CN115386086A - Preparation method of dimethyl silicone oil - Google Patents
Preparation method of dimethyl silicone oil Download PDFInfo
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- CN115386086A CN115386086A CN202210924614.3A CN202210924614A CN115386086A CN 115386086 A CN115386086 A CN 115386086A CN 202210924614 A CN202210924614 A CN 202210924614A CN 115386086 A CN115386086 A CN 115386086A
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 67
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000003513 alkali Substances 0.000 claims abstract description 59
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 239000003292 glue Substances 0.000 claims abstract description 30
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 24
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229940083037 simethicone Drugs 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 58
- 238000000034 method Methods 0.000 claims description 37
- 239000000126 substance Substances 0.000 claims description 37
- 239000003921 oil Substances 0.000 claims description 29
- 230000035484 reaction time Effects 0.000 claims description 19
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 18
- 229920001296 polysiloxane Polymers 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 8
- 239000002585 base Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 229940008099 dimethicone Drugs 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 5
- -1 tetramethylammonium hydroxide silicon alkoxide Chemical class 0.000 claims description 3
- YFCGDEUVHLPRCZ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C YFCGDEUVHLPRCZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims description 2
- JEULYRSRLMIJQJ-UHFFFAOYSA-N silyloxy(tetradecylsilyloxysilyloxysilyloxysilyloxy)silane Chemical compound C(CCCCCCCCCCCCC)[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH3] JEULYRSRLMIJQJ-UHFFFAOYSA-N 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 238000001914 filtration Methods 0.000 description 9
- MYXKPFMQWULLOH-UHFFFAOYSA-M tetramethylazanium;hydroxide;pentahydrate Chemical compound O.O.O.O.O.[OH-].C[N+](C)(C)C MYXKPFMQWULLOH-UHFFFAOYSA-M 0.000 description 9
- 239000002994 raw material Substances 0.000 description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 6
- 208000005156 Dehydration Diseases 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000010292 electrical insulation Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000007171 acid catalysis Methods 0.000 description 2
- 238000005815 base catalysis Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 1
- IUMSDRXLFWAGNT-UHFFFAOYSA-N Dodecamethylcyclohexasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 IUMSDRXLFWAGNT-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- ADANNTOYRVPQLJ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-[[dimethyl(trimethylsilyloxy)silyl]oxy-dimethylsilyl]oxy-dimethylsilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C ADANNTOYRVPQLJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 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
- 230000009965 odorless effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 229940008424 tetradecamethylhexasiloxane Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of dimethyl silicone oil, and relates to the technical field of dimethyl silicone oil. The preparation method comprises the following steps: s1, dehydrating a first organic silicon intermediate, adding an alkali glue and an end-capping reagent, and heating to 95-115 ℃ in a nitrogen atmosphere to react to obtain a first mixture; s2, heating the first mixture to 150-170 ℃, and reacting to obtain a second mixture; s3, continuously reacting under the first negative pressure condition to obtain a third mixture; s4, continuously heating the third mixture to 175-185 ℃, reducing the pressure, and reacting under a second negative pressure condition to obtain a fourth mixture; and S5, introducing inert gas into the fourth mixture, and reacting to obtain the simethicone. The preparation method can prepare the dimethyl silicone oil with no smell and adjustable viscosity.
Description
Technical Field
The invention relates to the technical field of dimethyl silicone oil, in particular to a preparation method of dimethyl silicone oil.
Background
With the rapid development of the power industry, more and more cable accessories are used. The cable accessories need to have good insulating properties to meet the requirements of high-voltage power transmission. The simethicone is colorless and odorless transparent liquid, has good heat resistance, acid resistance and cold resistance, stable chemical property, high boiling point and low freezing point, and is widely applied to motors, electric appliances and electronic instruments as a temperature-resistant, arc corona-resistant, corrosion-resistant, moisture-proof and dust-proof insulating medium.
