CN108641469A - A kind of ultraviolet curing solder mask and preparation method thereof - Google Patents
A kind of ultraviolet curing solder mask and preparation method thereof Download PDFInfo
- Publication number
- CN108641469A CN108641469A CN201810473900.6A CN201810473900A CN108641469A CN 108641469 A CN108641469 A CN 108641469A CN 201810473900 A CN201810473900 A CN 201810473900A CN 108641469 A CN108641469 A CN 108641469A
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- China
- Prior art keywords
- parts
- ultraviolet curing
- solder mask
- double methacrylate
- photoinitiator
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
Abstract
The present invention discloses a kind of ultraviolet curing solder mask and preparation method thereof; including 25~40 parts of modified epoxy double methacrylate; 15~20 parts of polyurethane double methacrylate; 8~15 parts of acrylic monomers; first 2~5 parts of photoinitiator; second 1~4 part of photoinitiator; 10~25 parts of azo everbright fast yellow; 1~3 part of antifoaming agent; 1~3 part of water-reducing agent; 1~3 part of levelling agent, the modified epoxy double methacrylate are obtained by the reaction by the way that epoxy double methacrylate, maleic anhydride, concentrated sulfuric acid catalyst and polymerization inhibitor to be placed in the container of inert gas shielding.The present invention is organically combined using modified epoxy double methacrylate, polyurethane double methacrylate and acrylic monomers three, it cooperates using between its molecular structure, synergistic effect, it is prepared for the ultraviolet curing solder mask that a kind of cure times are short, compatibility is high, its adhesive force is significantly improved compared to single resin ink, significantly improves the precision of ultraviolet curing printing.
Description
Technical field
The present invention relates to a kind of ultraviolet curing solder masks and preparation method thereof, belong to solder mask field.
Background technology
Solder mask divides several kinds：Such as liquid photosensitive development solder mask, heat curing type solder mask, ultraviolet hardening
Solder mask etc. is a kind of ink being exclusively used on pcb board.The UV cured anti-solder paste developed for printed circuit board
Ink is free of solvent, and pollution-free and hardening is quick, has excellent adhesive force, heat resistance and insulating properties after hardening.
Existing ultraviolet curing solder mask printed pattern tolerance is ± 0.2mm, is mainly used in the simple of single side
On product, the complexity of dual platen is generally higher than single sided board, and precision requirement is also higher, so general ultraviolet curing resistance
Solder paste ink is not suitable for doubling plate.
Invention content
It is high the technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of printing precision, adhere to
The strong ultraviolet curing solder mask of power.
The technical solution adopted by the present invention is as follows：
A kind of ultraviolet curing solder mask, includes the component of following parts by weight：
25~40 parts of modified epoxy double methacrylate,
15~20 parts of polyurethane double methacrylate,
8~15 parts of acrylic monomers,
First 2~5 parts of photoinitiator,
Second 1~4 part of photoinitiator,
10~25 parts of azo everbright fast yellow,
1~3 part of antifoaming agent,
1~3 part of water-reducing agent,
1~3 part of levelling agent,
The modified epoxy double methacrylate is by by epoxy double methacrylate, maleic anhydride, concentrated sulfuric acid catalyst and resistance
Poly- agent is placed in the container of inert gas shielding, is heated to 80~100 DEG C of reactions to the half that acid value is initial acid value, is cooled to
50~70 DEG C are added dimethylethanolamine and water, are stirred to react 0.5~0.6h postcoolings to room temperature and obtain.
Preferably, in the polyurethane double methacrylate ,-NCO linkage contents are not less than 10%.
The acrylic monomers is by difunctional acrylic monomers and monofunctional acrylates' monomer composition, the difunctionality
The weight ratio of group's acrylic monomers and monofunctional acrylates' monomer is 0.8~1:1.
First photoinitiator is benzophenone.
The second photoinitiator model 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173).
The antifoaming agent is Germany's 057 antifoaming agent of BYK.
The water-reducing agent is polycarboxylate water-reducer.
The levelling agent is Germany's 307 levelling agents of BYK.
