CN103224828A - Aircraft-grade high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof - Google Patents
Aircraft-grade high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof Download PDFInfo
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- CN103224828A CN103224828A CN2013101205803A CN201310120580A CN103224828A CN 103224828 A CN103224828 A CN 103224828A CN 2013101205803 A CN2013101205803 A CN 2013101205803A CN 201310120580 A CN201310120580 A CN 201310120580A CN 103224828 A CN103224828 A CN 103224828A
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Abstract
The present invention relates to an aircraft-grade high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof, and the aircraft-grade high-pressure anti-combustible oil includes the following components of tricresyl phosphate T306 and di-(tert-butyl phenyl) phenyl phosphate at weight ratio of (3.5-4.5):(1.5-3.0), and other components of 0.3wt%-0.5wt% of epoxy soybean oil isooctyl phenyl, 0.5wt% and 0.6wt% of antioxidant-0197, 0.8wt% and 1.1wt% of benzotriazole and 0.4wt% and 0.5wt% of dimethyl silicone oil. The high-pressure anti-combustible oil provided by the present invention has characteristics of low chlorine content and acid value, high ignition point and boiling point, and advantages of good lubricity, abrasion resistance, aging resistance, anti-foam, anti-flammability and thermal stability etc.
Description
Technical field
The invention belongs to the fire resistant oil field, especially a kind of aviation-grade high pressure fireresistant oil and production method thereof of making base oil with Tritolyl Phosphate.
Background technology
To doing the selection of the exclusive base oil of the used one of aviation-grade high-pressure oil: Tritolyl Phosphate (TCP) is a comparison new type of phosphate class flame-retardant plasticizer, and it is low to have volatility, water-tolerant, and excellent flame-retardant performance and non-flame properties, thermal oxidation stability are arranged; The lubricity of this base oil is good simultaneously, is lubricated oil of anti-extreme pressure and thickening agent, admittedly select this product to make a kind of key foundation oil of the fire resistant oil that is mixed.
Summary of the invention
The objective 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 Tritolyl 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, good oilness is arranged, resistance to abrasion, resistance to deterioration, anti-spumescence, advantages such as non-flame properties and heat-resistant quality energy.
The present invention realizes that the technical scheme of purpose is as follows:
A kind ofly do the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, composition is as follows:
Tritolyl Phosphate T306: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5 ~ 4.5:1.5 ~ 3, and it is as follows that other compositions account for the per-cent of gross weight:
Do the production method of the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, step is as follows:
Processed oil is an aviation-grade high-pressure oil allotment of labor process flow
⑴ qualified base oil Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight: 3.5 ~ 4.5:1.5 ~ 3 are mixed, and fully stir 1.5 ~ 2.5 hours;
Get ⑴ be mixed oil put into the regulation drying, clean, do not have the constant volume device that dyes and add and reach required several multiple agent and several auxiliary multiple agent in accordance with regulations, fully stir into mother liquor;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3 ~ 5 o'clock.
⑷ will filter the ⑶ that finishes through the 50-60 order, and temperature is controlled at 65 ± 2 ℃, balance 14 ~ 17 o'clock.
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. aviation-grade high pressure fireresistant oil; The back is packaged as processed oil with the cleaning-drying pail pack and weighs, warehouse-in.
And the production method of described Tritolyl Phosphate is:
Adopt stock yard, p-cresol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, catalyst levels be 0.22-0.3wt% between, p-cresol, acid discharge; 145 ℃ of neutral equilibrium temperature controls, about underpressure distillation 730-750mmHg, 380-390 ℃, rectification and purification 730-750mmHg again, 380-390 ℃, filter the 50-60 order and filter, getting its elaboration is base oil.
Stock yard, p-cresol do not have the ratio requirement.
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 p-tert-butylphenol of 0.15wt%, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 ℃, rectifying 740-755mmHg again, 390-400 ℃ of purification, the 50-60 order filters again, and getting its elaboration is base oil.
