CN107760033A - A kind of methyl-silicone oil composition and preparation method thereof - Google Patents
A kind of methyl-silicone oil composition and preparation method thereof Download PDFInfo
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- CN107760033A CN107760033A CN201710979566.7A CN201710979566A CN107760033A CN 107760033 A CN107760033 A CN 107760033A CN 201710979566 A CN201710979566 A CN 201710979566A CN 107760033 A CN107760033 A CN 107760033A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/057—Metal alcoholates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/10—Esters; Ether-esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention provides a kind of methyl-silicone oil composition, including：Methyl-silicone oil 95wt%~99wt%；Heat-resisting additive A0.005wt%~1wt%；Heat-resisting additive B 0.05wt%~2wt%；Heat-resisting additive C 0.1wt%~5wt%；All component dosage sums are 100wt%；The heat-resisting additive A is selected from the one or more of organic titanium；The heat-resisting additive B is selected from the one or more of zirconates；One or more of the heat-resisting additive C in organic phenols and aminated compounds.Inventor creatively has found, the heat endurance that heat-resisting additive A, heat-resisting additive B and heat-resisting additive C not can effectively improve methyl-silicone oil is used alone, and heat-resisting additive A, heat-resisting additive B and heat-resisting additive C in combination are used, combined additive can effectively improve the heat endurance of methyl-silicone oil, significantly improve the temperature in use of methyl-silicone oil.
Description
Technical field
The present invention relates to a kind of novel silicon oil technical field, more particularly to a kind of methyl-silicone oil composition and its preparation side
Method.
Background technology
Silicone oil is a kind of polysiloxane of different polymerization degree chain structure, and methyl-silicone oil is the most frequently used in silicone oil
Kind.Because methyl-silicone oil has unique physical and chemical performance, as water white transparency, it is nontoxic it is odorless, flash-point is high, freezing point is low,
Viscosity-temperature coefficient is small, compression ratio is big, surface tension is small, excellent electrical insulation capability and heat resistance etc., therefore, extensively should in military project
For fields such as Aeronautics and Astronautics, navigation, precision instruments, it is civilian on be mainly used in the fields such as chemical industry, automobile, scientific research, be mainly used as
Be electrically insulated liquid, heat transfer oil, defoamer, brightener, releasing agent, softening agent, extraordinary hydraulic oil, food-grade silicone oil, various silicone grease
Base oil etc., can be long-term use of in -50~+180 DEG C of temperature ranges.
With the development of science and technology, the particularly development of national defence and sophisticated technology, the heat resistance of methyl-silicone oil is proposed
Higher requirement, it is desirable to which it is resistant to 250 DEG C even more than 300 DEG C of high temperature, and in general methyl-silicone oil can not meet
It is required that.Although the heat endurance of methyl-silicone oil can be improved by changing molecular structure, implement cumbersome, cost
Height, meanwhile, the heat endurance of obtained methyl-silicone oil needs to improve.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of methyl-silicone oil composition and its preparation side
Method, the heat endurance of the methyl-silicone oil composition are higher.
The invention provides a kind of methyl-silicone oil composition, including：
All component dosage sums are 100wt%；
The heat-resisting additive A is selected from the one or more of organic titanium；The heat-resisting additive B be selected from zirconates one kind or
It is several；One or more of the heat-resisting additive C in organic phenols and aminated compounds.
Preferably, dynamic viscosity of the methyl-silicone oil at 25 DEG C is 80~120mm2/s。
Preferably, mass content of the methyl-silicone oil in the methyl-silicone oil composition is 96wt%~98wt%.
Preferably, the heat-resisting additive A is selected from isooctanol titanium, trimethoxy pentamethylcyclopentadiene base titanium, 2- ethyls
The one or more of caproic acid titanium and methyl -3,5- pimelic acid titaniums.
Preferably, mass contents of the heat-resisting additive A in the methyl-silicone oil composition be 0.005wt%~
0.9wt%.
