CN1834133A - Branched benzene siliconic oil - Google Patents
Branched benzene siliconic oil Download PDFInfo
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- CN1834133A CN1834133A CN 200610034998 CN200610034998A CN1834133A CN 1834133 A CN1834133 A CN 1834133A CN 200610034998 CN200610034998 CN 200610034998 CN 200610034998 A CN200610034998 A CN 200610034998A CN 1834133 A CN1834133 A CN 1834133A
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- silicone oil
- phenyl
- phenyl silicone
- structural formula
- water
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 title 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 37
- 229920002545 silicone oil Polymers 0.000 claims abstract description 34
- 239000002537 cosmetic Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 7
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 125000003118 aryl group Chemical group 0.000 claims abstract description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 3
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000010792 warming Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 4
- -1 siloxanes Chemical class 0.000 claims description 4
- 230000009967 tasteless effect Effects 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 230000009965 odorless effect Effects 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 238000000967 suction filtration Methods 0.000 description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004166 Lanolin Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 description 2
- 229940039717 lanolin Drugs 0.000 description 2
- 235000019388 lanolin Nutrition 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000005051 trimethylchlorosilane Substances 0.000 description 2
- VSIKJPJINIDELZ-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octakis-phenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VSIKJPJINIDELZ-UHFFFAOYSA-N 0.000 description 1
- IRVZFACCNZRHSJ-UHFFFAOYSA-N 2,4,6,8-tetramethyl-2,4,6,8-tetraphenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 IRVZFACCNZRHSJ-UHFFFAOYSA-N 0.000 description 1
- MVHZHMKEBJJTCH-UHFFFAOYSA-N CN(C)C.CO[SiH3] Chemical compound CN(C)C.CO[SiH3] MVHZHMKEBJJTCH-UHFFFAOYSA-N 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003845 household chemical Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- NYMPGSQKHIOWIO-UHFFFAOYSA-N hydroxy(diphenyl)silicon Chemical group C=1C=CC=CC=1[Si](O)C1=CC=CC=C1 NYMPGSQKHIOWIO-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
This invention relates to a branch-type silicone oil with a structural formula which R1, R2 and R3 represent alkyl or aryl and methyl, ethyl and phenyl are considered in prior. R1, R2 and R3 can be the same or not. The polymerization degree n is an integral between 1 and 100. This invention also relates to the method to prepare the branch-type phenyl silicone oil. The branch-type phenyl silicone oil is smell-less and colorless transparent liquid, with the characteristics of low viscosity and high refractive index. It is compatible with kinds of cosmetic raw materials and contains no heavy metal.
Description
Technical field
The present invention relates to a kind of silicone oil and preparation method, relate in particular to a kind of branched chain type phenyl silicone oil and preparation method thereof.
Background technology
Phenyl silicone oil is one of principal item of silicone oil, because it has good chemical stability, resistant of high or low temperature, electrical insulating property, performances such as radiation resistance and physiology inertia are widely used in aspects such as household chemicals, electronics, machinery.
The polydimethylsiloxane of traditional phenyl silicone oil linearity that to be part methyl replaced by phenyl, its structure is as follows:
Wherein R can be methyl or phenyl, and m, n, p also may be 0.
Their synthetic route is divided into two kinds of hydrolytie polycondensation and ring-opening polymerizations:
1, obtains by hydrolysis condensation reaction
With any or several synthetic main chains in dimethyldichlorosilane(DMCS), dimethyl dialkoxy silicane, phenylmethyldichloroislane, phenyl methyl dialkoxy silicane, diphenyl dichlorosilane, the phenylbenzene dialkoxy silicane, with in trimethylchlorosilane, trimethylammonium organoalkoxysilane, methyldiphenyl base chlorosilane, the methyldiphenyl base organoalkoxysilane any or several be end-capping reagent, obtain by hydrolytie polycondensation.
2, obtain by ring-opening polymerization
Mainly be octamethylcyclotetrasiloxane, dimethyl cyclosiloxane and tetramethyl tetraphenyl cyclotetrasiloxane, octaphenyl cyclotetrasiloxane etc., ring-opening polymerization under the catalysis of acid or alkali, and obtain with end-blockings such as hexamethyldisiloxane.