The preparation method of above-mentioned ultraviolet curing solder mask, includes the following steps：
Step 1：By modified epoxy double methacrylate, polyurethane double methacrylate, acrylic monomers, the first photoinitiator
It feeds intake in channel with the second photoinitiator；
Step 2：With high speed dispersor under the rotating speed of 800~1200r/min, disperse 0.5~0.8h in 50~80 DEG C,
Stop stirring and keeping the temperature；
Step 3：Azo everbright fast yellow, antifoaming agent, water-reducing agent and levelling agent are added in the feed liquid that step 2 obtains, continues
0.3~0.5h is stirred with 500~800r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
The invention firstly uses maleic anhydrides to be modified epoxy double methacrylate so that the double propylene of modified epoxy
Acid esters double bond content at least improves twice, and in the case where being illuminated by the light excitation, fracture, which occurs, for these unsaturated double-bonds makes linear polymeric wink
Between crosslinking become reticular structure, therefore modified epoxy double methacrylate light-cured performance is significantly improved.
- NCO linkage contents are not less than 10% in polyurethane double methacrylate, can be with modified epoxy double methacrylate and third
Acrylic monomer is arranged in pairs or groups, and under the irradiation of ultraviolet light, system can continue heat cure, and then realize double solidification effects.
Acrylic monomers can be interspersed in modification by difunctional acrylic monomers and monofunctional acrylates' monomer composition
Between epoxy double methacrylate and polyurethane double methacrylate so that system combines more secured, and significantly improves modified ring
The compatibility of oxygen double methacrylate and polyurethane double methacrylate.
It is more sensitive to water to cure component, by introducing water-reducing agent to improve preservation and the working performance of curing agent.
Advantageous effect：
The present invention uses modified epoxy double methacrylate, polyurethane double methacrylate and the organic knot of acrylic monomers three
It closes, cooperates using between its molecular structure, synergistic effect is prepared for that a kind of cure times are short, compatibility is high
Ultraviolet curing solder mask, adhesive force are significantly improved compared to single resin ink, significantly improve ultraviolet curing print
The precision of brush.
Specific implementation mode
According to following embodiments, the present invention may be better understood.
Embodiment 1
By epoxy double methacrylate, maleic anhydride, concentrated sulfuric acid catalyst and di-tert-butyl p-cresol polymerization inhibitor according to mole
Than 3:1:0.3:0.2 is placed in the container of inert gas shielding, is heated to 95 DEG C of reactions to the half that acid value is initial acid value, drop
To 65 DEG C dimethylethanolamines and water is added in temperature, and (molar ratio of epoxy double methacrylate, dimethylethanolamine and water is 3:2:1),
It being stirred to react 0.6h postcoolings to room temperature and obtains modified epoxy double methacrylate, measurement C=C double bond contents are 0.354 (bromine number),
Acid value 10.89mgg.
Embodiment 2
By epoxy double methacrylate, maleic anhydride, concentrated sulfuric acid catalyst and di-tert-butyl p-cresol polymerization inhibitor according to mole
Than 3:2:0.3:0.2 is placed in the container of inert gas shielding, is heated to half of 100 DEG C of reactions to acid value for initial acid value,
70 DEG C are cooled to dimethylethanolamines and water to be added (molar ratio of epoxy double methacrylate, dimethylethanolamine and water is 3:3:
1) it, is stirred to react 0.6h postcoolings to room temperature and obtains modified epoxy double methacrylate, measurement C=C double bond contents are 0.248 (bromine
Value), acid value 16.89mgg.
