CN102731559A - Alkyl-substituted disiloxane and preparation method thereof - Google Patents

Abstract

The invention discloses an alkyl-substituted disiloxane represented by chemical structural formula (I) and a preparation method thereof. The preparation method of the compound is as follows: magnesium: brominated alkane: silicon tetrachloride is 3-3.5: 3-3.3 : Take each raw material in a molar ratio of 1; add magnesium to the reactor, add bromoalkane-tetrahydrofuran or anhydrous ether solution and silicon tetrachloride-petroleum ether solution under nitrogen protection; at 20 ^o C ~ 60 ^o C temperature React for 2 to 6 hours; add ammonium chloride aqueous solution or dilute hydrochloric acid to mix and stop the reaction; separate the organic phase and the water phase, extract the water phase with an organic solvent, combine the organic phases, wash with deionized water, dry with a desiccant, and suction filter the filtrate After distillation and concentration, dehydrate at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours, and then go through silica gel column chromatography to obtain alkyl substituted disiloxane. The invention has good thermal stability, oxidation resistance and high flash point, and is suitable for hydraulic oil, diffusion pump oil and heat transfer oil.

Description

Alkyl substituted disiloxane and its preparation method

technical field

The invention belongs to an organic compound with one or more C—Si bonds, and relates to an alkyl-substituted disiloxane and a preparation method thereof. The prepared siloxane compound is especially suitable for heat-resistant and anti-oxidation medium oil.

Background technique

Organosilicon compounds can be used in hydraulic oil, heat transfer oil and diffusion pump oil due to their high thermal stability, oxidation resistance and high flash point. In the prior art, the commonly used polysiloxane-based synthetic oils cannot meet the requirements for use in harsh environments for a long time, and are prone to gelation; therefore, people have been looking for alternative synthetic oils with better performance.

Contents of the invention

The object of the present invention is to overcome the deficiencies in the prior art, and provide alkyl-substituted disiloxane and its preparation method, or alkylphenyl-substituted disiloxane and its preparation method. The organosilicon compound of the invention has good heat resistance, high flash point and strong oxidation resistance, and can be used for a long time under severe working conditions.

The content of the present invention is: alkyl substituted disiloxane, which is characterized in that the compound has the chemical structural formula of (I):

                                                 

In the formula: R= C ₈ H ₁₇ , C ₁₀ H ₂₁ , C ₁₂ H ₂₅ , C ₁₈ H ₃₇ etc.

The preparation method of the described alkyl-substituted disiloxane of the content of the present invention is characterized in that it comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: brominated alkane: silicon tetrachloride is 3 ~ 3.5: 3 ~ 3.3: 1, take each raw material component; take tetrahydrofuran or anhydrous ether with 1 to 40 times the volume of brominated alkane , and mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 1 to 40 times the volume of silicon tetrachloride, and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride ^- petroleum ether solution with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system ^; React at high temperature for 2 to 6 hours to obtain the reacted material;

c. Separation and purification: add 5-20 times the volume of silicon tetrachloride to ammonium chloride aqueous solution with a mass percentage of 5-10% or dilute hydrochloric acid solution with a mass percentage of 5-10% to the reacted material and mix to stop the reaction After the reaction is terminated, separate the organic phase and the water phase, and after the water phase is extracted three times with an organic solvent of 1 to 2 times its volume, all the organic phases are combined, and the combined organic phase is washed with deionized water for 2 to 6 times to After the pH is 6.5-7.5, add desiccant to dry, filter with suction, after the filtrate is distilled and concentrated to remove the solvent, dehydrate at a temperature of 160 ^oC to 260 ^oC for 3 to 4 hours and distill out low boiling point components, and then dehydrate the dehydrated material After silica gel column chromatography, the alkyl-substituted disiloxane can be obtained.

The reaction process of the preparation method of the alkyl substituted disiloxane is as follows:

 

The prepared alkyl-substituted disiloxane is a light yellow liquid, and the product is characterized when R = C ₈ H ₁₇ :

IR (KBr, coating film): 2922, 2854, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m, 14H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=750,735,637.

When R=C ₁₀ H ₂₁ :

IR (KBr, coating film): 2922, 2854, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m, 18H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=920,905,778.

