CN103224827A - High-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof - Google Patents
High-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof Download PDFInfo
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Abstract
The present invention relates to a high-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof, which includes the following components of tricresyl phosphate and di-(tert-butyl phenyl) phenyl phosphate at weight ratio of (1.5-2.0):(3.5-4.0), 1wt%-1.2wt% of epoxy soybean oil isooctyl phenyl, 0.1wt%-0.25wt% of dimethyl silicone oil, 0.05wt%-0.08wt% of adsorbent-803 and 0.5wt% of antioxidant-1030. 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 high pressure fireresistant oil and production method thereof of making base oil with Tritolyl Phosphate.
Background technology
KR series fire resistant lubricant is to aim at high temperature, high pressure or the high-performance fire resistant oil that uses is arranged under the naked light Working environment, this product is to be basic material from ISOPROPYL PHENYL DIPHENYL PHOSPHATE, and in addition other auxiliary agent modulation forms, be widely used in generating, lubricated and the hydraulic efficiency system of metallurgy and main equipment also can be used for military project and aviation field.KR-99-G(high pressure wherein) and among the KR-99-Z(press) fire resistant oil is the dedicated hydraulic fire resistant oil of the height, pressure speed governing and the Controlling System that are used for the automobile generating unit, the use temperature height that KR-99-G and KR-99-Z fire resistant oil are had, compressive resistance is big, the spontaneous ignition temperature height, resistivity is big, and lubricity is good, good cooling results, advantages such as rapid heat dissipation are the ideal products that substitutes the import fire resistant oil.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of 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 high pressure fireresistant oil of base oil with Tritolyl Phosphate, composition is as follows:
Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester weight ratio=1.5 ~ 2.0:3.5 ~ 4.0, the epoxy soybean oil monooctyl ester of gross weight 1% ~ 1.2%, 0.1% ~ 0.25% dimethyl silicone oil, the oxidation inhibitor of 0.05% ~ 0.08% sorbent material-803,0.5%-1030.
A kind ofly do the production method of the high pressure fireresistant oil of base oil with Tritolyl Phosphate, step is as follows:
⑴ qualified base oil Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester is mixed by weight 1.5 ~ 2.0:3.5 ~ 4.0, and fully stirs 2-5 hour;
⑵ get the oil product that is mixed among the ⑴ and put into by joining oil product quantity, adds 1% ~ 1.2% epoxy soybean oil monooctyl ester, adds 0.1% ~ 0.25% dimethyl silicone oil, add 0.05% ~ 0.08% sorbent material-803, add 0.5% oxidation inhibitor-1030, fully stir into mother liquor, temperature is controlled at 60 ± 2 ℃;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 5 ~ 6 o'clock;
⑷ will filter the ⑶ that finishes through the 50-70 order, and temperature is controlled at 65 ± 2 ℃, balance 15 ~ 17 o'clock;
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. high pressure fireresistant oil.
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.
Between, 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 tertiary butyl phenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4 ~ 3.1:1.8 ~ 2.2, esterification under the effect of calcium magnesium composite catalyst, catalyst levels is the amount of the tertiary butyl phenol 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.
Per-cent with lower volume all is weight percentage.
A kind ofly do the high pressure fireresistant oil of base oil with Tritolyl Phosphate, composition is as follows:
Tritolyl Phosphate (TCP): two (tert-butyl-phenyl) phenyl phosphate ester (TBPP) weight ratio=1.5 ~ 2.0:3.5 ~ 4.0, the epoxy soybean oil monooctyl ester that adds gross weight 1% ~ 1.2% again, 0.1% ~ 0.25% dimethyl silicone oil, the oxidation inhibitor of 0.05% ~ 0.08% sorbent material-803,0.5%-1030.
Production method is as follows:
⑴ qualified base oil Tritolyl Phosphate (TCP): two (tert-butyl-phenyl) phenyl phosphate ester (TBPP) by a certain percentage: 1.5 ~ 2.0:3.5 ~ 4.0 are mixed, and fully stir 3 hours;
⑵ get that the oil product that is mixed among the ⑴ is put into the regulation drying, clean constant volume device adds by joining oil product quantity, add 1% ~ 1.2% epoxy soybean oil monooctyl ester, add 0.1% ~ 0.25% dimethyl silicone oil, add 0.05% ~ 0.08% sorbent material-803, add 0.5% oxidation inhibitor-1030, fully stir into mother liquor, temperature is controlled at 60 ± 2 ℃;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 5 ~ 6 o'clock;
⑷ will filter the ⑶ that finishes through the 50-60 order, and temperature is controlled at 65 ± 2 ℃, balance 15 ~ 17 o'clock;
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. 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 tertiary butyl phenol, phenol and phosphorus oxychloride, in molar ratio: 2:2.4 ~ 3.1:1.8 ~ 2.2, pressing tertiary butyl phenol 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.