The existing methods for synthesizing the simethicone comprise an acid catalysis method, a cation resin exchange resin method, a temporary base catalysis method and the like. Wherein, the acid catalysis method needs neutralization subsequently, and the post-treatment is troublesome; the cation resin exchange resin method has high cost and cannot produce high-viscosity silicone oil; the temporary base catalysis method utilizes tetramethylammonium hydroxide as a catalyst, the prepared dimethyl silicone oil has residual smell, and the density of the molten tetramethylammonium hydroxide is higher, so that the tetramethylammonium hydroxide is deposited at the bottom and is not beneficial to the synthesis of the subsequent dimethyl silicone oil. Therefore, a method for preparing dimethyl silicone oil is needed, and the dimethyl silicone oil prepared by the method has no smell and adjustable viscosity.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of the dimethyl silicone oil, and the preparation method can prepare the dimethyl silicone oil which is free of smell and adjustable in viscosity.
The invention also provides the simethicone prepared by the preparation method.
The invention also provides application of the simethicone.
According to the embodiment of the first aspect of the invention, the preparation method of the simethicone comprises the following steps:
s1, dehydrating a first organic silicon intermediate, adding an alkali glue and an end-capping reagent, and heating to 95-115 ℃ in a nitrogen atmosphere to react to obtain a first mixture;
s2, heating the first mixture to 150-170 ℃, and reacting to obtain a second mixture;
s3, continuously reacting under the first negative pressure condition to obtain a third mixture;
s4, continuously heating the third mixture to 175-185 ℃, reducing the pressure, and reacting under a second negative pressure condition to obtain a fourth mixture;
and S5, introducing inert gas into the fourth mixture, and reacting to obtain the simethicone.
The preparation method provided by the embodiment of the invention has at least the following beneficial effects:
the preparation method of the embodiment has the advantages of low cost, no need of using a solvent, simple process and no complex post-treatment. The viscosity of the dimethyl silicone oil can be controlled by controlling the feeding ratio of the end-capping reagent to the alkali glue, and the viscosity of the synthesized dimethyl silicone oil is between 100mpa & s and 100000mpa & s. The comprehensive utilization of low-boiling-point substances is realized, the comprehensive utilization rate of the first organic silicon intermediate reaches more than 95%, the dimethyl silicone oil with excellent electrical insulation performance is obtained, and the residual odor in the silicone oil is reduced.
The decomposition of the tetramethylammonium hydroxide can generate trimethylamine which has fishy smell and is partially dissolved in a silicone oil system, and the two-stage devolatilization process (steps S3 and S4) and the inert gas (such as nitrogen) devolatilization process are adopted to facilitate the discharge of the trimethylamine dissolved in the system, so that the residual smell in the silicone oil is reduced.
Water in the raw materials can form hydroxyl silicone oil in the reaction, and the hydroxyl silicone oil can be polarized at high temperature to influence the high-temperature volume resistivity; the low-boiling-point substance has strong movement capability at high temperature, and can affect the dielectric loss and the high-temperature volume resistivity of the dimethyl silicone oil. The low-boiling-point substances are removed by dehydration, a two-section devolatilization process and a nitrogen devolatilization process, so that the electrical insulation property of the dimethyl silicone oil is effectively improved.
Through the reaction of the step S1, the viscosity of the silicone oil is favorably controlled. By the reaction of step S2, tetramethylammonium hydroxide can be rapidly decomposed, and the catalyst residue can be reduced. By the reaction of step S3, unreacted small molecule substances can be removed. The reaction in step S4 can further reduce the residue of small molecule substances. By the reaction of step S5, the residual odor of the silicone oil can be reduced while improving the electrical insulating properties of the silicone oil. Wherein the small molecular substance is a side reaction product, namely a low-boiling-point substance.
According to some embodiments of the present invention, the first silicone intermediate comprises at least one of hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6), and decatetramethylcycloheptasiloxane (D7).
According to some embodiments of the invention, the end-capping agent comprises at least one of hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane, dodecamethylwuasiloxane, tetradecamethylhexasiloxane, and first dimethylsilicone oil.
According to some embodiments of the invention, the viscosity of the first dimethyl silicone oil is between 1mPa · s and 100mPa · s.
According to some embodiments of the invention, the base catalyst is tetramethylammonium hydroxide and its silicon alkoxide.
According to some embodiments of the invention, the mass ratio of the first silicone intermediate to the alkali gum is 100:0.1 to 1.5.
According to some embodiments of the present invention, the mass ratio of the first silicone intermediate to the alkali gum is 100:0.25 to 1.
