CN104961897A - Phenyl alkyl silicone oil preparation method - Google Patents
Phenyl alkyl silicone oil preparation method Download PDFInfo
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Abstract
The present invention discloses a phenyl alkyl silicone oil preparation method, which comprises: under the protection of an inert gas, mixing high hydrogen content silicone oil, a methyl phenyl hybrid ring body, an end capping agent and a strong acid, reacting for 6-24 h at a temperature of 25-80 DEG C, carrying out post-treatment to obtain methyl phenyl hydrogen-containing silicone oil; and under the protection of an inert gas, mixing alpha-olefin, an organic solvent and a chloroplatinic acid/isopropyl alcohol solution, heating to a temperature of 60-120 DEG C, mixing with the methyl phenyl hydrogen-containing silicone oil, reacting, and carrying out a purification treatment to obtain the phenyl alkyl silicone oil. According to the present invention, the phenyl alkyl silicone oil preparation method is provided and has characteristics of wide raw material source, low cost, mild reaction conditions, easy control and easy industrialization; and the synthesized product has characteristics of uniform organic group distribution, good transparency, good heat resistance and high refractive index, and is especially suitable for the compounding oil for the mineral lubricating oil base oil.
Description
Technical field
The present invention relates to technical field prepared by organic silicone oil, particularly relate to a kind of preparation method of phenylalkyl silicone oil.
Background technology
Silicone oil typically refers to the linear polysiloxane for liquid state under room temperature, has that viscosity index is high, good, the good thermostability of viscosity-temperature characteristics energy, oxidation-resistance, low-temperature fluidity and an advantage such as anti-shear stability is good, various in style, is of wide application.
Modal silicone oil organic group is all methyl, is called methyl-silicone oil.Phenylalkyl silicone oil can be regarded as part methyl in methyl-silicone oil replaced by phenyl and alkyl after product, have excellent high/low temperature mobility, oilness, radioresistance, to the adsorptivity of metal and with organic consistency, be the wide product of development prospect.
Phenylalkyl silicone oil is a kind of lubricant base, and its molecular chain structure, molecular weight distribution directly have influence on its lubricity and operating temperature range.The preparation of existing phenylalkyl silicone oil mainly adopts methylhydracyclosiloxane, dimethicone and hexamethyldisiloxane ring opening copolymer to obtain silicon oil of low hydrogen content; Silicon oil of low hydrogen content carries out addition reaction of silicon with hydrogen with alpha-olefin, vinylbenzene and obtains again.But there is a lot of shortcoming in this method:
First, the monomer purity used in silicon oil of low hydrogen content preparation process is difficult to ensure, if wherein retain a small amount of impurity, then ring-opening reaction is wayward, easily occur crosslinked between Si-H, affect the viscosity of product, light transmission and structure distribution etc., in addition, also can make a big impact to second step Si―H addition reaction.
The second, the phenyl of introducing is in γ position, and the fracture of silicone oil side base usually occurs on the carbon atom of β position, causes the lifting of phenyl to silicone oil thermostability not obvious.
In addition, the preparation method of phenyl hydrogen-containing silicon oil also also exists certain defect in some reports at present.Such as, the containing hydrogen silicone oil by synthesizing containing phenylbenzene silica chain link containing silicon hydride chlorid, dimethylchlorosilane and diphenyl dichlorosilane hydrolytie polycondensation.This synthetic method, the composition very different of products therefrom under different proportioning raw materials and hydrolysising condition, the repeatability of product and poor controllability.And due to diphenyl siloxane chain link space steric effect large, differ greatly with the reactive behavior of methyl hydrogen silica chain link and dimethyl silicone oil chain link and consistency, be difficult to obtain the dimethyl diphenyl containing hydrogen silicone oil that segment distribution is even, functional, molar mass is high.The product transparency obtained is poor, and raw materials cost is high, low temperature properties and package stability poor, affect its usability.
Summary of the invention
The invention provides a kind of preparation method of phenylalkyl silicone oil, raw material sources are wide, cost is low, reaction conditions is gentle, be easy to control, be convenient to industrialization; In synthetic product organic group be more evenly distributed, transparency and thermotolerance is better, specific refractory power is high, be specially adapted to the composite oil of mineral lubricant oil base oil.
