CN100362087C - Liquid float-type gyroscope suspension - Google Patents
Liquid float-type gyroscope suspension Download PDFInfo
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- CN100362087C CN100362087C CNB021366233A CN02136623A CN100362087C CN 100362087 C CN100362087 C CN 100362087C CN B021366233 A CNB021366233 A CN B021366233A CN 02136623 A CN02136623 A CN 02136623A CN 100362087 C CN100362087 C CN 100362087C
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- floated gyroscope
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Abstract
The present invention relates to suspension used in liquid floated gyroscopes, which is prepared from perfluoroether carbonyl fluoride and substituted phenol compounds in an organic solvent in the presence of inorganic alkali monovalent metal and ammonia or an organic or inorganic amine compound, and the compound comprises arc-paired electrons on nitrogen atoms. The present invention has the structural formula of *, wherein N is 0 or 1, M is 1, 2 or 3, x is Br, z is H or Br, Y is Br or C(CH3)3.
Description
Invention field
The present invention relates generally to a kind of liquid float-type gyroscope suspension, Preparation method and use.
Background of invention:
Many instruments, instrument need be with suspension as working mediums, and are also more and more high to the requirement of suspension along with the continuous expansion of use field and environment, and good suspension must have high specific gravity, high viscosity and low advantage such as solidify.
Suspension at present commonly used mainly is the polymkeric substance of trifluorochloroethylene, trifluoro bromine ethene and the triaizine compounds that has the halo side switch etc. (as U.S.P.5248432 etc.).Owing to consider suitable proportion, viscosity, reach bigger molecular weight, this has just caused the general higher shortcoming of zero pour of these compounds.In addition, the above suspension is a quasi-oligomer, and range of molecular weight distributions is big, thereby causes the unusual of instrument function.Therefore limited their use prospect.
Summary of the invention
The purpose of this invention is to provide the suspension in a kind of liquid floated gyroscope, be called gyro oil again.
Another object of the present invention provides the synthetic method of the suspension in a kind of above-mentioned liquid floated gyroscope.
Purpose of the present invention also provides the purposes of the suspension in a kind of above-mentioned liquid floated gyroscope.
Suspension in a kind of liquid floated gyroscope of the present invention, its structural formula is as follows:
Wherein, N=0 or 1, M=1,2 or 3, X=Br, Z=H or Br, Y=Br or C (CH
3)
3In the described liquid floated gyroscope, suspension can be row with the following structural formula:
Suspension in the described liquid floated gyroscope can contain in the presence of the organic or inorganic amine compound of lone-pair electron in organic solvent and on mineral alkali, ammonia or the nitrogen-atoms of monovalence metal, made by perfluor ether carbonyl fluoride and 5-substituted phenol compounds reaction, reaction formula is as follows:
Above-mentioned perfluor ether carbonyl fluoride structural formula is
The structural formula of 5-substituted phenol compounds is
N=0 or 1 wherein, M=1,2 or 3, X=Br, Z=H or Br, Y=Br or C (CH
3)
3
In the method for the invention, the organic amine compound mol ratio that contains lone-pair electron on the mineral alkali of described perfluor ether carbonyl fluoride, 5-substituted phenol compounds and monovalence metal or the nitrogen-atoms is 1: 0.8-2: 1-10, adopt the organic amine compound that contains lone-pair electron on the mineral alkali of more monovalence metal or the nitrogen-atoms to not influence of reaction.Temperature of reaction is 0-40 ℃, recommends 10-30 ℃.Reaction times is 0.5-5 hour.Described organic solvent can be sherwood oil, chloroform, methylene dichloride, tetracol phenixin, benzene,toluene,xylene etc.
Described monovalence metal inorganic alkali is hydride, oxyhydroxide, carbonate or the supercarbonate of monovalence metal.As potassium hydride KH, sodium hydride, lithium hydroxide, potassium hydroxide, sodium hydroxide, salt of wormwood, yellow soda ash, saleratus, sodium bicarbonate etc.The organic amine compound that contains lone-pair electron on the described nitrogen-atoms is benzyl lauryl amine, triethylamine, Tributylamine, trioctylamine, pyridine, dimethyl amine yl pyridines, bipyridine, 1,8-diazacyclo [4.3.0]-5-nonene, 4-(N, the N-dimethyl)-and pyridine or 1,4-diazacyclo [2.2.2] octane.
