CN103881096B - Large scale integrated circuit solvent-free silicone resin and preparation method thereof - Google Patents
Large scale integrated circuit solvent-free silicone resin and preparation method thereof Download PDFInfo
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- CN103881096B CN103881096B CN201410065605.9A CN201410065605A CN103881096B CN 103881096 B CN103881096 B CN 103881096B CN 201410065605 A CN201410065605 A CN 201410065605A CN 103881096 B CN103881096 B CN 103881096B
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Abstract
The invention discloses a kind of large scale integrated circuit solvent-free silicone resin, it is by dimethyldichlorosilane 50 ~ 100 parts, dichloromethyl vinyl silanes 30 ~ 60 parts, phenyl trichlorosilane 70 ~ 140 parts, butyl acetate 90 ~ 180 parts, reaction dissolvent 500 ~ 1000 parts, coupling agent 2 ~ 5 parts is made.The large scale integrated circuit solvent-free silicone resin that the present invention provides, preferably gone out each component proportioning by great many of experiments, this resin has wearability, oxidative resistance, resistant of high or low temperature, radiation resistance, weatherability, insulating properties, hydrophobicity and the low surface potential energy of excellence.And the preparation method that the present invention provides, whole technological design is reasonable, use continuous hydrolysis technology, complete hydrolyzing, wash, be concentrated in a step, and use efficient catalyst zirconium ester coupling agent, the response time can be greatly reduced, improve production efficiency, cost-effective, improve the combination property of product.
Description
Technical field
The present invention relates to a kind of resin, solvent-free silicone resin being specifically related to a kind of large scale integrated circuit and preparation method thereof.
Background technology
Solvent-free silicone resin as integrated circuit packaging material have the wearability more excellent than conventional encapsulation materials epoxy resin,
The advantages such as oxidative resistance, resistant of high or low temperature, radiation resistance, weatherability, insulating properties, hydrophobicity and low surface potential energy, envelope
Dress solvent-free silicone resin should meet: bulk resistor is higher than 1014Ω, thermal conductivity is higher than 1.80W/mK, and coefficient of thermal expansion is less than
30 × 10-6/K, is resistant to be not less than 109Still keep favorable elasticity after drawing the irradiation of spy, be used by high-end large scale integrated circuit
Novel encapsulated material.
The sales volume of whole nation IC Packaging Industry is 1035.6 hundred million yuan, and annual with the speed increment more than about 12%,
Expect high-end macromolecule silicon materials used for packing material in 2014 more than 10,000 tons (adding up according to integrated circuit industry association).
Tradition solvent-free silicone resin uses batch (-type) hydrolysis process, there is the process time long, and production efficiency is low, and yield is low, and cost is high
Deng not enough.
Summary of the invention
Goal of the invention: the technical problem to be solved is to overcome the deficiencies in the prior art, it is provided that a kind of component proportioning section
Learn rationally, there is the wearability of excellence, oxidative resistance, resistant of high or low temperature, radiation resistance, weatherability, insulating properties, hydrophobic
The solvent-free silicone resin of the large scale integrated circuit of the advantage such as property and low surface potential energy；Another object of the present invention is to provide
The preparation method of this solvent-free silicone resin.
Technical scheme: for realizing object above, the present invention adopts the following technical scheme that:
A kind of large scale integrated circuit solvent-free silicone resin, it is made up of the raw material of following parts by weight: dimethyldichlorosilane
50～100 parts, dichloromethyl vinyl silanes 30～60 parts, phenyl trichlorosilane 70～140 parts, butyl acetate 90～180 parts,
Reaction dissolvent 500～1000 parts, coupling agent 2～5 parts；
Described reaction dissolvent is made up of the raw material of following parts by weight: concentration 10% sodium hydrate aqueous solution 100～120 parts, fourth
Ketone 90～110 parts, butyl acetate 300～400 parts.
