CN109929490A - A kind of normal temperature cure conducting resinl and preparation method thereof - Google Patents
A kind of normal temperature cure conducting resinl and preparation method thereof Download PDFInfo
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- CN109929490A CN109929490A CN201910134770.8A CN201910134770A CN109929490A CN 109929490 A CN109929490 A CN 109929490A CN 201910134770 A CN201910134770 A CN 201910134770A CN 109929490 A CN109929490 A CN 109929490A
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- conducting resinl
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- temperature cure
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Abstract
Present invention relates particularly to a kind of normal temperature cure conducting resinls and preparation method thereof, the normal temperature cure conducting resinl is prepared by the following method to obtain: thermoplasticity alcohol-soluble acrylic resin and absolute ethyl alcohol and stirring are mixed, addition dispersing agent, levelling agent, thickening anti-settling agent, white carbon black, nano-silver powder and micro-silver powder is then proceeded to be stirred, ball milling filters, is filling.Conducting resinl curing rate obtained is fast, working life is long, caking property is good, can function well as conducting resinl of the electronic devices such as LCD liquid crystal display for static conductive function.
Description
Technical field
The present invention relates to conducting resinl technical fields, and in particular to a kind of normal temperature cure conducting resinl and preparation method thereof.
Background technique
Conducting resinl is the adhesive with certain adhesive property after a kind of solidification, it is usually based on conductive filler and base rubber
Raw material is wanted, conducting particles is combined together by the cementation of base rubber, forms conductive path, realizes leading by binding material
Electrical connection.
Traditional conducting resinl has three categories type, epoxy systems, silicone system, organosilicon systems.Epoxy systems, need using
Curing agent is just able to achieve film-forming, and most of epoxy hardeners, which need to heat, can just crosslink reaction, and normal temperature cure agent is latent
Volt property is shorter, and working life only has even a few minutes a few hours.Silicone system, although normal temperature cured type working life is longer, solidification
Reaction has the generation of the by-products such as ethyl alcohol, acetone, easily causes the phenomenon that generating corrosion by bonding substrates.Organosilicon systems, after solidification
The glue film of formation is softer, and there are the technical problems such as adhesion strength is low.Therefore, it is necessary to overcome the existing conducting resinl normal temperature cure time
The technical problems such as length, room temperature lower working life short, bad adhesion, improve the applicability of conducting resinl.
Summary of the invention
One of the objects of the present invention is to provide a kind of normal temperature cure conducting resinls, are prepared from the following raw materials in parts by weight:
As optimal technical scheme, the molecular weight of the thermoplasticity alcohol-soluble acrylic resin is 20000~50000, is glued
Degree is 1000-10000cps.
Technical solution more preferably, the viscosity of the thermoplasticity alcohol-soluble acrylic resin are 1000-6000cps.
As optimal technical scheme, the white carbon black is one of H18, H20, H21 or more than one combination.
As optimal technical scheme, the levelling agent is water and oil applicable type Siloxane-Oxyalkylene Copolymers levelling agent.
As optimal technical scheme, the thickening anti-settling agent is polyamide wax.
As optimal technical scheme, the dispersing agent is alcohol ethers solvent dispersing agent.
As optimal technical scheme, the partial size of the nano-silver powder is 100-200nm.
As optimal technical scheme, the partial size of the micro-silver powder is 1-3 μm.
The second purpose of the present invention is to provide the preparation methods of above-mentioned normal temperature cure conducting resinl, comprising the following steps:
(1) thermoplasticity alcohol-soluble acrylic resin and dehydrated alcohol are added in reaction kettle and are stirred；
(2) dispersing agent, levelling agent, thickening anti-settling agent, white carbon black, nano-silver powder and micro-silver powder are added to step (1)
Obtained in be stirred in mixture；
(3) mixture obtained in step (2) is subjected to ball milling, filters, is filling.
As optimal technical scheme, the temperature being stirred described in step (1) is 15-25 DEG C, and the time is 1-12 hours.
As optimal technical scheme, the temperature being stirred described in step (2) is room temperature, and the time is 0.5-5 hours.
As optimal technical scheme, Ball-milling Time described in step (3) is 1-12 hours；Ball milling partial size is 1-3 μm.