Preferably, the heat-resisting additive B be selected from zirconium caprylate, tetrabutyl zirconate, zirconium-n-butylate and zirconium acetate one kind or
It is several.
Preferably, mass contents of the heat-resisting additive B in the methyl-silicone oil composition be 0.05wt%~
1.8wt%.
Preferably, the heat-resisting additive C is selected from BHT, 4,4- di-2-ethylhexylphosphine oxides (2,6- bis- tertiary fourths
Base) it is phenol, right, to '-di-iso-octyldiphenylamine, N phenyl N ' secondary-butyl-p-phenylenediamines one or more.
Preferably, mass contents of the heat-resisting additive C in the methyl-silicone oil composition be 0.2wt%~
4wt%.
Present invention also offers a kind of preparation method of methyl-silicone oil composition described above, including：
Heat-resisting additive A, heat-resisting additive B and heat-resisting additive C are mixed with methyl-silicone oil, methyl silicon is obtained after reaction
Fluid composition；
The temperature of the reaction is 180~220 DEG C；The time of the reaction is 8~12h.
The invention provides a kind of methyl-silicone oil composition, including：Methyl-silicone oil 95wt%~99wt%；Heat-resisting additive
A0.005wt%~1wt%；Heat-resisting additive B 0.05wt%~2wt%；Heat-resisting additive C 0.1wt%~5wt%；It is all
Component dosage sum is 100wt%；The heat-resisting additive A is selected from the one or more of organic titanium；The heat-resisting additive B choosings
From the one or more of zirconates；One or more of the heat-resisting additive C in organic phenols and aminated compounds.Grinding
In studying carefully, inventor creatively has found, heat-resisting additive A, heat-resisting additive B and heat-resisting additive C, which is used alone, to be had
Effect improves the heat endurance of methyl-silicone oil, and heat-resisting additive A, heat-resisting additive B and heat-resisting additive C in combination are used, and
It is added in methyl-silicone oil, combined additive can be compatible well with methyl-silicone oil, and can be effectively improved methyl-silicone oil
Heat endurance, significantly improve the temperature in use of methyl-silicone oil.Therefore, the thermostabilization of methyl-silicone oil composition provided by the invention
Property and heat resistance are higher.In addition, the preparation method of methyl-silicone oil composition disclosed by the invention is simple and easy, cost is relatively low.It is real
Test result to show, the initial oxidation temperature of methyl-silicone oil is brought up to more than 350 DEG C by methyl-silicone oil composition provided by the invention.
Embodiment
Below in conjunction with the embodiment of the present invention, technical scheme is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, belongs to this hair
The scope of bright protection.
The invention provides a kind of methyl-silicone oil composition, including：
All component dosage sums are 100wt%.
The methyl-silicone oil is the base oil of the methyl-silicone oil composition.In the present invention, the methyl-silicone oil is in institute
It is 95wt%~99wt%, preferably 96wt%~98wt% to state the mass content in methyl-silicone oil composition.The present invention's
In some embodiments, mass content of the methyl-silicone oil in the methyl-silicone oil composition is 97.1wt%, 96.1wt%
Or 96.0wt%.Dynamic viscosity of the methyl-silicone oil at 25 DEG C is preferably 80~120mm2/s.In some realities of the present invention
Apply in example, the methyl-silicone oil is preferably No. 100 methyl-silicone oils.
The heat-resisting additive A is selected from the one or more of organic titanium；Preferably isooctanol titanium, trimethoxy pentamethyl ring
The one or more of pentadienyl titanium, 2 ethyl hexanoic acid titanium and methyl -3,5- pimelic acid titaniums.In the present invention, it is described heat-resisting to add
It is 0.005wt%~1wt% to add mass contents of the agent A in the methyl-silicone oil composition；Preferably 0.005wt%~
0.9wt%.In certain embodiments of the present invention, quality of the heat-resisting additive A in the methyl-silicone oil composition contains
Measure as 0.9wt% or 0.5wt%.