When R=C ₁₂ H ₂₅ :

IR (KBr, coating film): 2922, 2854, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m,22H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=1088,1073,919.

In the preparation method of the alkyl-substituted disiloxane: the organic solvent described in step c can be petroleum ether, diethyl ether, n-hexane, cyclohexane, ethyl acetate, dichloromethane, chloroform, benzene, toluene any of the.

In the preparation method of the alkyl-substituted disiloxane: the desiccant described in step c can be anhydrous sodium sulfate or anhydrous magnesium sulfate.

In the preparation method of the alkyl-substituted disiloxane: the chromatographic solvent used in the silica gel column chromatography described in step c can be petroleum ether or n-hexane.

Another content of the present invention is: alkylphenyl substituted disiloxane, which is characterized in that the compound has the chemical structural formula (II):

 

In the formula: R= C ₈ H ₁₇ , C ₁₀ H ₂₁ , C ₁₂ H ₂₅ , C ₁₈ H ₃₇ etc.

The preparation method of the alkylphenyl substituted disiloxane described in another content of the present invention is characterized in that it comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium:bromoalkane:diphenyldichlorosilane of 1~1.5:1~1.5:1, take each raw material component; take bromoalkane volume 1~40 times the volume of tetrahydrofuran or no Water ether, and mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take 1 to 40 times the volume of diphenyldichlorosilane in petroleum ether, and mix it into a diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ^ether solution with ^the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; React at a temperature of C for 2 to 6 hours to obtain the reacted material;

c. Separation and purification: adding 5 to 20 times the volume of diphenyldichlorosilane to 5 to 10% ammonium chloride aqueous solution or 5 to 10% dilute hydrochloric acid solution to the reacted material to mix Stop the reaction; separate the organic phase and the water phase after the reaction is stopped, extract the water phase three times with an organic solvent 1 to 2 times its volume, combine the organic phases, and wash the combined organic phases with deionized water for 2 to 6 times After the pH is 6.5-7.5, add a desiccant to dry, and filter with suction. After the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^oC to 260 ^oC for 3 to 4 hours and distill out low boiling point components, and then the dehydrated The material is subjected to silica gel column chromatography to obtain alkyl-substituted diphenyldisiloxane.

The reaction process of the preparation method of the alkylphenyl substituted disiloxane is as follows:

   

 

The prepared alkyl-substituted diphenyldisiloxane is a light yellow liquid, and the product is characterized when R = C ₈ H ₁₇ :

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which: 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): δ 7.58 – 7.30 (m, 10H), 1.48 – 1.06 (m, 14H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=606,591,529,493.

When R = C ₁₀ H ₂₁ :

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which: 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): δ 7.58 – 7.30 (m, 10H), 1.48 – 1.06 (m, 18H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=663,648,586,522.

When R = C ₁₂ H ₂₅ :

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which: 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): δ 7.58 – 7.30 (m, 10H), 1.48 – 1.06 (m, 22H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=721, 706, 586, 552.

In the preparation method of the alkylphenyl substituted disiloxane: the organic solvent in step c can be petroleum ether, diethyl ether, n-hexane, cyclohexane, ethyl acetate, dichloromethane, chloroform, benzene , any one of toluene.

In the preparation method of the alkylphenyl substituted disiloxane: the desiccant in step c can be anhydrous sodium sulfate or anhydrous magnesium sulfate.

In the preparation method of the alkylphenyl substituted disiloxane: the chromatographic solvent used in the silica gel column chromatography in step c can be petroleum ether or n-hexane.

Compared with the prior art, the present invention has the following characteristics and beneficial effects:

(1) Adopting the present invention, the structure of the product is controllable, the reaction process is simple, and the purification of the product is convenient; on the other hand, the organosilicon compound of the present invention combines siloxane and silane structures, and has Good thermal stability, oxidation resistance and high flash point, it will be well applied in hydraulic oil, diffusion pump oil and heat transfer oil;

(2) Compared with the existing medium oil and high-temperature-resistant silicone oil, the present invention has stable heat resistance and oxidation resistance at about 300 ^o C, the flash point is about 300 ^o C, and can be used at 300 ^o C for a long time;

(3) With the present invention, compared with the existing traditional high-temperature-resistant silicone oil, disiloxane has good fluidity because the molecular segment contains long-chain alkane structures and the molecules are small; at the same time, because the molecules in disiloxane The silicon atom in the middle is only connected to one oxygen atom, so disiloxane with this structure has no high-temperature rearrangement compared with traditional silicone oil;

(4) The preparation process of the product of the present invention is simple, the product is easy to separate and purify, the product yield is high, and the cost is reduced due to the use of a mixed solvent, so it has extremely strong economic benefits and strong practicability.