Embodiment 3
Step 1：35 parts of modified epoxy double methacrylate prepared by Example 1,18 parts of polyurethane double methacrylate, third
12 parts of acrylic monomer (dipropylene glycol diacrylate and tetrahydrofuran acrylate monomer, weight ratio 1:1), first is light-initiated
In (1173) 2 parts of channels that feed intake of 4 parts of agent benzophenone and the second photoinitiator；
Step 2：With high speed dispersor under the rotating speed of 1000r/min, disperse 0.6h in 65 DEG C, stops stirring and keeping the temperature；
Step 3：23 parts of azo everbright fast yellow, 2 parts of antifoaming agent, 2 parts of water-reducing agent and stream are added in the feed liquid that step 2 obtains
2 parts of flat agent continues to stir 0.4h with 800r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
Embodiment 4
Step 1：25 parts of modified epoxy double methacrylate prepared by Example 1,20 parts of polyurethane double methacrylate, third
(dipropylene glycol diacrylate and lauric acid acrylate weight ratio are 0.8 to 15 parts of acrylic monomer:1), the first photoinitiator two
In (1173) 4 parts of channels that feed intake of 2 parts of Benzophenone and the second photoinitiator；
Step 2：With high speed dispersor under the rotating speed of 800r/min, disperse 0.8h in 50 DEG C, stops stirring and keeping the temperature；
Step 3：10 parts of azo everbright fast yellow, 1 part of antifoaming agent, 1 part of water-reducing agent and stream are added in the feed liquid that step 2 obtains
1 part of flat agent continues to stir 0.5h with 500r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
Embodiment 5
Step 1：40 parts of modified epoxy double methacrylate prepared by Example 1,15 parts of polyurethane double methacrylate, third
8 parts of acrylic monomer (hexanediyl ester and tetrahydrofuran acrylate monomer, weight ratio 1:1), the first photoinitiator
In (1173) 1 parts of channels that feed intake of 5 parts of benzophenone and the second photoinitiator；
Step 2：With high speed dispersor under the rotating speed of 1200r/min, disperse 0.5h in 80 DEG C, stops stirring and keeping the temperature；
Step 3：25 parts of azo everbright fast yellow, 3 parts of antifoaming agent, 3 parts of water-reducing agent and stream are added in the feed liquid that step 2 obtains
3 parts of flat agent continues to stir 0.3h with 500r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
Comparative example 1
Step 1：35 parts of modified epoxy double methacrylate prepared by Example 1,18 parts of polyurethane double methacrylate, the
In (1173) 2 parts of channels that feed intake of one 4 parts of photoinitiator benzophenone and the second photoinitiator；
Step 2：With high speed dispersor under the rotating speed of 1000r/min, disperse 0.6h in 65 DEG C, stops stirring and keeping the temperature；
Step 3：23 parts of azo everbright fast yellow, 2 parts of antifoaming agent, 2 parts of water-reducing agent and stream are added in the feed liquid that step 2 obtains
2 parts of flat agent continues to stir 0.4h with 800r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
Comparative example 2
Step 1：35 parts of modified epoxy double methacrylate prepared by Example 1,12 parts of (dipropylene glycol of acrylic monomers
Diacrylate and tetrahydrofuran acrylate monomer, weight ratio 1:1), 4 parts of the first photoinitiator benzophenone and the second light
In (1173) 2 parts of channels that feed intake of initiator；
Step 2：With high speed dispersor under the rotating speed of 1000r/min, disperse 0.6h in 65 DEG C, stops stirring and keeping the temperature；
Step 3：23 parts of azo everbright fast yellow, 2 parts of antifoaming agent, 2 parts of water-reducing agent and stream are added in the feed liquid that step 2 obtains
2 parts of flat agent continues to stir 0.4h with 800r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
Comparative example 3
Step 1：Take 35 parts of epoxy double methacrylate, 12 parts of 18 parts of polyurethane double methacrylate, acrylic monomers (dipropyls
Omega-diol diacrylate and tetrahydrofuran acrylate monomer, weight ratio 1:1), 4 parts of the first photoinitiator benzophenone and
In two (1173) 2 parts of the photoinitiator channels that feed intake；
Step 2：With high speed dispersor under the rotating speed of 1000r/min, disperse 0.6h in 65 DEG C, stops stirring and keeping the temperature；
Step 3：23 parts of azo everbright fast yellow, 2 parts of antifoaming agent, 2 parts of water-reducing agent and stream are added in the feed liquid that step 2 obtains
2 parts of flat agent continues to stir 0.4h with 800r/min；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
The solder mask that above-described embodiment 3~5 and comparative example 1~3 are prepared carries out conventional performance test, as a result
It is shown in Table 1：Pcb board spray printing is carried out using UV ink-jet screen printers, solidification ultraviolet source power is 250W/cm, under 25 DEG C of environment
The viscosity of test ink, adhesive force are measured according to GB/T 9286-1998 test methods, hardness according to GB/T6739-2006, resistance
It is 288 DEG C of dippings 10 seconds of solder furnace four times to weld performance condition, and see whether to fall off enters phenomenon with scolding tin, and no discoloration, is floated at stripping
It rises and scolding tin infiltration is excellent.It can be seen from the data in Table 1 that epoxy double methacrylate light-cured performance after modified is shown
It writes and improves, can reach better light-cured performance with the use of polyurethane double methacrylate and acrylic monomers, strong adhesive force,
Printing precision is high.
