CN103408759B - A kind of preparation method of methyl phenyl silicone oil with high refractive index - Google Patents
A kind of preparation method of methyl phenyl silicone oil with high refractive index Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of methyl phenyl silicone oil with high refractive index, belong to organosilicon synthesis technical field.The method is for polymerization single polymerization monomer with dimethyldichlorosilane(DMCS), diphenyl dichlorosilane and dichloromethyl phenylsilane, under stirring at 30 DEG C, monomer is joined in solvent, stirring, then drip a certain amount of hydrolyzed solution wherein, dropwising rear continuation reaction to being hydrolyzed end.Stratification, separate lower floor's sour water, upper organic phase is washed to neutrality, obtain siloxane prepolymer, add a certain amount of end-capping reagent wherein and condensation catalyst carries out condensation reaction, after reaction terminates, wash away catalyzer to neutral, then steam solvent xylene and low-boiling-point substance at reduced pressure conditions, obtain silicone oil product.Methyl phenyl silicone oil prepared by the present invention is clear oily liquids, and specific refractory power is high, product good uniformity, and purity is high, and high thermal resistance is good, and preparation technology is simple, is easy to industrialization.
Description
technical field:
The present invention relates to the preparation method of silicone oil, specifically refer to a kind of preparation method of methyl phenyl silicone oil with high refractive index.
background technology:
Methyl phenyl silicone oil is one of main products of silicone oil, owing to introducing phenyl group, methyl phenyl silicone oil has good thermotolerance, chemical stability, electrical insulating property, radiation resistance etc., methyl phenyl silicone oil is widely used in a lot of field, especially in personal care, national defense industry, aerospace, be the wide product of development prospect.Methyl phenyl silicone oil demand rises year by year, the research of its new variety, novel process is become to the focus of organosilicon industry.
At present, the preparation method about methyl phenyl silicone oil is more, primarily of hydrolytic condensation method and the two kinds of method preparations of catalytic equilibration method.Such as, patent CN102070785A discloses and a kind ofly prepares the method for hydroxyl-terminated polymethylphenyl sioxane with dichloromethyl phenylsilane hydrolyzate, Dimethyldichlorosilane hydrolysate, methyl phenyl ring siloxane for raw material; Patent CN101851333A discloses one with methyl phenyl ring siloxane, dimethicone, methylhydracyclosiloxane for raw material, and rare earth super acid is catalyst preparing methyl and phenyl hydrogen-containing silicon oil.Aforesaid method is mainly that methyl phenyl silicone oil prepared by raw material with cyclosiloxane, adds cost prepared by product, is not conducive to suitability for industrialized production, simultaneously with above-mentioned monomer for raw material can not prepare the methyl phenyl silicone oil of high phenyl content.And patent CN102516546A to disclose a kind of be raw material with dichloromethyl phenylsilane, the weak organic bases aqueous solution is that low viscosity aminomethyl phenyl hydroxy silicon oil prepared by neutralizing agent, although the method raw material is inexpensive, add a large amount of weak organic bases, add the cost of suitability for industrialized production.
With dimethyldichlorosilane(DMCS), dichloromethyl phenylsilane and diphenyl dichlorosilane for raw material, the mutual solubility with other monomers can be increased by the introducing of dichloromethyl phenylsilane, thus prepare the good product of homogeneity, the silicone oil of different phenyl content can be prepared by the ratio of raw material simultaneously, the method raw material is simple, industrialization cost is low, is prepare methyl phenyl silicone oil to compare effective means.
summary of the invention:
The present invention proposes a kind of preparation method of methyl phenyl silicone oil with high refractive index, the method technique is simple, reaction conditions is gentle, raw material is easy to get, cost is low, be easy to suitability for industrialized production; Obtained product clear, specific refractory power is high, good uniformity, and purity is high, and high thermal resistance is good.
The present invention is achieved by following technical proposals:
A preparation method for methyl phenyl silicone oil with high refractive index, is characterized in that carrying out in the steps below:
(1) in the there-necked flask with stirring, backflow, Dropping feeder, add 2.58 ~ 10.32g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 5.06 ~ 20.26g diphenyl dichlorosilane by every 80mL dimethylbenzene, 50mL acetone, be uniformly mixed at 30 DEG C; Configure the mixed hydrolysis liquid that the volume ratio be made up of acetone and distilled water is 100:57.6, stir, dropwise drip in there-necked flask with constant voltage titration funnel, dripping quantity is: drip 157.6mL mixed hydrolysis liquid by above-mentioned every 80mL dimethylbenzene, control rate of addition and keep 1d/2s, at 30 DEG C, continue reaction 5 ~ 30h after dropwising, hydrolysis terminates;
(2) stratification, separate lower floor's sour water, the hydrolyzate distilled water of 50 ~ 60 DEG C in upper strata is washed till neutrality, obtain silane prepolymer, then at 80 ~ 120 DEG C, add a certain amount of end-capping reagent and condensation catalyst carries out condensation reaction 2 ~ 10h, after reaction terminates, wash away catalyzer to neutrality with the distilled water of 50 ~ 60 DEG C, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain silicone oil product.