Detailed ways

The embodiment given below intends to further illustrate the present invention, but can not be interpreted as the restriction to protection scope of the present invention, those skilled in the art make some non-essential improvements and adjustments to the present invention according to the above-mentioned content of the present invention, still Belong to the protection scope of the present invention.

Example 1:

Preparation of 1,2,3,1',2',3'hexaoctyldisiloxane

Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C ₈ H ₁₇ Br (31mmol, 5.986g)-THF (tetrahydrofuran) (10ml) solution to the constant pressure dropping funnel under nitrogen protection, slowly drop a small amount of C ₈ H ₁₇ Br-THF solution into the system to initiate the reaction . After the Grignard reagent in the system is stable, add SiCl ₄ (10mmol, 1.7g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^o C to continue Reaction 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate and the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours and distilled off low boiling point components, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain a light yellow liquid (5.94g , yield 79.1%).

IR (KBr, coating film): 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak. ¹ HNMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m, 14H), 0.91 (t, J = 6.8 Hz, 3H). Mass spectrum: [M ⁺ ] m/z=750.75,735,637.

Example 2:

Preparation of 1,2,3,1',2',3'hexadecyldisiloxane

Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant-pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C ₁₀ H ₂₁ Br (31mmol, 6.851g)-THF (10ml) solution to the constant pressure dropping funnel under nitrogen protection, and slowly drop a small amount of C ₁₀ H ₂₁ Br-THF solution into the system to initiate the reaction. After the Grignard reagent in the system is stable, add SiCl ₄ (10mmol, 1.7g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^o C to continue Reaction 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate, and then the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours and the low boiling point components were distilled off, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain a light yellow liquid.

IR (KBr, coating film): 2922, 2854, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m, 18H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=920,905,778.

Example 3:

Preparation of 1,2,3,1',2',3'hexa-dodecyldisiloxane

Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant-pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C ₁₂ H ₂₅ Br (31mmol, 7.726g)-THF (10ml) solution to the constant pressure dropping funnel under nitrogen protection, and slowly drop a small amount of C ₁₂ H ₂₅ Br-THF solution into the system to initiate the reaction. After the Grignard reagent in the system is stable, add SiCl ₄ (10mmol, 1.7g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^o C to continue Reaction 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate, and then the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours and the low boiling point components were distilled off, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain a light yellow liquid.

IR (KBr, coating film): 2922, 2854, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): 1.48 – 1.06 (m,22H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=1088,1073,919.

Example 4:

Preparation of 1,1'-dioctyl 2,3,2',3'tetraphenyldisiloxane

Magnesium chips (11 mmol, 0.264 g) were added to a three-necked flask equipped with a condenser tube, a constant pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated, and nitrogen was blown three times. Add C ₈ H ₁₇ Br (10mmol, 1.931g)-THF (5ml) solution to the constant pressure dropping funnel under nitrogen protection, and slowly drop a small amount of C ₈ H ₁₇ Br-THF solution into the system to initiate the reaction. After the Grignard reagent in the system is stable, add Ph ₂ SiCl ₂ (10mmol, 2.532g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, and after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^°C C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate, and then the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours, and the low boiling point components were distilled off, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain light yellow phenyl disilica Oxygen liquid.

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which 1076 is the Si-O-Si vibration absorption peak. ¹ H NMR (400 MHz, CDCl3): δ 7.58 – 7.30 (m, 20H), 1.48 – 1.06 (m,28H), 0.91 (t, J = 6.8 Hz, 6H). Mass spectrum: [M ⁺ ] m/z=606,591,529,493.