Suspension in the liquid floated gyroscope of the present invention not only can be used for the liquid floated gyroscope of satellite, aerospacecraft, guided missile etc., also can be used for naval vessel, automobile, boiler and as the lubricant of instrument with change the additive of shape product.Method of the present invention is easy, is fit to suitability for industrialized production.
Embodiment
To help to understand the present invention by following embodiment, but not limit content of the present invention.
Embodiment 1
The preparation of perfluor-(2,5-dimethyl-3,6-dioxy base n-nonanoic acid) (2 ' 4 ' 6 '-tribromo-benzene) ester:
Successively with 26.48g (0.08mol) 2,4, the 6-tribromophenol, prolong is equipped with in the adding of 100ml methylene dichloride and 6.32g (0.08mol) pyridine, and dropping funnel is in the 500ml three-necked bottle of thermometer and nitrogen mouth, under induction stirring and logical nitrogen situation, Dropwise 5 0g (0.1mol) perfluor-2 slowly, 5-dimethyl-3,6-dioxy base nonanoyl fluorine, during dropping, temperature is controlled between 10-35 ℃, adds 0.4g dimethyl amine yl pyridines subsequently, reacts after 3 hours, reactant distilled water wash three times, each 80ml, organic phase is filtered with silicagel column, and filtrate is evaporate to dryness on Rotary Evaporators, and mistake column separating purification, obtain the colourless sticking shape liquid of 50g,, be pure product through gas-chromatography and mass spectroscopy.
Mass spectrum (MS): 813 (20), 812 (29), 811 (71), 810 (89), 809 (69), 808 (57), 665 (100), 379 (15), 329 (68)
Infrared (IR): 1808,1559,1435,1283,747cm
-1
Hydrogen nuclear magnetic resonance (
1H NMR): 7.80 (S)
Embodiment 2
Perfluor-2,5,8,11-tetramethyl--3,6,9, the preparation of 12-four oxygen bases 15 carbonic acid (2 ', 3 ', 4 ', 5 ', 6 '-pentabromobenzene) ester:
Successively with 25g (0.051mol) 2,3,4,5,6-pentabromobenzene Fen, 120ml tetracol phenixin (through the hydrolith reflow treatment) and 5.2g (0.065mol) pyridine add prolong are housed, and dropping funnel is in the 250ml three-necked bottle of thermometer and nitrogen inlet.Under induction stirring and logical nitrogen situation, slowly be added dropwise to 46.6g (0.0561mol) perfluor-2,5,8,11-tetramethyl--3,6,9,12 four oxygen base pentadecanoyl fluorine, temperature is controlled at 0-30 ℃, add 0.4g dimethyl amine yl pyridines subsequently, react after 3 hours reactant distilled water wash three times, each 80ml, organic phase is filtered in silicagel column, gained filtrate evaporate to dryness on Rotary Evaporators, and cross column separating purification, get the colourless jelly of 53g, through gas-chromatography, mass spectrum and infrared analysis, be pure product.
Infrared (IR): 1808,1306,1239,983,748cm
-1
Embodiment 3
Perfluor-(2,5,8-trimethylammonium-3,6,9-three oxygen base laurostearic acids) (preparation of 2 ', 6 '-two bromo-4-tert.-butyl phenols:
Successively with 24.64g (0.08mol) 2,6-two bromo-4-tert.-butyl phenols, 100ml sherwood oil and 7.9g pyridine add prolong are housed, dropping funnel, in the 500ml three-necked bottle of thermometer and nitrogen mouth, under induction stirring and logical nitrogen situation, slowly drip 67g perfluor-2,5,8-trimethylammonium-3,6,9-three oxygen bases 12 carbonyl fluorides, during dropping, temperature is controlled between 10-30 ℃.Add 0.4g dimethyl amine yl pyridines subsequently, react afterreaction thing distilled water wash three times in 3 hours, each 80ml, organic phase is filtered in silicagel column, and filtrate is evaporate to dryness on Rotary Evaporators, and crosses column separating purification, gets the colourless sticking shape liquid of 68g.Through gas-chromatography, mass spectrum and infrared analysis are pure product.
