CN104151555A - Preparation method of methyl phenyl vinyl silicone resin - Google Patents
Preparation method of methyl phenyl vinyl silicone resin Download PDFInfo
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- CN104151555A CN104151555A CN201410392116.4A CN201410392116A CN104151555A CN 104151555 A CN104151555 A CN 104151555A CN 201410392116 A CN201410392116 A CN 201410392116A CN 104151555 A CN104151555 A CN 104151555A
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Abstract
The invention relates to a preparation method of methyl phenyl vinyl silicone resin. The invention relates to a silicone resin preparation method. The invention aims at solving problems of low light transmittance, low refractive index, low viscosity and high silicon hydroxyl content of existing silicon resin. The method comprises the following steps: 1, phenyl chlorosilane, dimethyl dichlorosilane and methylvinyl chlorosilane are well mixed; 2, toluene is well mixed with water, and the mixed liquid obtained in the step 1 is dropped into the mixture; a reaction is allowed for 2-8h under a temperature of 40-50 DEG C, such that a reaction liquid is obtained; 3, the reaction liquid obtained in the step 2 is subjected to a reflux reaction, such that a reflux mixed liquid is obtained; and 4, extraction, filtration and reduced-pressure distillation are sequentially carried out, such that methyl phenyl vinyl silicone resin is obtained. The product provided by the invention has a refractive index no lower than 1.50, a light transmittance no lower than 90%, a viscosity no lower than 7000mPa.s, and a silicon hydroxyl content no higher than 1000ppm.
Description
Technical field
The present invention relates to a kind of preparation method of silicone resin.
Background technology
LED is a kind of semi-conductor electricity sub-element solid-state, that inorganic semiconductor produces light source that uses.As light source, the advantage of LED is embodied in three aspects: energy-saving and environmental protection and long lifetime.In LED manufacturing processed, need the electronic devices and components such as chip reasonably to arrange on request, assemble, recycling packaging plastic makes it to isolate with environment.Optical grade epoxy resin has high transmittance, specific refractory power, has applied for many years as the packaged material of LED.In recent years, along with the development of semi-conductor industry, highlighted LED (HBLED) is the main flow of development, and this chip needs driving, the welding temperature of higher electric current also higher.Easily there is Yellowing because epoxy resin encapsulating material is exposed under ultraviolet ray or under hot environment, stable light source output can not be provided under high electric current, be not suitable with LED growth requirement.At present, use and caused enough attention organosilicon as packaged material.As packaged material, organosilyl advantage is the stability of thermodynamics and optics, and this stability is to be determined by the stable connection of Si-O-Si skeleton in polymkeric substance.The joint sealant that meets LED production requirement of being prepared by silicone resin should have high mechanical strength, suitable hardness, high transmittance and specific refractory power.
One of universal method of synthetic silicone resin by hydrolyzing chlorosilane, condensation reaction:
R
1, R
2=methyl, phenyl, vinyl
The silicone resin refractive index of full methyl is 1.41, and the refractive index of the silicone resin that full phenyl replaces is 1.57.According to snell ' s law, by reducing the difference of specific refractory power between LED chip and packaged material, the light that can reduce in LED chip is caught, and then increases light output.Therefore the refractive index of packaged material is higher, and the light output efficiency of LED is larger.But the too high silicone resin transmittance of phenyl content is lower, shows thermoplasticity, is not suitable for use in packaged material.
The conventional chlorosilane that contains phenyl comprises phenyl-trichloro-silicane, diphenyl dichlorosilane, dichloromethyl phenylsilane.Conventional methyl chlorosilane comprises: dimethyldichlorosilane(DMCS), methyl ethylene dichlorosilane.Prepare in the process of silicone resin in hydrolyzing chlorosilane, condensation, because the reactive behavior of various chlorosilanes differs greatly, thereby reaction product composition is complicated.When lower than 60 DEG C of reactions, the silicone resin molecular weight obtaining is lower, and remaining Si-OH content is high.This resin adds the joint sealant making after linking agent, catalyzer, in hot setting process, dehydration condensation occurs, and discharges vaporous water molecule.
