CN108610483A - A kind of high-purity dimethicone of resistance to oxidation and its synthetic method - Google Patents
A kind of high-purity dimethicone of resistance to oxidation and its synthetic method Download PDFInfo
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- CN108610483A CN108610483A CN201810517658.8A CN201810517658A CN108610483A CN 108610483 A CN108610483 A CN 108610483A CN 201810517658 A CN201810517658 A CN 201810517658A CN 108610483 A CN108610483 A CN 108610483A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
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Abstract
The present invention relates to technical field of organic synthesis, and in particular to a kind of synthetic method of the high-purity dimethicone of resistance to oxidation, the synthetic method of the high-purity dimethicone of resistance to oxidation include the following steps：Octaphenylcyclotetrasiloxane and dimethyltetraphenyldisiloxane are uniformly mixed in octamethylcy-clotetrasiloxane, decompression dehydration is then carried out, obtains mixed system 1；Hexamethyldisiloxane, organic rare-earth ligand, silane coupling agent, end-capping reagent and the concentrated sulfuric acid are added in mixed system 1 to be reacted, mixed system 2 is obtained；Mixed system 2 is kept the temperature into 0.5~1h at 140~150 DEG C, continues to be warming up to 180~220 DEG C, 2~4h of balanced reaction obtains crude product；Neutralizer is added in the crude product, then washes, be evaporated under reduced pressure and remove low-boiling-point substance to get to the high-purity dimethicone of resistance to oxidation.Good, the excellent oxidation resistent susceptibility of the storage stability of the high-purity dimethicone of resistance to oxidation of the present invention and purity is high.
Description
Technical field
The present invention relates to technical field of organic synthesis, and in particular to a kind of high-purity dimethicone of resistance to oxidation and its synthesis side
Method.
Background technology
Dimethicone is the transparency liquid of colorless and odorless, and surface tension is low, has high surface-active, excellent disappears
Steep anti-foaming property and good film forming.Dimethicone has hydrophobicity, not soluble in water.Dimethicone has good with other substances
Good isolation, greasy property are more excellent.In the case where not influencing ventilative, there is the performance of barrier humidity.Dimethicone is in width
Within the temperature range of viscosity change it is small.Heat resistance acid-proof.Chemical property is stablized, and boiling point is high, and solidification point is low, as liquid
Existing wide temperature range.The electrical property of dimethicone is good, especially in various frequency ranges when rate factor it is small, surface
Power is small, and anti-shear performance is excellent.Based on the above excellent property, dimethicone can be directly used for damp proof insulation, damps, subtracts
Shake defoams, lubrication, polishing etc., is widely used as insulation lubrication, shockproof, grease proofing dirt, dielectric liquid and heat carrier.
Although dimethicone itself has preferable oxidative resistance, usual non-refractory.But in order to further prevent
Or continue silicone oil and aoxidized, antioxidant is usually added in silicone oil, but the change of antioxidant high temperature resistance is bad；It cannot
Solve the oxidation resistent susceptibility of dimethicone.
Invention content
Of the existing technology in order to overcome the problems, such as, an object of the present invention is to provide a kind of high-purity dimethyl of resistance to oxidation
Silicone oil, the oxidation resistent susceptibility and purity that it has storage stability good, excellent are high.
The second object of the present invention is to provide a kind of synthetic method of the high-purity dimethicone of resistance to oxidation, it is produced with product
Rate is high, simple for process, the characteristics of being easy to control.
To achieve the goals above, the present invention provides a kind of synthetic method of the high-purity dimethicone of resistance to oxidation, including with
Lower step：
(1) octaphenylcyclotetrasiloxane and dimethyltetraphenyldisiloxane are mixed in octamethylcy-clotetrasiloxane
It is even, decompression dehydration is then carried out, mixed system 1 is obtained；
(2) in mixed system 1 be added hexamethyldisiloxane, organic rare-earth ligand, silane coupling agent, end-capping reagent and
The concentrated sulfuric acid is passed through 5~15min of nitrogen, is then decompressed to -0.09MPa after mixing, and heat is sealed at 85~120 DEG C
10~15min is reacted, 90~100 DEG C is then heated to, and react 0.5~2h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature to 0.5~1h at 140~150 DEG C, continues to be warming up to 180 DEG C~220 DEG C, balance is anti-
2~4h is answered, crude product is obtained；
(4) neutralizer will be added in crude product, it is neutrality to adjust its pH, is then washed, and it is low to carry out vacuum distillation removing
Object is boiled to get to the high-purity dimethicone of resistance to oxidation.