Example 5:

Preparation of 1,1'-didecyl 2,3,2',3'tetraphenyldisiloxane

Magnesium chips (11 mmol, 0.264 g) were added to a three-necked flask equipped with a condenser tube, a constant pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C ₁₀ H ₂₁ Br (10mmol, 2.212g)-THF (5ml) solution to the constant pressure dropping funnel under nitrogen protection, and slowly drop a small amount of C ₁₀ H ₂₁ Br-THF solution into the system to initiate the reaction. After the Grignard reagent in the system is stable, add Ph ₂ SiCl ₂ (10mmol, 2.532g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, and after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^°C C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate, and then the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours, and the low boiling point components were distilled off, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain light yellow phenyl disilica Oxygen liquid.

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which: 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): δ 7.58 – 7.30 (m, 10H), 1.48 – 1.06 (m, 18H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=663,648,586,522.

Embodiment 6:

Preparation of 1,1'-docosyl 2,3,2',3'tetraphenyldisiloxane

Magnesium chips (11 mmol, 0.264 g) were added to a three-necked flask equipped with a condenser tube, a constant pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C ₁₂ H ₂₅ Br (10mmol, 2.212g)-THF (5ml) solution to the constant pressure dropping funnel under nitrogen protection, and slowly drop a small amount of C ₁₂ H ₂₅ Br-THF solution into the system to initiate the reaction. After the Grignard reagent in the system is stable, add Ph ₂ SiCl ₂ (10mmol, 2.532g)-petroleum ether (5ml) solution to the constant pressure dropping funnel, and after the mixed solution is added dropwise within 2h, the temperature is raised to 50 ^°C C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, and the organic phases were combined. The organic phase was dried with anhydrous sodium sulfate, and then the solvent was distilled off, dehydrated at 160 ^oC ~ 260 ^oC for 3 ~ 4 hours, and the low boiling point components were distilled off, and the dehydrated organic phase was subjected to silica gel column chromatography to obtain light yellow phenyl disilica Oxygen liquid.

IR (KBr, coating film): 3049, 2922, 2854, 1465, 1378, 1245, 1076, 832, 771, 721, of which: 1076 is the Si-O-Si vibration absorption peak;

¹ H NMR (400 MHz, CDCl ₃ ): δ 7.58 – 7.30 (m, 10H), 1.48 – 1.06 (m, 22H), 0.91 (t, J = 6.8 Hz, 3H);

Mass spectrum: [M ⁺ ] m/z=721, 706, 586, 552.

Embodiment 7:

The preparation method of alkyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: silicon tetrachloride is 3:3:1, take each raw material component; take tetrahydrofuran or anhydrous ether that is 1 times the volume of bromoalkane, and mix it into bromoalkane Alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 40 times the volume of silicon tetrachloride and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride-petroleum ether solution with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and drop ^them into the reaction system; , to obtain the reacted material;

C, separation and purification: the mass percentage of silicon tetrachloride volume 5 times volume is 10% ammonium chloride aqueous solution or the mass percentage is that 10% dilute hydrochloric acid solution joins in the material after reaction and mixes and stops reaction; After reaction stops, separate organic phase and water phase, and the water phase was extracted three times with an organic solvent of 1 times its volume, then all the organic phases were combined, and the combined organic phase was washed 2 to 6 times with deionized water until the pH was 6.5 to 7.5, and then added Drying with desiccant, suction filtration, after the filtrate is distilled and concentrated to remove the solvent, dehydrated at 160 ^oC ~ 260 ^oC for 3 hours and distilled out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted disiloxanes are yellow liquids.

Embodiment 8:

The preparation method of alkyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: silicon tetrachloride is 3.5: 3.3: 1, take each raw material component; take tetrahydrofuran or anhydrous ether 40 times the volume of bromoalkane, and mix it into bromoalkane Alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether of 1 times the volume of silicon tetrachloride, and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, the silicon tetrachloride-petroleum ether solution is mixed with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and added dropwise to ^the reaction system ^; Reaction 6h, obtains the post-reaction material;

C, separation and purification: 5% ammonium chloride aqueous solution or 5% dilute hydrochloric acid solution with 20 times the volume of silicon tetrachloride volume is added to the reacted material and mixed to stop the reaction; after the reaction is stopped, separate the organic phase and water phase, and the water phase was extracted three times with an organic solvent twice its volume, then all the organic phases were combined, and the combined organic phase was washed 2 to 6 times with deionized water until the pH was 6.5 to 7.5, and then added Drying with desiccant, suction filtration, after the filtrate is concentrated by distillation to remove the solvent, dehydrated at a temperature of 160 ^oC ~ 260 ^oC for 4 hours and distilled out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted disiloxanes are yellow liquids.