Therefore in joint sealant, form bubble, have a strong impact on mechanical strength and transmittance.When higher than 60 DEG C of reactions, the silicone resin molecular weight obtaining is higher, and remaining Si-OH content is lower.But due to excess Temperature, cause being hydrolyzed too fast, the rapid autohemagglutination of silanol of generation or further crosslinked and form gel, prepared silicone resin transmittance is low, can not meet LED production requirement.
Summary of the invention
The present invention is in order to solve the problem that existing silicone resin transmittance is low, refractive index is low, viscosity is low and silicon hydroxy radical content is high, and a kind of preparation method of methyl phenyl vinyl silicone resin is provided.
The preparation method of a kind of methyl phenyl vinyl silicone resin of the present invention carries out according to the following steps:
One, phenyl chlorosilane, dimethyldichlorosilane(DMCS) and methyl ethylene chlorosilane are mixed, obtain chlorosilane mixed solution; Described phenyl chlorosilane and the mol ratio of dimethyldichlorosilane(DMCS) are (80～160): 100; The mol ratio of described phenyl chlorosilane and methyl ethylene chlorosilane is (200～500): 100;
Two, toluene and water are mixed, obtain the mixed solution of toluene and water, then in the mixed solution of toluene and water, drip the chlorosilane mixed solution that step 1 obtains, then be to react 2h～8h under the condition of 40～50 DEG C in temperature, obtain reaction solution; Described chlorosilane mixed solution and the mass ratio of toluene are 1:(4.5～5.5); Described chlorosilane mixed solution and the mass ratio of water are 1:(1.5～2.5);
Three, reaction solution step 2 being obtained is warming up to temperature as 80～90 DEG C by temperature as 40～50 DEG C taking heat-up rate as 0.5 DEG C/min～4 DEG C/min, and is back flow reaction 2h～4h at 80～90 DEG C in temperature, obtains backflow mixed liquor;
Four, the backflow mixed liquor 1. step 3 being obtained is cooled to after room temperature, pours separating funnel into, and stratification discards the water of middle level floss thin layer and lower floor, obtains organic phase A; 2. the organic phase A after is 1. added to distilled water, stir after 8min～12min, then pour separating funnel into, stratification, discards after lower floor's water, obtains organic phase B; Wherein said distilled water equates with the volume of organic phase A; 3., till repeating being operated to organic phase that stratification obtains and being neutrality 2., obtain neutral organic phase; 4. by sand formula funnel filtering and impurity removing for the neutral organic phase after 3.; 5. toluene and small-molecule substance are removed in underpressure distillation, obtain methyl phenyl vinyl silicone resin; Described underpressure distillation parameter is: vacuum tightness is 0.05MPa～1MPa, 25～35 DEG C of fore-running temperature, 120～180 DEG C of dry points.
Beneficial effect of the present invention:
1. the present invention is by the strict ratio of controlling phenyl chlorosilane, dimethyldichlorosilane(DMCS) and methyl ethylene chlorosilane, refractive index >=1.50 of the silicone resin obtaining, transmittance >=90%.
2. the reactive behavior difference of chlorosilane is larger, only 40～50 DEG C of temperature ranges, reactive behavior difference minimum, between various chlorosilane monomers, polymerization forms multipolymer mutually, the silicone resin clear obtaining, now the molecular weight of resin, viscosity are lower.
3. under reflux temperature, molecular weight, the silicone resin that viscosity is lower further complete Si-OH condensation reaction, obtain the silicone resin that molecular weight is higher, viscosity is larger, the viscosity >=7000mPa.s of its resin, silicon hydroxy radical content≤1000ppm.The increase of molecular weight is conducive to the raising of molecular resin cohesive strength, has also reduced Si-OH content in resin, has avoided the generation of bubble in packaging plastic.