As optimal technical scheme, filter condition described in step (3) are as follows: sieve mesh number 300-800 mesh.
As optimal technical scheme, canned described in step (3) is that syringe is filling.
Advantageous effects of the invention:
Normal temperature cure conducting resinl provided by the invention, it is attached with glass baseplate using thermoplasticity alcohol-soluble acrylic resin
Put forth effort preferably, the conducting resinl made of thermoplasticity alcohol-soluble acrylic resin has relatively strong in glass baseplate, especially LCD screen
Cementability；Curing reaction is carried out without adding curing agent；Conductive peptizing agent is done using dehydrated alcohol, dehydrated alcohol is at normal temperature
Evaporation rate is fast, so that rate of drying is fast at normal temperature for manufactured conducting resinl；Thixotropic agent, manufactured conducting resinl are done using white carbon black
Thixotropy is higher, has good dispensing performance；Final conducting resinl obtained is with the normal temperature cure time is short, working life is long, body
The product advantage that resistivity is small, adhesive force is strong, the conduction of static conductive function is used for be especially suitable for electronic devices such as LCD liquid crystal displays
Glue.
As optimal technical scheme, normal temperature cure conducting resinl provided by the invention, white carbon black is in H18, H20, H21
One or more kinds of combinations, can have more perfect compatibility with resin solvent system, give full play to its thixotropic property.
As optimal technical scheme, normal temperature cure conducting resinl provided by the invention, thickening anti-settling agent is selected from polyamide wax,
Sedimentation phenomenon does not occur for the silver powder particles in conducting resinl made of capable of making, and extends the working life of conducting resinl.
As optimal technical scheme, normal temperature cure conducting resinl provided by the invention, levelling agent is that water and oil applicable type polyethers changes
Property polysiloxane leveling agents, can have better compatibility with thermoplasticity alcohol-soluble acrylic resin and anhydrous ethanol solvent, make
Conducting resinl obtained is not stratified, and has preferable levelability.
As optimal technical scheme, the dispersing agent is alcohol ethers solvent dispersing agent, with thermoplasticity alcohol-soluble propylene
Acid resin and anhydrous ethanol solvent can have better compatibility, keep conducting resinl obtained not stratified, and there is preferable dispersion to lead
The performance of electric silver powder.
The preparation method of normal temperature cure conducting resinl provided by the invention, it is easy to operate, by selecting specific composition of raw materials
And operation conditions optimization, so that the normal temperature cure conducting resinl of preparation has the normal temperature cure time short, the advantage of working life length.
As optimal technical scheme, the preparation method of normal temperature cure conducting resinl provided by the invention is mixed by optimization stirring
Conjunction condition controls the evaporation rate of conductive peptizing agent, to improve the stability of conducting resinl.
As optimal technical scheme, the preparation method of normal temperature cure conducting resinl provided by the invention, filter condition can have
The silver powder of effect removal bulky grain, improves the stability of conducting resinl.
Specific embodiment
Detailed description of the preferred embodiments below.
Normal temperature cure conducting resinl provided by the invention, is made by following raw material: thermoplasticity alcohol-soluble acrylic resin, anhydrous
Ethyl alcohol, white carbon black, levelling agent, dispersing agent, thickening anti-settling agent, nano-silver powder and micro-silver powder；
Wherein, the parts by weight composition of each raw material is as follows:
The thermoplasticity alcohol-soluble acrylic resin is 5-30 parts, specifically, such as can be 5,10,15,20,25,30
Part；
The dehydrated alcohol is 30-60 parts, specifically, such as can be 30,40,50,60 parts；
The white carbon black is 5-10 parts, specifically, such as can be 5,6,7,8,9,10 parts；
The levelling agent is 1-4 parts, specifically, such as can be 1,2,3,4 part；
The dispersing agent is 1-4 parts, specifically, such as can be 1,2,3,4 part；
The thickening anti-settling agent be 0.1-1 part, specifically, for example, can be 0.1,0.2,0.3,0.4,0.5,0.6,0.7,
0.8,0.9,1.0 part；
The nano-silver powder is 20-50 parts, specifically, such as can be 20,30,40,50 parts；
The micro-silver powder is 30-50 parts, specifically, such as can be 30,35,40,45,50 parts.