Traditional phenyl silicone oil has limited its application in cosmetic field owing to have following weak point:
1, have certain polar material with ethanol, glycerol etc. and have paraffin, the mineral wet goods material intermiscibility of long carbochain bad;
2, be difficult to accomplish to have high refractive index under the low viscosity;
3, cosmetic material is very strict to the requirement of smell and color and luster, is difficult to accomplish colorless and odorless, and the silicone oil smell that particularly has the diphenyl siloxane chain link is more obvious.
Summary of the invention
Technical problem to be solved by this invention provides a kind of branched chain type phenyl silicone oil.This branched chain type phenyl silicone oil, outward appearance are colourless transparent liquid, and tasteless; With low-pole material such as ethanol commonly used in the makeup, glycerol with to have the plurality of raw materials intermiscibilities such as paraffin, white mineral oil of long carbochain all fine, and also has higher refractive index under the low viscosity, be particularly suitable as cosmetic material, be used in the products such as skin care product, sunscreen, lipstick.
Another technical problem to be solved by this invention is the preparation method of above-mentioned branched chain type phenyl silicone oil.
The present invention solves the technical scheme that its technical problem adopts: a kind of branched chain type phenyl silicone oil, and its structural formula is:
R wherein
1, R
2, R
3Be alkyl or aryl, preferable methyl, ethyl or phenyl; R
1, R
2, R
3Can be identical, also can be inequality;
The integer of polymerization degree n=1～100;
It is synthesized into by following weight per-cent proportioning raw material:
A, phenyl silane 15～30%
B, end-capping reagent 20～45%
C, catalyzer 0～15%
D, water 20～65%;
Its fundamental property is:
Outward appearance: colourless transparent liquid
Smell: tasteless
General 15～the 100mPa.s of viscosity in the time of 20 ℃: 15～500mPa.s
Refractive index in the time of 20 ℃: 1.4550～1.5000
Proportion in the time of 20 ℃: 0.9700～1.1000.
Above-mentioned phenyl silane is to satisfy any in the following structural formula:
Wherein X can select halogen or alkoxyl group for use, preferred chlorine, methoxy or ethoxy.
Above-mentioned end-capping reagent is to satisfy the silane of following structural formula I or satisfy any in the siloxanes of structural formula II:
R wherein
1, R
2, R
3Be alkyl or aryl, preferable methyl, ethyl or phenyl, R
1, R
2, R
3Can be identical, also can be inequality; X can be halogen or alkoxyl group, preferred chlorine, methoxy or ethoxy.
Above-mentioned catalyzer is any in protonic acid or the strong-acid ion exchange resin, preferred hydrochloric acid.
Above-mentioned water can be selected distilled water, deionized water, process water and tap water for use, preferred deionized water.
The present invention solves the technical scheme that another technical problem adopts:
The preparation method of above-mentioned branched chain type phenyl silicone oil, it comprises the steps: water and catalyzer joined in the reactor and stirs, and phenyl silane and end-capping reagent are mixed, and evenly is added drop-wise in 1～8 hour in the reactor, and control reaction temperature is at 5～60 ℃; Drip and be warming up to 50～80 ℃, reacted again 1～6 hour; Reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 1.3～11.3KPa, 80～150 ℃ of following underpressure distillation 1～4 hour; Be cooled to room temperature, add gac, be warming up to 40～80 ℃, stirred 0.5～4 hour, filter then and obtain product.
Synthetic route of the present invention:
According to used end-capping reagent difference, reaction scheme has following two kinds:
Reaction formula 1:
Reaction formula 2;
Excellent effect of the present invention:
The present invention has prepared the branched chain type phenyl silicone oil with phenyl silane and end-capping reagent, and n can reconcile within the specific limits, by changing and reconcile the consumption of four kinds of raw materials, can obtain different viscosity, and the phenyl silicone oil of different refractive index can reach following fundamental property:
Outward appearance: colourless transparent liquid
Smell: tasteless
General 15～the 100mPa.s of viscosity in the time of 20 ℃: 15～500mPa.s
Refractive index in the time of 20 ℃: 1.4550～1.5000
Proportion in the time of 20 ℃: 0.9700～1.1000.
The product that the present invention obtains is compared with traditional phenyl silicone oil, has colorless and odorless, and is transparent, has high refractive index under the low viscosity, and for example viscosity is the phenyl silicone oil of 15mPa.s, and refractive index can reach 1.455; Comprise that with multiple cosmetic material ethanol, glycerine, white mineral oil, paraffin, lanolin etc. all have good intermiscibility; Safe, do not contain heavy metal.Table 1 is the intermiscibility of raw material commonly used in the phenyl silicone oil for preparing of the present invention and the makeup.