Embodiment 9:

The preparation method of alkyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: silicon tetrachloride is 3.3:3.1:1, take each raw material component; take tetrahydrofuran or anhydrous ether 20 times the volume of bromoalkane, and mix it into bromoalkane Alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 20 times the volume of silicon tetrachloride and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride-petroleum ether ^solution with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; , to obtain the reacted material;

C, separation and purification: 7% ammonium chloride aqueous solution or 8% dilute hydrochloric acid solution is added in the reacted material with a mass percentage of 12 times the volume of silicon tetrachloride to stop the reaction; after the reaction is terminated, separate the organic phase and water phase, and the water phase was extracted three times with an organic solvent twice its volume, then all the organic phases were combined, and the combined organic phase was washed 2 to 6 times with deionized water until the pH was 6.5 to 7.5, and then added Drying with a desiccant, suction filtration, after the filtrate is concentrated by distillation to remove the solvent, dehydrated at a temperature of 160 ^oC ~ 260 ^oC for 3.5 hours and distilled out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted disiloxanes are pale yellow liquids.

Example 10:

The preparation method of alkyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: silicon tetrachloride is 3.1: 3.1: 1, take each raw material component; take tetrahydrofuran or anhydrous ether 10 times the volume of bromoalkane, and mix it into bromoalkane Alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 10 times the volume of silicon tetrachloride and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride-petroleum ether solution with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; after the dropwise addition, react at a temperature of 30 ^o C for 5 hours , to obtain the reacted material;

C, separation and purification: 9 times the volume of silicon tetrachloride volume is 6% ammonium chloride aqueous solution or 6% dilute hydrochloric acid solution is added in the reacted material and mixed to stop the reaction; after the reaction is stopped, separate the organic phase and water phase, and the water phase was extracted three times with an organic solvent 1.5 times its volume, then all the organic phases were combined, and the combined organic phase was washed 2 to 6 times with deionized water until the pH was 6.5 to 7.5, and then added Drying with desiccant, suction filtration, after the filtrate is distilled and concentrated to remove the solvent, dehydrated at 160 ^oC ~ 260 ^oC for 3 hours and distilled out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted disiloxanes are yellow liquids.

Example 11:

The preparation method of alkyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: brominated alkane: silicon tetrachloride is 3:3 ~ 3.3: 1, take each raw material component; take tetrahydrofuran or anhydrous ether with 1 to 40 times the volume of brominated alkane, and Mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 1 to 40 times the volume of silicon tetrachloride, and mix it into a silicon tetrachloride-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride ^- petroleum ether solution with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system ^; React at high temperature for 2 to 6 hours to obtain the reacted material;

c. Separation and purification: add 5-20 times the volume of silicon tetrachloride to ammonium chloride aqueous solution with a mass percentage of 5-10% or dilute hydrochloric acid solution with a mass percentage of 5-10% to the reacted material and mix to stop the reaction After the reaction is terminated, separate the organic phase and the water phase, and after the water phase is extracted three times with an organic solvent of 1 to 2 times its volume, all the organic phases are combined, and the combined organic phase is washed with deionized water for 2 to 6 times to After the pH is 6.5-7.5, add desiccant to dry, filter with suction, after the filtrate is distilled and concentrated to remove the solvent, dehydrate at a temperature of 160 ^oC to 260 ^oC for 3 to 4 hours and distill out low boiling point components, and then dehydrate the dehydrated material After silica gel column chromatography, the alkyl-substituted disiloxane of light yellow liquid is obtained.

Example 12:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium:bromoalkane:diphenyldichlorosilane of 1~1.5:1~1.5:1, take each raw material component; take bromoalkane volume 1~40 times the volume of tetrahydrofuran or no Water ether, and mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take 1 to 40 times the volume of diphenyldichlorosilane in petroleum ether, and mix it into a diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ^ether solution with ^the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; React at a temperature of C for 2 to 6 hours to obtain the reacted material;

c. Separation and purification: adding 5 to 20 times the volume of diphenyldichlorosilane to 5 to 10% ammonium chloride aqueous solution or 5 to 10% dilute hydrochloric acid solution to the reacted material to mix Stop the reaction; separate the organic phase and the water phase after the reaction is stopped, extract the water phase three times with an organic solvent 1 to 2 times its volume, combine the organic phases, and wash the combined organic phases with deionized water for 2 to 6 times After the pH is 6.5-7.5, add a desiccant to dry, and filter with suction. After the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^oC to 260 ^oC for 3 to 4 hours and distill out low boiling point components, and then the dehydrated The material was subjected to silica gel column chromatography to obtain a pale yellow liquid alkyl-substituted diphenyldisiloxane.