According to some embodiments of the present invention, the mass ratio of the first silicone intermediate to the endcapping agent is 100:1 to 30.
According to some embodiments of the present invention, the mass ratio of the first silicone intermediate to the endcapping agent is 100:2 to 24.
According to some embodiments of the invention, the viscosity of the alkali gum is 1500 to 2500 mpa-s.
According to some embodiments of the invention, the method of making the alkali gum comprises the steps of: and mixing and dehydrating the alkali catalyst and the second organic silicon intermediate, and reacting at 85-100 ℃ in a nitrogen atmosphere under a third negative pressure condition to obtain the alkali glue. Thus, an alkali gel having a stable viscosity (1500 to 2500mPa · s) can be obtained, and the alkali gel can be stably stored at room temperature for 15 days or more. The alkali catalyst contains crystal water, and the crystal water participates in the reaction, so that the finally prepared dimethyl silicone oil contains a small amount of hydroxyl, and the electrical insulation performance of the dimethyl silicone oil is influenced. The influence of oxygen and moisture on the alkali glue is effectively prevented through a dehydration process and a nitrogen environment in the synthesis process, so that the electric insulation performance of the synthesized dimethyl silicone oil is improved.
According to some embodiments of the invention, the dehydration treatment of the base catalyst with the second silicone intermediate comprises the steps of: reacting at 85-100 ℃ under the conditions of nitrogen atmosphere and negative pressure of 0.085-0.095 MPa. The reaction time is 0.5-1.5 h.
According to some embodiments of the invention, the temperature of the reaction in the dehydration treatment of the base catalyst and the second silicone intermediate is between 90 ℃ and 95 ℃. The pressure of the reaction was 0.09MPa negative pressure. The reaction time is 1h.
According to some embodiments of the present invention, in the method for preparing the alkali paste, the mass ratio of the alkali catalyst to the second silicone intermediate is 1:20 to 30.
According to some embodiments of the present invention, in the method for preparing the alkali paste, the mass ratio of the alkali catalyst to the second silicone intermediate is 1:23 to 27.
According to some embodiments of the present invention, in the method for preparing the alkali paste, the mass ratio of the alkali catalyst to the second silicone intermediate is 1:25.
according to some embodiments of the invention, the base catalyst comprises at least one of tetramethylammonium hydroxide and tetramethylammonium hydroxide silicon alkoxide.
According to some embodiments of the invention, the third negative pressure is 0.09MPa to 0.1MPa negative pressure.
According to some embodiments of the invention, the third negative pressure is 0.095MPa negative pressure.
According to some embodiments of the present invention, in the preparation method of the alkali glue, the reaction is further continued under a negative pressure of 0.1MPa after the reaction. The reaction time is 0.2 h-1 h; preferably 0.5h.
According to some embodiments of the invention, step S1 further comprises, prior to the dehydrating, mixing the first organosilicon intermediate with a low boiler. By adding low-boiling-point substances, the utilization rate of raw materials is improved, and the cost is saved.
According to some embodiments of the invention, the low boiling substance comprises at least one of a second silicone intermediate and a second dimethylsilicone oil. The second simethicone is a low molecular weight silicone oil. The second silicone intermediate includes at least one of D3, D4, D5, D6, D7, and a low molecular weight silicone oil. The boiling point of the low molecular weight silicone oil is 140-200 ℃; preferably 160 ℃ to 180 ℃.
According to some embodiments of the invention, the mass ratio of the first organosilicon intermediate to the low boilers is 100:3 to 15.
According to some embodiments of the invention, the mass ratio of the first organosilicon intermediate to the low boilers is 100:5 to 12.
According to some embodiments of the invention, the temperature of the reaction in step S1 is between 98 ℃ and 112 ℃.
According to some embodiments of the invention, the temperature of the reaction in step S1 is between 100 ℃ and 110 ℃.
According to some embodiments of the invention, in step S1, the reaction time is 2h to 6h.
According to some embodiments of the invention, in step S1, the reaction time is between 3h and 5h.
According to some embodiments of the invention, in step S1, the reaction time is 4h.
According to some embodiments of the invention, the temperature of the reaction in step S2 is 155 ℃ to 165 ℃.