Table 1 Tritolyl Phosphate quality and technical index
| Project | Index |
| Color and luster (Pt-Co) # ≤ | 60 |
| 20 ℃ of g/cm of density 3 ≤ | 1.178 |
| Acid number mgKOH/g≤ | 0.070 |
| 40 ℃ of mm of viscosity 2/s ≥ | 33 |
| Flash-point ℃ 〉= | 225 |
| Spontaneous ignition temperature ℃ 〉= | 430 |
| Cl content mg/g≤ | 30 |
Table 2 two (tert-butyl-phenyl) phenyl phosphate ester quality and technical index
| Project | Index |
| Color and luster (Pt-Co) # ≤ | 60 |
| 20 ℃ of g/cm of density 3 ≤ | 1.170 |
| Acid number mgKOH/g≤ | 0.070 |
| 40 ℃ of mm of viscosity 2/s ≥ | 48 |
| Flash-point ℃ 〉= | 240 |
| Spontaneous ignition temperature ℃ 〉= | 530 |
| Cl content mg/g≤ | 40 |
Mass analysis of table 3 high pressure fireresistant oil such as following table
| Project | Index |
| Color and luster (Pt-C o） #≤ | 60 |
| Acid number mgKOH/ g≤ | 0.070 |
| 20 ℃ of density. g/ CM 3 | 1.130-1.170 |
| 40 ℃ of viscosity. MM 2/s | 38-45 |
| Flash-point ℃ | 240 |
| Granularity SAEA-6D level≤ | 4 |
| Pour point ℃≤ | -18 |
| Spontaneous ignition temperature (triangle is also) ℃ 〉= | 530 |
| (hot plate) ℃ 〉= | 700 |
| Chlorinity %≤ | 0.005 |
| Moisture ppm≤ | 80 |
| 20 ℃ of resistivity. Ω cm 〉= | 5.0×10 9 |
| Foam property, the high mm of foam | 25 |
Claims (5)
1. do the high pressure fireresistant oil of base oil with Tritolyl Phosphate for one kind, it is characterized in that: composition is as follows:
Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester weight ratio=1.5 ~ 2.0:3.5 ~ 4.0, the epoxy soybean oil monooctyl ester of gross weight 1% ~ 1.2%, 0.1% ~ 0.25% dimethyl silicone oil, the oxidation inhibitor of 0.05% ~ 0.08% sorbent material-803,0.5%-1030.
2. a claim 1 is described does the production method of the high pressure fireresistant oil of base oil with Tritolyl Phosphate, and it is characterized in that: step is as follows:
⑴ qualified base oil Tritolyl Phosphate: two (tert-butyl-phenyl) phenyl phosphate ester is mixed by weight 1.5 ~ 2.0:3.5 ~ 4.0, and fully stirs 2-5 hour;
⑵ get the oil product that is mixed among the ⑴ and put into by joining oil product quantity, adds 1% ~ 1.2% epoxy soybean oil monooctyl ester, adds 0.1% ~ 0.25% dimethyl silicone oil, add 0.05% ~ 0.08% sorbent material-803, add 0.5% oxidation inhibitor-1030, fully stir into mother liquor, temperature is controlled at 60 ± 2 ℃;
⑶ be added to the ⑵ mother liquor finished in the ⑴ still, fully stirs 65 ± 2 ℃ of temperature controls, balance 5 ~ 6 o'clock;
⑷ will filter the ⑶ that finishes through the 50-70 order, and temperature is controlled at 65 ± 2 ℃, balance 15 ~ 17 o'clock;
⑸ do total analysis to the ⑷ that finishes through sampling, qualified, becomes the finished product, i.e. high pressure fireresistant oil.
3. according to claim 2ly do the production method of the 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 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 tertiary butyl phenol, 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 tertiary butyl phenol 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. according to claim 2ly do the production method of the high pressure fireresistant oil of base oil with Tritolyl Phosphate, 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 |
|---|---|---|---|
| CN2013101204302A CN103224827A (en) | 2013-04-09 | 2013-04-09 | High-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof |
| CN201410078831.0A CN103897786A (en) | 2013-04-09 | 2014-03-06 | High-pressure fire-resistant oil using tritolyl phosphate as base oil and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101204302A CN103224827A (en) | 2013-04-09 | 2013-04-09 | High-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof |
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| CN2013101204302A Pending CN103224827A (en) | 2013-04-09 | 2013-04-09 | High-pressure anti-combustible oil with base oil of tricresyl phosphate and production method thereof |
| CN201410078831.0A Pending CN103897786A (en) | 2013-04-09 | 2014-03-06 | High-pressure fire-resistant oil using tritolyl phosphate as base oil and production method thereof |
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| CN114181757B (en) * | 2020-09-14 | 2022-06-28 | 安美科技股份有限公司 | Phosphate fire-resistant oil |
| CN113073000A (en) * | 2021-03-08 | 2021-07-06 | 安徽中天石化股份有限公司 | Method for improving performance of phosphate flame-retardant hydraulic oil |
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 |
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- 2013-04-09 CN CN2013101204302A patent/CN103224827A/en active Pending
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- 2014-03-06 CN CN201410078831.0A patent/CN103897786A/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 |
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Application publication date: 20130731 |