And the preparation method's of described calcium magnesium composite catalyst step is as follows:
⑴ claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor that adds water to;
⑵ stir, heating, and control reaction temperature heats 6 ~ 8h at 80 ± 5 ℃;
⑶ filter reaction product, and suction filtration washes with water;
⑷ the product oven dry after will wash grinds, and gets≤100 purpose catalyzer, and roasting gets calcium magnesium composite catalyst.
Raw materials in part by weight is as follows:
Advantage of the present invention and beneficial effect are:
1, to have a 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, advantages such as non-flame properties and heat-resistant quality energy.
2, this product application also extends near the system of working other high temperature heat source or the naked light in industry high temperature, high pressure, oil pumping systems such as metallurgy, machinery, military projects.
3, preparation method of the present invention is simple, process control is thin, and acid number is obvious, and the every index of the product of producing is all good than the currently available products index.
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.
A kind ofly do the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, composition is as follows:
Tritolyl Phosphate T306: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5 ~ 4.5:1.5 ~ 3, and it is as follows that other compositions account for the per-cent of gross weight:
Production method is as follows:
Processed oil is the technical process of aviation-grade high-pressure oil
⑴ qualified base oil Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight: 3.5 ~ 4.5:1.5 ~ 3 are mixed, and fully stir 1.5 ~ 2.5 hours;
Get ⑴ be mixed oil put into the regulation drying, clean, do not have the constant volume device that dyes and add and reach required several multiple agent and several auxiliary multiple agent in accordance with regulations, fully stir into mother liquor;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3 ~ 5 o'clock.
⑷ will filter the ⑶ that finishes through the 50-60 order, and temperature is controlled at 65 ± 2 ℃, balance 14 ~ 17 o'clock.
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. aviation-grade high pressure fireresistant oil; The back is packaged as processed oil with the cleaning-drying pail pack and weighs, warehouse-in.
The main component production method of described fire resistant oil is as follows:
A. the technical process of Tritolyl Phosphate: (TCP)
Adopt stock yard, p-cresol and phosphorus oxychloride in proportion: 2.2-2.6:1-1.3 between catalyzer (calcium magnesium composite catalyst) 0.22%-0.3%(presses, p-cresol calculates) act under esterification, acid discharge; 145 ℃ of neutral equilibrium temperature controls, underpressure distillation (about 730-750mmHg, 380-390 ℃), rectification and purification (730-750mmHg, 380-390 ℃) again, negative pressure is controlled at more than 680 mmhg, back secondary filter 50-60 order filters, and getting its elaboration is used base oil.
B. the technical process of two (tert-butyl-phenyl) phenyl phosphate ester: (TBPP)
Adopt the raw material p-tert-butylphenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4 ~ 3.1:1.8 ~ 2.2, pressing p-tert-butylphenol at catalyzer (calcium magnesium composite catalyst) 0.15%(calculates) esterification under the effect, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation (740-755mmHg, 390-400 ℃), rectifying (740-755mmHg again, 390-400 ℃) purify, the control negative pressure is more than 690 mmhg, and secondary filter 50-60 order filters, and getting its elaboration is used base oil.
C. the preparation method of calcium magnesium composite catalyst, it is characterized in that: step is as follows:
⑴ claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor that adds water to;
⑵ stir, heating, and control reaction temperature heats 6 ~ 8h at 80 ± 5 ℃;
⑶ filter reaction product, and suction filtration washes with water;
⑷ the product oven dry after will wash grinds, and gets≤100 purpose catalyzer, and roasting gets calcium magnesium composite catalyst.