According to some embodiments of the invention, the temperature of the reaction in step S2 is 157 ℃ to 162 ℃.
According to some embodiments of the invention, the temperature of the reaction in step S2 is 160 ℃.
According to some embodiments of the invention, in step S2, the reaction time is 1h to 3h.
According to some embodiments of the invention, in step S2, the reaction time is 1.5h to 2.5h.
According to some embodiments of the invention, in step S2, the reaction time is 2h.
According to some embodiments of the invention, in step S3, the first negative pressure is 0.085MPa to 0.095MPa negative pressure.
According to some embodiments of the invention, in step S3, the first negative pressure is a negative pressure of 0.09 MPa.
According to some embodiments of the invention, in step S3, the reaction time is 1h to 3h.
According to some embodiments of the invention, in step S3, the reaction time is 1.5h to 2.5h.
According to some embodiments of the invention, in step S3, the reaction time is 2h.
According to some embodiments of the invention, the temperature of the reaction in step S4 is 178 ℃ to 182 ℃.
According to some embodiments of the invention, in step S4, the temperature of the reaction is 180 ℃.
According to some embodiments of the invention, in step S4, the second negative pressure is 0.09MPa to 0.1MPa negative pressure.
According to some embodiments of the invention, in step S4, the second negative pressure is a negative pressure of 0.1 MPa.
According to some embodiments of the invention, in step S4, the reaction time is 1h to 3h.
According to some embodiments of the invention, in step S4, the reaction time is 2h.
According to some embodiments of the invention, in step S5, the reaction time is 1h to 3h.
According to some embodiments of the invention, in step S5, the reaction time is 2h.
According to some embodiments of the invention, in step S5, the inert gas comprises at least one of nitrogen, helium and argon.
The dimethicone prepared by the method for preparing the dimethicone according to the embodiment of the second aspect of the invention.
According to some embodiments of the present invention, the viscosity of the dimethylsilicone oil can be controlled to 100mPa · s to 100000mPa · s.
According to some embodiments of the present invention, the viscosity of the dimethylsilicone fluid can be controlled to be 100 to 40000mPa · s.
According to some embodiments of the invention, the resistivity of the dimethicone at 25 ℃ can be controlled to be higher than 1 x 10 13 Ω·m。
According to some embodiments of the present invention, the resistivity of the dimethylsilicone oil at 25 ℃ can be controlled to be 1 × 10 13 Ω·m～2×10 14 Ω·m。
According to some embodiments of the present invention, the dielectric loss of the dimethylsilicone oil at 25 ℃ can be controlled to 0 to 0.0001.
According to some embodiments of the present invention, the dimethylsilicone fluid may be controlled to have a resistivity higher than 1X 10 at 90 ℃ 12 Ω·m。
According to some embodiments of the present invention, the resistivity of the dimethylsilicone oil at 90 ℃ can be controlled to be 1 × 10 12 Ω·m～9×10 12 Ω·m。
According to some embodiments of the present invention, the dielectric loss of the dimethylsilicone fluid at 90 ℃ can be controlled to 0 to 0.0003.
The dimethyl silicone oil provided by the embodiment of the invention has at least the following beneficial effects:
the dimethylsilicone fluids of the examples have excellent insulating properties and controlled viscosity.
The dimethylsilicone oil prepared by the above method for preparing dimethylsilicone oil according to the third aspect of the present invention is used in the fields of machinery, electricity or paint.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, if there are first, second, etc. described, it is only for the purpose of distinguishing technical features, and it is not understood that relative importance is indicated or implied or that the number of indicated technical features is implicitly indicated or that the precedence of the indicated technical features is implicitly indicated.