Preferably, the molecular weight of the thermoplasticity alcohol-soluble acrylic resin is 20000~50000, viscosity 1000-
10000cps, specifically, such as can for 1000,2000,3000,4000,5000,6000,7000,8000,9000,
10000cps.It is highly preferred that the viscosity of the alcohol-soluble acrylic resin is 1000-6000cps, specifically, such as can be
1000,2000,3000,4000,5000,6000cps.The thermoplasticity alcohol-soluble acrylic resin can by commercially available acquisition,
Such as it can be thermoplasticity alcohol-soluble acrylic resin B725, thermoplasticity alcohol-soluble acrylic resin B731, thermoplasticity alcohol-soluble
Acrylic resin B736, thermoplasticity alcohol-soluble acrylic resin B805, thermoplasticity alcohol-soluble acrylic resin B817, thermoplasticity alcohol
One or more of soluble acrylic resin B875, but not limited to this.
Preferably, the white carbon black is one of H18, H20, H21 or more than one combination；
Preferably, the levelling agent is water and oil applicable type Siloxane-Oxyalkylene Copolymers levelling agent.The water and oil applicable type is poly-
Ether modified polyorganosiloxane levelling agent can be by commercially available acquisition, such as can be water and oil applicable type Siloxane-Oxyalkylene Copolymers levelling
Agent SP-931, water and oil applicable type Siloxane-Oxyalkylene Copolymers levelling agent SP-963 or water and oil applicable type Siloxane-Oxyalkylene Copolymers stream
One or more of flat agent SP-983, but not limited to this.
Preferably, the thickening anti-settling agent is polyamide wax.
Preferably, the dispersing agent is alcohol ethers solvent dispersing agent.The alcohol ethers solvent dispersing agent can pass through
Commercially available acquisition, such as can be alcohol ethers solvent dispersing agent LD-1211, alcohol ethers solvent dispersant B YK-P104S or alcohol
One or more of ether solvent class dispersant B YK-163, but not limited to this.
Preferably, the partial size of the nano-silver powder is 100-200nm, specifically, such as can for 100,110,120,
130,140,150,160,170,180,190,200nm.It is highly preferred that the partial size of the nano-silver powder is 100-160nm, specifically
Ground, such as can be 100,110,120,130,140,150,160nm.
Preferably, the partial size of the micro-silver powder can be 1-3 μm, specifically, such as can be 1,1.5,2,2.5,3 μ
m。
Above-mentioned normal temperature cure conducting resinl is to be prepared by the following method:
(1) thermoplasticity alcohol-soluble acrylic resin and dehydrated alcohol are added in reaction kettle and are stirred；
(2) dispersing agent, levelling agent, thickening anti-settling agent, white carbon black, nano-silver powder and micro-silver powder are added to step (1)
Obtained in be stirred in mixture；
(3) mixture obtained in step (2) is subjected to ball milling, filters, is filling.
Preferably, the condition being stirred described in step (1) are as follows: temperature is 15-25 DEG C, specifically, such as can be
15,20,25℃；Mixing time is 1-12 hours, specifically, such as can be small for 1,2,3,4,5,6,7,8,9,10,11,12
When.
Preferably, what the process being stirred described in step (2) carried out at room temperature, the time being stirred is 0.5-
5 hours, specifically, such as can be 0.5,1,2,3,4,5 hour.
Preferably, Ball-milling Time described in step (3) be 1-12 hour, specifically, for example, can be 1,2,3,4,5,6,
7,8,9,10,11,12 hours；Ball milling partial size is 1-3 μm；
Preferably, filter condition described in step (3) are as follows: sieve mesh number 300-800 mesh specifically, such as can be 300
Mesh, 400 mesh, 500 mesh, 600 mesh, 700 mesh, 800 mesh.
Preferably, canned described in step (3) is that syringe is filling.
The present invention will be described in detail by way of examples below, but protection scope of the present invention is not limited to that.
