 3
Part；4 parts of isocyanuric acid three-glycidyl ester；12 parts of calcium carbonate；15 parts of aluminium hydroxide；10 parts of carbon black；1 part of defoamer；Levelling agent 1
Part；1 part of antioxidant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 130 DEG C by test.
Quick-drying solidifies 2 minutes in 130-150 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
140 DEG C cure 60 minutes 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）：4H.
Glossiness（GB/T 1743-1979）：68.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Start shedding off, find that scolding tin enters phenomenon.
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 solder mask ink composition, is made up of the component of following parts by weight：
20 parts of hyperbranched resin；3 parts of ethylene glycol diglycidylether；3 parts of polypropylene glycol diglycidyl ether；Isocyanuric acid
4 parts of three-glycidyl ester；12 parts of calcium carbonate；15 parts of aluminium hydroxide；10 parts of carbon black；1 part of defoamer；1 part of levelling agent；Antioxidant
1 part；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 solidifies 2 minutes in 110-130 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
120 DEG C cure 60 minutes 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）：2 grades.
Hardness（GB/T 6739-2006）：5H.
Glossiness（GB/T 1743-1979）：45.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Start shedding off, find that scolding tin enters phenomenon.
Tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 300 DEG C.
Comparative example 3
A kind of thermosetting solder mask ink composition, is made up of the component of following parts by weight：
End group is 18 parts of the linear polyester of carboxyl；20 parts of hyperbranched resin；3 parts of ethylene glycol diglycidylether；Calcium carbonate
12 parts；15 parts of aluminium hydroxide；10 parts of carbon black；1 part of defoamer；1 part of levelling agent；1 part of antioxidant；13 parts of acetone；Triethylene four
2 parts of amine.
Understand that the solidification temperature of the present embodiment is 130 DEG C by test.
Quick-drying solidifies 2 minutes in 130-150 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
140 DEG C cure 60 minutes 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）：50.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Start shedding off, find that scolding tin enters phenomenon.
Tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 350 DEG C.
Comparative example 4
A kind of thermosetting solder mask ink composition, is made up of the component of following parts by weight：
End group is 18 parts of the linear polyester of carboxyl；20 parts of hyperbranched resin；12 parts of calcium carbonate；15 parts of aluminium hydroxide；Carbon black
10 parts；1 part of defoamer；1 part of levelling agent；1 part of antioxidant；13 parts of acetone；2 parts of triethylene tetramine.
Understand that the solidification temperature of the present embodiment is 150 DEG C by test.
Quick-drying solidifies 2 minutes in 150-170 DEG C during use.Thickness of dry film is controlled at 25-30 μm.Then dried in air blast
160 DEG C cure 60 minutes 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）：4H.
Glossiness（GB/T 1743-1979）：44.
Welding resistance performance（288 DEG C of solder furnaces impregnate 10s, three times）：Start shedding off, find that scolding tin enters phenomenon.
Tested by thermogravimetric, the heat resisting temperature of the solder mask of the present embodiment is 330 DEG C.
By above-described embodiment and the test data of comparative example, solder mask of the invention is specific linear poly-
Under the synergy of ester, hyperbranched resin and reactive diluent, institute has curing rate fast, solidification temperature, excellent into solder mask
Heat resistance, soldering resistance, yellowing resistance the features such as.
Embodiment described above only expresses embodiments of the present invention, and its 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, it all should fall within the scope and spirit of the invention.
Claims (7)
1. a kind of thermosetting solder mask ink composition, it is characterised in that be made up of the component of following parts by weight：
End group is 15 ~ 30 parts of the linear polyester of carboxyl；
10 ~ 25 parts of hyperbranched resin；
5 ~ 20 parts of reactive diluent；
10 ~ 35 parts of inorganic filler；
0 ~ 15 part of pigment；
0 ~ 8 part of function additive；
0 ~ 20 part of solvent；
1 ~ 3 part of curing agent；
Wherein, 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 into closed container, is then added the concentrated sulfuric acid as catalyst, is stirred at 160 ~ 180 DEG C
The matrix G1 of hyperbranched resin is obtained after condensation reaction occurring within 1 ~ 2 hour；
（2）Then 2 parts of (methylol) benzoic acid of 3,5- bis- 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 being stirred 1 ~ 2 hour at 160 ~ 180 DEG C, then this step is repeated 5 times, obtains hyperbranched tree
The matrix G7 of fat；
（3）Then by step（2）Reaction temperature be down to 80 DEG C, add excessive epoxychloropropane and sodium hydrate aqueous solution,
Reaction is washed after 3 hours and obtains described hyperbranched resin；
Wherein, the end group is that the hydroxyl value of the linear polyester of carboxyl is 120~180 mgKOH/g, weight average molecular weight 10000
~30000；
Wherein, the reactive diluent is ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether and isocyanuric acid three
The mixture of ethylene oxidic ester.
2. a kind of thermosetting solder mask ink composition according to claim 1, it is characterised in that the hyperbranched resin closes
Into step（2）In the obtained matrix G7 of hyperbranched resin contain 100 ~ 118 terminal hydroxy groups.
3. a kind of thermosetting solder mask ink composition according to claim 1, it is characterised in that the inorganic filler is carbon
At least one of sour calcium, aluminium hydroxide, barium sulfate, titanium dioxide.
4. a kind of thermosetting solder mask ink composition according to claim 1, it is characterised in that the function additive is to disappear
At least one of infusion, levelling agent, antioxidant.
5. a kind of thermosetting solder mask ink composition according to claim 1, it is characterised in that the solvent is that alcohols is molten
At least one of agent, esters solvent, ketones solvent, solvent of ether ester type.
6. a kind of thermosetting solder mask ink composition according to claim 1, it is characterised in that the curing agent is amine
Curing agent.
7. a kind of thermosetting solder mask ink composition according to claim 1 ~ 6 any one, it is characterised in that by as follows
The component composition of parts by weight：
End group is 15 ~ 30 parts of the linear polyester of carboxyl；
10 ~ 25 parts of hyperbranched resin；
1 ~ 5 part of ethylene glycol diglycidylether；
2 ~ 4 parts of polypropylene glycol diglycidyl ether；
3 ~ 7 parts of isocyanuric acid three-glycidyl ester；
10 ~ 35 parts of inorganic filler；
0 ~ 15 part of pigment；
0 ~ 8 part of function additive；
0 ~ 20 part of solvent；
1 ~ 3 part of curing agent.
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Effective date of registration: 20211229 Address after: 212413 No.18, chengshang Industrial Park, Huangmei Town, Jurong City, Zhenjiang City, Jiangsu Province Patentee after: JIANGSU HIMONIA ELECTRONIC MATERIALS CO.,LTD. Address before: 4 / F, No.1 warehouse, no.4987, Binhai Third Road, Wenzhou Economic and Technological Development Zone, Wenzhou City, Zhejiang Province 325000 Patentee before: Yu Qing |