Preferably, above-described large scale integrated circuit solvent-free silicone resin, it is by the raw material of following parts by weight
Make: dimethyldichlorosilane 50～80 parts, dichloromethyl vinyl silanes 30～40 parts, phenyl trichlorosilane 70～100 parts,
Butyl acetate 90～140 parts, reaction dissolvent 500～800 parts, coupling agent 2～5 parts；
Described reaction dissolvent is made up of the raw material of following parts by weight: concentration 10% sodium hydrate aqueous solution 100～110 parts, fourth
Ketone 90～100 parts, butyl acetate 300～350 parts.
Preferably, above-described large scale integrated circuit solvent-free silicone resin, it is by the raw material of following parts by weight
Make: dimethyldichlorosilane 50～65 parts, dichloromethyl vinyl silanes 30～40 parts, phenyl trichlorosilane 70～80 parts,
Butyl acetate 90～100 parts, reaction dissolvent 500～550 parts, coupling agent 2～5 parts；
Described reaction dissolvent is made up of the raw material of following parts by weight: concentration 10% sodium hydrate aqueous solution 100～110 parts, fourth
Ketone 90～100 parts, butyl acetate 300 parts.
Preferably, above-described large scale integrated circuit solvent-free silicone resin, described coupling agent is that zirconate is even
Connection agent, i.e. coupling agent are four n-pro-pyl zirconates.
The preparation method of large scale integrated circuit solvent-free silicone resin of the present invention, comprises the following steps:
(1) parts by weight as described in claims 1 to 3 take dimethyldichlorosilane, methylvinyldichlorosilane, phenyl
Trichlorosilane and butyl acetate are made into mixed liquor, instill parts by weight described in claims 1 to 3 by sodium hydrate aqueous solution,
Butanone, the reaction dissolvent that butyl acetate is made into, within about 1 hour, drip off, after dripping off, continue stirring reaction 1～2 hour；
(2) dividing and fall down a layer neutral water, solids content is surveyed in sampling；Add the zirconate of solid part 5/2000ths to thousand/1000ths weight
Coupling agent, carries out back flow reaction at 120～135 degree, until not having water to generate, both.
Preferably, the preparation method of above-described large scale integrated circuit solvent-free silicone resin, step (2) is described
Acid esters coupling agent be four n-pro-pyl zirconates.
Beneficial effect: compared to the prior art the large scale integrated circuit solvent-free silicone resin that the present invention provides has the advantage that
The large scale integrated circuit solvent-free silicone resin that the present invention provides, is applicable to large-scale integrated electricity by great many of experiments screening
The composition of the solvent-free silicone resin on road and proportioning, each component proportioning preferably gone out is scientific and reasonable, has the wearability, resistance to of excellence
The advantages such as oxidisability, resistant of high or low temperature, radiation resistance, weatherability, insulating properties, hydrophobicity and low surface potential energy.
The large scale integrated circuit preparation method of solvent-free silicone resin that the present invention provides, filters out optimal by great many of experiments
Process conditions, whole technological design is reasonable, in particular by continuous hydrolysis technology, hydrolyzing, wash, be concentrated in a step
Complete, and use efficient catalyst zirconium ester coupling agent, the response time can be greatly reduced, improve production efficiency, save into
This, improve the combination property of product.
Detailed description of the invention
Below in conjunction with specific embodiment, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate the present invention and need not
In limiting the scope of the present invention, after having read the present invention, those skilled in the art repair the various equivalent form of values of the present invention
Change and all fall within the application claims limited range.
Embodiment 1
(1) take dimethyldichlorosilane 50g, methylvinyldichlorosilane 30g, phenyl trichlorosilane 80g and butyl acetate 90g to join
Become mixed liquor, be added dropwise to by 100g10% sodium hydrate aqueous solution, 90g butanone, in the mixed liquor that 300g butyl acetate is made into, about
Within 1 hour, drip off, after dripping off, continue stirring reaction 1 hour；
(2) then dividing and fall down a layer neutral water, then, solids content is surveyed in sampling；Then, the zirconate of solid part 2/1000ths is added
Coupling agent, under 120～135 degree of reflux temperatures, carries out reaction until not having water to generate, sampling.
