CN103304818B - A kind of preparation method of methyl phenyl silicone oil - Google Patents
A kind of preparation method of methyl phenyl silicone oil Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of methyl phenyl silicone oil, belong to organosilicon synthesis technical field.The method a certain proportion of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane monomer is joined in the mixed solvent of dimethylbenzene and acetone to mix, solution is against the current adopted to drip the mixed hydrolysis liquid of acetone and water wherein, a certain amount of end-capping reagent is added after dropwising, at 30 DEG C, continue reaction for some time, hydrolysis terminates.Stratification, separate lower floor's sour water, upper strata hydrolyzate hot distilled water is washed till neutrality, obtain siloxane prepolymer, adding a certain amount of condensation catalyst wherein carries out after condensation reaction terminates, wash away catalyzer to neutral with hot distilled water, then steam solvent xylene and low-boiling-point substance at reduced pressure conditions, obtain methyl phenyl silicone oil product.Methyl phenyl silicone oil prepared by the present invention is the translucent oily liquids of clarification, and product homogeneity is better, and purity is high, and preparation process condition is simple, and solvent recoverable, is easy to suitability for industrialized production.
Description
technical field:
The present invention relates to the preparation method of silicone oil, specifically refer to a kind of preparation method of dimethyl diphenyl silicone oil of trimethicone end-blocking, product is the translucent oily liquids of clarification, and good uniformity, purity is high.
background technology:
Silicone oil keeps the linear polysiloxanes of liquid state under being often referred to room temperature, the most frequently used silicone oil organic group is all methyl, be called methyl-silicone oil, and methyl phenyl silicone oil be in methyl-silicone oil part methyl be substituted by phenyl after product, having excellent resistant of high or low temperature, oilness and radioresistance, is the wide product of development prospect.
At present, preparation method about methyl phenyl silicone oil is more, such as, patent CN 102070785A 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 CN 101851333A 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.It is raw material with dichloromethyl phenylsilane that patent CN 102516546A discloses a kind of, the weak organic bases aqueous solution is that acid binding agent prepares low viscosity aminomethyl phenyl hydroxy silicon oil, although the method raw material is inexpensive, add a large amount of weak organic bases, add the cost of suitability for industrialized production.
summary of the invention:
The present invention proposes a kind of preparation method of methyl phenyl silicone oil, specifically refer to a kind of preparation method of dimethyl diphenyl silicone oil of trimethicone end-blocking, 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.
The present invention is achieved by following technical proposals:
A preparation method for methyl phenyl silicone oil, is characterized in that carrying out in the steps below:
(1) in 500 mL there-necked flasks, add 5.06 ~ 35.45 g diphenyl dichlorosilanes, 80 mL dimethylbenzene, 50 mL acetone by every 7.74 ~ 23.23 g dimethyldichlorosilane(DMCS)s, be uniformly mixed at 30 DEG C; With acetone and distilled water configuration hydrolyzed solution, the consumption of acetone and distilled water is for add 100 mL acetone and 57.6 g distilled water by every 7.74 ~ 23.23g dimethyldichlorosilane(DMCS) and 5.06 ~ 35.45 g diphenyl dichlorosilanes, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, add a certain amount of end-capping reagent after dropwising, continue reaction 5 h at 30 DEG C, 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 siloxane prepolymer, then at 80 ~ 120 DEG C, add condensation catalyst carry out condensation reaction 1 ~ 8 h, after reaction terminates, wash away catalyzer to neutral, then 130 DEG C of reduced pressure with the distilled water of 50 ~ 60 DEG C
Under steam solvent xylene and low-boiling-point substance, obtain methyl phenyl silicone oil product.
The dimethyldichlorosilane(DMCS) wherein added in step (1), the amount of diphenyl dichlorosilane are: the integral molar quantity of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 0.2 mol, the preferred 18.07:15.19 of mass ratio of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane;
Wherein the end-capping reagent described in step (1) is trimethylchlorosilane, and add-on is: total mol ratio of trimethylchlorosilane and dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 1:10 ~ 1:80, is 0.2716 ~ 2.1728 g;
Wherein add condensation catalyst in step (2) when carrying out condensation reaction, condensation catalyst add-on is 0.01% ~ 0.2% of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane total mass, is 0.0133 g ~ 0.2660 g;
Wherein the condensation catalyst described in step (2) is the ethanolic soln of 25wt% sodium ethylate;
The optimal reaction temperature of the catalyzer condensation reaction wherein described in step (2) is 100 DEG C, and best condensation reaction time is 3h.