The intermiscibility of raw material commonly used in table 1 phenyl silicone oil and the makeup
| Raw material | The phenyl silicone oil (weight ratio) of cosmetic material/the present invention's preparation | ||
| 1/10 | 1/1 | 10/1 | |
| Water | I | I | I |
| Dehydrated alcohol | C | C | C |
| Ethanol (75%) | I | I | I |
| Virahol | C | C | C |
| Virahol (70%) | I | I | I |
| Stearyl alcohol | C | C | C |
| White mineral oil (26#) | C | C | C |
| Lanolin | C | C | C |
| Whiteruss | C | C | C |
| Glycerine | C | C | C |
| Solid paraffin | C | C | C |
C represents to mix fully, and I represents that part is immiscible or immiscible fully.
Describe the present invention in detail below in conjunction with specific embodiment
Embodiment
Embodiment 1
With stirring in the 565g deionized water adding 1L four-hole boiling flask, 131g phenyl-trichloro-silicane and 174g trimethylchlorosilane are mixed, in 8 hours, evenly be added drop-wise in the flask, control reaction temperature is at 5 ℃; Drip and be warming up to 60 ℃, reacted again 1 hour, reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then under 1.3KPa, 100 ℃, underpressure distillation 4 hours; After reducing to room temperature, add gac, be warming up to 50 ℃, stirred 0.5 hour, suction filtration obtains the product 132g of colorless and odorless then, and viscosity is 28mPa.s, and refractive index is 1.4669, and proportion is 1.005.
Embodiment 2
With 290g deionized water and 52g mass concentration is that 36% hydrochloric acid adds in the 1L four-hole boiling flask and stirs, and 162g phenyl triethoxysilane and 350g trimethylethoxysilane are mixed, and evenly is added drop-wise in 1 hour in the flask, and control reaction temperature is at 50 ℃; Drip and be warming up to 80 ℃, reacted again 6 hours, reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 1.3KPa, 80 ℃ of following underpressure distillation 4 hours; Add gac after reducing to room temperature, be warming up to 80 ℃, stirred 2 hours, suction filtration obtains the product 160g of colorless and odorless then, and viscosity is 15mPa.s, and refractive index is 1.4552, and proportion is 0.9726.
Embodiment 3
With 222g deionized water and 72g mass concentration is that 38% hydrochloric acid adds in the 1L four-hole boiling flask and stirs, and 196g phenyl triethoxysilane and 400g hexamethyldisiloxane are mixed, and evenly is added drop-wise in 2 hours in the flask, and control reaction temperature is at 60 ℃; Drip and be warming up to 75 ℃, reacted again 3 hours, reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 11.3KPa, 150 ℃ of following underpressure distillation 2 hours; Add gac after reducing to room temperature, be warming up to 40 ℃, stirred 4 hours, suction filtration obtains the product 210g of colorless and odorless then, and viscosity is 20mPa.s, and refractive index is 1.4600, and proportion is 0.9804.
Embodiment 4
290g deionized water and 131g strong-acid ion exchange resin joined in the 1L four-hole boiling flask stir, after 203g phenyl triethoxysilane and 250g hexamethyldisiloxane mixed, evenly be added drop-wise in 7 hours in the flask, control reaction temperature is at 15 ℃; Drip and be warming up to 75 ℃, reacted again 6 hours, reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 6.3KPa, 125 ℃ of following underpressure distillation 3.5 hours; Add gac after reducing to room temperature, be warming up to 45 ℃, stirred 3.5 hours, suction filtration obtains the product 140g of colorless and odorless then, and viscosity is 98mPa.s, and refractive index is 1.4786, and proportion is 1.0550.
Embodiment 5
600g water and the 40g vitriol oil joined in the 2L four-hole boiling flask stir, after 400g phenyl triethoxysilane and 300g trimethylethoxysilane are mixed, evenly be added drop-wise in 4 hours in the flask, control reaction temperature is at 50 ℃; Drip and be warming up to 80 ℃, reacted again 4 hours, reacted and left standstill branch water; Oil phase is carried out alkali cleaning and washing repeatedly until neutrality, then 2KPa, 130 ℃ of following underpressure distillation 2 hours; Add gac after reducing to room temperature, be warming up to 40 ℃, stirred 1 hour, suction filtration obtains the product 420g of colorless and odorless then, and viscosity is 52mPa.s, and refractive index is 1.4700, and proportion is 1.011.
