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Preparation method of high-purity tricresyl phosphate

A high-purity technology of tricresyl phosphate, which is applied in the field of preparation of high-purity tricresyl phosphate, can solve problems such as slow hydrolysis of tricresyl phosphate, difficult environmental protection process improvement, and impact on storage stability, etc., to achieve economical and fast High purity, low loss, and loss reduction effect

Active Publication Date: 2019-04-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If it contains unremoved free cresols, it will have a negative impact on the oxidation stability of tricresyl phosphate; if it contains unremoved acidic impurities like phosphodiesters or phosphate monoesters, it will Affect the storage stability of tricresyl phosphate, because the presence of acid and trace water will cause the slow hydrolysis of tricresyl phosphate, resulting in an increase in its acid value
At the same time, the above-mentioned methods have not yet broken away from the influence of traditional methods. Processes such as adsorbent adsorption, alkali washing and water washing still appear in the newly developed preparation methods, and it is difficult to say that the process improvement of green environmental protection has been realized.
Therefore, there are significant differences between the above-mentioned patent and this patent in the preparation method and the quality control of the final product.

Method used

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  • Preparation method of high-purity tricresyl phosphate
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  • Preparation method of high-purity tricresyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] In a 5000mL three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, a condenser, and a hydrogen chloride tail gas absorption device, 2703 g of m-p-cresol was added (o-cresol was not detected, and the total content of m-p-cresol was 99.53%. The molar ratio of phenol to p-cresol is 6.5:3.5), phosphorus oxychloride 1128g, catalyst anhydrous aluminum chloride 3.8g, start stirring and slowly heat up to 150°C, and react at this temperature for 12 hours. After the reaction product was distilled under reduced pressure at 150° C. and 5 kPa vacuum for 10 h, its acid value was detected. When detecting that its acid value is 2.64mgKOH / g, stop vacuum distillation.

[0045] The above-mentioned crude product is introduced into molecular distillation equipment for the first stage of light phase impurity removal treatment. Set the evaporation temperature at 155°C and the vacuum degree at 15Pa, adjust the other molecular distillation parameters, and keep the...

Embodiment 2

[0048] In a 5000mL three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, a condenser, and a hydrogen chloride tail gas absorption device, add 2703 g of m-p-cresol (o-cresol has not been detected, and the total content of m-p-cresol is 99.76%, and m-p-cresol The molar ratio of phenol to p-cresol is 7:3), phosphorus oxychloride 1100g, catalyst anhydrous aluminum chloride 3.8g, start stirring and slowly heat up to 150°C, and react at this temperature for 12 hours. After the reaction product was distilled under reduced pressure at 140° C. and 5 kPa vacuum for 10 h, its acid value was detected. When the acid value was detected to be 2.71 mgKOH / g, the vacuum distillation was stopped.

[0049] The above-mentioned crude product is introduced into molecular distillation equipment for the first stage of light phase impurity removal treatment. Set the evaporation temperature at 155°C and the vacuum degree at 10Pa, adjust the other molecular distillation pa...

Embodiment 3

[0052] In a 5000mL three-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, a condenser, and a hydrogen chloride tail gas absorption device, add m-p-cresol 2703g (o-cresol is not detected, and the total content of m-p-cresol is 99.46%, m-p-cresol The molar ratio of phenol to p-cresol is 6.3:3.7), phosphorus oxychloride 1100g, catalyst anhydrous aluminum chloride 3.8g, start stirring and slowly heat up to 150°C, and react at this temperature for 12 hours. After the reaction product was distilled under reduced pressure at 150° C. and 4 kPa vacuum for 10 h, its acid value was detected. When the acid value was detected to be 1.34 mgKOH / g, the vacuum distillation was stopped.

[0053] The above-mentioned crude product is introduced into molecular distillation equipment for the first stage of light phase impurity removal treatment. Set the evaporation temperature at 156°C and the vacuum degree at 2Pa, adjust the other molecular distillation parameters, a...

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Abstract

The invention relates to a preparation method of high-purity tricresyl phosphate. The preparation method comprises the following steps: (S1) with mixed cresol and phosphorus oxychloride as the raw materials and Lewis acid as a catalyst, simultaneously adding the raw materials and the catalyst into a reactor, and reacting to obtain a crude product of tricresyl phosphate, wherein the mass percentageof o-cresol in mixed cresol is lower than 0.01%; (S2) carrying out reduced-pressure distillation on the crude product of tricresyl phosphate until the acid value of the crude product of tricresyl phosphate is less than or equal to 3mgKOH / g; and (S3) carrying out molecular distillation on the tricresyl phosphate crude product with the acid value less than or equal to 3mgKOH / g. The preparation method is simple, convenient, low in production cost, high in product purity and suitable for industrial production. High-purity tricresyl phosphate prepared by virtue of the preparation method is suitable for the fields of aviation fuel base oil, plasticizers, flame retardants, lubricating oil extreme-pressure anti-wear agents and the like.

Description

technical field [0001] The invention relates to a preparation method of tricresyl phosphate, in particular to a preparation method of green and environment-friendly high-purity tricresyl phosphate. Background technique [0002] Tricresyl phosphate (Tricresyl phosphate) has low volatility, good water resistance, good flame retardancy and flame resistance, thermal oxidation stability and extreme pressure and anti-wear properties. Combustible agent and extreme pressure antiwear agent, which can increase the flexibility of paint film when used in paint; used in polymers to give it good wear resistance, weather resistance, mildew resistance, radiation resistance and electrical properties, It is widely used as a plasticizing flame retardant in cable materials, conveyor belts, plastic sheets and other products; it can be used in lubricating oil products to endow it with excellent extreme pressure and anti-wear capabilities, and is widely used in vehicle gear oils, hydraulic oils an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 王俊明段况华张建荣徐小红周旭光陈馥婧
Owner PETROCHINA CO LTD
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