The heat-resisting additive B is selected from the one or more of zirconates；Preferably zirconium caprylate, tetrabutyl zirconate, zirconium-n-butylate
With the one or more of zirconium acetate.In the present invention, quality of the heat-resisting additive B in the methyl-silicone oil composition contains
Measure as 0.05wt%~2wt%；Preferably 0.05wt%~1.8wt%.In certain embodiments of the present invention, it is described heat-resisting to add
It is 0.3wt%, 0.4wt% or 0.5wt% to add mass contents of the agent B in the methyl-silicone oil composition.
One or more of the heat-resisting additive C in organic phenols and aminated compounds；The preferably uncles of 2,6- bis-
It is butyl paracresol, 4,4- di-2-ethylhexylphosphine oxides (2,6- di-t-butyls) phenol, right, to '-di-iso-octyldiphenylamine, N phenyl N ' sec-butyls pair
The one or more of phenylenediamine.In the present invention, mass contents of the heat-resisting additive C in the methyl-silicone oil composition
For 0.1wt%~5wt%；Preferably 0.2wt%~4wt%.In certain embodiments of the present invention, the heat-resisting additive C
Mass content in the methyl-silicone oil composition is 1.5wt%, 1.6wt% or 2.7wt%.
Under study for action, inventor creatively has found, heat-resisting additive A, heat-resisting additive B and heat-resisting addition is used alone
Agent C not can effectively improve the heat endurance of methyl-silicone oil, and by heat-resisting additive A, heat-resisting additive B and heat-resisting additive C
It is applied in combination, and is added in methyl-silicone oil, combined additive can be compatible well with methyl-silicone oil, and can effectively change
The heat endurance of kind methyl-silicone oil, significantly improve the temperature in use of methyl-silicone oil.Therefore, methyl-silicone oil combination provided by the invention
The heat endurance and heat resistance of thing are higher.
Present invention also offers a kind of preparation method of methyl-silicone oil composition, including：
Heat-resisting additive A, heat-resisting additive B and heat-resisting additive C are mixed with methyl-silicone oil, methyl silicon is obtained after reaction
Fluid composition.
Specifically, it is preferably：Heat-resisting additive A, heat-resisting additive B and heat-resisting additive C are added in methyl-silicone oil,
Methyl-silicone oil composition is obtained after reaction.
The component and dosage of the heat-resisting additive A, heat-resisting additive B and heat-resisting additive C and methyl-silicone oil are same as above,
This is repeated no more.The present invention has no special limitation to the source of above-mentioned used raw material components, can be general commercially available.
In the present invention, the temperature of the reaction is 180~220 DEG C；Preferably 190~210 DEG C.In some of the present invention
In embodiment, the temperature of the reaction is 200 DEG C.The time of the reaction is 8~12h；Preferably 10~12h.In the present invention
Some embodiments in, the time of the reaction is 10h.The reaction is carried out preferably under conditions of stirring.The present invention is to institute
The mode for stating stirring has no special limitation, using agitating mode well known to those skilled in the art.
After the reaction, preferably also include cooling.The present invention has no special limitation to the mode of the cooling, using this
The type of cooling known to art personnel.The temperature of the cooling is preferably room temperature.
The invention provides a kind of methyl-silicone oil composition, including：Methyl-silicone oil 95wt%~99wt%；Heat-resisting additive
A0.005wt%~1wt%；Heat-resisting additive B 0.05wt%~2wt%；Heat-resisting additive C 0.1wt%~5wt%；It is all
Component dosage sum is 100wt%；The heat-resisting additive A is selected from the one or more of organic titanium；The heat-resisting additive B choosings
From the one or more of zirconates；One or more of the heat-resisting additive C in organic phenols and aminated compounds.Grinding
In studying carefully, inventor creatively has found, heat-resisting additive A, heat-resisting additive B and heat-resisting additive C, which is used alone, to be had
Effect improves the heat endurance of methyl-silicone oil, and heat-resisting additive A, heat-resisting additive B and heat-resisting additive C in combination are used, and
It is added in methyl-silicone oil, combined additive can be compatible well with methyl-silicone oil, and can be effectively improved methyl-silicone oil
Heat endurance, significantly improve the temperature in use of methyl-silicone oil.Therefore, the thermostabilization of methyl-silicone oil composition provided by the invention
Property and heat resistance are higher.In addition, the preparation method of methyl-silicone oil composition disclosed by the invention is simple and easy, cost is relatively low.It is real
Test result to show, the initial oxidation temperature of methyl-silicone oil is brought up to more than 350 DEG C by methyl-silicone oil composition provided by the invention.
