CN103408759A - Preparation method of methyl phenyl silicone oil with high refractive index - Google Patents
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Abstract
The invention relates to a preparation method of methyl phenyl silicone oil with high refractive index, and belongs to the technical field of organosilicon synthesis. The method is as below: using dimethyl dichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane as polymerization monomers; adding the monomers into a solvent while stirring at 30 DEG C; uniformly stirring; dropwise adding a proper amount of a hydrolysate; continuing to react until the end of hydrolysis; standing for layering; separating out a lower layer of acid water; washing an upper layer organic phase to a neutral state to obtain a siloxane prepolymer; adding a proper amount of an end-capping reagent and a condensation catalyst into the siloxane prepolymer to carry out a condensation reaction; after the reaction, washing out the catalyst to a neutral state; and steaming out the solvent of xylene and low-boiling-point substances under reduced pressure to obtain the silicone oil. The methyl phenyl silicone oil prepared by the invention is a clarified transparent oily liquid with high refractive index, good product uniformity, high purity and good high temperature resistance; and the preparation technology is simple and easy for industrialization.
Description
Technical field:
The present invention relates to the preparation method of silicone oil, specifically refer to a kind of preparation method of high refractive index methyl phenyl silicone oil.
Background technology:
Methyl phenyl silicone oil is one of main products of silicone oil, owing to having introduced phenyl group, methyl phenyl silicone oil has good thermotolerance, chemical stability, electrical insulating property, radiation resistance etc., make methyl phenyl silicone oil be widely used in a lot of fields, especially in personal care, national defense industry, aerospace, be the wide product of development prospect.The 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, more about the preparation method of methyl phenyl silicone oil, mainly by hydrolytic condensation method and two kinds of method preparations of catalytic equilibration method.For example, patent CN 102070785A has announced and a kind ofly take dichloromethyl phenylsilane hydrolyzate, Dimethyldichlorosilane hydrolysate, methyl phenyl ring siloxane and prepare the method for hydroxyl-terminated polymethylphenyl sioxane as raw material; Patent CN 101851333A has announced a kind ofly take methyl phenyl ring siloxane, dimethyl cyclosiloxane, methylhydracyclosiloxane and is raw material, and rare earth super acid prepares methyl and phenyl hydrogen-containing silicon oil for catalyzer.Aforesaid method mainly be take cyclosiloxane as raw material prepares methyl phenyl silicone oil, has increased cost prepared by product, is not conducive to suitability for industrialized production, and the above-mentioned monomer of take simultaneously can not prepare the methyl phenyl silicone oil of high phenyl content as raw material.And patent CN 102516546A has announced and a kind ofly take dichloromethyl phenylsilane and be raw material, the weak organic bases aqueous solution is that neutralizing agent prepares low viscosity aminomethyl phenyl hydroxy silicon oil, although the method raw material is inexpensive, added a large amount of weak organic basess, increased the cost of suitability for industrialized production.
Take dimethyldichlorosilane(DMCS), dichloromethyl phenylsilane and diphenyl dichlorosilane is raw material, introducing by dichloromethyl phenylsilane can increase the mutual solubility with other monomers, thereby prepare homogeneity product preferably, simultaneously can prepare by the ratio of raw material the silicone oil of different phenyl contents, the method raw material is simple, the industrialization cost is low, is to prepare relatively effective means of methyl phenyl silicone oil.
Summary of the invention:
The present invention proposes a kind of preparation method of high refractive index methyl phenyl silicone oil, 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; Prepared product clear, specific refractory power is high, good uniformity, purity is high, and high thermal resistance is good.