A preparation method for phenylalkyl silicone oil, comprises the following steps:
(1) under protection of inert gas, high containing hydrogen silicone oil, aminomethyl phenyl mixed methylcyclosiloxane, end-capping reagent and strong acid are mixed, react 6 ~ 24h at 25 ~ 80 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil through aftertreatment;
The mass ratio of described high containing hydrogen silicone oil, aminomethyl phenyl mixed methylcyclosiloxane, end-capping reagent and strong acid is 1: 5 ~ 50: 1 ~ 5: 1 ~ 12;
(2) under protection of inert gas, by alpha-olefin, organic solvent and Platinic chloride/aqueous isopropanol mixing, be heated to 60 ~ 120 DEG C, and mix with methyl and phenyl hydrogen-containing silicon oil prepared by step (1), after reaction, obtain phenylalkyl silicone oil through purification process;
The mass ratio of described alpha-olefin, organic solvent, Platinic chloride/aqueous isopropanol and methyl and phenyl hydrogen-containing silicon oil is 1: 0.3 ~ 200: 0.001 ~ 1: 1 ~ 250.
As preferably, the chemical structural formula of described high containing hydrogen silicone oil is such as formula shown in (I):
Wherein, a is selected from natural number, and b is selected from the natural number not comprising 0, and a, b are separate, and a+b=1 ~ 50.
As preferably, the chemical structural formula of described aminomethyl phenyl mixed methylcyclosiloxane is such as formula shown in (II):
Wherein, x, y are independently selected from the natural number not comprising 0, and x+y=3 ~ 6.Further preferably, in described aminomethyl phenyl mixed methylcyclosiloxane, phenyl content is 5 ~ 20mol.%.
As preferably, described end-capping reagent be hexamethyldisiloxane, trimethylmethoxysilane, trimethylethoxysilane, tetramethyl-phenylbenzene sily oxide, dimethyl benzene methoxylsilane, 3,5-dimethylphenyl Ethoxysilane, dimethyltetraphenyldisiloxane, methyldiphenyl methoxylsilane, methyldiphenylethoxysilane, hexaphenyldisiloxane, triphenylmethoxy silane, triphenyl Ethoxysilane, in one or more;
Described strong acid is selected from the one in the vitriol oil, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, trifluoromethanesulfonic acid, acidic white earth, solid super-strong acid, macropore strong acid cation exchange resin.Its consumption is 1 ~ 8% of raw material total mass (i.e. the total mass of high containing hydrogen silicone oil, aminomethyl phenyl mixed methylcyclosiloxane, end-capping reagent and strong acid).Further preferably, described strong acid is the vitriol oil of 98%, and consumption is 1 ~ 2% of raw material total mass.
As preferably, in step (1), temperature of reaction is 20 ~ 60 DEG C, and the reaction times is 16 ~ 24h.
As preferably, the preparation method of described Platinic chloride/aqueous isopropanol is: dissolved in by Platinic chloride in Virahol, obtain Virahol and Platinic chloride complex compound, Platinic chloride concentration is 0.1 ~ 2wt.%, and the consumption participating in reaction is 5 ~ 100ppm of methyl and phenyl hydrogen-containing silicon oil quality (molar ratio computing with Si-H key contained in Pt and methyl and phenyl hydrogen-containing silicon oil).As preferably, described Platinic chloride concentration is 0.8 ~ 1wt.%, and the consumption participating in reaction is the 20 ~ 50ppm (molar ratio computing with Pt and Si-H key) of addition raw material.
As preferably, described alpha-olefin is the straight or branched type alkene that carbon number is selected from 2 ~ 20, and in Si-H key contained in methyl and phenyl hydrogen-containing silicon oil and alpha-olefin, the mol ratio of C=C is 1: 1.1 ~ 1.5; Further preferably, described alpha-olefin carbon number is the straight or branched alkene of 8 ~ 16, and consumption is (Si-H): (C=C)=1: 1.2 ~ 1.3; Most preferably, described alpha-olefin is 1-laurylene.