Mass spectrum (MS): 953 (13), 952 (12), 951 (10), 938 (100), 937 (91), 910 (15), 794 (24), 793 (23), 228 (15), 226 (15), 169 (52)
Infrared (IR): 2970,1807,1451,1305,1240,993,747cm
-1
Hydrogen nuclear magnetic resonance (
1H NMR): 1.32 (S, 9H), 7.59 (S, 1H)
Claims (9)
1. the suspension in the liquid floated gyroscope, its structural formula is as follows:
N=0 or 1 wherein, M=1,2 or 3, X=Br, Z=H or Br, Y=Br or C (CH
3)
3
2. the suspension in a kind of liquid floated gyroscope as claimed in claim 1 is characterized in that structural formula is as follows:
3. the suspension in a kind of liquid floated gyroscope as claimed in claim 1 is characterized in that structural formula is as follows:
4. the suspension in a kind of liquid floated gyroscope as claimed in claim 1 is characterized in that structural formula is as follows:
5. the suspension preparation method in a kind of liquid floated gyroscope as claimed in claim 1, it is characterized in that in organic solvent and mineral alkali, ammonia or the nitrogen-atoms of monovalence metal on contain in the presence of the organic or inorganic amine compound of lone-pair electron, the organic amine compound mol ratio that contains lone-pair electron on the mineral alkali of perfluor ether carbonyl fluoride, 5-substituted phenol compounds and monovalence metal or the nitrogen-atoms is 1: 0.8-2: during 1-10,0-40 ℃ of reaction 0.5-5 hour, described perfluor ether carbonyl fluoride structural formula was
The structural formula of 5-substituted phenol compounds is
6. the suspension preparation method in a kind of liquid floated gyroscope as claimed in claim 5 is characterized in that described organic solvent is sherwood oil, chloroform, methylene dichloride, tetracol phenixin, benzene, toluene or dimethylbenzene.
7. the suspension preparation method in a kind of liquid floated gyroscope as claimed in claim 5 is characterized in that described monovalence metal inorganic alkali is hydride, oxyhydroxide, carbonate or the supercarbonate of monovalence metal.
8. the suspension preparation method in a kind of liquid floated gyroscope as claimed in claim 5, the organic amine compound that it is characterized in that containing on the described nitrogen-atoms lone-pair electron is benzyl lauryl amine, triethylamine, Tributylamine, trioctylamine, pyridine, dimethyl amine yl pyridines, bipyridine, 1,8-diazacyclo [4.3.0]-5-nonene, 4-(N, the N-dimethyl)-and pyridine or 1,4-diazacyclo [2.2.2] octane.
9. the purposes of the suspension in a kind of liquid floated gyroscope as claimed in claim 1 is characterized in that the lubricant of instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021366233A CN100362087C (en) | 2002-08-23 | 2002-08-23 | Liquid float-type gyroscope suspension |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021366233A CN100362087C (en) | 2002-08-23 | 2002-08-23 | Liquid float-type gyroscope suspension |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1400294A CN1400294A (en) | 2003-03-05 |
| CN100362087C true CN100362087C (en) | 2008-01-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021366233A Expired - Fee Related CN100362087C (en) | 2002-08-23 | 2002-08-23 | Liquid float-type gyroscope suspension |
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|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4975212A (en) * | 1988-12-27 | 1990-12-04 | Allied-Signal Inc. | Fluorinated lubricating compositions |
| US5248432A (en) * | 1987-05-01 | 1993-09-28 | Charles Stark Draper Laboratory, Inc. | Halogenated aryl ester damping fluids and lubricants |
-
2002
- 2002-08-23 CN CNB021366233A patent/CN100362087C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5248432A (en) * | 1987-05-01 | 1993-09-28 | Charles Stark Draper Laboratory, Inc. | Halogenated aryl ester damping fluids and lubricants |
| US4975212A (en) * | 1988-12-27 | 1990-12-04 | Allied-Signal Inc. | Fluorinated lubricating compositions |
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| Publication number | Publication date |
|---|---|
| CN1400294A (en) | 2003-03-05 |
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Granted publication date: 20080116 Termination date: 20110823 |