Example 13:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: diphenyldichlorosilane of 1:1:1, take each raw material component; take tetrahydrofuran or anhydrous ether that is 40 times the volume of bromoalkane, and mix them into Bromoalkane-tetrahydrofuran or anhydrous ether solution; take 1 times the volume of diphenyldichlorosilane in petroleum ether and mix it into a diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, the diphenyldichlorosilane-petroleum ether ^solution was mixed with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and added dropwise to the reaction system; Reaction 2h, obtains the post-reaction material;

c. Separation and purification: adding 10% ammonium chloride aqueous solution or 10% dilute hydrochloric acid solution to 5 times the volume of diphenyldichlorosilane by volume and mixing the materials after the reaction to stop the reaction; Separate the organic phase and the water phase, extract the water phase three times with an organic solvent of 1 times its volume, combine the organic phases, wash the combined organic phases with deionized water for 2 to 6 times until the pH is 6.5 to 7.5, Add desiccant to dry, filter with suction, after the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^oC ~ 260 ^oC for 3 hours and distill off low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted diphenyldisiloxanes are pale yellow liquids.

Example 14:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: diphenyldichlorosilane of 1.5: 1.5: 1, take each raw material component; take tetrahydrofuran or anhydrous ether that is 40 times the volume of bromoalkane, and mix them into Bromoalkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether with 40 times the volume of diphenyldichlorosilane and mix it into diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ether ^solution with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; Reaction 6h, obtains the post-reaction material;

c, separation and purification: 20 times the volume of diphenyl dichlorosilane volume is 5% ammonium chloride aqueous solution or 5% dilute hydrochloric acid solution is added to the reaction and the materials are mixed to stop the reaction; after the reaction is stopped Separate the organic phase and the aqueous phase, extract the aqueous phase three times with an organic solvent twice its volume, combine the organic phases, wash the combined organic phases with deionized water for 2 to 6 times until the pH is 6.5 to 7.5, Add desiccant to dry, filter with suction, after the filtrate is distilled and concentrated to remove the solvent, dehydrate at 160 ^oC ~ 260 ^oC for 4 hours and distill off low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted diphenyldisiloxanes are pale yellow liquids.

Example 15:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: diphenyldichlorosilane of 1.3:1.3:1, take each raw material component; take tetrahydrofuran or anhydrous ether 20 times the volume of bromoalkane, and mix them into Bromoalkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 20 times the volume of diphenyldichlorosilane and mix it into diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ether ^solution with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; Reaction 4h, obtains the material after reaction;

C, separation and purification: 12 times the volume of diphenyl dichlorosilane volume is 7% ammonium chloride aqueous solution or 7% dilute hydrochloric acid solution is added to the reaction after the reaction material is mixed to stop the reaction; after the reaction is stopped Separate the organic phase and the water phase, extract the water phase three times with an organic solvent of 1.5 times its volume, combine the organic phases, wash the combined organic phases with deionized water for 2 to 6 times until the pH is 6.5 to 7.5, Add desiccant to dry, filter with suction, after the filtrate is distilled and concentrated to remove the solvent, dehydrate at a temperature of 160 ^oC ~ 260 ^oC for 3.5 hours and distill out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain the product Alkyl-substituted diphenyldisiloxane was obtained as light yellow liquid.