Described organic solvent is at least one in toluene, dimethylbenzene, tetrahydrofuran (THF), Virahol, propyl carbinol, normal hexane, sherwood oil.Its consumption is 20 ~ 80% of reactant total mass (i.e. the total mass of alpha-olefin, organic solvent, Platinic chloride/aqueous isopropanol and methyl and phenyl hydrogen-containing silicon oil).As preferably, described organic solvent is toluene, and consumption is 30 ~ 50% of reactant total mass.
As preferably, methyl and phenyl hydrogen-containing silicon oil step (1) prepared instills in the mixing solutions be made up of alpha-olefin, organic solvent and Platinic chloride/aqueous isopropanol, and in dropping process, in guarantee system, temperature is no more than 90 DEG C.
As preferably, the aftertreatment described in step (1) is:
The reaction solution that step (1) obtains is cooled to room temperature, adds excessive neutralizing agent and fully stir, neutralize, then through high speed centrifugation removing solid wherein, vacuum removal retained material and low-boiling-point substance;
Described neutralizing agent is at least one in carbonate, supercarbonate, oxidized metal;
Described vacuum removal condition is: vacuum tightness is-0.075 ~-0.096Mpa, and temperature is 150 ~ 210 DEG C, and the time of removing is 1 ~ 4h.
As preferably, in step (2), react extremely: at v
si-H=2158cm
-1place, through infrared detection without till Si-H absorption peak, then carries out purification process.Further preferably, in step (2), temperature of reaction is 70 ~ 100 DEG C, and the reaction times is 8 ~ 12h.
As preferably, in step (2), described purification process is vacuum removal organic solvent, residual reaction raw materials and low-boiling-point substance;
Described vacuum removal condition is: vacuum tightness is-0.075 ~-0.096Mpa, and temperature is 150 ~ 210 DEG C, and the time of removing is 1 ~ 4h.
According to phenylalkyl silicone oil prepared by aforesaid method, its number-average molecular weight is 0.5 × 10
4~ 6 × 10
4between, alkyl content is between 0.1 ~ 2.0mmol/g, phenyl content is between 1 ~ 25mol.%, refractive index is adjustable between 1.40 ~ 1.54, there is radiation hardness, high temperature resistant, weather-proof, oilness is good, to the excellent adsorption of metal, with the advantage such as organic consistency is good, be specially adapted to the composite oily of mineral lubricant oil base oil.
Compared with prior art, tool of the present invention has the following advantages:
1) raw material sources are wide, cost is low;
2) reaction conditions gentle, be easy to control;
3) in synthetic product organic group be more evenly distributed, transparency and thermotolerance is better, specific refractory power is high.
Embodiment
The present invention further illustrates by following embodiment, but embodiment is not limiting the scope of the invention.
Embodiment 1
At N
2under protection, to one, reflux condensate device is housed, thermometer, aminomethyl phenyl mixed methylcyclosiloxane 47.48g (phenyl content is 10mol.%) is added in the dry four-hole bottle of 100mL of mechanical stirrer, hexamethyldisiloxane 1.5228g, high containing hydrogen silicone oil (Jiaxing Joint Chemical Co., Ltd, UC202, lower same) 0.9972g, 98% vitriol oil 0.5g, 24h is reacted at 25 DEG C, then add 2g anhydrous sodium bicarbonate fully to neutralize, through high speed centrifugation desalination, at vacuum tightness-0.096Mpa, unreacting material and low-boiling-point substance 2h is pulled out at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add toluene 10g, 1-laurylene 1.89g, Platinic chloride/aqueous isopropanol (Platinic chloride concentration is 0.8wt.%) 1; be warming up to 75 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 6h.At vacuum tightness-0.096Mpa, pull out toluene, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 5500, PDI is 1.67, and wherein alkyl content is 0.296mmol/g, and phenyl content is 8.4mol.%, refractive index n
d 25=1.4233; 10% thermal degradation temperature is 398 DEG C; With layering in 3 ~ 4 days after mineral oil.Embody preparation method and property relationship
Embodiment 2
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 45.08g (phenyl content is 10mol.%), hexamethyldisiloxane 1.2636g, high containing hydrogen silicone oil 3.6564g, 98% vitriol oil 0.5g; 24h is reacted at 25 DEG C; then add 2g anhydrous sodium bicarbonate fully to neutralize; through high speed centrifugation desalination; at vacuum tightness-0.096Mpa; pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add sherwood oil 10g, 1-laurylene 6.94g, Platinic chloride/aqueous isopropanol 3; be warming up to 75 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 10h.At vacuum tightness-0.096Mpa, pull out sherwood oil, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 6900, PDI is 1.69, and wherein alkyl content is 0.998mmol/g, and phenyl content is 7.4mol.%, refractive index n
d 25=1.4346; 10% thermal degradation temperature is 407 DEG C; Not stratified after dissolving each other with mineral oil.