The invention has the advantages that:
1. the raw material that the present invention adopts is chlorosilane monomer, and raw material is simple, can be produced by direct method, output is large, cost is low, be easy to get, and make methyl phenyl silicone oil be more prone to suitability for industrialized production, technique is simple simultaneously, reaction conditions is gentle; Solvent xylene can pass through underpressure distillation recycling.
2. the present invention adopts highly basic sodium ethylate to be catalyzer, and consumption is few, effectively the condensation of catalyze siloxane prepolymer can prepare methyl phenyl silicone oil.
3. the silicone oil of the present invention's synthesis is the translucent oily liquids of clarification, and molecular weight distribution is little, good uniformity, and purity is high.
4. the present invention produces a large amount of waste hydrochloric acids when hydrolyzing chlorosilane, can mix with bauxite, gets supernatant liquid and carries out heating evaporation and obtain aluminum chloride crystal, as water purification agent, reach the effect of comprehensive reutilization, reduce environmental pollution simultaneously.
Accompanying drawing explanation
Fig. 1 is Ph/R ratio methyl phenyl silicone oil gpc chromatogram prepared when being 0.1.
Methyl phenyl silicone oil infrared spectrogram prepared when being 0.3 that Fig. 2 is Ph/R ratio.
Fig. 3 is Ph/R ratio methyl phenyl silicone oil gpc chromatogram prepared when being 0.3.
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 0.1.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 23.23 g dimethyldichlorosilane(DMCS)s, 5.06 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0570 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.Its gpc chromatogram is shown in Fig. 1.Its gpc chromatogram is unimodal dispersing mode, silicone oil good uniformity, and purity is higher, and molecular weight distribution is little.
Embodiment 2
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.Its infrared spectrogram is shown in Fig. 2, and gpc chromatogram is shown in Fig. 3.3051.6 cm in its infrared spectrogram
-1with 3071.1 cm
-1the stretching vibration that absorption peak belongs to the unsaturated hydrogen of phenyl absorbs; Be CH at the absorption peak at 2962.2 and 2904.2 places
3c-H stretching vibration peak in-Si; At 1429.7 cm
-1strong absorption peak belongs to the vibration absorption peak of aromatic ring in Si-Ph; The sharp-pointed absorption peak produced at 1261.4 places is Si-CH
3absorption peak; At 1000 ~ 1120 cm
-1a wide and strong absorption band is had to belong to the antisymmetric stretching vibration of Si-O-Si.Its gpc chromatogram is unimodal dispersing mode, silicone oil good uniformity, and purity is higher, and molecular weight distribution is little.
Embodiment 3
Ph/R ratio (mol ratio) is 0.7.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 7.74 g dimethyldichlorosilane(DMCS)s, 35.45 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0864 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 white comparatively soft solid methyl phenyl silicone oil product.
Embodiment 4
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 2.1728 g end-capping reagent trimethylchlorosilanes after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.
Embodiment 5
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.2716 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.
Embodiment 6
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 1 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.
Embodiment 7
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 8 h, after reaction terminates, wash away catalyzer 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 yellow translucent liquid methyl phenyl silicone oil product.
Embodiment 8
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.
Embodiment 9
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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, add 0.0665 g condensation catalyst sodium ethylate (quality is monomer total mass 0.05%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 yellow translucent liquid methyl phenyl silicone oil product.
Embodiment 10
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.0133 g condensation catalyst sodium ethylate (quality is monomer total mass 0.01%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 liquid methyl phenyl silicone oil product.
Embodiment 11
Ph/R ratio (mol ratio) is 0.3.In 500 mL there-necked flasks, add 80 mL dimethylbenzene, 50 mL acetone and 18.07 g dimethyldichlorosilane(DMCS)s, 15.19 g diphenyl dichlorosilanes, be uniformly mixed at 30 DEG C; Configure a certain proportion of hydrolyzed solution, wherein acetone 100 mL and distilled water 57.6 g, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, total titration time is about 3 h, adds 0.5432 g end-capping reagent trimethylchlorosilane after dropwising, at 30 DEG C, continue reaction 5h, 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 0.2660 g condensation catalyst sodium ethylate (quality is monomer total mass 0.2%) carry out condensation reaction 3 h, after reaction terminates, wash away catalyzer 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 yellow translucent liquid methyl phenyl silicone oil product.