Embodiment 6
150g water and 38g strong-acid ion exchange resin joined in the 1L four-hole boiling flask stir, after 225g phenyltrimethoxysila,e and 337g trimethylammonium methoxy silane are mixed, evenly be added drop-wise in 6 hours in the flask, control reaction temperature is at 40 ℃; Drip and be warming up to 50 ℃, reacted again 6 hours, reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 2.6KPa, 115 ℃ of following underpressure distillation 1 hour; Add gac after reducing to room temperature, be warming up to 55 ℃, stirred 2 hours, suction filtration obtains the product 245g of colorless and odorless then, and viscosity is 32mPa.s, and refractive index is 1.4631, and proportion is 0.9857.
Claims (10)
1, a kind of branched chain type phenyl silicone oil, it is characterized in that: its structural formula is:
R wherein
1, R
2, R
3Be alkyl or aryl, R
1, R
2, R
3Can be identical, also can be inequality;
The integer of polymerization degree n=1～100;
It is synthesized into by following weight per-cent proportioning raw material:
A, phenyl silane 15～30%
B, end-capping reagent 20～45%
C, catalyzer 0～15%
D, water 20～65%;
Its fundamental property is:
Outward appearance: colourless transparent liquid
Smell: tasteless
General 15～the 100mPa.s of viscosity in the time of 20 ℃: 15～500mPa.s
Refractive index in the time of 20 ℃: 1.4550～1.5000
Proportion in the time of 20 ℃: 0.9700～1.1000.
2, branched chain type phenyl silicone oil according to claim 1 is characterized in that: the R in the structural formula of described branched chain type phenyl silicone oil
1, R
2, R
3Be methyl, ethyl or phenyl, R
1, R
2, R
3Can be identical, also can be inequality.
3, branched chain type phenyl silicone oil according to claim 1 is characterized in that: described phenyl silane is to satisfy any in the following structural formula:
Wherein X can select halogen or alkoxyl group for use.
4, branched chain type phenyl silicone oil according to claim 3, it is characterized in that: the X in the structural formula of described phenyl silane can select chlorine, methoxy or ethoxy for use.
5, used for cosmetic phenyl silicone oil according to claim 1 is characterized in that: described end-capping reagent is to satisfy the silane of following structural formula I or satisfy any in the siloxanes of structural formula II:
R wherein
1, R
2, R
3Be alkyl or aryl, R
1, R
2, R
3Can be identical, also can be inequality; X can be halogen or alkoxyl group.
6, used for cosmetic phenyl silicone oil according to claim 5 is characterized in that: described end-capping reagent is to satisfy the silane of following structural formula I or satisfy any in the siloxanes of structural formula II, the R in their structural formula
1, R
2, R
3Be methyl, ethyl or phenyl; X can be chlorine, methoxy or ethoxy.
7, used for cosmetic phenyl silicone oil according to claim 1 is characterized in that: described catalyzer is any in protonic acid or the strong-acid ion exchange resin.
8, used for cosmetic phenyl silicone oil according to claim 1 is characterized in that: described catalyzer is a hydrochloric acid.
9, used for cosmetic phenyl silicone oil according to claim 1, it is characterized in that: described water can be selected distilled water, deionized water, process water and tap water for use.