Example 16:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: diphenyldichlorosilane of 1.1:1.1:1, take each raw material component; take tetrahydrofuran or anhydrous ether 10 times the volume of bromoalkane, and mix them into Bromoalkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 30 times the volume of diphenyldichlorosilane and mix it into a diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ether ^solution with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; React 3h, obtain the material after reaction;

c. Separation and purification: add 8% ammonium chloride aqueous solution or 6% dilute hydrochloric acid solution with 9 times the volume of diphenyldichlorosilane to the reaction and mix the materials to stop the reaction; Separate the organic phase and the aqueous phase, extract the aqueous phase three times with an organic solvent twice its volume, combine the organic phases, wash the combined organic phases with deionized water for 2 to 6 times until the pH is 6.5 to 7.5, Add desiccant to dry, filter with suction, after the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^oC ~ 260 ^oC for 3 hours and distill off low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography to obtain Alkyl-substituted diphenyldisiloxanes are pale yellow liquids.

Example 17:

The preparation method of alkylphenyl substituted disiloxane comprises the following steps:

a. Ingredients: According to the molar ratio of magnesium: bromoalkane: diphenyldichlorosilane of 1.4:1.4:1, take each raw material component; take tetrahydrofuran or anhydrous ether 30 times the volume of bromoalkane, and mix them into Bromoalkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 30 times the volume of diphenyldichlorosilane and mix it into a diphenyldichlorosilane-petroleum ether solution;

The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, brominated octadecane, etc.;

b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ether ^solution with the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; React 5h, obtain the material after reaction;

c, separation and purification: 15 times the volume of diphenyl dichlorosilane volume is 8% ammonium chloride aqueous solution or 8% dilute hydrochloric acid solution is added to the reaction and the materials are mixed to stop the reaction; after the reaction is stopped Separate the organic phase and the aqueous phase, extract the aqueous phase three times with an organic solvent twice its volume, combine the organic phases, wash the combined organic phases with deionized water for 2 to 6 times until the pH is 6.5 to 7.5, Add desiccant to dry, filter with suction, after the filtrate is distilled and concentrated to remove the solvent, dehydrate at a temperature of 160 ^oC ~ 260 ^oC for 3 ~ 4 hours and distill out low boiling point components, and then the dehydrated material is subjected to silica gel column chromatography, that is Alkyl-substituted diphenyldisiloxanes were obtained as pale yellow liquids.

Among the above-mentioned embodiments 7-17: the organic solvent described in the step c is any one in sherwood oil, ether, n-hexane, cyclohexane, ethyl acetate, methylene chloride, chloroform, benzene, toluene.

Among the above-mentioned embodiments 7-17: the desiccant described in step c can be anhydrous sodium sulfate or anhydrous magnesium sulfate.

Among the above-mentioned Examples 7-17: the chromatographic solvent used in the silica gel column chromatography described in step c is sherwood oil or normal hexane.

In above-mentioned embodiment: each raw material that adopts is commercially available product.

In the above-mentioned embodiments: among the percentages used, those not specified are all percentages by weight (mass); the parts by weight (mass) can all be grams or kilograms.

Among the above-mentioned embodiments: the process parameters (temperature, time, concentration, etc.) in each step and the numerical values of the amounts of each component are within the range, and any point is applicable.

The content of the present invention and the technical content not specifically described in the above embodiments are the same as the prior art.

The present invention is not limited to the above-mentioned embodiments, and all of the contents of the present invention can be implemented and have the above-mentioned good effects.

Claims (10)