Embodiment 3
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 47.69g (phenyl content is 10mol.%), hexamethyldisiloxane 0.648g, high containing hydrogen silicone oil 1.662g, acidic white earth (Anji County Zhong Xin atlapulgite company limited of Zhejiang Province; trade mark HT-1A) 2g; 12h is reacted at 60 DEG C; then suction filtration removing catalyzer; at vacuum tightness-0.096Mpa; pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add Virahol 10g, 1-laurylene 3.1558g, Platinic chloride/aqueous isopropanol 2; be warming up to 75 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 8h.At vacuum tightness-0.096Mpa, pull out Virahol, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 9900, PDI is 1.80, and wherein alkyl content is 0.493mmol/g, and phenyl content is 8.1mol.%, refractive index n
d 25=1.4319; 10% thermal degradation temperature is 432 DEG C; Not stratified after dissolving each other with mineral oil.
Embodiment 4
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 46.295g (phenyl content is 10mol.%), hexamethyldisiloxane 0.0486g, high containing hydrogen silicone oil 3.6564, macropore strong acid cation exchange resin (sky tunami letter resin Science and Technology Ltd.; D001 type) 3g; 12h is reacted at 60 DEG C; then suction filtration removing catalyzer; at vacuum tightness-0.096Mpa; pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add dimethylbenzene 12g, 1-laurylene 6.94g, Platinic chloride/aqueous isopropanol 4; be warming up to 100 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 8h.At vacuum tightness-0.096Mpa, pull out dimethylbenzene, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 20700, PDI is 2.31, and wherein alkyl content is 0.979mmol/g, and phenyl content is 7.8mol.%, refractive index n
d 25=1.4377; 10% thermal degradation temperature is 469 DEG C; Not stratified after dissolving each other with mineral oil.
Embodiment 5
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 47.48g (phenyl content is 5mol.%), hexamethyldisiloxane 1.5228g, high containing hydrogen silicone oil 0.9972, perchloric acid 0.5g; 24h is reacted at 25 DEG C; then add 2g anhydrous sodium bicarbonate fully to neutralize; through high speed centrifugation desalination; at vacuum tightness-0.096Mpa; pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add Virahol 12g, 1-laurylene 1.89g, Platinic chloride/aqueous isopropanol 1; be warming up to 75 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 8h.At vacuum tightness-0.096Mpa, pull out Virahol, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 5700, PDI is 1.61, and wherein alkyl content is 0.295mmol/g, and phenyl content is 3.6mol.%, refractive index n
d 25=1.4174; 10% thermal degradation temperature is 367 DEG C; With layering in 3 ~ 4 days after mineral oil.
Embodiment 6
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 47.48g (phenyl content is 20mol.%), dimethyltetraphenyldisiloxane 3.9292g, high containing hydrogen silicone oil 0.9972, vitriol oil 0.5g; 24h is reacted at 25 DEG C; then add 2g anhydrous sodium bicarbonate fully to neutralize; through high speed centrifugation desalination; at vacuum tightness-0.096Mpa; pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add propyl carbinol 12g, 1-laurylene 6.94g, Platinic chloride/aqueous isopropanol 4; be warming up to 90 DEG C; slowly instill in reaction system with the methyl and phenyl hydrogen-containing silicon oil 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 10h.At vacuum tightness-0.096Mpa, pull out propyl carbinol, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by the present embodiment, outward appearance clear, its molecular weight is 4500, PDI is 1.71, and wherein alkyl content is 0.295mmol/g, and phenyl content is 14.6mol.%, refractive index n
d 25=1.4529; 10% thermal degradation temperature is 407 DEG C; Not stratified after dissolving each other with mineral oil.