The present invention is achieved by following technical proposals:
A kind of preparation method of high refractive index methyl phenyl silicone oil is characterized in that carrying out in the steps below:
(1) in the there-necked flask with stirring, backflow, Dropping feeder, add 2.58～10.32 g dimethyldichlorosilane(DMCS)s, 19.11g dichloromethyl phenylsilane, 5.06～20.26 g diphenyl dichlorosilanes by every 80 mL dimethylbenzene, 50 mL acetone, be uniformly mixed under 30 ℃; The volume ratio that configuration is comprised of acetone and distilled water is the mixed hydrolysis liquid of 100:57.6, stir, with constant voltage titration funnel, dropwise drip in there-necked flask, dripping quantity is: drip 157.6 mL mixed hydrolysis liquid by above-mentioned every 80 mL dimethylbenzene, control rate of addition and keep 1d/2s, after dropwising, continue reaction 5 ~ 30 h under 30 ℃, hydrolysis finishes;
(2) stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with the distilled water of 50～60 ℃, obtain the silane prepolymer, then under 80～120 ℃, add a certain amount of end-capping reagent and condensation catalyst to carry out condensation reaction 2～10 h, after reaction finishes, wash away catalyzer to neutral with the distilled water of 50～60 ℃, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the 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.
Wherein the optimum reacting time of the described hydrolysis reaction of step (1) is 10 h.
Wherein the end-capping reagent described in step (2) is hexamethyldisiloxane, and add-on is: add end-capping reagent 0.40 g～3.24 g by the every 80 mL dimethylbenzene in step (1).
Wherein the condensation catalyst described in step (2) is stannous octoate, condensation catalyst add-on: add catalyzer 0.0395 g～0.7893 g by the every 80 mL dimethylbenzene in step (1), wherein preferably add catalyzer 0.3947 g by the every 80 mL dimethylbenzene in step (1).
Wherein the optimal reaction temperature of the described catalyzer condensation reaction of step (2) is 100 ℃, and best condensation reaction time is 4 h.
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 by direct method production, 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 for preparing of the present invention, the mol ratio (Ph/R) of phenyl and organic group is 35% ~ 65%, can control by the ratio of regulating monomer the content of phenyl.
3. to adopt stannous octoate be condensation catalyst in the present invention, and consumption is few, and catalytic activity is high, and the condensation of catalyze siloxane prepolymer prepares methyl phenyl silicone oil effectively.
4. the silicone oil clear that synthesizes of the present invention, 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, the product excellent storage stability.
The accompanying drawing explanation
Fig. 1 is that Ph/R ratio is 0.55 o'clock prepared methyl phenyl silicone oil infrared spectrogram.
Fig. 2 is that Ph/R ratio is 0.55 o'clock prepared methyl phenyl silicone oil gpc chromatogram.
Embodiment:
Be below preferred embodiment of the present invention, can understand better the present invention, but embodiments of the invention be not limited to this, shown in it, data do not represent the restriction to characteristic range of the present invention simultaneously.
Ph/R ratio (mol ratio) is 0.35.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 10.32 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 5.06 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3450 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ 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 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, 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 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 2.58 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 20.26 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811g hexamethyldisiloxane and 0.4195 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ 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 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 5 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 30 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the faint yellow methyl phenyl silicone oil product of clear.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.40 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear high viscosity methyl phenyl silicone oil product.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 3.24 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 2 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ 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 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 10 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clarifying faint yellow transparent methyl phenyl silicone oil product.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 80 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clear methyl phenyl silicone oil product.
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 120 ℃, add 0.811 g hexamethyldisiloxane and 0.3947 g condensation catalyst stannous octoate (quality is monomer total mass 1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain clarifying faint yellow transparent methyl phenyl silicone oil product.