Table 1
| Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Viscosity cP | 17.8 | 18.9 | 18.7 | 21.4 | 20.8 | 24.6 |
| Adhesive force | 1 grade | 1 grade | 1 grade | 3 grades | 3 grades | 4 grades |
| Hardness | 6H | 6H | 6H | 4H | 4H | 3H |
| Solidification rate m/min | 15 | 16 | 18 | 11 | 10 | 5 |
| Welding resistance performance | It is excellent | It is excellent | It is excellent | Slight stripping | Slightly float | Scolding tin penetrates into |
| Printing precision mm | ±0.08 | ±0.09 | ±0.1 | ±0.12 | ±0.13 | ±0.2 |
The present invention provides the thinking and method of a kind of ultraviolet curing solder mask and preparation method thereof, specific implementation should
There are many method and approach of technical solution, the above is only a preferred embodiment of the present invention, it is noted that for this technology
For the those of ordinary skill in field, various improvements and modifications may be made without departing from the principle of the present invention, this
A little improvements and modifications also should be regarded as protection scope of the present invention.Existing skill can be used in each component part being not known in the present embodiment
Art is realized.
Claims (9)
1. a kind of ultraviolet curing solder mask, which is characterized in that include the component of following parts by weight：
25~40 parts of modified epoxy double methacrylate,
15~20 parts of polyurethane double methacrylate,
8~15 parts of acrylic monomers,
First 2~5 parts of photoinitiator,
Second 1~4 part of photoinitiator,
10~25 parts of azo everbright fast yellow,
1~3 part of antifoaming agent,
1~3 part of water-reducing agent,
1~3 part of levelling agent,
The modified epoxy double methacrylate is by by epoxy double methacrylate, maleic anhydride, concentrated sulfuric acid catalyst and polymerization inhibitor
It is placed in the container of inert gas shielding, is heated to 80~100 DEG C of reactions to the half that acid value is initial acid value, it is cooled to 50~
70 DEG C are added dimethylethanolamine and water, are stirred to react 0.5~0.6h postcoolings to room temperature and obtain.
2. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the double acrylic acid of the polyurethane
In ester ,-NCO linkage contents are not less than 10%.
3. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the acrylic monomers is by double
Functional group's acrylic monomers and monofunctional acrylates' monomer composition, the difunctional acrylic monomers and simple function group propylene
The weight ratio of acid monomers is 0.8~1:1.
4. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that first photoinitiator is
Benzophenone.
5. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the second light-initiated dosage form
Number be 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173).
6. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the antifoaming agent is Germany
057 antifoaming agent of BYK.
7. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the water-reducing agent is polycarboxylic acids
Water-reducing agent.
8. a kind of ultraviolet curing solder mask according to claim 1, which is characterized in that the levelling agent is Germany
307 levelling agents of BYK.
9. the preparation method of ultraviolet curing solder mask described in claim 1~8 any one, which is characterized in that including such as
Lower step：
Step 1：By modified epoxy double methacrylate, polyurethane double methacrylate, acrylic monomers, the first photoinitiator and
Two photoinitiators feed intake in channel；
Step 2：With high speed dispersor under the rotating speed of 800~1200r/min, disperses 0.5~0.8h in 50~80 DEG C, stop
It stirs and keeps the temperature；
Step 3：Azo everbright fast yellow, antifoaming agent, water-reducing agent and levelling agent are added in the feed liquid that step 2 obtains, continues with 500
~800r/min stirs 0.3~0.5h；
Step 4：After stirring and evenly mixing, it is 300 nanometers or less to be ground to grain size with hydraulic three-roller machine；
Step 5：After being filtered using 1 μm of filter element filtering machine to obtain the final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810473900.6A CN108641469A (en) | 2018-05-17 | 2018-05-17 | A kind of ultraviolet curing solder mask and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810473900.6A CN108641469A (en) | 2018-05-17 | 2018-05-17 | A kind of ultraviolet curing solder mask and preparation method thereof |
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| CN108641469A true CN108641469A (en) | 2018-10-12 |
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| CN201810473900.6A Pending CN108641469A (en) | 2018-05-17 | 2018-05-17 | A kind of ultraviolet curing solder mask and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776756A (en) * | 2019-01-21 | 2019-05-21 | 深圳市道尔顿电子材料有限公司 | A kind of dual modified epoxy acrylate and its photoresist |
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| CN104277519A (en) * | 2014-10-28 | 2015-01-14 | 成都纳硕科技有限公司 | Ultraviolet curable antifouling flame-retardant coating for plastic circuit board |
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| CN101295142A (en) * | 2007-04-27 | 2008-10-29 | 太阳油墨制造株式会社 | Printed circuit board and manufacturing method thereof |
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