CN102558226A - Method for preparing aviation tricresyl phosphate additive - Google Patents
Method for preparing aviation tricresyl phosphate additive Download PDFInfo
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- CN102558226A CN102558226A CN2011104206527A CN201110420652A CN102558226A CN 102558226 A CN102558226 A CN 102558226A CN 2011104206527 A CN2011104206527 A CN 2011104206527A CN 201110420652 A CN201110420652 A CN 201110420652A CN 102558226 A CN102558226 A CN 102558226A
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- aviation
- paaam
- tricresyl phosphate
- tritolyl phosphate
- aerospace
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Abstract
The invention relates to a method for preparing an aviation tricresyl phosphate additive. The method comprises the following steps of: reacting pure m.p-cresol with phosphorus trichloride in the presence of Lewis acid serving as a catalyst to obtain a crude tricresyl phosphate product; distilling the crude tricresyl phosphate product under reduced pressure to evaporate low-fraction unreacted m.p-cresol for recycling; adding sodium hydroxide, heating to the temperature of 60 DEG C, violently stirring for 1 hour, demixing, and rinsing to remove free phenol and water; and heating, stirring, adding a mixture of poly(acrylic acid-co-acrylamide) (PAAAM) and anhydrous potassium carbonate, heating, and stirring to ensure that trace water is fully absorbed by the PAAAM. The aviation tricresyl phosphate additive product is special for aerospace and aviation oil, has high purity and the water content of less than 300ppm, has water solubility, does not have acidity or alkalinity, cannot corrode precision instrument parts of aerospace and aviation equipment or influence the safety and service life of the aerospace and aviation equipment, and is completely suitable for special-grade aerospace and aviation oil.
Description
Technical field
The present invention relates to tritolyl phosphate, particularly a kind of tritolyl phosphate additive product preparation method of space flight and aviation private-use class.
Background technology
Safe, at a high speed and the needs of leading-edge field development according to the space flight and aviation industry; Tritolyl phosphate is selected for use the additive for the high-tech content proportioning; Thereby this product proposed to reach requirement of high purity; Must satisfy the technical requirements of space flight and aviation oil plant specialized requirement in addition, that is: moisture is less than 300ppm, water miscible no acid-basicity.If moisture is high, with the speed and the performance that greatly influence space flight and aviation flight; And the existence of water soluble acid basicity will bring corrosion to the high precision of space flight and aviation equipment, high most advanced and sophisticated instrument component, also will greatly influence the safety and the life-span of aerospace craft.
In view of this, the tritolyl phosphate additive product preparation method who seeks a kind of space flight and aviation private-use class becomes pursuing one's goal of these those skilled in the art.
Summary of the invention
Task of the present invention provides a kind of aviation and uses the tritolyl phosphate addictive preparation method, and it has solved the existing in prior technology problem effectively, is suitable for space flight and aviation oil plant private-use class fully.In the preparation process, the tritolyl phosphate product bullion that reaction generates under the catalyzer condition boils off the low unreacted M-and P-cresols of cut to reach recovery set usefulness through underpressure distillation, not only reduces the environmental protection treatment expense but also economize on resources; At last guaranteeing that fraction is the tritolyl phosphate product of aviation private-use class under associated vacuum degree, the high temperature.
Technical solution of the present invention is following:
The tritolyl phosphate addictive preparation method is used in a kind of aviation, and it may further comprise the steps:
Pure M-and P-cresols and phosphorus trichloride are reacted generation tritolyl phosphate product bullion under Liwis acid as catalyst condition;
Tritolyl phosphate product bullion is boiled off the low unreacted M-and P-cresols of cut through underpressure distillation to be used to reach recovery set;
Add 10% sodium hydroxide, be heated to 60 ℃ of vigorous stirring after 1 hour the layering rinsing remove free phenol and moisture;
When being warming up to 110 ℃, stir after 30 minutes, the PAAAM of adding 0.2% and 0.3% Anhydrous potassium carbonate mixture are warming up to 150 ℃ again and continue to stir 30 minutes, so that micro-moisture is fully absorbed by PAAAM; Said PAAAM is: vinylformic acid/2-acrylamido-2-methyl propane sulfonic acid multipolymer, and 1g can absorb 93g water;
After PAAAM and Anhydrous potassium carbonate mixture process absorb, guaranteeing that fraction is that the tritolyl phosphate product is used in aviation under vacuum 400 handkerchiefs, 250 ℃ again.
The technical requirements of space flight and aviation oil plant specialized requirement has been satisfied in aviation of the present invention with the tritolyl phosphate additive product; This kind additive purity is high; Moisture is less than 300ppm; Water miscible no acid-basicity can not produce corrosion to the precision instrument parts of space flight and aviation equipment, can not influence the safety and the life-span of aerospace craft yet.
Aviation of the present invention, can reduce the environmental protection treatment expense and economize on resources again in the preparation process with the tritolyl phosphate additive product, can also use portioned product by recovery set.
Embodiment
The invention provides a kind of aviation and use the tritolyl phosphate addictive preparation method, this preparation method may further comprise the steps:
Pure M-and P-cresols and phosphorus trichloride are reacted generation tritolyl phosphate product bullion under Liwis acid as catalyst condition.
Tritolyl phosphate product bullion is boiled off the low unreacted M-and P-cresols of cut to reach recovery set usefulness through underpressure distillation, not only reduce the environmental protection treatment expense but also economize on resources.