Embodiment 12
Ph/R ratio (mol ratio) is 0.55.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.0395 g condensation catalyst stannous octoate (quality is monomer total mass 0.1 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ 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 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 5.16 g dimethyldichlorosilane(DMCS)s, 19.11 g dichloromethyl phenylsilanes, 15.19 g diphenyl dichlorosilanes, be uniformly mixed under 30 ℃; With constant voltage titration funnel, dropwise drip 100 mL acetone and 57.6 g distilled water mixed hydrolysis liquid in there-necked flask, control rate of addition and keep 1d/2s, total titration time is 3 h left and right, after dropwising, continues reaction 10 h under 30 ℃, and hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with 50～60 ℃ of distilled water, obtain siloxane prepolymer, then under 100 ℃, add 0.811 g hexamethyldisiloxane and 0.7893 g condensation catalyst stannous octoate (quality is monomer total mass 2 %) to carry out condensation reaction 4 h, after reaction finishes, with 50～60 ℃ of distilled water, wash away catalyzer to neutral, then under 130 ℃ 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. the preparation method of a high refractive index methyl phenyl silicone oil, carry out according to following step:
In the there-necked flask with stirring, backflow, Dropping feeder, add 2.58～10.32 g dimethyldichlorosilane(DMCS)s, 19.11g dichloromethyl phenylsilane, 5.06～20.26 g diphenyl dichlorosilanes by every 80 mL dimethylbenzene, 50 mL acetone, be uniformly mixed under 30 ℃; The volume ratio that configuration is comprised of acetone and distilled water is the mixed hydrolysis liquid of 100:57.6, stir, with constant voltage titration funnel, dropwise drip in there-necked flask, dripping quantity is: drip 157.6 mL mixed hydrolysis liquid by above-mentioned every 80 mL dimethylbenzene, control rate of addition and keep 1d/2s, after dropwising, continue reaction 5 ~ 30 h under 30 ℃, hydrolysis finishes; Stratification, separate lower floor's sour water, the upper strata hydrolyzate is washed till neutrality with the distilled water of 50～60 ℃, obtain the silane prepolymer, then under 80～120 ℃, add a certain amount of end-capping reagent and condensation catalyst to carry out condensation reaction 2～10 h, after reaction finishes, wash away catalyzer to neutral with the distilled water of 50～60 ℃, then under 130 ℃ of reduced pressure, steam solvent xylene and low-boiling-point substance, obtain the silicone oil product.
2. the preparation method of a kind of high refractive index methyl phenyl silicone oil according to claim 1 is characterized in that: wherein in step (1), 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 high refractive index methyl phenyl silicone oil according to claim 1, it is characterized in that: wherein the reaction times of the described hydrolysis reaction of step (1) is 10 h.
4. the preparation method of a kind of high refractive index methyl phenyl silicone oil according to claim 1, it is characterized in that: wherein the end-capping reagent described in step (2) is hexamethyldisiloxane, and add-on is: add end-capping reagent 0.40 g～3.24 g by the every 80 mL dimethylbenzene in step (1).
5. the preparation method of a kind of high refractive index methyl phenyl silicone oil according to claim 1, it is characterized in that: wherein the condensation catalyst described in step (2) is stannous octoate, the condensation catalyst add-on: add catalyzer 0.0395 g～0.7893 g by the every 80 mL dimethylbenzene in step (1).
6. the preparation method of a kind of high refractive index methyl phenyl silicone oil according to claim 1, it is characterized in that: wherein the condensation catalyst add-on is for to add catalyzer 0.3947 g by the every 80 mL dimethylbenzene in step (1).
7. the preparation method of a kind of high refractive index methyl phenyl silicone oil according to claim 1, it is characterized in that: wherein the optimal reaction temperature of the described catalyzer condensation reaction of step (2) is 100 ℃, and best condensation reaction time is 4 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329475A (en) * | 2018-01-30 | 2018-07-27 | 广东省石油与精细化工研究院 | A kind of 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 |
| CN110669221A (en) * | 2019-10-31 | 2020-01-10 | 周民主 | Hydrolysis method of high-boiling silicone oil |
| CN111978544A (en) * | 2020-09-07 | 2020-11-24 | 江西星火狮达科技有限公司 | Methyl phenyl high-boiling silicone oil and preparation method thereof |
| CN115612104A (en) * | 2022-11-08 | 2023-01-17 | 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 |
-
2013
- 2013-08-13 CN CN201310351131.XA patent/CN103408759B/en not_active Expired - Fee Related
Patent 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 |
Non-Patent Citations (1)
| Title |
|---|
| 律微波 等: "国内苯基硅油产品现状和应用", 《有机硅材料》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329475A (en) * | 2018-01-30 | 2018-07-27 | 广东省石油与精细化工研究院 | A kind of 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 |
| CN110669221A (en) * | 2019-10-31 | 2020-01-10 | 周民主 | Hydrolysis method of high-boiling silicone oil |
| CN111978544A (en) * | 2020-09-07 | 2020-11-24 | 江西星火狮达科技有限公司 | Methyl phenyl high-boiling silicone oil and preparation method thereof |
| 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 |
| CN115612104A (en) * | 2022-11-08 | 2023-01-17 | 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 |
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