In order to further illustrate the present invention, with reference to embodiments to a kind of methyl-silicone oil composition provided by the invention and
Its preparation method is described in detail, but can not be understood as limiting the scope of the present invention.
Reagent used is commercially available in following examples.
Embodiment 1
Weigh No. 100 97.1 grams of methyl-silicone oils, add 0.5 gram of methyl -3,5- pimelic acid titanium, 0.4 gram of isooctanol titanium, 0.5
Gram zirconium caprylate, 0.2 gram of BHT, 1.3 grams are right, to '-di-iso-octyldiphenylamine, under conditions of stirring,
200 DEG C of reaction 10h, after being cooled to room temperature, obtain methyl-silicone oil composition.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil combination that the present embodiment obtains
The initial oxidation temperature of thing is 353.5 DEG C.
Embodiment 2
Weigh No. 100 96.1 grams of methyl-silicone oils, add 0.9 gram of 2 ethyl hexanoic acid titanium, 0.3 gram of zirconium-n-butylate, 2.7 gram 4,4-
Di-2-ethylhexylphosphine oxide (2,6- di-t-butyl) phenol, under conditions of stirring, 10h is reacted at 200 DEG C, after being cooled to room temperature, obtains methyl
Silicone oil composite.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil combination that the present embodiment obtains
The initial oxidation temperature of thing is 351.4 DEG C.
Embodiment 3
No. 100 96 grams of methyl-silicone oils are weighed, add 0.5 gram of trimethoxy pentamethylcyclopentadiene base titanium, 0.4 gram of four fourth oxygen
Base zirconium, 1.5 grams are right, to '-di-iso-octyldiphenylamine, 1.6 grams of N phenyl N ' secondary-butyl-p-phenylenediamines, under conditions of stirring,
200 DEG C of reaction 10h, after being cooled to room temperature, obtain methyl-silicone oil composition.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil combination that the present embodiment obtains
The initial oxidation temperature of thing is 356.8 DEG C.
Comparative example 1
No. 100 100 grams of methyl-silicone oils are weighed, hydrocarbon is determined with differential scanning calorimetry according to standard ASTM E2009-1999
The test method of class oxidation onset temperature, determine the obtained initial oxidation temperature of methyl-silicone oil, the results showed that, this comparative example obtains
The initial oxidation temperature of the methyl-silicone oil arrived is 278.5 DEG C.
Comparative example 2
No. 100 99.5 grams of methyl-silicone oils are weighed, add 0.5 gram of isooctanol titanium, under conditions of stirring, in 200 DEG C of reactions
10h, after being cooled to room temperature, obtain methyl-silicone oil composition.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil that this comparative example obtains rises
Beginning oxidizing temperature is 294.6 DEG C.
Comparative example 3
No. 100 98.5 grams of methyl-silicone oils are weighed, 1.5 grams of addition is right, to '-di-iso-octyldiphenylamine, in the condition of stirring
Under, 10h is reacted at 200 DEG C, after being cooled to room temperature, obtains methyl-silicone oil composition.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil that this comparative example obtains rises
Beginning oxidizing temperature is 294.8 DEG C.
Comparative example 4
No. 100 99.5 grams of methyl-silicone oils are weighed, add 0.5 gram of zirconium caprylate, under conditions of stirring, in 200 DEG C of reactions
10h, after being cooled to room temperature, obtain methyl-silicone oil composition.