Add 10% sodium hydroxide, be heated to 60 ℃ of vigorous stirring after 1 hour the layering rinsing remove free phenol and moisture.
When being warming up to 110 ℃, stir after 30 minutes, the PAAAM of adding 0.2% and 0.3% Anhydrous potassium carbonate mixture are warming up to 150 ℃ again and continue to stir 30 minutes, so that micro-moisture is fully absorbed by PAAAM.Said PAAAM is: vinylformic acid/2-acrylamido-2-methyl propane sulfonic acid multipolymer, 1g can absorb 93g water.Anhydrous potassium carbonate not only has very strong water-absorbent, more can react the effect that reaches absorption with free phenol, the free acid in the product.
After PAAAM and Anhydrous potassium carbonate mixture process absorb, guaranteeing that fraction is that the tritolyl phosphate product is used in aviation under vacuum 400 handkerchiefs, 250 ℃ again.
In sum; The technical requirements of space flight and aviation oil plant specialized requirement has been satisfied in aviation of the present invention with the tritolyl phosphate additive product; This kind additive purity is high, and moisture is less than 300ppm, water miscible no acid-basicity; Can not produce corrosion, can not influence the safety and the life-span of aerospace craft yet the precision instrument parts of space flight and aviation equipment.Tritolyl phosphate additive product of the present invention is suitable for space flight and aviation oil plant private-use class fully.
Certainly; Those skilled in the art in the present technique field will be appreciated that; The foregoing description only is to be used for explaining the present invention; And be not with opposing qualification of the present invention, as long as in connotation scope of the present invention, all will drop in the scope of claim of the present invention the variation of the foregoing description, modification etc.
Claims (1)
1. the tritolyl phosphate addictive preparation method is used in an aviation, it is characterized in that it may further comprise the steps:
Pure M-and P-cresols and phosphorus trichloride are reacted generation tritolyl phosphate product bullion under Liwis acid as catalyst condition;
Tritolyl phosphate product bullion is boiled off the low unreacted M-and P-cresols of cut through underpressure distillation to be used to reach recovery set;
Add 10% sodium hydroxide, be heated to 60 ℃ of vigorous stirring after 1 hour the layering rinsing remove free phenol and moisture;
When being warming up to 110 ℃, stir after 30 minutes, the PAAAM of adding 0.2% and 0.3% Anhydrous potassium carbonate mixture are warming up to 150 ℃ again and continue to stir 30 minutes, so that micro-moisture is fully absorbed by PAAAM; Said PAAAM is: vinylformic acid/2-acrylamido-2-methyl propane sulfonic acid multipolymer, and 1g can absorb 93g water;
After PAAAM and Anhydrous potassium carbonate mixture process absorb, guaranteeing that fraction is that the tritolyl phosphate product is used in aviation under vacuum 400 handkerchiefs, 250 ℃ again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104206527A CN102558226A (en) | 2011-12-15 | 2011-12-15 | Method for preparing aviation tricresyl phosphate additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104206527A CN102558226A (en) | 2011-12-15 | 2011-12-15 | Method for preparing aviation tricresyl phosphate additive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102558226A true CN102558226A (en) | 2012-07-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104206527A Pending CN102558226A (en) | 2011-12-15 | 2011-12-15 | Method for preparing aviation tricresyl phosphate additive |
Country Status (1)
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| CN (1) | CN102558226A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593099A (en) * | 2017-09-30 | 2019-04-09 | 中国石油天然气股份有限公司 | A kind of preparation method of high-purity phosphoric acid front three phenolic ester |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049848A (en) * | 1989-08-29 | 1991-03-13 | 中国科学院长春应用化学研究所 | The new preparation process of tri aromatic ester of phosphic acid |
| CN101117405A (en) * | 2007-09-11 | 2008-02-06 | 天津市联瑞化工有限公司 | Method for preparing non-toxicity organophosphorus ester flame-proof plasticizing agent |
| CN102153953A (en) * | 2010-12-31 | 2011-08-17 | 长兴化学工业股份有限公司 | Photocurable adhesive composition |
-
2011
- 2011-12-15 CN CN2011104206527A patent/CN102558226A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049848A (en) * | 1989-08-29 | 1991-03-13 | 中国科学院长春应用化学研究所 | The new preparation process of tri aromatic ester of phosphic acid |
| CN101117405A (en) * | 2007-09-11 | 2008-02-06 | 天津市联瑞化工有限公司 | Method for preparing non-toxicity organophosphorus ester flame-proof plasticizing agent |
| CN102153953A (en) * | 2010-12-31 | 2011-08-17 | 长兴化学工业股份有限公司 | Photocurable adhesive composition |
Non-Patent Citations (3)
| Title |
|---|
| 杨锦飞: "TiSiW12O40/TiO2催化合成磷酸三甲苯酯的研究", 《有机化学》 * |
| 江芝良，等: "磷酸三甲苯酯合成工艺研究", 《化工时刊》 * |
| 秦海芳，王乾: "磷酸三甲苯酯合成方法的研究", 《天津化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593099A (en) * | 2017-09-30 | 2019-04-09 | 中国石油天然气股份有限公司 | A kind of preparation method of high-purity phosphoric acid front three phenolic ester |
| CN109593099B (en) * | 2017-09-30 | 2021-04-30 | 中国石油天然气股份有限公司 | Preparation method of high-purity tricresyl phosphate |
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Application publication date: 20120711 |