Example 1
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of pentahydrate tetramethylammonium hydroxide and 100 parts of DMC in a three-neck flask, heating to 90-95 ℃ in nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The temperature was maintained and the reaction was continued for 2h under a negative pressure of 0.095 MPa.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the transparent alkali glue with the viscosity of 1800mPa & s.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of DMC were added to a three-necked flask, stirring was switched on, the mixture was heated to 90 ℃ and dehydrated for 2h under a negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 2 parts of hexamethyldisiloxane and 0.5 part of alkali gel are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 100 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Maintaining the temperature and vacuum pressure constant, in the direction ofIntroducing N into the bottom of the reaction bottle 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 2
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of D4 in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain transparent alkali glue with the viscosity of 1750mPa & s.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of D4 are added into a three-neck flask, stirred, heated to 90 ℃ and dehydrated for 2h under the negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 7.4 parts of dimethyl silicone oil with the viscosity of 50 mPas and 0.5 part of alkali gum are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously raising the temperature to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N to the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 3
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of D4 in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 90 parts of D4 and 10 parts of low-boiling substances are added into a three-neck flask, stirred, heated to 90 ℃ and dehydrated for 2 hours under the negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 7.4 parts of dimethyl silicone oil with the viscosity of 50 mPas and 0.5 part of alkali gum are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously raising the temperature to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N to the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 4
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of DMC in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 95 parts of DMC and 5 parts of low-boiling substance are added into a three-neck flask, stirring is started, heating is carried out to 90 ℃, and dehydration is carried out for 2 hours under the negative pressure of 0.09 MPa.
(2) Temperature ofRecovering normal pressure without changing, adding 2 parts of dimethyl silicone oil with viscosity of 5 mPa.s and 0.5 part of alkali gel, and pumping N 2 And thirdly, under the nitrogen atmosphere, continuously raising the temperature to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N into the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 5 (differing from example 2 only in the amount of dimethylsilicone oil having a viscosity of 50 mPas)
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of D4 in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of D4 are added into a three-neck flask, stirred, heated to 90 ℃ and dehydrated for 2h under the negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 24 parts of dimethyl silicone oil with the viscosity of 50 mPas and 0.5 part of alkali gum are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N into the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 6 (differing from example 2 only in the amount of the dimethylsilicone oil having a viscosity of 50 mPas)
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of D4 in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The temperature was maintained and the reaction was continued for 2h under a negative pressure of 0.095 MPa.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of D4 are added into a three-neck flask, stirred, heated to 90 ℃ and dehydrated for 2h under the negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 10 parts of dimethyl silicone oil with the viscosity of 50 mPas and 0.5 part of alkali gel are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N into the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 7 (differing from example 2 only in the amount of dimethylsilicone oil having a viscosity of 50 mPas)
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of D4 in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of D4 are added into a three-neck flask, stirred, heated to 90 ℃ and dehydrated for 2h under the negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 5 parts of dimethyl silicone oil with the viscosity of 50 mPas and 0.5 part of alkali gum are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 110 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N to the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 8 (differing from example 1 only in the amount of the alkali gum used)
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of DMC in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of DMC were added in a three-necked flask, stirring was switched on, the mixture was heated to 90 ℃ and dehydrated under a negative pressure of 0.09MPa for 2h.
(2) The temperature is not changed, the normal pressure is recovered, 2 parts of hexamethyldisiloxane and 0.25 part of alkali gel are added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 100 ℃ and reacting for 4 hours.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N into the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Example 9 (differing from example 1 only in the amount of the alkali gum used)
The embodiment provides a preparation method of simethicone, which comprises the following steps:
(1) Synthesizing alkali glue:
(1) mixing 4 parts of tetramethylammonium pentahydrate hydroxide and 100 parts of DMC in a three-neck flask, heating to 90-95 ℃ under the nitrogen atmosphere, and reacting for 1h under the negative pressure of 0.09 MPa.
(2) The reaction was continued for 2h at 0.095MPa of negative pressure, maintaining the temperature.
(3) Reacting for 0.5h under the negative pressure of 0.1MPa to obtain the alkali glue.
(2) And (3) synthesizing dimethyl silicone oil:
(1) 100 parts of DMC were added to a three-necked flask, stirring was switched on, the mixture was heated to 90 ℃ and dehydrated for 2h under a negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 2 parts of hexamethyldisiloxane and 1 part of alkali gel are added, and N is pumped and discharged 2 Three times under nitrogen atmosphere, andthe temperature is continuously increased to 100 ℃ and the reaction is carried out for 4h.
(3) The temperature is increased to 160 ℃ and the reaction is carried out for 2h.
(4) Keeping the temperature unchanged, reacting for 2h under the negative pressure of 0.09MPa, and vacuumizing to remove unreacted micromolecule substances.