4. underpressure distillation goes out toluene and small-molecule substance, obtains the silicone resin that contains methyl, phenyl and vinyl, and outward appearance is almost completely transparent, the viscosity >=7000mPa.s of resin, silicon hydroxy radical content≤1000ppm.
Brief description of the drawings
Fig. 1 is the methyl phenyl vinyl silicone resin infrared spectrogram of test one preparation;
Embodiment
Embodiment one: the preparation method of a kind of methyl phenyl vinyl silicone resin of present embodiment carries out according to the following steps:
One, phenyl chlorosilane, dimethyldichlorosilane(DMCS) and methyl ethylene chlorosilane are mixed, obtain chlorosilane mixed solution; Described phenyl chlorosilane and the mol ratio of dimethyldichlorosilane(DMCS) are (80～160): 100; The mol ratio of described phenyl chlorosilane and methyl ethylene chlorosilane is (200～500): 100;
Two, toluene and water are mixed, obtain the mixed solution of toluene and water, then in the mixed solution of toluene and water, drip the chlorosilane mixed solution that step 1 obtains, then be to react 2h～8h under the condition of 40～50 DEG C in temperature, obtain reaction solution; Described chlorosilane mixed solution and the mass ratio of toluene are 1:(4.5～5.5); Described chlorosilane mixed solution and the mass ratio of water are 1:(1.5～2.5);
Three, reaction solution step 2 being obtained is warming up to temperature as 80～90 DEG C by temperature as 40～50 DEG C taking heat-up rate as 0.5 DEG C/min～4 DEG C/min, and is back flow reaction 2h～4h at 80～90 DEG C in temperature, obtains backflow mixed liquor;
Four, the backflow mixed liquor 1. step 3 being obtained is cooled to after room temperature, pours separating funnel into, and stratification discards the water of middle level floss thin layer and lower floor, obtains organic phase A; 2. the organic phase A after is 1. added to distilled water, stir after 8min～12min, then pour separating funnel into, stratification, discards after lower floor's water, obtains organic phase B; Wherein said distilled water equates with the volume of organic phase A; 3., till repeating being operated to organic phase that stratification obtains and being neutrality 2., obtain neutral organic phase; 4. by sand formula funnel filtering and impurity removing for the neutral organic phase after 3.; 5. toluene and small-molecule substance are removed in underpressure distillation, obtain methyl phenyl vinyl silicone resin; Described underpressure distillation parameter is: vacuum tightness is 0.05MPa～1MPa, 25～35 DEG C of fore-running temperature, 120～180 DEG C of dry points.
Fore-running temperature described in this embodiment step 4 refers to the temperature while distilling out the first drop of liquid, and dry point refers to the temperature while not having liquid to distill out.
1. present embodiment is by the strict ratio of controlling phenyl chlorosilane, dimethyldichlorosilane(DMCS) and methyl ethylene chlorosilane, refractive index >=1.50 of the silicone resin obtaining, transmittance >=90%.
2. the reactive behavior difference of chlorosilane is larger, only 40～50 DEG C of temperature ranges, reactive behavior difference minimum, between various chlorosilane monomers, polymerization forms multipolymer mutually, the silicone resin clear obtaining, now the molecular weight of resin, viscosity are lower.
3. under reflux temperature, molecular weight, the silicone resin that viscosity is lower further complete Si-OH condensation reaction, obtain the silicone resin that molecular weight is higher, viscosity is larger, the viscosity >=7000mPa.s of its resin, silicon hydroxy radical content≤1000ppm.The increase of molecular weight is conducive to the raising of molecular resin cohesive strength, has also reduced Si-OH content in resin, has avoided the generation of bubble in packaging plastic.
4. underpressure distillation goes out toluene and small-molecule substance, obtains the silicone resin that contains methyl, phenyl and vinyl, and outward appearance is almost completely transparent, the viscosity >=7000mPa.s of resin, silicon hydroxy radical content≤1000ppm.
