Preparation method of rubber plasticizer tricresyl phosphate
A technology of tricresyl phosphate and rubber plasticizer, applied in the field of preparation of tricresyl phosphate, can solve the problems of difficult separation, unstable catalyst, pollute the environment and the like, and achieve the effect of simple treatment
Inactive Publication Date: 2015-05-06
QINGDAO WANGYU RUBBER
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Problems solved by technology
Tricresyl phosphate is produced by one-step reaction of phosphorus oxychloride and mixed cresols. The synthesis process is simple, but the choice of catalyst is very important to the whole reaction. At present, Lewis acid is used as catalyst in the production process, but these catalysts are unstable in themselves, It is easy to decompose in the medium, the post-reaction treatment is troublesome, the separation is difficult, the catalyst cannot be recycled and reused, and the environment is polluted
Method used
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Embodiment
[0015] 1. Add 17.8g mixed cresols and 0.37g catalyst TiSiW in a three-necked flask 12 o 40 / TiO 2 , stirred and heated to 60°C, added dropwise 5ml of phosphorus oxychloride, the dropwise addition was completed within 1 hour, and the temperature was raised to 100°C, and reacted for 8 hours;
[0016] 2. Filter out the catalyst, distill under reduced pressure, and the resulting fraction is tricresyl phosphate.
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Abstract
The invention discloses a preparation method of a rubber plasticizer tricresyl phosphate. The method includes the following steps: 1, adding mixed cresol and TiSiW12O40 / TiO2 in a three-neck flask, heating withle stirring to 60 DEG C, dropwise adding phosphorus oxychloride within 1 h, heating to 100 DEG C, and reacting for 8 h; and 2, filtering out the catalyst, and conducting reduced pressure distillation to obtain a fraction of tricresyl phosphate. According to the preparation method of the rubber plasticizer tricresyl phosphate provided by the invention, supported heteropoly acid is used to substitute Lewis acid for synthesis of tricresyl phosphate; and the catalyst has the advantages of stabilization simple post-treatment for the reaction, recyclability, green and environment-friendliness.
Description
[0001] technical field [0002] The invention relates to a method for preparing a rubber plasticizer, in particular to a method for preparing tricresyl phosphate. [0003] Background technique [0004] Tricresyl phosphate is a standard flame retardant plasticizer for synthetic rubber, polyester, and polyvinyl chloride. It can endow high polymers with good wear resistance, weather resistance, mildew resistance, radiation resistance, and electrical properties. It can also be used Used as gasoline additive, lubricating oil additive and hydraulic oil. Tricresyl phosphate is produced by one-step reaction of phosphorus oxychloride and mixed cresols. The synthesis process is simple, but the choice of catalyst is very important to the whole reaction. At present, Lewis acid is used as catalyst in the production process, but these catalysts are unstable in themselves, It is easy to decompose in the medium, the post-reaction treatment is troublesome, the separation is difficult, the ...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
Inventor 梁松杰
Owner QINGDAO WANGYU RUBBER
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