Processed oil mass analysis such as following table
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Color and luster (Pt-C o） # | 50 | 45 | 60 | 50 | 60 |
| Acid number mgKOH/ g | 0.062 | 0.049 | 0.053 | 0.050 | 0.055 |
| 20 ℃ of density. g/ CM 3 | 1.152 | 1.152 | 1.152 | 1.151 | 1.153 |
| 40 ℃ of viscosity. MM 2/s | 44.33 | 41.35 | 41.50 | 43.43 | 41.65 |
| Flash-point ℃ | 246 | 250 | 246 | 248 | 246 |
| Granularity SAEA-6D level | 5 | 3 | 5 | 4 | 5 |
| Pour point ℃ | -20 | -18 | -20 | -19 | -19 |
| Spontaneous ignition temperature (triangle also) ℃ | 530 | 540 | 530 | 530 | 540 |
| (hot plate) ℃ | 710 | 705 | 720 | 720 | 710 |
| Moisture PPm | 60 | 50 | 70 | 40 | 40 |
| Chlorinity % | 0.005 | 0.005 | 0.005 | 0.005 | 0.005 |
| The high me of foam | 20 | 22 | 24 | 20 | 22 |
| 20 ℃ of resistivity. Ω cm 3 | 5.0×10 10 | 5.0×10 10 | 5.0×10 9 | 5.0×10 10 | 5.0×10 10 |
Tritolyl Phosphate mass analysis such as following table (TCPT306)
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Acid number mgKOH/ g | 0.042 | 0.054 | 0.050 | 0.049 | 0.060 |
| 20 ℃ of density. g/ CM 3 | 1.170 | 1.174 | 1.171 | 1.174 | 1.172 |
| 40 ℃ of viscosity. MM 2/s | 36 | 34 | 37 | 34 | 36 |
| Flash-point ℃ | 227 | 225 | 230 | 227 | 225 |
| Spontaneous ignition temperature ℃ | 475 | 470 | 485 | 480 | 480 |
| Cl content/g | 22 | 25 | 27 | 24 | 24 |
| Color and luster (Pt-C o） # | 40 | 50 | 40 | 40 | 50 |
Two (tert-butyl-phenyl) phenyl phosphate ester mass analysis such as following table (TBPP)
| Project | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 |
| Acid number mgKOH/ g | 0.040 | 0.060 | 0.045 | 0.040 | 0.050 |
| 20 ℃ of density. g/ CM 3 | 1.143 | 1.143 | 1.144 | 1.143 | 1.145 |
| 40 ℃ of viscosity. MM 2/s | 58.2 | 53.6 | 50.8 | 53.7 | 56.2 |
| Flash-point ℃ | 250 | 253 | 250 | 253 | 253 |
| Spontaneous ignition temperature ℃ | 586 | 579 | 576 | 565 | 564 |
| Cl content/g | 28 | 25 | 24 | 27 | 22 |
| Color and luster (Pt-C o） # | 50 | 50 | 60 | 70 | 60 |
Claims (5)
1. do the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate for one kind, it is characterized in that: composition is as follows:
Tritolyl Phosphate T306: two (tert-butyl-phenyl) phenyl phosphate ester is by weight=3.5 ~ 4.5:1.5 ~ 3, and it is as follows that other compositions account for the per-cent of gross weight:
2. as claimed in claim 1ly do the production method of the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, it is characterized in that: step is as follows:
Processed oil is an aviation-grade high-pressure oil allotment of labor process flow
⑴ qualified base oil Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester by weight: 3.5 ~ 4.5:1.5 ~ 3 are mixed, and fully stir 1.5 ~ 2.5 hours;
Get ⑴ be mixed oil put into the regulation drying, clean, do not have the constant volume device that dyes and add and reach required several multiple agent and several auxiliary multiple agent in accordance with regulations, fully stir into mother liquor;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 3 ~ 5 o'clock.
⑷ will filter the ⑶ that finishes through the 50-60 order, and temperature is controlled at 65 ± 2 ℃, balance 14 ~ 17 o'clock.
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. aviation-grade high pressure fireresistant oil; The back is packaged as processed oil with the cleaning-drying pail pack and weighs, warehouse-in.