Embodiment 2
(1) take dimethyldichlorosilane 65g, methylvinyldichlorosilane 30g, phenyl trichlorosilane 70g and butyl acetate 95g to join
Become mixed liquor, be added dropwise to by 110g10% sodium hydrate aqueous solution, 100g butanone, in the mixed liquor that 300g butyl acetate is made into,
Within about 1 hour, drip off, after dripping off, continue stirring reaction 1 hour；
(2) then dividing and fall down a layer neutral water, then, solids content is surveyed in sampling；The zirconate being subsequently adding solid part 3/1000ths is even
Connection agent, carries out back flow reaction at 120～135 degree, until not having water to generate, both, sampling.
Embodiment 3
(1) dimethyldichlorosilane 100g, dichloromethyl vinyl silanes 60g, phenyl trichlorosilane 140g, butyl acetate 180g are taken
It is made into mixed liquor, is added dropwise to by 220g10% sodium hydrate aqueous solution, 200g butanone, in the mixed liquor that 600g butyl acetate is made into,
Within about 1 hour, drip off, after dripping off, continue stirring reaction 1 hour；
(2) then dividing and fall down a layer neutral water, then, solids content is surveyed in sampling；It is subsequently adding the zirconate of solid part 3/1000ths
Coupling agent, under 120～135 degree of reflux temperatures, carries out reaction until not having water to generate, sampling.
Embodiment 4 performance test experience
Take the large scale integrated circuit solvent-free silicone resin that above example 1 to 3 prepares respectively, carry out various performance inspection
Surveying, specific experiment result is as shown in table 1:
The table 1 large scale integrated circuit performance test results of solvent-free silicone resin
More than test result indicate that, the large scale integrated circuit solvent-free silicone resin that the present invention prepares, superior performance, tool
There are resistant of high or low temperature, radiation resistance, weatherability, insulating properties and the low surface potential energy of excellence, can be widely applied to collect on a large scale
Become in circuit.
The above is only the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as the present invention
Protection domain.
Claims (1)
1. the preparation method of a large scale integrated circuit silicones, it is characterised in that comprise the following steps:
(1) dimethyldichlorosilane 50～100 parts, dichloromethyl vinyl silanes 30～60 are taken by weight
Part, phenyl trichlorosilane 70～140 parts and butyl acetate 90～180 parts are made into mixed liquor, instill by concentration 10%
Sodium hydrate aqueous solution 100～120 parts, butanone 90～110 parts and butyl acetate 300～400 parts of reactions being made into
Solvent, drips off for 1 hour, after dripping off, continues stirring reaction 1～2 hour；
(2) dividing and fall down a layer neutral water, solids content is surveyed in sampling；Add solid part 3/2000ths to thousand/1000ths
The zirconium ester coupling agent of weight, carries out back flow reaction at 120～135 degree, until not having water to generate, both；
Zirconium ester coupling agent described in step (2) is four n-pro-pyl zirconates.
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| CN201410065605.9A CN103881096B (en) | 2014-02-26 | 2014-02-26 | Large scale integrated circuit solvent-free silicone resin and preparation method thereof |
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| CN201410065605.9A CN103881096B (en) | 2014-02-26 | 2014-02-26 | Large scale integrated circuit solvent-free silicone resin and preparation method thereof |
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| CN103881096A CN103881096A (en) | 2014-06-25 |
| CN103881096B true CN103881096B (en) | 2016-11-23 |
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| CN115746304B (en) * | 2022-12-07 | 2023-08-04 | 嘉兴联合化学有限公司 | Method for preparing phenyl silicone resin without solvent and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
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