Embodiment 1
A kind of normal temperature cure conducting resinl, is prepared by the following method to obtain:
It (1) is the thermoplasticity alcohol-soluble acrylic resin B725 of 3000cps and 30 parts by 10 parts of viscosity under the conditions of 25 DEG C
Dehydrated alcohol, which is added in reaction kettle, to be stirred 5 hours；
(2) under the conditions of 25 DEG C, by 1 part of alcohol ethers solvent dispersing agent LD-1211, the polyether-modified poly- silicon of water and oil applicable type
Oxygen alkane levelling agent SP-931,0.3 part of polyamide wax, 5 parts of white carbon black H18, the nano-silver powder and 30 parts of grains that 20 parts of partial sizes are 100nm
Diameter is that 1 μm of micro-silver powder is added in mixture obtained in step (1) and is stirred 2 hours；
(3) mixture obtained in step (2) is carried out ball milling 5 hours, test fineness of materials can be received to 3 μm or less
Material has been filtered and filling has been saved into syringe with 400 mesh net filtrations after rewinding.
Conducting resinl obtained is solidified at 25 DEG C, curing time 13min, adhesive force is 4B, resistivity after solidification
For 2.5 × 10-4 Ω cm, working life 45h.
Embodiment 2
It (1) is the thermoplasticity alcohol-soluble acrylic resin B731 of 6000cps and 35 parts by 10 parts of viscosity under the conditions of 25 DEG C
Dehydrated alcohol, which is added in reaction kettle, to be stirred 5 hours；
(2) under the conditions of 25 DEG C, by 1 part of alcohol ethers solvent dispersant B YK-P104S, 1 part of water and oil applicable type polyethers changes
Property polysiloxane leveling agents SP-963,0.1 part of polyamide wax, 5 parts of white carbon black H20, nano-silver powder that 40 parts of partial sizes are 150nm and
The micro-silver powder that 30 parts of partial sizes are 1 μm, which is added in mixture obtained in step (1), to be stirred 2 hours；
(3) mixture obtained in step (2) is carried out ball milling 5 hours, test fineness of materials can be received to 3 μm or less
Material has been filtered and filling has been saved into syringe with 400 mesh net filtrations after rewinding.
Conducting resinl obtained is solidified at 25 DEG C, curing time 12min, adhesive force is 4B, resistivity after solidification
For 2.1 × 10-4 Ω cm, working life 46h.
Embodiment 3
It (1) is the thermoplasticity alcohol-soluble acrylic resin B736 of 4000cps and 35 parts by 15 parts of viscosity under the conditions of 25 DEG C
Dehydrated alcohol, which is added in reaction kettle, to be stirred 5 hours；
(2) under the conditions of 25 DEG C, by 1 part of alcohol ethers solvent dispersant B YK-163,1 part of water and oil applicable type is polyether-modified
Polysiloxane leveling agents SP-983,0.2 part of polyamide wax, 5 parts of white carbon black H21, the nano-silver powder and 35 that 30 parts of partial sizes are 100nm
It is 2 hours that the micro-silver powder that part partial size is 1 μm, which is added to the time being stirred in mixture obtained in step (1),；
(3) mixture obtained in step (2) is carried out ball milling 5 hours, test fineness of materials can be received to 3 μm or less
Material has been filtered and filling has been saved into syringe with 400 mesh net filtrations after rewinding.
Conducting resinl obtained is solidified at 25 DEG C, curing time 11min, adhesive force is 4B, resistivity after solidification
For 2.3 × 10-4 Ω cm, working life 47h.
Embodiment 4
It (1) is the thermoplasticity alcohol-soluble acrylic resin B805 of 4000cps and 50 parts by 20 parts of viscosity under the conditions of 25 DEG C
Dehydrated alcohol, which is added in reaction kettle, to be stirred 5 hours；
(2) under the conditions of 25 DEG C, by 1 part of alcohol ethers solvent dispersing agent LD-1211,1 part of water and oil applicable type is polyether-modified
Polysiloxane leveling agents SP-931,0.3 part of polyamide wax, 5 parts of white carbon black H18, the nano-silver powder and 50 that 50 parts of partial sizes are 100nm
The micro-silver powder that part partial size is 1 μm, which is added in mixture obtained in step (1), to be stirred 2 hours；
(3) mixture obtained in step (2) is carried out ball milling 5 hours, test fineness of materials can be received to 3 μm or less
Material has been filtered and filling has been saved into syringe with 400 mesh net filtrations after rewinding.