Wherein in step (1), the mass ratio of dimethyldichlorosilane(DMCS), dichloromethyl phenylsilane and diphenyl dichlorosilane is preferably 5.16:19.11:15.19.
The optimum reacting time of the hydrolysis reaction wherein described in step (1) is 10h.
Wherein the end-capping reagent described in step (2) is hexamethyldisiloxane, and add-on is: add end-capping reagent 0.40g ~ 3.24g by the every 80mL dimethylbenzene in step (1).
Wherein the condensation catalyst described in step (2) is stannous octoate, condensation catalyst add-on: add catalyzer 0.0395g ~ 0.7893g by the every 80mL dimethylbenzene in step (1), wherein preferably adds catalyzer 0.3947g by the every 80mL dimethylbenzene in step (1).
The optimal reaction temperature of the catalyzer condensation reaction wherein described in step (2) is 100 DEG C, and best condensation reaction time is 4h.
The invention has the advantages that:
1. the present invention proposes a kind of method that direct hydrolysis chlorosilane monomer prepares silicone oil, raw material is simple, can be produced by direct method, output is large, cost is low, be easy to get, make methyl phenyl silicone oil be more prone to suitability for industrialized production, technique is simple simultaneously, reaction conditions is gentle, easy handling.
2. in the methyl phenyl silicone oil prepared of the present invention, the mol ratio (Ph/R) of phenyl and organic group is 35% ~ 65%, can by the content regulating the ratio of monomer control phenyl.
3. the present invention adopts stannous octoate to be condensation catalyst, and consumption is few, and catalytic activity is high, effectively the condensation of catalyze siloxane prepolymer can prepare methyl phenyl silicone oil.
4. the silicone oil clear of the present invention's synthesis, specific refractory power high (1.51 ~ 1.56), good uniformity, molecular weight distribution is little, and purity is high, and high thermal resistance is good, product excellent storage stability.
Accompanying drawing explanation
Methyl phenyl silicone oil infrared spectrogram prepared when being 0.55 that Fig. 1 is Ph/R ratio.
Fig. 2 is Ph/R ratio methyl phenyl silicone oil gpc chromatogram prepared when being 0.55.
embodiment:
Be below preferred embodiment of the present invention, can understand the present invention better, but embodiments of the invention be not limited thereto, shown in it, data do not represent the restriction to characteristic range of the present invention simultaneously.
Embodiment 1
Ph/R ratio (mol ratio) is 0.35.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 10.32g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 5.06g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3450g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Embodiment 2
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, solvent xylene and low-boiling-point substance is steamed, obtain clear methyl phenyl silicone oil product, refractive index is 1.5521.Its infrared spectra is shown in Fig. 1; Gpc chromatogram is shown in Fig. 2.
Embodiment 3
Ph/R ratio (mol ratio) is 0.65.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 2.58g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 20.26g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.4195g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clarifying translucent methyl phenyl silicone oil product.
Embodiment 4
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 5h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Embodiment 5
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 30h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the faint yellow methyl phenyl silicone oil product of clear.
Embodiment 6
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.40g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear high viscosity methyl phenyl silicone oil product.
Embodiment 7
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, add 3.24g hexamethyldisiloxane and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, wash away catalyzer to neutrality with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Embodiment 8
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 2h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Embodiment 9
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 10h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the transparent methyl phenyl silicone oil product of clear light yellow.
Embodiment 10
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 80 DEG C, add 0.811g hexamethyldisiloxane and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, wash away catalyzer to neutrality with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Embodiment 11
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 120 DEG C, 0.811g hexamethyldisiloxane is added and 0.3947g condensation catalyst stannous octoate (quality is monomer total mass 1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the transparent methyl phenyl silicone oil product of clear light yellow.
Embodiment 12
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.0395g condensation catalyst stannous octoate (quality is monomer total mass 0.1%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear low viscosity methyl phenyl silicone oil product.