The present inventor has found during the experiment, organic dilute by being added in the preparation process of dimethicone
Native complex can significantly improve the antioxygenic property and high temperature resistance of dimethicone, and wherein organic rare-earth ligand makes
Dosage is an important factor for influencing dimethicone oxidative resistance, under optimum condition, the octaphenylcyclotetrasiloxane with it is described
The weight ratio of organic rare-earth ligand is 1：(0.01~0.08).The organic rare-earth ligand can be Eu, Tb and Sm element
Deng complex, ligand can be benzoic acid, p-methylbenzoic acid, p-aminobenzoic acid, paranitrobenzoic acid, to methoxyl group
Benzoic acid, 1,3,5 trimesic acids, 3- nitros -4-aminobenzoic acid, the chloro- 3- nitrobenzoic acids of 4-, thenoyl trifluoropropyl
Ketone, 1,10- Phen, 2,2 '-bipyridyls, one kind in 4,4 '-bipyridyls.
The disadvantage that system is muddy, viscosity is excessive caused by the excessive polymerization of reactant can be avoided by the way that end-capping reagent is added
It holds, under optimum condition, the end-capping reagent is selected from divinyl tetramethyl disiloxane, Vinyldimethylethoxysilane, six
Tetramethyldisiloxane or dimethylvinylmethoxysiiane.
Under optimum condition, in step (1), the technique of the decompression dehydration is -0.08Mpa, is kept the temperature at 70~90 DEG C
0.5~2h.
Under optimum condition, octaphenylcyclotetrasiloxane, dimethyltetraphenyldisiloxane and hexamethyldisiloxane weight
Amount is than being 1:(1.2~1.8):(1.5~2).
Under optimum condition, the silane coupling agent is selected from aminopropyl triethoxysilane, aminopropyl trimethoxysilane, 2-
Aminoethyl amino propyl trimethoxy silane, divinyl triammonium base propyl trimethoxy silicane, aminoethylaminopropyl methyl dimethoxy oxygen
In base silane, aminoethylaminopropyl triethoxysilane, urea propyl-triethoxysilicane and urea propyl trimethoxy silicane extremely
Few one kind.
Under optimum condition, in step (4), the technique of the vacuum distillation is：Temperature is 180~220 DEG C, vacuum degree
For -0.09~-0.10MPa.
The present invention also provides a kind of high-purity dimethicones of resistance to oxidation, are prepared according to the preparation method.
Through the above technical solutions, the present invention has the following technical effects：
The present invention can significantly improve diformazan by the way that organic rare-earth ligand is added in the preparation process of dimethicone
The antioxygenic property and high temperature resistance of base silicone oil disclosure satisfy that the performance of dimethicone at high temperature.
The preparation method of the offer of the present invention also has products collection efficiency height, product storage stability good, abundant raw material, technique
Simply, the characteristics of being easy to control is convenient for industrialization.
Specific implementation mode
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
Embodiment 1
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 60g dimethyltetraphenyldisiloxanes in four silica of 55g prestoxs ring
It is uniformly mixed in alkane, then carries out decompression dehydration (technique of decompression dehydration is -0.08Mpa, and 1h is kept the temperature at 75 DEG C), mixed
Zoarium system 1；
(2) 80g hexamethyldisiloxane, the cooperation of 2g p-methylbenzoic acid-Eu organic REs are added in mixed system 1
Object, 3g divinyl triammonium bases propyl trimethoxy silicane, 5g divinyl tetramethyl disiloxanes and the 5mL concentrated sulfuric acids (98%),
After mixing, it is passed through nitrogen 10min, is then decompressed to -0.09MPa, 10~15min of thermal response is sealed at 100 DEG C,
100 DEG C are then heated to, and reacts 1h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature into 1h at 150 DEG C, continues to be warming up to 220 DEG C, balanced reaction 4h obtains crude product；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 180~220 DEG C, vacuum degree is -0.09~-0.10MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Heat stability testing：The thermostabilization of product is measured using the TG209C type thermogravimetric analyzers of German Nai Chi companies production
Property (5% mass loss rate and temperature when 10% mass loss rate in air).
Light transmittance test method：Prepared product is spin-coated on slide, then in the purple of Perkins Elmer companies
It is tested on outside-visible spectrophotometer, wave-length coverage is 300~800nm.
Viscosity test：Using the NDJ-1 type rotational viscometers of Shanghai Precision Scientific Apparatus Co., Ltd's production at 25 DEG C
Measure viscosity.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 95.1% (500nm), viscosity 47950mPa/s, in air
In 5% mass loss rate when temperature be 465 DEG C, in air temperature when 10% mass loss rate be 505 DEG C.
