CN103897770A - Aircraft grade high-pressure fire-resistant oil using trixylenyl phosphate as base oil and production method thereof - Google Patents
Aircraft grade high-pressure fire-resistant oil using trixylenyl phosphate as base oil and production method thereof Download PDFInfo
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Abstract
The invention relates to aircraft grade high-pressure fire-resistant oil using trixylenyl phosphate as base oil and a production method thereof. The aircraft grade high-pressure fire-resistant oil comprises the following components: trixylenyl phosphate and di(tert-butyl-phenyl)phenyl phosphate having a weight ratio of (3.5-4.5):(1.5-3); and the aircraft grade high-pressure fire-resistant oil comprises the following other components in percentage by weight: 0.3-0.5% of 2-ethyl hexyl ester of epoxidized soybean oil, 0.5-0.6% of antioxidant TH-1010, 0.8-1.1% of triazole and 0.4-0.5% of dimethyl silicone oil. The high-pressure fire-resistant oil provided by the invention has the characteristics of low chlorine content, low acid value and high self-ignition point and boiling point, and has the advantages of favorable lubricating property, abrasion resistance, aging resistance, foaming resistance, flame resistance, heat stability and the like.
Description
Technical field
The invention belongs to fire resistant oil field, especially a kind of trixylyl phosphate does aviation-grade high pressure fireresistant oil and the production method thereof of base oil.
Background technology
To doing the selection of the exclusive base oil of aviation-grade high-pressure oil one used: trixylyl phosphate (TXP) is comparison new type of phosphate class flame-retardant plasticizer, has volatility low, water-tolerant, and have good flame retardant resistance and non-flame properties, thermal oxidation stability; The lubricity of this base oil is good simultaneously, is the lubricated oil of anti-extreme pressure and thickening agent, admittedly select this product to make a kind of key foundation oil of mixture fire resistant oil.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of aviation-grade high pressure fireresistant oil and production method thereof of making base oil with trixylyl phosphate is provided, this fire resistant oil has that cl content is low, acid number is low, spontaneous ignition temperature and the high characteristic of boiling point, there is good oilness, resistance to abrasion, resistance to deterioration, anti-spumescence, the advantages such as non-flame properties and heat-resistant quality energy.
The technical scheme that the present invention realizes object is as follows:
Trixylyl phosphate does an aviation-grade high pressure fireresistant oil for base oil, and composition is as follows:
Trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5～4.5:1.5～3, and other compositions and weight percent are as follows:
Prepare the method that trixylyl phosphate does the aviation-grade high pressure fireresistant oil of base oil, production method is as follows:
(1) qualified base oil trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight proportion: mixture is carried out in 3.5～4.5:1.5～3, and fully stirs 1.5～2.5 hours;
(2) get part (1) mixture oil put into dry, clean, add required several auxiliary agents without the constant volume device that dyes, fully stir into mother liquor;
(3) (1) the (2) mother liquor completing is added in still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3～5 hours;
(4) (3) will filtering through 50-60 order of completing, temperature is controlled at 65 ± 2 ℃, balance 14～17 hours;
(5) (4) do total analysis through sampling what complete, qualified, become the finished product, i.e. aviation-grade high pressure fireresistant oil.
And the preparation method of described trixylyl phosphate is as follows:
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium Mg catalyst, the 0.22wt%-0.3wt% that catalyst levels is xylenol, acid discharge; 145 ℃ of neutral equilibrium temperature controls, underpressure distillation: 720-750mmHg, 380-410 ℃, then rectifying: 720-750mmHg, 400-410 ℃ of purification, then the filtration of 50-60 order, getting its fine work is base oil.
And the production method of described two (tert-butyl-phenyl) phenyl phosphate ester is as follows:
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4～3.1:1.8～2.2, esterification under the effect of catalyzer calcium magnesium composite catalyst, catalyst levels is the 0.15wt% of p-tert-butylphenol, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 ℃, then rectifying 740-755mmHg, 390-400 ℃ of purification, 50-60 order filters again, and getting its fine work is base oil.
And the preparation method's of described calcium magnesium composite catalyst step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in reactor, add water;
(2) stir, heat, control temperature of reaction at 80 ± 5 ℃, heating 6～8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) the product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst;
The parts by weight of raw material are as follows:
Advantage of the present invention and beneficial effect are:
1, to have cl content low for high pressure fireresistant oil provided by the invention, and acid number is low, and the characteristic that spontaneous ignition temperature and boiling point are high has good oilness, resistance to abrasion, resistance to deterioration, anti-spumescence, the advantages such as non-flame properties and heat-resistant quality energy.
2, this product application, in industry high temperature, high pressure, oil pumping systems such as metallurgy, machinery, military projects, also extends near the system of working other high temperature heat source or naked light.
3, simple, the process control of preparation method of the present invention, acid number is obvious, and the product indices of producing is all good compared with currently available products high target.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Following per-cent is all weight percentage.