(5) Further heating to 180 ℃, reacting for 2h under the negative pressure of 0.1MPa, and further removing unreacted micromolecular substances.
(6) Keeping the temperature and the vacuum pressure unchanged, and introducing N into the bottom of the reaction flask 2 And reacting for 2 hours. And filtering to obtain transparent dimethyl silicone oil after the reaction is finished.
Comparative example 1
Compared to example 4, the only difference is: n is not introduced into the process (6) in the step (2) 2 。
Comparative example 2
Compared to example 2, the only difference is: process (1) of step (2) is missing.
Comparative example 3
Compared to example 2, the only difference is: replacing the processes (1) and (2) of the step (2) with the following processes:
(1) 100 parts of D4 and 7.4 parts of dimethylsilicone oil having a viscosity of 50 mPas were added to a three-necked flask, stirred and heated to 90 ℃ and dehydrated for 2 hours under a negative pressure of 0.09 MPa.
(2) The temperature is not changed, the normal pressure is recovered, 0.5 part of alkali gel is added, and N is pumped and discharged 2 And thirdly, under the nitrogen atmosphere, continuously heating to 110 ℃ and reacting for 4 hours.
Example of detection
The dimethylsilicone fluids prepared in the above examples and comparative examples were examined for viscosity, volume resistivity, dielectric loss, odor, yield of dimethylsilicone fluid and yield of low boiling substances. The specific detection method comprises the following steps:
the detection method of the viscosity comprises the following steps: GB/T2794-2013.
The detection method of the volume resistivity and the dielectric loss comprises the following steps: GB/T5654-2007.
The calculation formula of the yield of the dimethyl silicone oil is as follows: the dimethicone yield = dimethicone mass/raw material mass;
the formula for calculating the yield of the low-boiling-point substance is as follows: low boiler yield = low boiler mass/feedstock mass;
wherein, the raw materials are an organic silicon intermediate, an alkali glue and an end-capping reagent; if the low-boiling-point substance is added during the preparation of the dimethyl silicone oil, the raw material also comprises the low-boiling-point substance.
The detection results are as follows:
TABLE 1
Comparative example 1 is different from example 4 only in that N is not introduced during the removal of the low boiling components in step (2) 2 This causes the dimethylsilicone oil prepared in comparative example 1 to have some residual odor and the insulating properties thereof to be lower than those of example 4, which greatly affects the use of the silicone oil. The nitrogen gas is introduced to carry out not only the trimethylamine generated by the decomposition of the tetramethylammonium hydroxide, but also small molecular substances which are not removed completely by the combination of van der Waals force.
Comparative example 2 differs from example 2 only in that: process (1) of step (1) is missing. The volume resistivity and the viscosity of the silicone oil are greatly reduced at high temperature, and the dielectric loss is greatly increased. The trace moisture in the raw material can influence the electrical insulation performance of the silicone oil, because the moisture can be used as an end-capping agent to participate in the end capping of the silicone oil, the obtained product can not meet the actual use requirement.
After repeating the preparation method of comparative example 3 twice, the prepared dimethylsilicone fluids each had a viscosity of 12900mm 2 At 25 ℃ and 14600mm 2 At 25 ℃ for a period of time. After repeating the preparation method of example 2 two more times, the prepared dimethylsilicone fluids each had a viscosity of 11520mm 2 S (25 ℃) and 11200mm 2 At 25 ℃ for a period of time. It can be seen that, although the preparation method provided in comparative example 3 also enables the preparation of transparent dimethylsilicone fluids, the dimethylsilicone fluids obtainedThe viscosity of the dimethylsilicone oil is unstable, the viscosity fluctuation of the dimethylsilicone oil among batches is large, the viscosity of the dimethylsilicone oil cannot be well controlled, and the properties of the dimethylsilicone oil are unstable. In addition, viscosity instability of the dimethylsilicone fluids may also affect its application. For example: the viscosity of the insulating oil is in the range of 1500 mPas to 13000 mPas as specified in the national standard DL/T2412-2021 "guide for selecting insulating oil for power cable terminals", and it is apparent that the preparation method of comparative example 3 cannot provide a simethicone having a viscosity stabilized at 13000 mPas or less.