Embodiment 2
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 68g dimethyltetraphenyldisiloxanes in four silica of 50g prestoxs ring
It is uniformly mixed in alkane, then carries out decompression dehydration (technique of decompression dehydration is -0.08Mpa, and 2h is kept the temperature at 90 DEG C), mixed
Zoarium system 1；
(2) 80g hexamethyldisiloxane, the cooperation of 1g 1,10- Phen-Tb organic REs are added in mixed system 1
Object, 3g divinyl triammonium bases propyl trimethoxy silicane, 4g divinyl tetramethyl disiloxanes and the 8mL concentrated sulfuric acids (98%),
After mixing, be passed through 5~15min of nitrogen, be then decompressed to -0.09MPa, be sealed at 90 DEG C thermal response 10~
15min then heats to 95 DEG C, and reacts 1h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature into 0.5h at 150 DEG C, continues to be warming up to 220 DEG C, balanced reaction 2.5h is slightly produced
Object；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 195 DEG C, vacuum degree is -0.10MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Light transmittance test method, viscosity determining procedure, heat stability testing method are the same as embodiment 1.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 97.2% (500nm), viscosity 49560mPa/s, in air
In 5% mass loss rate when temperature be 449 DEG C, in air temperature when 10% mass loss rate be 487 DEG C.
Embodiment 3
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 85g dimethyltetraphenyldisiloxanes in four silica of 75g prestoxs ring
It is uniformly mixed in alkane, then carries out decompression dehydration (technique of decompression dehydration is -0.08Mpa, and 1h is kept the temperature at 80 DEG C), mixed
Zoarium system 1；
(2) 75~100g hexamethyldisiloxane, 3g p-methylbenzoic acid-Eu organic REs are added in mixed system 1
Complex, 2g aminoethylaminopropyls triethoxysilane, 5g Vinyldimethylethoxysilanes and the 10mL concentrated sulfuric acids (98%),
After mixing, it is passed through nitrogen 10min, is then decompressed to -0.09MPa, 10~15min of thermal response is sealed at 110 DEG C,
100 DEG C are then heated to, and reacts 1h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature into 1h at 140 DEG C, continues to be warming up to 210 DEG C, balanced reaction 3h obtains crude product；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 205 DEG C, vacuum degree is -0.09MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Light transmittance test method, viscosity determining procedure, heat stability testing method are the same as embodiment 1.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 95.2% (500nm), viscosity 51740mPa/s, in air
In 5% mass loss rate when temperature be 468 DEG C, in air temperature when 10% mass loss rate be 503 DEG C.
Embodiment 4
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 90g dimethyltetraphenyldisiloxanes in four silica of 80g prestoxs ring
In alkane be uniformly mixed, then carry out decompression dehydration (technique of decompression dehydration be -0.08Mpa, at 70~90 DEG C keep the temperature 0.5~
2h), mixed system 1 is obtained；
(2) it is organic dilute that 100g hexamethyldisiloxane, 0.5g thioyl trifluoroacetone-Sm are added in mixed system 1
Native complex, 5g aminoethylaminopropyls triethoxysilane, 2g Vinyldimethylethoxysilanes and the 12mL concentrated sulfuric acids
(98%), it after mixing, is passed through 5~15min of nitrogen, is then decompressed to -0.09MPa, thermal response is sealed at 120 DEG C
10~15min then heats to 100 DEG C, and reacts 2h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature into 1h at 140 DEG C, continues to be warming up to 180 DEG C, balanced reaction 4h obtains crude product；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 180 DEG C, vacuum degree is -0.09MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Light transmittance test method, viscosity determining procedure, heat stability testing method are the same as embodiment 1.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 97.3% (500nm), viscosity 48630mPa/s, in air
In 5% mass loss rate when temperature be 438 DEG C, in air temperature when 10% mass loss rate be 478 DEG C.
Embodiment 5
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 60g dimethyltetraphenyldisiloxanes in four silica of 50g prestoxs ring
In alkane be uniformly mixed, then carry out decompression dehydration (technique of decompression dehydration be -0.08Mpa, at 70~90 DEG C keep the temperature 0.5~
2h), mixed system 1 is obtained；
(2) 75g hexamethyldisiloxane, the cooperation of 4g 1,10- Phen-Tb organic REs are added in mixed system 1
Object, 1g aminoethylaminopropyls triethoxysilane, 6g Vinyldimethylethoxysilanes and the 5mL concentrated sulfuric acids (98%), mixing
After uniformly, it is passed through 5~15min of nitrogen, is then decompressed to -0.09MPa, 10~15min of thermal response is sealed at 85 DEG C, so
After be warming up to 90 DEG C, and react 0.5h under normal pressure, obtain mixed system 2；
(3) mixed system 2 is kept the temperature into 0.5h at 150 DEG C, continues to be warming up to 180 DEG C, balanced reaction 2h is slightly produced
Object；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 220 DEG C, vacuum degree is -0.10MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Light transmittance test method, viscosity determining procedure, heat stability testing method are the same as embodiment 1.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 91.5% (500nm), viscosity 49780mPa/s, in air
In 5% mass loss rate when temperature be 417 DEG C, in air temperature when 10% mass loss rate be 467 DEG C.