Trixylyl phosphate does an aviation-grade high pressure fireresistant oil for base oil, and composition is as follows:
Trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5～4.5:1.5～3, and other compositions and weight percent are as follows:
Oxidation inhibitor TH-1010 is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
Production method is as follows:
Processed oil is the technical process of aviation-grade high-pressure oil
(1) qualified base oil trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight proportion: mixture is carried out in 3.5～4.5:1.5～3, and fully stirs 1.5～2.5 hours;
(2) get (1) mixture oil put into regulation dry, clean, add in accordance with regulations and required several multiple agent without the constant volume device dying, fully stir into mother liquor;
(3) (1) the (2) mother liquor completing is added in still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3～5 hours;
(4) (3) will filtering through 50-60 order of completing, temperature is controlled at 65 ± 2 ℃, balance 14～17 hours;
(5) (4) do total analysis through sampling what complete, qualified, become the finished product, i.e. aviation-grade high pressure fireresistant oil; Be packaged as processed oil with cleaning-drying pail pack afterwards and weigh, warehouse-in.
The main component production method of described fire resistant oil is as follows:
A. the technical process of trixylyl phosphate: (TXP)
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 press xylenol calculating at catalyzer (calcium magnesium composite catalyst) 0.22%-0.3%() act under esterification, acid discharge; 145 ℃ of neutral equilibrium temperature controls, underpressure distillation (720-750mmHg left and right, 400-410 ℃/380-400 ℃), (the 720-750mmHg left and right of rectifying again, 400-410 ℃/380-400 ℃) purify, negative pressure control, more than 680 mmhg, filters in (50-60 order), and getting its fine work is base oil 93-95%.
B. the technical process of two (tert-butyl-phenyl) phenyl phosphate ester: (TBPP)
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4～3.1:1.8～2.2, catalyzer (calcium magnesium composite catalyst) 0.15%(press p-tert-butylphenol calculate) effect under esterification, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation (740-755mmHg, 390-400 ℃), then rectifying (740-755mmHg, 390-400 ℃) purify, control negative pressure more than 690 mmhg, secondary filter 50-60 order filters, and getting its fine work is base oil used.
C. the preparation method of calcium magnesium composite catalyst, is characterized in that: step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor adding water to;
(2) stir, heat, control temperature of reaction at 80 ± 5 ℃, heating 6～8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) the product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst;
The parts by weight of raw material are as follows:
The mass analysis of tricresyl phosphate benzhydryl ester is as following table (TXP)
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Acid number mgKOH/g | 0.060 | 0.080 | 0.050 | 0.072 | 0.063 |
| 20 ℃ of .g/CM of density 3 | 1.139 | 1.137 | 1.142 | 1.140 | 1.142 |
| 40 ℃ of .MM of viscosity 2/s | 48.7 | 46.91 | 49.58 | 52.15 | 50.09 |
| Flash-point ℃ | 248 | 251 | 249 | 255 | 253 |
| Spontaneous ignition temperature ℃ | 538 | 543 | 540 | 549 | 542 |
| Cl content mg/g | 24 | 31 | 23 | 19 | 25 |
| Color and luster (Pt-C o） # | 75 | 80 | 60 | 50 | 60 |
Tertiary butyl ester mass analysis is as following table (TBPP)
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Acid number mgKOH/g | 0.050 | 0.045 | 0.072 | 0.063 | 0.058 |
| 20 ℃ of .g/CM of density 3 | 1.144 | 1.144 | 1.147 | 1.145 | 1.144 |
| 40 ℃ of .MM of viscosity 2/s | 54.6 | 61.4 | 52.5 | 50.92 | 57.14 |
| Flash-point ℃ | 253 | 251 | 254 | 253 | 254 |
| Spontaneous ignition temperature ℃ | 593 | 586 | 569 | 572 | 563 |
| Cl content/g | 23 | 29 | 25 | 22 | 20 |
| Color and luster (Pt-C o） # | 70 | 60 | 55 | 70 | 60 |
Processed oil mass analysis is as following table
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Color and luster (Pt-C o） # | 60 | 50 | 60 | 70 | 60 |
| Acid number mgKOH/g | 0.043 | 0.038 | 0.042 | 0.051 | 0.048 |
| 20 ℃ of .g/CM of density 3 | 1.151 | 1.153 | 1.150 | 1.153 | 1.154 |
| 40 ℃ of .MM of viscosity 2/s | 42.50 | 40.30 | 42.20 | 40.15 | 41.42 |
| Flash-point ℃ | 248 | 246 | 251 | 246 | 249 |
| Granularity SAEA-6D level | 3 | 5 | 3 | 4 | 4 |
| Pour point ℃ | -18 | -19 | -18 | -20 | -18 |
| Spontaneous ignition temperature (triangle also) ℃ | 530 | 530 | 540 | 530 | 540 |
| (hot plate) ℃ | 710 | 715 | 728 | 725 | 715 |
| Moisture PPm | 80 | 60 | 60 | 50 | 60 |
| Chlorinity % | 0.005 | 0.005 | 0.005 | 0.005 | 0.005 |
| The high me of foam | 24 | 20 | 22 | 19 | 20 |
| 20 ℃ of resistivity. Ω cm 3 | 5.0×10 9 | 5.0×10 10 | 5.0×10 9 | 5.0×10 10 | 5.0×10 10 |
Claims (5)
1. trixylyl phosphate does an aviation-grade high pressure fireresistant oil for base oil, it is characterized in that: composition is as follows:
Trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5～4.5:1.5～3, and other compositions and weight percent are as follows:
2. prepare the method that trixylyl phosphate as claimed in claim 1 does the aviation-grade high pressure fireresistant oil of base oil, it is characterized in that: production method is as follows:
(1) qualified base oil trixylyl phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight proportion: mixture is carried out in 3.5～4.5:1.5～3, and fully stirs 1.5～2.5 hours;
(2) get part (1) mixture oil put into dry, clean, add required several auxiliary agents without the constant volume device that dyes, fully stir into mother liquor;
(3) (1) the (2) mother liquor completing is added in still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3～5 hours;
(4) (3) will filtering through 50-60 order of completing, temperature is controlled at 65 ± 2 ℃, balance 14～17 hours;
(5) (4) do total analysis through sampling what complete, qualified, become the finished product, i.e. aviation-grade high pressure fireresistant oil.
