CN101684126A - Silicon-containing fluorine-containing poly-alpha-olefin and preparation method thereof - Google Patents

Silicon-containing fluorine-containing poly-alpha-olefin and preparation method thereof Download PDF

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Publication number
CN101684126A
CN101684126A CN200810231635A CN200810231635A CN101684126A CN 101684126 A CN101684126 A CN 101684126A CN 200810231635 A CN200810231635 A CN 200810231635A CN 200810231635 A CN200810231635 A CN 200810231635A CN 101684126 A CN101684126 A CN 101684126A
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polyalphaolefin
olefin
fluorine
alpha
siliceous
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王海忠
冯大鹏
刘维民
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The invention discloses silicon-containing fluorine-containing poly-alpha-olefin and a preparation method thereof. The poly-alpha-olefin is represented by a molecular structural formula (I). The poly-alpha-olefin is prepared by polymerizing methyl trifluoro-propyl 2-allyl silane and alpha olefin under an anhydrous AlCl3 catalysis condition. The poly-alpha-olefin has high viscosity and viscosity index under conditions of high temperature and lower temperature and can be used as base oil of lubricant.

Description

A kind of siliceous fluorine-containing polyalphaolefin and preparation method thereof
Technical field
The present invention relates to a kind of siliceous fluorine-containing polyalphaolefin and preparation method thereof.
Background technology
Polyalphaolefin (PAO) is a kind of lubricating oil commonly used, is widely used in all kinds of friction means.It has the use temperature wide ranges, and pour point is low, the viscosity index height, and vaporization losses is little, the high-temperature thermal oxidation good security, advantage such as coking is few, and is nontoxic has shear stability in addition, unreactiveness, electrical property is good, can be used as damping fluid, hydraulic efficiency oil and lubricant etc. that wide temperature range uses.Because its these premium propertiess, its use face is very wide, has also obtained to use widely in space flight and aviation industry.The PAO ucon oil is mainly used in engine, removes in addition, also obtains considerable development and application in industrial gear oil, turning oil, automatic transmission fluid, hydraulic efficiency oil, grease base oil, thermal oil and technology wet goods field.
Generally speaking, fluorinated organic compound all has good lubricating property, therefore if pass through chemical synthesis process, the organic group that will contain active element F is incorporated in the PAO molecular structure, then can improve the lubricity of PAO on the one hand, resulting fluorine-containing PAO also has the excellent properties of PAO oil itself simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of siliceous fluorine-containing polyalphaolefin and preparation method thereof.
In the present invention, in synthetic PAO process, introduce molecular flexibility methyl trifluoro propyl silane molecule preferably, on the one hand F is introduced in the PAO molecular structure, simultaneously, because the silane molecule structure has relative good low-temperature flowing property, is introduced into, and helps to improve the viscosity temperature characteristic of PAO.
A kind of siliceous fluorine-containing polyalphaolefin is characterized in that: molecular structure represents that with formula (I) it is connected with two polyalphaolefin structures at the methyl trifluoro propyl silane two ends, and alhpa olefin is that carbon number is alhpa olefin or its composition of 6-16; Abbreviate FSiPAO as,
Figure A20081023163500031
In the formula (I): m is the siliceous fluorine-based polyalphaolefin chain link quantity that contains, and equals 1-10.
The synthetic of fluorine-containing polyalphaolefin of the present invention can be represented with following chemical equation:
Figure A20081023163500041
Involved in the present invention to raw material make by the organometallic chemistry reaction by methyl trifluoro propyl dichlorosilane and bromopropylene for the methyl trifluoro propyl diallylsilane, employed alhpa olefin is that carbon number is alhpa olefin or its composition of 6-16.
The synthetic method of compound may further comprise the steps:
A, polyreaction: the methyl trifluoro propyl diallylsilane reacted than 1: 4 according to metering with alhpa olefin, added anhydrous AlCl 3Catalyzed polymerization, temperature of reaction are 100~150 ℃, and the reaction times is 2-6 hour, and reaction finishes back adding aqueous sodium hydroxide washes and washs away catalyzer, promptly obtains primary product;
The aftertreatment of B, siliceous fluorine-containing polyalphaolefin: will add Na in the prepared siliceous fluorine-containing polyalphaolefin 2SO 4Solution washing is to pH neutrality, and dry back is removed and desolvated, and underpressure distillation to 200-250 ℃ of steaming removes lighting end wherein, and residuum is required product.
By above technical scheme, the synthetic compound has very high viscosity and viscosity index under high/low temperature condition, and the base oil that can be used as lubricating oil uses.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment:
Embodiment 1
Siliceous fluorine-containing poly-α octene (is abbreviated as FSiPAO 8): get methyl trifluoro propyl diallyl silane 12.1g and octene 25.7g and mix the anhydrous AlCl of adding 0.95g 3, be warming up to 120 ℃, reacted 3 hours, add H 2The O termination reaction.Add sherwood oil, the dissolving organic phase adds aqueous sodium hydroxide solution (5%) washing and removes catalyzer, uses anhydrous Na 2SO 4Washing is to neutral.Dry filter removes and desolvates, and is heated to 150-250 ℃ of underpressure distillation, removes lighting end wherein, and obtain required target compound: weak yellow liquid, viscosity (25 ℃) is 511.1mm 2/ s, viscosity index is 146, and zero pour is less than-25 ℃, and the DSC heat decomposition temperature is 425 ℃.
Embodiment 2
Siliceous fluorine-containing poly-α laurylene (is abbreviated as FSiPAO 12): get methyl trifluoro propyl diallyl silane 16.2g and α laurylene 48.7g and mix the anhydrous AlCl of adding 1.65g 3, be warming up to 120 ℃, reacted 3 hours, add H 2The O termination reaction.Add sherwood oil, the dissolving organic phase adds aqueous sodium hydroxide solution (5%) washing and removes catalyzer, uses anhydrous Na 2SO 4Washing is to neutral.Dry filter removes and desolvates, and is heated to 150-250 ℃ of underpressure distillation, removes lighting end wherein, and promptly obtain required target compound: weak yellow liquid, viscosity (25 ℃) is 157.6mm 2/ s, viscosity index is 147, and zero pour is less than-25 ℃, and the DSC heat decomposition temperature is 423 ℃.
Siliceous fluorine-containing polyalphaolefin involved in the present invention is compared with general polyalphaolefin has tribological property preferably.Table 1 and table 2 have been listed two kinds of siliceous fluorine-containing polyalphaolefin (FSiPAO respectively 8And FSiPAO 12) with general polyalphaolefin respectively as the SRV fine motion rub(bing)test result of steel-steel-steel pair and steel-gunmetal friction lubricating agent, as can be seen from the test results, as steel-steel-steel pair lubricant, siliceous fluorine-containing polyalphaolefin has relatively low frictional coefficient and wear volume and advantages of high bearing capacity, illustrates that the introducing of F element helps to improve the tribological property of PAO lubricating oil.As steel-gunmetal friction lubricating agent, siliceous fluorine-containing polyalphaolefin has relatively low frictional coefficient and wear volume equally.
Table 1, SRV fine motion rub(bing)test result (steel-steel, frequency 25Hz, 30 minutes)
Figure A20081023163500051
Table 2, SRV fine motion rub(bing)test result (steel-gunmetal, frequency 25Hz, 30 minutes)