Claims (5)
1. a preparation method for methyl phenyl silicone oil, carries out in the steps below:
(1) in there-necked flask, add 5.06 ~ 35.45 g diphenyl dichlorosilanes, 80 mL dimethylbenzene, 50 mL acetone by every 7.74 ~ 23.23 g dimethyldichlorosilane(DMCS)s, be uniformly mixed at 30 DEG C; With acetone and distilled water configuration hydrolyzed solution, the consumption of acetone and distilled water is for add 100 mL acetone and 57.6 g distilled water by every 7.74 ~ 23.23g dimethyldichlorosilane(DMCS) and 5.06 ~ 35.45 g diphenyl dichlorosilanes, stir, dropwise drip in there-necked flask with constant voltage titration funnel, control rate of addition and keep 1d/2s, add a certain amount of end-capping reagent after dropwising, continue reaction 5 h at 30 DEG C, 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 siloxane prepolymer, then at 80 ~ 120 DEG C, add condensation catalyst carry out condensation reaction 1 ~ 8 h, after reaction terminates, wash away catalyzer to neutral, then 130 DEG C of reduced pressure with the distilled water of 50 ~ 60 DEG C
Under steam solvent xylene and low-boiling-point substance, obtain methyl phenyl silicone oil product;
The dimethyldichlorosilane(DMCS) wherein added in step (1), the amount of diphenyl dichlorosilane are: the integral molar quantity of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 0.2 mol, and the mass ratio of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 18.07:15.19.
2. the preparation method of methyl phenyl silicone oil according to claim 1, it is characterized in that, wherein the end-capping reagent described in step (1) is trimethylchlorosilane, add-on is: total mol ratio of trimethylchlorosilane and dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 1:10 ~ 1:80, is 0.2716 ~ 2.1728 g.
3. the preparation method of methyl phenyl silicone oil according to claim 1, it is characterized in that, wherein add condensation catalyst in step (2) when carrying out condensation reaction, condensation catalyst add-on is 0.01% ~ 0.2% of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane total mass, is 0.0133 g ~ 0.2660 g.
4. the preparation method of methyl phenyl silicone oil according to claim 1, is characterized in that, wherein the condensation catalyst described in step (2) is the ethanolic soln of 25wt% sodium ethylate.
5. the preparation method of methyl phenyl silicone oil according to claim 1, is characterized in that, the temperature of reaction of the catalyzer condensation reaction described in step (2) is 100 DEG C, and condensation reaction time is 3h.
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| CN106893618A (en) * | 2017-02-08 | 2017-06-27 | 江苏大学 | A kind of composite titan-based grease preparation method based on PSI |
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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 |
| 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 |
| CN111534222A (en) * | 2020-06-08 | 2020-08-14 | 无锡米克新材料有限公司 | Organopolysiloxane rubber protective coating paint |
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| US3706775A (en) * | 1970-12-17 | 1972-12-19 | Wacker Chemie Gmbh | Method of preparing high molecular weight linear organopolysiloxanes |
| GB1513310A (en) * | 1974-09-16 | 1978-06-07 | Gen Electric | Organopolysiloxanes |
| US4390651A (en) * | 1974-09-16 | 1983-06-28 | General Electric Company | Phenyl-containing organopolysiloxanes |
| CN1037158A (en) * | 1988-12-12 | 1989-11-15 | 营口市熊岳制药厂 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
| DE102005047394A1 (en) * | 2005-10-04 | 2007-04-05 | Wacker Chemie Ag | Production of organopolysiloxane for use e.g. in buildings protection, involves reaction of chlorosilane with water and alcohol, continuous addition of water and immiscible solvent, and then phase separation |
| CN102585226A (en) * | 2012-02-13 | 2012-07-18 | 江苏大学 | Preparation method for thermoset high temperature resistant methyl phenyl silicone resin |
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