Embodiment 13
Ph/R ratio (mol ratio) is 0.55.In 500mL there-necked flask, add 80mL dimethylbenzene, 50mL acetone and 5.16g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 15.19g diphenyl dichlorosilane, be uniformly mixed at 30 DEG C; In there-necked flask, dropwise drip 100mL acetone and 57.6g distilled water mixed hydrolysis liquid with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3h, and at 30 DEG C, continue reaction 10h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, hydrolyzate 50 ~ 60 DEG C of distilled water in upper strata are washed till neutrality, obtain siloxane prepolymer, then at 100 DEG C, 0.811g hexamethyldisiloxane is added and 0.7893g condensation catalyst stannous octoate (quality is monomer total mass 2%) carries out condensation reaction 4h, after reaction terminates, catalyzer is washed away to neutral with 50 ~ 60 DEG C of distilled water, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the faint yellow methyl phenyl silicone oil product of clear high viscosity.
Claims (7)
1. a preparation method for methyl phenyl silicone oil with high refractive index, carries out according to following step:
In the there-necked flask with stirring, backflow, Dropping feeder, add 2.58 ~ 10.32g dimethyldichlorosilane(DMCS), 19.11g dichloromethyl phenylsilane, 5.06 ~ 20.26g diphenyl dichlorosilane by every 80mL dimethylbenzene, 50mL acetone, be uniformly mixed at 30 DEG C; Configure the mixed hydrolysis liquid that the volume ratio be made up of acetone and distilled water is 100:57.6, stir, dropwise drip in there-necked flask with constant voltage titration funnel, dripping quantity is: drip 157.6mL mixed hydrolysis liquid by above-mentioned every 80mL dimethylbenzene, control rate of addition and keep 1d/2s, at 30 DEG C, continue reaction 5 ~ 30h after dropwising, hydrolysis terminates; Stratification, separate lower floor's sour water, the hydrolyzate distilled water of 50 ~ 60 DEG C in upper strata is washed till neutrality, obtain silane prepolymer, then at 80 ~ 120 DEG C, add a certain amount of end-capping reagent and condensation catalyst carries out condensation reaction 2 ~ 10h, after reaction terminates, wash away catalyzer to neutrality with the distilled water of 50 ~ 60 DEG C, then under 130 DEG C of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain silicone oil product.
2. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: wherein the mass ratio of dimethyldichlorosilane(DMCS), dichloromethyl phenylsilane and diphenyl dichlorosilane is 5.16:19.11:15.19.
3. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: the reaction times of wherein said hydrolysis reaction is 10h.
4. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: wherein said end-capping reagent is hexamethyldisiloxane, and add-on is: add end-capping reagent 0.40g ~ 3.24g by every 80mL dimethylbenzene.
5. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: wherein said condensation catalyst is stannous octoate, condensation catalyst add-on: add catalyzer 0.0395g ~ 0.7893g by every 80mL dimethylbenzene.
6. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: wherein condensation catalyst add-on is for add catalyzer 0.3947g by every 80mL dimethylbenzene.
7. the preparation method of a kind of methyl phenyl silicone oil with high refractive index according to claim 1, is characterized in that: the optimal reaction temperature of wherein said catalyzer condensation reaction is 100 DEG C, and best condensation reaction time is 4h.
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| CN108329475B (en) * | 2018-01-30 | 2020-10-16 | 广东省石油与精细化工研究院 | Synthetic method of methyl phenyl silicone oil |
| CN110358089A (en) * | 2018-04-11 | 2019-10-22 | 苏州润特新材料科技有限公司 | A kind of preparation method of alkylaryl modified silicon oil |
| CN110669221B (en) * | 2019-10-31 | 2021-11-30 | 河北科盛瑞化工有限公司 | Hydrolysis method of high-boiling silicone oil |
| CN111978544B (en) * | 2020-09-07 | 2022-05-20 | 江西星火狮达科技有限公司 | Methyl phenyl high-boiling silicone oil and preparation method thereof |
| CN115612104B (en) * | 2022-11-08 | 2023-04-28 | 广州盛泰诺新材料科技有限公司 | Production process of electronic grade 107 with low ring body content |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508776B (en) * | 2009-03-13 | 2011-04-20 | 杭州师范大学 | Method of preparing methyl phenyl polysiloxane |
| CN103087320A (en) * | 2013-01-06 | 2013-05-08 | 溧阳巨神科技材料有限公司 | Preparation method of hydroxyl-terminated polymethylphenyl silicone oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101508776B (en) * | 2009-03-13 | 2011-04-20 | 杭州师范大学 | Method of preparing methyl phenyl polysiloxane |
| CN103087320A (en) * | 2013-01-06 | 2013-05-08 | 溧阳巨神科技材料有限公司 | Preparation method of hydroxyl-terminated polymethylphenyl silicone oil |
Non-Patent Citations (1)
| Title |
|---|
| 国内苯基硅油产品现状和应用;律微波 等;《有机硅材料》;20091125;第23卷(第6期);第402-405页 * |
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