1. Alkyl-substituted disiloxane, characterized in that the compound has the chemical structural formula of (I):                                                  

In the formula: R= C ₈ H ₁₇ , C ₁₀ H ₂₁ , C ₁₂ H ₂₅ , C ₁₈ H ₃₇ . 2. the preparation method of alkyl substituted disiloxane, it is characterized in that comprising the following steps: a. Ingredients: According to the molar ratio of magnesium: brominated alkane: silicon tetrachloride is 3 ~ 3.5: 3 ~ 3.3: 1, take each raw material component; take tetrahydrofuran or anhydrous ether with 1 to 40 times the volume of brominated alkane , and mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take petroleum ether 1 to 40 times the volume of silicon tetrachloride, and mix it into a silicon tetrachloride-petroleum ether solution; The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, and brominated octadecane; b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the silicon tetrachloride ^- petroleum ether solution with the remaining brominated alkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system ^; React at high temperature for 2 to 6 hours to obtain the reacted material; c. Separation and purification: add 5-20 times the volume of silicon tetrachloride to ammonium chloride aqueous solution with a mass percentage of 5-10% or dilute hydrochloric acid solution with a mass percentage of 5-10% to the reacted material and mix to stop the reaction After the reaction is terminated, separate the organic phase and the water phase, and after the water phase is extracted three times with an organic solvent of 1 to 2 times its volume, all the organic phases are combined, and the combined organic phase is washed with deionized water for 2 to 6 times to After the pH is 6.5~7.5, add a desiccant to dry, and filter with suction. After the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^o C ~ 260 ^o C for 3 ~ 4 hours and distill out the low boiling point components, and then the dehydrated The material is subjected to silica gel column chromatography to obtain an alkyl-substituted disiloxane. 3. by the preparation method of the described alkyl-substituted disiloxane of claim 2, it is characterized in that: the organic solvent described in step c is sherwood oil, ether, normal hexane, hexanaphthene, ethyl acetate, methylene dichloride , Chloroform, benzene, toluene in any one. 4. according to the preparation method of the described alkyl substituted disiloxane of claim 2, it is characterized in that: desiccant described in step c is anhydrous sodium sulfate or anhydrous magnesium sulfate. 5. by the preparation method of the described alkyl-substituted disiloxane of claim 2, it is characterized in that: the used chromatographic solvent of silica gel column chromatography described in step c is sherwood oil or n-hexane. 6. Alkylphenyl substituted disiloxane, characterized in that the compound has the chemical structural formula (II):   In the formula: R= C ₈ H ₁₇ , C ₁₀ H ₂₁ , C ₁₂ H ₂₅ , C ₁₈ H ₃₇ . 7. the preparation method of alkylphenyl substituted disiloxane, it is characterized in that comprising the following steps: a. Ingredients: According to the molar ratio of magnesium:bromoalkane:diphenyldichlorosilane of 1~1.5:1~1.5:1, take each raw material component; take bromoalkane volume 1~40 times the volume of tetrahydrofuran or no Water ether, and mixed into a brominated alkane-tetrahydrofuran or anhydrous ether solution; take 1 to 40 times the volume of diphenyldichlorosilane in petroleum ether, and mix it into a diphenyldichlorosilane-petroleum ether solution; The brominated alkane is any one of brominated n-octane, brominated n-decane, brominated dodecane, and brominated octadecane; b. Reaction: After anhydrous and oxygen-free treatment of the reaction kettle, magnesium is added to the reaction kettle, and bromoalkane-tetrahydrofuran or anhydrous ether solution is added dropwise to the reaction kettle to react with magnesium under the protection of nitrogen, and a part of the reaction kettle is formed. After the alkyl Grignard reagent, mix the diphenyldichlorosilane-petroleum ^ether solution with ^the remaining bromoalkane-tetrahydrofuran or anhydrous ether and drop them into the reaction system; React at a temperature of C for 2 to 6 hours to obtain the reacted material; c. Separation and purification: adding 5 to 20 times the volume of diphenyldichlorosilane to 5 to 10% ammonium chloride aqueous solution or 5 to 10% dilute hydrochloric acid solution to the reacted material to mix Stop the reaction; separate the organic phase and the water phase after the reaction is stopped, extract the water phase three times with an organic solvent 1 to 2 times its volume, combine the organic phases, and wash the combined organic phases with deionized water for 2 to 6 times After the pH is 6.5~7.5, add a desiccant to dry, and filter with suction. After the filtrate is concentrated by distillation to remove the solvent, dehydrate at a temperature of 160 ^o C ~ 260 ^o C for 3 ~ 4 hours and distill out low boiling point components, and then dehydrate The final material is subjected to silica gel column chromatography to obtain alkyl-substituted diphenyldisiloxane. 8. by the preparation method of the described alkylphenyl substituted disiloxane of claim 7, it is characterized in that: the organic solvent described in the step c is sherwood oil, ether, normal hexane, hexanaphthene, ethyl acetate, diacetate Any of methyl chloride, chloroform, benzene, and toluene. 9. According to the preparation method of the described alkylphenyl substituted disiloxane of claim 7, it is characterized in that: the desiccant described in the step c is anhydrous sodium sulfate or anhydrous magnesium sulfate. 10. by the preparation method of the described alkylphenyl substituted disiloxane of claim 7, it is characterized in that: the used chromatographic solvent of silica gel column chromatography described in the step c is sherwood oil or n-hexane.