Example 2 differs from examples 5 to 7 in the amount of dimethylsilicone oil having a viscosity of 50 mPas. As is clear from Table 1, the viscosity of the dimethylsilicone fluid obtained gradually increased as the amount of the dimethylsilicone fluid having a viscosity of 50 mPas was decreased. This is because, after the blocking agent is decreased, the chain growth of the silicone oil is less restricted, the molecular chain growth is longer, and the entanglement between molecular chains is larger, resulting in an increase in viscosity.
Example 1 differs from examples 8-9 in the amount of alkali gum used. As can be seen from Table 1, the viscosity of the resulting dimethylsilicone fluids increased as the amount of the base gum was decreased. This is because the alkali gum is the active center in the chain initiation process, and the reduction of the active center makes the small molecules participate in the chain growth more, and therefore the resulting molecular chain is also longer, resulting in an increase in viscosity.
While the embodiments of the present invention have been described in detail with reference to the specific embodiments, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A preparation method of dimethyl silicone oil is characterized by comprising the following steps: the method comprises the following steps:
s1, dehydrating a first organic silicon intermediate, adding an alkali glue and an end-capping reagent, and heating to 95-115 ℃ in a nitrogen atmosphere to react to obtain a first mixture;
s2, heating the first mixture to 150-170 ℃, and reacting to obtain a second mixture;
s3, continuously reacting under the first negative pressure condition to obtain a third mixture;
s4, continuously heating the third mixture to 175-185 ℃, reducing the pressure, and reacting under a second negative pressure condition to obtain a fourth mixture;
and S5, introducing inert gas into the fourth mixture, and reacting to obtain the simethicone.
2. The method for preparing dimethylsilicone fluid according to claim 1, comprising the steps of: the first silicone intermediate comprises at least one of D3, D4, D5, D6, and D7; preferably, the mass ratio of the first organosilicon intermediate to the alkali glue is 100:0.1 to 1.5; preferably, the mass ratio of the first organosilicon intermediate to the alkali glue is 100:0.25 to 1.
3. The method for preparing dimethylsilicone oil according to claim 1, characterized in that: the mass ratio of the first organosilicon intermediate to the end-capping reagent is 100:1 to 30; preferably, the mass ratio of the first silicone intermediate to the end-capping agent is 100:2 to 24; preferably, the end-capping agent comprises at least one of hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane, dodecamethylwu-siloxane, tetradecylhexasiloxane, and first dimethicone.
4. The method for preparing dimethylsilicone oil according to claim 1, characterized in that: the preparation method of the alkali glue comprises the following steps: mixing and dehydrating an alkali catalyst and a second organic silicon intermediate, and reacting at 85-100 ℃ under the conditions of nitrogen atmosphere and third negative pressure to obtain alkali glue;
preferably, the mass ratio of the base catalyst to the second silicone intermediate is 1:20 to 30 percent;
preferably, the base catalyst comprises at least one of tetramethylammonium hydroxide and tetramethylammonium hydroxide silicon alkoxide.
5. The method for preparing dimethylsilicone oil according to claim 4, comprising the steps of: the reaction temperature under the third negative pressure condition is 90-95 ℃; preferably, the reaction time under the third negative pressure condition is 1 h-3 h.
6. The method for preparing dimethylsilicone oil according to claim 1, characterized in that: in the step S1, before dehydration, the first organic silicon intermediate is mixed with a low-boiling-point substance; preferably, the low boiling substance includes at least one of a second silicone intermediate and a second dimethylsilicone oil; preferably, the mass ratio of the first organosilicon intermediate to the low boilers is 100:3 to 15.
7. The method for preparing dimethylsilicone oil according to claim 1, characterized in that: in the step S1, the reaction temperature is 98-112 ℃; preferably, the reaction time is 2h to 6h.
8. The method for preparing dimethylsilicone oil according to claim 1, characterized in that: in the step S2, the reaction temperature is 155-165 ℃; preferably, the reaction time is 1h to 3h.
9. The dimethylsilicone oil produced by the production method according to any one of claims 1 to 8.
10. Use of the dimethylsilicone oil prepared by the process according to any one of claims 1 to 8 in the mechanical, electrical or paint field.
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