Comparative example 1
A kind of synthetic method of the high-purity dimethicone of resistance to oxidation, includes the following steps：
(1) by 50g octaphenylcyclotetrasiloxanes and 60g dimethyltetraphenyldisiloxanes in four silica of 55g prestoxs ring
It is uniformly mixed in alkane, then carries out decompression dehydration (technique of decompression dehydration is -0.08Mpa, and 1h is kept the temperature at 75 DEG C), mixed
Zoarium system 1；
(2) be added in mixed system 1 80g hexamethyldisiloxane, 3g divinyl triammonium bases propyl trimethoxy silicane,
5g divinyl tetramethyl disiloxanes and the 5mL concentrated sulfuric acids (98%) are passed through nitrogen 10min, then depressurize after mixing
To -0.09MPa, it is sealed 10~15min of thermal response at 100 DEG C, then heats to 100 DEG C, and react 1h under normal pressure,
Obtain mixed system 2；
(3) mixed system 2 is kept the temperature into 1h at 150 DEG C, continues to be warming up to 220 DEG C, balanced reaction 4h obtains crude product；
(4) it is neutrality that sodium hydroxide will be added in crude product to system pH, is then washed, and it is low to carry out vacuum distillation removing
Object (temperature is 180~220 DEG C, vacuum degree is -0.09~-0.10MPa) is boiled to get to the high-purity dimethicone of resistance to oxidation.
Light transmittance test method, viscosity determining procedure, heat stability testing method are the same as embodiment 1.
The light transmittance of methyl-silicone oil manufactured in the present embodiment is 85.6% (500nm), viscosity 45710mPa/s, in air
In 5% mass loss rate when temperature be 315 DEG C, in air temperature when 10% mass loss rate be 348 DEG C.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (8)
1. a kind of synthetic method of the high-purity dimethicone of resistance to oxidation, which is characterized in that include the following steps：
(1) octaphenylcyclotetrasiloxane and dimethyltetraphenyldisiloxane are uniformly mixed in octamethylcy-clotetrasiloxane,
Then decompression dehydration is carried out, mixed system 1 is obtained；
(2) hexamethyldisiloxane, organic rare-earth ligand, silane coupling agent, end-capping reagent and dense sulphur are added in mixed system 1
Acid is passed through 5~15min of nitrogen, is then decompressed to -0.09MPa after mixing, and thermal response is sealed at 85~120 DEG C
10~15min then heats to 90~100 DEG C, and reacts 0.5~2h under normal pressure, obtains mixed system 2；
(3) mixed system 2 is kept the temperature to 0.5~1h at 140~150 DEG C, continues to be warming up to 180 DEG C~220 DEG C, balanced reaction 2
~4h, obtains crude product；
(4) neutralizer will be added in crude product, it is neutrality to adjust its pH, is then washed, and carries out vacuum distillation and remove low-boiling-point substance,
Obtain the high-purity dimethicone of resistance to oxidation.
2. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that in step (1)
In, the technique of the decompression dehydration is -0.08Mpa, and 0.5~2h is kept the temperature at 70~90 DEG C.
3. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that octaphenyl ring four
The weight ratio of siloxanes, dimethyltetraphenyldisiloxane and hexamethyldisiloxane is 1:(1.2~1.8):(1.5~2).
4. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that the end-capping reagent
Selected from divinyl tetramethyl disiloxane, Vinyldimethylethoxysilane, hexamethyldisiloxane or dimethylvinylsiloxy
Methoxylsilane.
5. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that the silane is even
Join agent and is selected from aminopropyl triethoxysilane, aminopropyl trimethoxysilane, 2- aminoethyl amino propyl trimethoxy silanes, diethyl
Alkene triamido propyl trimethoxy silicane, aminoethylaminopropyl methyl dimethoxysilane, aminoethylaminopropyl triethoxysilicane
At least one of alkane, urea propyl-triethoxysilicane and urea propyl trimethoxy silicane.
6. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that the octaphenyl
The weight ratio of cyclotetrasiloxane and the organic rare-earth ligand is 1：(0.01~0.08).
7. the synthetic method of the high-purity dimethicone of resistance to oxidation according to claim 1, which is characterized in that in step (4)
In, the technique of the vacuum distillation is：Temperature is 180~220 DEG C, vacuum degree is -0.09~-0.10MPa.
8. a kind of high-purity dimethicone of resistance to oxidation, which is characterized in that the system according to any one of claim 1~7
Preparation Method is prepared.
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|---|---|---|---|---|
| CN110483776A (en) * | 2019-08-27 | 2019-11-22 | 佛山市天宝利硅工程科技有限公司 | A kind of synthetic method and its synthesizer of high purity silicone oil |
| CN110483776B (en) * | 2019-08-27 | 2021-09-14 | 佛山市天宝利硅工程科技有限公司 | Synthesis method and synthesis device of high-purity silicone oil |
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