Embodiment two: present embodiment is different from embodiment one: the phenyl chlorosilane described in step 1 is one or both the mixture in phenyl-trichloro-silicane and diphenyl dichlorosilane.Other steps and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: the mol ratio of the phenyl chlorosilane described in step 1 and dimethyldichlorosilane(DMCS) is (100～140): 100.Other steps and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: the mol ratio of the phenyl chlorosilane described in step 1 and dimethyldichlorosilane(DMCS) is 120:100.Other steps and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: the mol ratio of the phenyl chlorosilane described in step 1 and methyl ethylene chlorosilane is (300～400): 100.Other steps and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the mol ratio of the phenyl chlorosilane described in step 1 and methyl ethylene chlorosilane is 350:100.Other steps and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: then drip the chlorosilane mixed solution that step 1 obtains in the mixed solution of toluene and water in step 2, under temperature is the condition of 45 DEG C, react 4h～5h again, obtain reaction solution.Other steps and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: the mass ratio of the chlorosilane mixed solution described in step 2 and toluene is 1:(4.2～5.2).Other steps and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: the mass ratio of the chlorosilane mixed solution described in step 2 and toluene is 1:5.Other steps and parameter are identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: the mass ratio of the chlorosilane mixed solution described in step 2 and water is 1:(1.2～2.2).Other steps and parameter are identical with one of embodiment one to nine.
Embodiment 11: present embodiment is different from one of embodiment one to ten: the mass ratio of the chlorosilane mixed solution described in step 2 and water is 1:2.Other steps and parameter are identical with one of embodiment one to ten.
Embodiment 12: present embodiment is different from one of embodiment one to 11: the reaction solution in step 3, step 2 being obtained is warming up to temperature as 84 DEG C by temperature as 45 DEG C taking heat-up rate as 2 DEG C/min, and be back flow reaction 2h at 84 DEG C in temperature, obtain backflow mixed liquor.Other steps and parameter are identical with one of embodiment one to 11.
Embodiment 13: present embodiment is different from one of embodiment one to 12: step 4 5. described in underpressure distillation parameter be: vacuum tightness is 0.08MPa, 30 DEG C of fore-running temperature, 150 DEG C of dry points.Other steps and parameter are identical with one of embodiment one to 12.
With following verification experimental verification beneficial effect of the present invention:
The preparation method of a kind of methyl phenyl vinyl silicone resin of test one, this test carries out according to the following steps:
One, 0.25mol phenyl-trichloro-silicane, 0.22mol dimethyldichlorosilane(DMCS) and 0.14mol methyl ethylene chlorosilane are mixed, obtain chlorosilane mixed solution;
Two, 500g toluene and 200g water are mixed, obtain the mixed solution of toluene and water, then in the mixed solution of toluene and water, drip the chlorosilane mixed solution that 100g step 1 obtains, then be to react 4h under the condition of 45 DEG C in temperature, obtain reaction solution;
Three, reaction solution step 2 being obtained is warming up to temperature as 84 DEG C by temperature as 45 DEG C taking heat-up rate as 2 DEG C/min, and is back flow reaction 2h at 84 DEG C in temperature, obtains backflow mixed liquor;
Four, the backflow mixed liquor 1. step 3 being obtained is cooled to after room temperature, pours separating funnel into, and stratification discards the water of middle level floss thin layer and lower floor, obtains organic phase; 2. the organic phase after is 1. added to 800g distilled water, stir after 10min, then pour separating funnel into, stratification, discards after lower floor's water, obtains organic phase; Wherein said distilled water equates with the volume of organic phase; 3., till repeating organic phase that operation 2. obtains to stratification for 5 times and being neutrality, obtain neutral organic phase; 4. by sand formula funnel filtering and impurity removing for the neutral organic phase after 3.; 5. toluene and small-molecule substance are removed in underpressure distillation, obtain methyl phenyl vinyl silicone resin.