10, the preparation method of any one described branched chain type phenyl silicone oil of claim 1-9, it is characterized in that, it comprises the steps: water and catalyzer joined in the reactor and stirs, phenyl silane and end-capping reagent are mixed, evenly be added drop-wise in 1～8 hour in the reactor, control reaction temperature is at 5～60 ℃; Drip and be warming up to 50～80 ℃, reacted again 1～6 hour; Reacted and left standstill branch water; Oil phase is carried out alkali cleaning repeatedly and washes until neutrality; Then 1.3～11.3KPa, 80～150 ℃ of following underpressure distillation 1～4 hour; Be cooled to room temperature, add gac, be warming up to 40～80 ℃, stirred 0.5～4 hour, filter then and obtain product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100349982A CN100396715C (en) | 2006-04-17 | 2006-04-17 | Branched benzene siliconic oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100349982A CN100396715C (en) | 2006-04-17 | 2006-04-17 | Branched benzene siliconic oil |
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| Publication Number | Publication Date |
|---|---|
| CN1834133A true CN1834133A (en) | 2006-09-20 |
| CN100396715C CN100396715C (en) | 2008-06-25 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100349982A Active CN100396715C (en) | 2006-04-17 | 2006-04-17 | Branched benzene siliconic oil |
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| Country | Link |
|---|---|
| CN (1) | CN100396715C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1998103A1 (en) * | 2007-06-01 | 2008-12-03 | Foxsemicon Integrated Technology, Inc. | Light source assembly and backlight module including the same |
| CN100471898C (en) * | 2007-02-09 | 2009-03-25 | 南京大学 | Method of preparing star-type multi-arm silicon oil |
| CN101875724B (en) * | 2009-04-30 | 2012-08-08 | 东莞市贝特利新材料有限公司 | Preparation method of phenyl silicone resin |
| CN103435806A (en) * | 2013-07-17 | 2013-12-11 | 烟台德邦先进硅材料有限公司 | Branched chain type phenyl silicone oil and preparation methods thereof |
| CN105199109A (en) * | 2015-09-29 | 2015-12-30 | 广州有色金属研究院 | Preparation method of MDT-type phenyl methyl silicone oil for cosmetics |
| CN106977721A (en) * | 2017-04-26 | 2017-07-25 | 中国石油化工股份有限公司 | A kind of method for hydrolysis of silicone oil monomer |
| CN109796597A (en) * | 2019-01-25 | 2019-05-24 | 江南大学 | A kind of preparation method of branched chain type silane, polyoxyalkylene alkyl co-modified silicone oil |
| CN116396479A (en) * | 2023-04-13 | 2023-07-07 | 广东雷邦高新材料有限公司 | Preparation method of methyl MT silicone oil for cosmetics |
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| GB2096631A (en) * | 1981-04-09 | 1982-10-20 | Gen Electric | Fluorosilicone rubber composition process and polymer |
| CN1230463C (en) * | 2002-01-10 | 2005-12-07 | 中国石油化工股份有限公司 | Prepn of phenyl sesquisiloxane prepolymer |
| CN1569925A (en) * | 2004-04-29 | 2005-01-26 | 上海高分子材料研究开发中心 | Novel configuration phenyl methyl silicon oil |
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2006
- 2006-04-17 CN CNB2006100349982A patent/CN100396715C/en active Active
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| CN100471898C (en) * | 2007-02-09 | 2009-03-25 | 南京大学 | Method of preparing star-type multi-arm silicon oil |
| EP1998103A1 (en) * | 2007-06-01 | 2008-12-03 | Foxsemicon Integrated Technology, Inc. | Light source assembly and backlight module including the same |
| CN101875724B (en) * | 2009-04-30 | 2012-08-08 | 东莞市贝特利新材料有限公司 | Preparation method of phenyl silicone resin |
| CN103435806A (en) * | 2013-07-17 | 2013-12-11 | 烟台德邦先进硅材料有限公司 | Branched chain type phenyl silicone oil and preparation methods thereof |
| CN103435806B (en) * | 2013-07-17 | 2015-09-02 | 烟台德邦先进硅材料有限公司 | A kind of branched chain type phenyl silicone oil and preparation method thereof |
| CN105199109A (en) * | 2015-09-29 | 2015-12-30 | 广州有色金属研究院 | Preparation method of MDT-type phenyl methyl silicone oil for cosmetics |
| CN105199109B (en) * | 2015-09-29 | 2017-10-10 | 广州有色金属研究院 | A kind of preparation method of MDT types polymethylphenyl siloxane fluid used for cosmetic |
| CN106977721A (en) * | 2017-04-26 | 2017-07-25 | 中国石油化工股份有限公司 | A kind of method for hydrolysis of silicone oil monomer |
| CN106977721B (en) * | 2017-04-26 | 2020-11-06 | 中国石油化工股份有限公司 | Hydrolysis method of silicone oil monomer |
| CN109796597A (en) * | 2019-01-25 | 2019-05-24 | 江南大学 | A kind of preparation method of branched chain type silane, polyoxyalkylene alkyl co-modified silicone oil |
| CN116396479A (en) * | 2023-04-13 | 2023-07-07 | 广东雷邦高新材料有限公司 | Preparation method of methyl MT silicone oil for cosmetics |
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| CN100396715C (en) | 2008-06-25 |
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