Conducting resinl obtained is solidified at 25 DEG C, curing time 10min, adhesive force is 5B, resistivity after solidification
For 2 × 10-4 Ω cm, working life 48h.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.The endpoint and any value of range disclosed by herein are not
It is limited to the accurate range or value, these ranges or value should be understood as comprising the value close to these ranges or value.For numerical value
For range, between the endpoint value of each range, between the endpoint value of each range and individual point value and individual point value
Between can be combined with each other and obtain one or more new numberical ranges, these numberical ranges should be considered as specific herein
It is open.It should be pointed out that for those of ordinary skill in the art, without departing from the inventive concept of the premise, also
Several modifications and improvements can be made, these are all within the scope of protection of the present invention.Therefore, the scope of protection of the patent of the present invention is answered
It is determined by the appended claims.
Claims (10)
1. a kind of normal temperature cure conducting resinl, which is characterized in that be prepared from the following raw materials in parts by weight:
2. normal temperature cure conducting resinl according to claim 1, which is characterized in that the thermoplasticity alcohol-soluble acrylic resin
Molecular weight be 2000-5000, viscosity 1000-10000cps, preferably 1000-6000cps.
3. normal temperature cure conducting resinl according to claim 1, which is characterized in that the white carbon black is in H18, H20, H21
One or more kinds of combinations.
4. normal temperature cure conducting resinl according to claim 1, which is characterized in that the levelling agent is water and oil applicable type polyethers
Modified polyorganosiloxane levelling agent.
5. normal temperature cure conducting resinl according to claim 1, which is characterized in that the thickening anti-settling agent is polyamide wax.
6. normal temperature cure conducting resinl according to claim 1, which is characterized in that the dispersing agent is alcohol ethers solvent point
Powder.
7. normal temperature cure conducting resinl according to claim 1, which is characterized in that the partial size of the nano-silver powder is 100-
200nm, the partial size of the micro-silver powder are 1-3 μm.
8. the preparation method of normal temperature cure conducting resinl described in -7 any one according to claim 1, which is characterized in that including with
Lower step:
(1) thermoplasticity alcohol-soluble acrylic resin and absolute ethyl alcohol and stirring are mixed；
(2) dispersing agent, levelling agent, thickening anti-settling agent, white carbon black, nano-silver powder and micro-silver powder are added to institute in step (1)
It is stirred in the mixture obtained；
(3) mixture obtained in step (2) is subjected to ball milling, filters, is filling.
9. preparation method according to claim 8, which is characterized in that the temperature being stirred described in step (1) is 15-
25 DEG C, the time is 1-12 hours；The temperature being stirred described in step (2) is room temperature, and the time is 0.5-5 hours.
10. preparation method according to claim 8, which is characterized in that Ball-milling Time described in step (3) is that 1-12 is small
When, ball milling partial size is 1-3 μm；Filter condition described in step (3) are as follows: sieve mesh number 300-800 mesh.
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Cited By (5)
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| CN110964462A (en) * | 2019-12-09 | 2020-04-07 | 南京金世家新材料科技有限公司 | Single-component conductive adhesive stored and cured at normal temperature and preparation method and application thereof |
| CN111925753A (en) * | 2020-07-20 | 2020-11-13 | 华南理工大学 | Cigarette phase change material of tipping paper for cigarettes and preparation method and application thereof |
| CN112614610A (en) * | 2020-11-06 | 2021-04-06 | 深圳市飞荣达科技股份有限公司 | Block conductive adhesive cable and preparation method thereof |
| CN114854340A (en) * | 2022-05-20 | 2022-08-05 | 长春艾德斯新材料有限公司 | Low-permeability conductive silver adhesive and preparation method thereof |
| CN115074052A (en) * | 2022-05-20 | 2022-09-20 | 长春艾德斯新材料有限公司 | Conductive silver adhesive capable of being rapidly cured at room temperature, preparation method and conductive film |
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Application publication date: 20190625 |