Claims (2)

1, a kind of siliceous fluorine-containing polyalphaolefin is characterized in that: molecular structure represents that with formula (I) it is connected with two polyalphaolefin structures at the methyl trifluoro propyl silane two ends, and alhpa olefin is that carbon number is alhpa olefin or its composition of 6-16;
Figure A2008102316350002C1
In the formula (I): m is the siliceous fluorine-based polyalphaolefin chain link quantity that contains, and equals 1-10.
2, the preparation method of siliceous fluorine-containing polyalphaolefin according to claim 1 is characterized in that this method may further comprise the steps:
A, polyreaction: the methyl trifluoro propyl diallylsilane reacted than 1: 4 according to metering with alhpa olefin, added anhydrous AlCl 3Catalyzed polymerization, temperature of reaction are 100~150 ℃, and the reaction times is 2-6 hour, and reaction finishes back adding aqueous sodium hydroxide washes and washs away catalyzer, promptly obtains primary product;
The aftertreatment of B, siliceous fluorine-containing polyalphaolefin: will add Na in the prepared siliceous fluorine-containing polyalphaolefin 2SO 4Solution washing is to PH neutrality, and dry back is removed and desolvated, and underpressure distillation to 200-250 ℃ of steaming removes lighting end wherein, and residuum is required product.
CN200810231635A 2008-09-26 2008-09-26 Silicon-containing fluorine-containing poly-alpha-olefin and preparation method thereof Pending CN101684126A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303428A (en) * 2020-02-24 2020-06-19 武汉高环新材料科技有限公司 High-temperature stable silicon-based base oil and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303428A (en) * 2020-02-24 2020-06-19 武汉高环新材料科技有限公司 High-temperature stable silicon-based base oil and preparation method thereof

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Application publication date: 20100331