3. trixylyl phosphate according to claim 2 does the aviation-grade high pressure fireresistant oil production method of base oil, it is characterized in that: the preparation method of described trixylyl phosphate is as follows:
Adopt raw material xylenol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium Mg catalyst, the 0.22wt%-0.3wt% that catalyst levels is xylenol, acid discharge; 145 ℃ of neutral equilibrium temperature controls, underpressure distillation: 720-750mmHg, 380-410 ℃, then rectifying: 720-750mmHg, 400-410 ℃ of purification, then the filtration of 50-60 order, getting its fine work is base oil.
4. trixylyl phosphate according to claim 2 does the aviation-grade high pressure fireresistant oil production method of base oil, it is characterized in that: the production method of described two (tert-butyl-phenyl) phenyl phosphate ester is as follows:
Adopt raw material p-tert-butylphenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4～3.1:1.8～2.2, esterification under the effect of catalyzer calcium magnesium composite catalyst, catalyst levels is the 0.15wt% of p-tert-butylphenol, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 ℃, then rectifying 740-755mmHg, 390-400 ℃ of purification, 50-60 order filters again, and getting its fine work is base oil.
5. the aviation-grade high pressure fireresistant oil production method of making base oil according to the trixylyl phosphate described in claim 3 or 4, is characterized in that: the preparation method's of described calcium magnesium composite catalyst step is as follows:
(1) claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in reactor, add water;
(2) stir, heat, control temperature of reaction at 80 ± 5 ℃, heating 6～8h;
(3) reaction product is filtered, suction filtration, washes with water;
(4) the product after washing is dried, grind, get≤100 object catalyzer, roasting, obtains calcium magnesium composite catalyst; The parts by weight of raw material are as follows:
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| CN201310121448.4 | 2013-04-09 | ||
| CN201410078835.9A CN103897770A (en) | 2013-04-09 | 2014-03-06 | Aircraft grade high-pressure fire-resistant oil using trixylenyl phosphate as base oil and production method thereof |
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| CN110628486A (en) * | 2019-09-09 | 2019-12-31 | 山东瑞兴阻燃科技有限公司 | Trixylyl phosphate fire-resistant hydraulic oil and preparation method thereof |
| CN110724582A (en) * | 2019-10-08 | 2020-01-24 | 山东瑞兴阻燃科技有限公司 | Tert-butylated triphenyl phosphate flame-retardant hydraulic oil and preparation method thereof |
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| WO2017075744A1 (en) * | 2015-11-02 | 2017-05-11 | 深圳市广昌达石油添加剂有限公司 | Compound additive for preventing spontaneous combustion of diesel antiwear agent |
| CN110305722A (en) * | 2019-07-12 | 2019-10-08 | 安徽中天石化股份有限公司 | A kind of phosphate fire resistant hydraulic oil |
| CN114181757B (en) * | 2020-09-14 | 2022-06-28 | 安美科技股份有限公司 | Phosphate fire-resistant oil |
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| CA918139A (en) * | 1967-09-06 | 1973-01-02 | J. Shatynski John | Functional fluid composition |
| US20090247436A1 (en) * | 2008-03-31 | 2009-10-01 | Exxonmobil Research And Engineering Company | Lubricant composition with improved varnish deposit resistance |
| JP5172839B2 (en) * | 2008-04-09 | 2013-03-27 | 住友電気工業株式会社 | Flame retardant tube and heat shrink tube using the same |
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| CN110628486A (en) * | 2019-09-09 | 2019-12-31 | 山东瑞兴阻燃科技有限公司 | Trixylyl phosphate fire-resistant hydraulic oil and preparation method thereof |
| CN110724582A (en) * | 2019-10-08 | 2020-01-24 | 山东瑞兴阻燃科技有限公司 | Tert-butylated triphenyl phosphate flame-retardant hydraulic oil and preparation method thereof |
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