Comparative example 1
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add octamethylcyclotetrasiloxane 47.48g, hexamethyldisiloxane 1.5228g, high containing hydrogen silicone oil 0.9972g, 98% vitriol oil 0.5g; 24h is reacted at 25 DEG C; then add 2g anhydrous sodium bicarbonate fully to neutralize; through high speed centrifugation desalination; at vacuum tightness-0.096Mpa, pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain Methyl Hydrogen Polysiloxane Fluid.
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add toluene 10g, 1-laurylene 1.89g, Platinic chloride/aqueous isopropanol 1; be warming up to 75 DEG C; slowly instill in reaction system with the Methyl Hydrogen Polysiloxane Fluid 25g of constant pressure funnel by above-mentioned synthesis, drip off in 2h.Continue reaction 6h.At vacuum tightness-0.096Mpa, pull out toluene, unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain phenylalkyl silicone oil.
Phenylalkyl silicone oil prepared by this comparative example, outward appearance clear, its molecular weight is 5500, PDI is 1.65, and wherein alkyl content is 0.292mmol/g, refractive index n
d 25=1.4104; 10% thermal degradation temperature is 285 DEG C; With layering in 3 ~ 4 days after mineral oil.
Comparative example 2
At N
2under protection; be equipped with in the dry four-hole bottle of 100mL of reflux condensate device, thermometer, mechanical stirrer to one and add aminomethyl phenyl mixed methylcyclosiloxane 48.4772g (phenyl content is 10mol.%), hexamethyldisiloxane 1.5228g, 98% vitriol oil 0.5g; 24h is reacted at 25 DEG C; then add 2g anhydrous sodium bicarbonate fully to neutralize; through high speed centrifugation desalination; at vacuum tightness-0.096Mpa, pull out unreacting material and low-boiling-point substance 2h at 205 DEG C, obtain methyl phenyl silicone oil.
Methyl phenyl silicone oil prepared by this comparative example, outward appearance clear, its molecular weight is 5300, PDI is 1.62, and wherein phenyl content is 7.9mol.%, refractive index n
d 25=1.4262; 10% thermal degradation temperature is 373 DEG C; Do not dissolve each other with mineral oil, layering at once after mixing.
Claims (9)
1. a preparation method for phenylalkyl silicone oil, is characterized in that, comprises the steps:
(1) under protection of inert gas, high containing hydrogen silicone oil, aminomethyl phenyl mixed methylcyclosiloxane, end-capping reagent and strong acid are mixed, react 6 ~ 24h at 25 ~ 80 DEG C, obtain methyl and phenyl hydrogen-containing silicon oil through aftertreatment;
The mass ratio of described high containing hydrogen silicone oil, aminomethyl phenyl mixed methylcyclosiloxane, end-capping reagent and strong acid is 1: 5 ~ 50: 1 ~ 5: 1 ~ 12:
(2) under protection of inert gas, by alpha-olefin, organic solvent and Platinic chloride/aqueous isopropanol mixing, be heated to 60 ~ 120 DEG C, and mix with methyl and phenyl hydrogen-containing silicon oil prepared by step (1), after reaction, obtain phenylalkyl silicone oil through purification process;
The mass ratio of described alpha-olefin, organic solvent, Platinic chloride/aqueous isopropanol and methyl and phenyl hydrogen-containing silicon oil is 1: 0.3 ~ 200: 0.001 ~ 1: 1 ~ 250.
2. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, the chemical structural formula of described high containing hydrogen silicone oil is such as formula shown in (I):
Wherein, a is selected from natural number, and b is selected from the natural number not comprising 0, and a, b are separate, and a+b=1 ~ 50.
3. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, the chemical structural formula of described aminomethyl phenyl mixed methylcyclosiloxane is such as formula shown in (II):
Wherein, x, y are independently selected from the natural number not comprising 0, and x+y=3 ~ 6.