The experiment side of hydrocarbon oxidation initial temperature is determined with differential scanning calorimetry according to standard ASTM E2009-1999
Method, determine the obtained initial oxidation temperature of methyl-silicone oil composition, the results showed that, the methyl-silicone oil that this comparative example obtains rises
Beginning oxidizing temperature is 293.5 DEG C.
Pass through above-described embodiment and comparative example, it can be seen that heat-resisting additive A, heat-resisting additive B and resistance to is used alone
Hot addition of C not can effectively improve the heat endurance of methyl-silicone oil, and by heat-resisting additive A, heat-resisting additive B and heat-resisting add
Add agent C in combination to use, and be added in methyl-silicone oil, combined additive can be compatible well with methyl-silicone oil, and can
The heat endurance of methyl-silicone oil is effectively improved, significantly improves the temperature in use of methyl-silicone oil.Therefore, methyl silicon provided by the invention
The heat endurance and heat resistance of fluid composition are higher.In addition, the preparation method of methyl-silicone oil composition disclosed by the invention is simple
Easy, cost is relatively low.Test result indicates that methyl-silicone oil composition provided by the invention is by the initial oxidation temperature of methyl-silicone oil
Bring up to more than 350 DEG C.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
1. a kind of methyl-silicone oil composition, including：
All component dosage sums are 100wt%；
The heat-resisting additive A is selected from the one or more of organic titanium；The heat-resisting additive B is selected from one kind or several of zirconates
Kind；One or more of the heat-resisting additive C in organic phenols and aminated compounds.
2. methyl-silicone oil composition according to claim 1, it is characterised in that motion of the methyl-silicone oil at 25 DEG C
Viscosity is 80~120mm2/s。
3. methyl-silicone oil composition according to claim 1, it is characterised in that the methyl-silicone oil is in the methyl-silicone oil
Mass content in composition is 96wt%~98wt%.
4. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive A is selected from isooctanol
Titanium, trimethoxy pentamethylcyclopentadiene base titanium, the one or more of 2 ethyl hexanoic acid titanium and methyl -3,5- pimelic acid titaniums.
5. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive A is in the methyl
Mass content in silicone oil composite is 0.005wt%~0.9wt%.
6. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive B be selected from zirconium caprylate,
The one or more of tetrabutyl zirconate, zirconium-n-butylate and zirconium acetate.
7. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive B is in the methyl
Mass content in silicone oil composite is 0.05wt%~1.8wt%.
8. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive C is selected from 2,6- bis-
It is Butylated Hydroxytoluene, 4,4- di-2-ethylhexylphosphine oxides (2,6- di-t-butyls) phenol, right, to '-di-iso-octyldiphenylamine, N phenyl N ' sec-butyls
The one or more of p-phenylenediamine.
9. methyl-silicone oil composition according to claim 1, it is characterised in that the heat-resisting additive C is in the methyl
Mass content in silicone oil composite is 0.2wt%~4wt%.
10. a kind of preparation method of the methyl-silicone oil composition described in claim 1, including：
Heat-resisting additive A, heat-resisting additive B and heat-resisting additive C are mixed with methyl-silicone oil, methyl-silicone oil group is obtained after reaction
Compound；
The temperature of the reaction is 180~220 DEG C；The time of the reaction is 8~12h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109735107A (en) * | 2018-12-26 | 2019-05-10 | 宜昌科林硅材料有限公司 | A method of low viscosity dimethyl silicone oil thermo oxidative stability in air is improved using the organo-metallic compound of nickel and zirconium |
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| CN102220004A (en) * | 2011-04-21 | 2011-10-19 | 中国科学院化学研究所 | Heat-resisting silicone oil composite |
| CN105886081A (en) * | 2016-04-27 | 2016-08-24 | 饶秀琴 | Lubricating oil and abrasion-resistant cleaning lubricating oil additive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735107A (en) * | 2018-12-26 | 2019-05-10 | 宜昌科林硅材料有限公司 | A method of low viscosity dimethyl silicone oil thermo oxidative stability in air is improved using the organo-metallic compound of nickel and zirconium |
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