The underpressure distillation parameter of step 4 described in is 5.: vacuum tightness is 0.08Mpa, 30 DEG C of fore-running temperature, 150 DEG C of dry points.
(1) adopt the VECTOR-22 of BRUKER company type infrared spectrometer to detect testing a methyl phenyl vinyl silicone resin obtaining, obtain infrared spectrogram as shown in Figure 1, as can be seen from the figure 1260cm
-1place is symmetrical Si-CH
3formation vibration charateristic avsorption band; 2960cm
-1place is symmetrical CH
3stretching vibration peak; 1593cm
-1place is vinyl absorption vibration peak; 1429cm
-1place is the characteristic peak of phenyl silica chain link; 1078-1127cm
-1wide and the strong absorption band at place is the antisymmetric stretching vibration of Si-O-Si, and this is the charateristic avsorption band of silicone resin.
Conclusion: determine that by infrared spectra IR synthetic resin is the silicone resin that contains methyl, phenyl and vinyl.
(2) resin viscosity is measured:
Bioassay standard: GB/T 22314-2008 " adopts plastic hoop epoxy resins viscosity measurement method ", and determining instrument is NDJ-97 type Rotary Viscosimeter.
(3) silicon hydroxy radical content is measured:
1. according to
principle will generate water after silicone resin polycondensation;
2. Water content determination: bioassay standard is GB/T 11146-2009 detecting crude oil water content karl Fischer coulometric titration, measures water-content, the then anti-silicon hydroxy radical content of releasing.
(4) transmittance testing method: bioassay standard is GB/T 2410-2008 " mensuration of transparent plastics transmittance and mist degree ", testing tool UVmini-1240 type spectrophotometer.
(5) refractive index testing method: bioassay standard is GB/T 614-2006 " chemical reagent index determination universal method ", testing tool DR-M4/1550 Abbe refractometer.
Conclusion: test in sum a methyl phenyl vinyl silicone resin outward appearance obtaining almost completely transparent, the viscosity 8000mPa.s of resin, silicon hydroxy radical content 550ppm, transmittance 97%, refractive index 1.50.
Claims (9)
1. a preparation method for methyl phenyl vinyl silicone resin, is characterized in that a kind of preparation method of methyl phenyl vinyl silicone resin carries out according to the following steps:
One, phenyl chlorosilane, dimethyldichlorosilane(DMCS) and methyl ethylene chlorosilane are mixed, obtain chlorosilane mixed solution; Described phenyl chlorosilane and the mol ratio of dimethyldichlorosilane(DMCS) are (80～160): 100; The mol ratio of described phenyl chlorosilane and methyl ethylene chlorosilane is (200～500): 100;
Two, toluene and water are mixed, obtain the mixed solution of toluene and water, then in the mixed solution of toluene and water, drip the chlorosilane mixed solution that step 1 obtains, then be to react 2h～8h under the condition of 40～50 DEG C in temperature, obtain reaction solution; Described chlorosilane mixed solution and the mass ratio of toluene are 1:(4.5～5.5); Described chlorosilane mixed solution and the mass ratio of water are 1:(1.5～2.5);
Three, reaction solution step 2 being obtained is warming up to temperature as 80～90 DEG C by temperature as 40～50 DEG C taking heat-up rate as 0.5 DEG C/min～4 DEG C/min, and is back flow reaction 2h～4h at 80～90 DEG C in temperature, obtains backflow mixed liquor;
Four, the backflow mixed liquor 1. step 3 being obtained is cooled to after room temperature, pours separating funnel into, and stratification discards the water of middle level floss thin layer and lower floor, obtains organic phase A; 2. the organic phase A after is 1. added to distilled water, stir after 8min～12min, then pour separating funnel into, stratification, discards after lower floor's water, obtains organic phase B; Wherein said distilled water equates with the volume of organic phase A; 3., till repeating being operated to organic phase that stratification obtains and being neutrality 2., obtain neutral organic phase; 4. by sand formula funnel filtering and impurity removing for the neutral organic phase after 3.; 5. toluene and small-molecule substance are removed in underpressure distillation, obtain methyl phenyl vinyl silicone resin; Described underpressure distillation parameter is: vacuum tightness is 0.05MPa～1MPa, 25～35 DEG C of fore-running temperature, 120～180 DEG C of dry points.
2. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 1, is characterized in that the phenyl chlorosilane described in step 1 is one or both the mixture in phenyl-trichloro-silicane and diphenyl dichlorosilane.
3. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 1 and 2, the mol ratio that it is characterized in that the phenyl chlorosilane described in step 1 and dimethyldichlorosilane(DMCS) is (100～140): 100, and the mol ratio of the phenyl chlorosilane described in step 1 and methyl ethylene chlorosilane is (300～400): 100.
4. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, the mol ratio that it is characterized in that the phenyl chlorosilane described in step 1 and dimethyldichlorosilane(DMCS) is 120:100, and the mol ratio of the phenyl chlorosilane described in step 1 and methyl ethylene chlorosilane is 350:100.
5. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, it is characterized in that then in the mixed solution of toluene and water, dripping the chlorosilane mixed solution that step 1 obtains in step 2, under temperature is the condition of 45 DEG C, react 4h～5h again, obtain reaction solution.
6. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, the mass ratio that it is characterized in that the chlorosilane mixed solution described in step 2 and toluene is 1:(4.2～5.2), the mass ratio of the chlorosilane mixed solution described in step 2 and water is 1:(1.2～2.2).
7. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, the mass ratio that it is characterized in that the chlorosilane mixed solution described in step 2 and toluene is 1:5, and the mass ratio of the chlorosilane mixed solution described in step 2 and water is 1:2.
8. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, it is characterized in that the reaction solution that in step 3, step 2 obtained is warming up to temperature as 84 DEG C by temperature as 45 DEG C taking heat-up rate as 2 DEG C/min, and be back flow reaction 2h at 84 DEG C in temperature, obtain backflow mixed liquor.
9. the preparation method of a kind of methyl phenyl vinyl silicone resin according to claim 3, is characterized in that described in step 4 5. that underpressure distillation parameter is: vacuum tightness is 0.08MPa, 30 DEG C of fore-running temperature, 150 DEG C of dry points.
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| US10815339B2 (en) | 2016-04-26 | 2020-10-27 | Guangdong Biomax Si&F New Material Co., Ltd. | Method for preparing organopolysiloxane resins |
| CN112708137A (en) * | 2020-08-24 | 2021-04-27 | 惠州市永卓科技有限公司 | Preparation method of low-hydroxyl-content MDT silicone oil with end capped by dimethylvinylsiloxy group |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10815339B2 (en) | 2016-04-26 | 2020-10-27 | Guangdong Biomax Si&F New Material Co., Ltd. | Method for preparing organopolysiloxane resins |
| CN109233712A (en) * | 2018-08-08 | 2019-01-18 | 无锡帝科电子材料股份有限公司 | A kind of semiconductor packages glue and preparation process |
| CN112708137A (en) * | 2020-08-24 | 2021-04-27 | 惠州市永卓科技有限公司 | Preparation method of low-hydroxyl-content MDT silicone oil with end capped by dimethylvinylsiloxy group |
| CN112708137B (en) * | 2020-08-24 | 2022-04-01 | 惠州市永卓科技有限公司 | Preparation method of low-hydroxyl-content MDT silicone oil with end capped by dimethylvinylsiloxy group |
| CN115353857A (en) * | 2022-07-11 | 2022-11-18 | 武汉飞恩微电子有限公司 | Packaging medium for pressure sensor chip and preparation method thereof |
| CN115353857B (en) * | 2022-07-11 | 2023-06-27 | 武汉飞恩微电子有限公司 | Packaging medium for pressure sensor chip and preparation method thereof |
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