3. according to claim 2ly do the production method of the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, it is characterized in that: the production method of described Tritolyl Phosphate is:
Adopt stock yard, p-cresol and phosphorus oxychloride in molar ratio: 2.2-2.6:1-1.3 is esterification under the effect of catalyzer calcium magnesium composite catalyst, catalyst levels be 0.22-0.3wt% between, p-cresol, acid discharge; 145 ℃ of neutral equilibrium temperature controls, about underpressure distillation 730-750mmHg, 380-390 ℃, rectification and purification 730-750mmHg again, 380-390 ℃, filter the 50-60 order and filter, getting its elaboration is base oil.
4. according to claim 2ly do the production method of the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate, 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 p-tert-butylphenol of 0.15wt%, temperature is controlled at 120-150 ℃, acid discharge, neutral equilibrium, underpressure distillation 740-755mmHg, 390-400 ℃, rectifying 740-755mmHg again, 390-400 ℃ of purification, the 50-60 order filters again, and getting its elaboration is base oil.
5. describedly do the production method of the aviation-grade high pressure fireresistant oil of base oil with Tritolyl Phosphate according to claim 3 or 4, it is characterized in that: the preparation method's of described calcium magnesium composite catalyst step is as follows:
⑴ claim HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, sesbania powder, in the reactor that adds water to;
⑵ stir, heating, and control reaction temperature heats 6 ~ 8h at 80 ± 5 ℃;
⑶ filter reaction product, and suction filtration washes with water;
⑷ the product oven dry after will wash grinds, and gets≤100 purpose catalyzer, and roasting gets calcium magnesium composite catalyst.
Raw materials in part by weight is as follows:
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101205803A CN103224828A (en) | 2013-04-09 | 2013-04-09 | Aircraft-grade high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof |
| CN201410078738.XA CN103897768A (en) | 2013-04-09 | 2014-03-06 | Aircraft grade high-pressure fire-resistant oil using tritolyl phosphate as base oil and production method thereof |
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| CN2013101205803A CN103224828A (en) | 2013-04-09 | 2013-04-09 | Aircraft-grade high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof |
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| CN201410078738.XA Pending CN103897768A (en) | 2013-04-09 | 2014-03-06 | Aircraft grade high-pressure fire-resistant oil using tritolyl phosphate as base oil and production method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367134A (en) * | 2016-09-30 | 2017-02-01 | 广西东奇能源技术有限公司 | Fuel capable of reducing sulfur dioxide emission |
| WO2022052424A1 (en) * | 2020-09-14 | 2022-03-17 | 安美科技股份有限公司 | Phosphate ester fire-resistant fluid |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1231458A (en) * | 1967-09-06 | 1971-05-12 | ||
| CN102695785A (en) * | 2009-11-12 | 2012-09-26 | 吉坤日矿日石能源株式会社 | Flame-retardant hydraulic oil composition |
| CN103013635A (en) * | 2012-12-27 | 2013-04-03 | 安陆市奥森石油化学有限责任公司 | Ester type fire-resistant hydraulic fluid and preparation method thereof |
-
2013
- 2013-04-09 CN CN2013101205803A patent/CN103224828A/en active Pending
-
2014
- 2014-03-06 CN CN201410078738.XA patent/CN103897768A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1231458A (en) * | 1967-09-06 | 1971-05-12 | ||
| CN102695785A (en) * | 2009-11-12 | 2012-09-26 | 吉坤日矿日石能源株式会社 | Flame-retardant hydraulic oil composition |
| CN103013635A (en) * | 2012-12-27 | 2013-04-03 | 安陆市奥森石油化学有限责任公司 | Ester type fire-resistant hydraulic fluid and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367134A (en) * | 2016-09-30 | 2017-02-01 | 广西东奇能源技术有限公司 | Fuel capable of reducing sulfur dioxide emission |
| WO2022052424A1 (en) * | 2020-09-14 | 2022-03-17 | 安美科技股份有限公司 | Phosphate ester fire-resistant fluid |
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| CN103897768A (en) | 2014-07-02 |
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Application publication date: 20130731 |