4. the preparation method of phenylalkyl silicone oil according to claim 1, it is characterized in that, described end-capping reagent is at least one in hexamethyldisiloxane, trimethylmethoxysilane, trimethylethoxysilane, tetramethyl-phenylbenzene sily oxide, dimethyl benzene methoxylsilane, 3,5-dimethylphenyl Ethoxysilane, dimethyltetraphenyldisiloxane, methyldiphenyl methoxylsilane, methyldiphenylethoxysilane, hexaphenyldisiloxane, triphenylmethoxy silane, triphenyl Ethoxysilane;
Described strong acid is selected from the one in the vitriol oil, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, trifluoromethanesulfonic acid, acidic white earth, solid super-strong acid, macropore strong acid cation exchange resin.
5. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, described organic solvent is at least one in toluene, dimethylbenzene, tetrahydrofuran (THF), Virahol, propyl carbinol, normal hexane, sherwood oil.
6. the preparation method of phenylalkyl silicone oil according to claim 1, it is characterized in that, methyl and phenyl hydrogen-containing silicon oil step (1) prepared instills in the mixing solutions be made up of alpha-olefin, organic solvent and Platinic chloride/aqueous isopropanol, and in dropping process, in guarantee system, temperature is no more than 90 DEG C.
7. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, the aftertreatment described in step (1) is:
The reaction solution that step (1) obtains is cooled to room temperature, adds excessive neutralizing agent and fully stir, neutralize, then through high speed centrifugation removing solid wherein, vacuum removal retained material and low-boiling-point substance;
Described neutralizing agent is at least one in carbonate, supercarbonate, oxidized metal;
Described vacuum removal condition is: vacuum tightness is-0.075 ~-0.096Mpa, and temperature is 150 ~ 210 DEG C, and the time of removing is 1 ~ 4h.
8. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, in step (2), reacts extremely: at V
si-H=2158cm
-1place, through infrared detection without till Si-H absorption peak, then carries out purification process.
9. the preparation method of phenylalkyl silicone oil according to claim 1, is characterized in that, in step (2), described purification process is vacuum removal organic solvent, residual reaction raw materials and low-boiling-point substance;
Described vacuum removal condition is: vacuum tightness is-0.075 ~-0.096Mpa, and temperature is 150 ~ 210 DEG C, and the time of removing is 1 ~ 4h.
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| CN105524284B (en) * | 2016-01-12 | 2018-12-11 | 浙江大学 | A kind of polysiloxanes-polyethylene graft copolymer and its preparation method and application |
| CN105524284A (en) * | 2016-01-12 | 2016-04-27 | 浙江大学 | Polyorganosiloxane-polyethylene grafted copolymer and preparation method and application thereof |
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| CN107233862A (en) * | 2017-08-02 | 2017-10-10 | 王艺霖 | A kind of preparation method of methyl phenyl silicone oil adsorbent |
| CN107814586B (en) * | 2017-10-26 | 2020-11-06 | 杭州瑞江新材料技术有限公司 | Organic silicon waterproof and oilproof emulsion and preparation method thereof |
| CN107814586A (en) * | 2017-10-26 | 2018-03-20 | 杭州瑞江新材料技术有限公司 | A kind of novel organosilicon waterproof and oilproof emulsion and preparation method thereof |
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| 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 |
| CN112574417A (en) * | 2020-11-27 | 2021-03-30 | 山东大易化工有限公司 | Preparation method of release agent suitable for medium-high temperature metal die casting |
| CN112778527A (en) * | 2021-01-05 | 2021-05-11 | 吉林大学 | Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low silicone oil agent for carbon fibers |
| CN112778527B (en) * | 2021-01-05 | 2022-05-27 | 吉林大学 | Polyol fatty acid ester/phenyl/polyether co-modified silicone oil, preparation method and special low silicone oil agent for carbon fibers |
| CN114133567A (en) * | 2021-09-11 | 2022-03-04 | 唐山三友硅业有限责任公司 | Preparation method of polysiloxane cross-linking agent |
| CN114133567B (en) * | 2021-09-11 | 2022-11-22 | 唐山三友硅业有限责任公司 | Preparation method of polysiloxane cross-linking agent |
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