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Preparation method of phosphite phenolic ester antioxidant additive

An anti-oxidant aid, phosphite phenol ester technology, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve high synthesis temperature, difficult waste liquid treatment, sub- The problem of low purity of phenolic phosphate antioxidant additives can be solved to improve the conversion rate, the solvent recovery process is simple and easy, and the effect of improving the anti-hydrolysis ability

Inactive Publication Date: 2021-04-06
RIANLON (ZHUHAI) NEW MATERIAL CO LTD +1
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  • Abstract
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  • Application Information

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Problems solved by technology

[0008] The main purpose of the present invention is to provide a preparation method of phosphite phenolic ester antioxidant additives to solve the problems of low purity, high synthesis temperature and difficulty in waste liquid treatment in the preparation of phosphite phenolic ester antioxidant additives by existing methods Major and other issues

Method used

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preparation example Construction

[0025] As described in the background technology, there are problems such as low purity, high synthesis temperature and difficulty in waste liquid treatment in the preparation of phosphite phenolic ester antioxidant additives by the existing method. In order to solve the above-mentioned technical problems, the application provides a preparation method of phosphite phenolic ester antioxidant additives, the preparation method of the phosphite phenolic ester antioxidant additives comprises: in the presence of a solvent and a catalyst, making phenol Compounds react with phosphorus trichloride to obtain phosphite phenolic ester antioxidant additives, and the solvent is C 8 ~C 10 Alkane compound, synthetic route is as shown in formula (I):

[0026] where R 1 Including but not limited to H, CH 3 or C(CH 3 ) 3 , R 2 Including but not limited to H, CH 3 , C(CH 3 ) 3 or C n h 2n+1 , n=5~9;

[0027] Preferably: R 1 for C(CH 3 ) 3 when R 2 for C(CH 3 ) 3 ; 1 For H, R ...

Embodiment 1

[0044] The preparation method of phosphite phenol ester antioxidant auxiliary agent is as follows:

[0045] 1) Add 178.0g 2,4-di-tert-butylphenol, 8.90g triethylamine and 72.98g n-octane into a four-neck flask with electric stirring, constant pressure dropping funnel and reflux condenser, and connect the tail gas In the absorption device, the weight ratio of catalyst, alkane compound and phenol compound is 5:41:100.

[0046] 2) The temperature was raised to 50°C, and 42.31 g of phosphorus trichloride was started to be added dropwise at this temperature. The dropwise addition time was 1 hour, and the molar ratio of phosphorus trichloride to phenolic compounds was 1:2.78.

[0047] 3) After the dropwise addition, keep the reaction at 50° C. for 1 hour, then raise the temperature to 110° C. and react under reduced pressure and reflux for 12 hours at this temperature. The vacuum degree is 0.050-0.065 MPa. After the reaction, the pH of the reaction solution is detected to be 5.5, an...

Embodiment 2

[0054] The preparation method of phosphite phenol ester antioxidant auxiliary agent is as follows:

[0055] 1) Add 178.0g 2-tert-butylphenol, 0.89g tripropylamine and 169.10g nonane into a four-neck flask equipped with electric stirring, constant pressure dropping funnel and reflux condenser, and connect the tail gas absorption device, catalyst, alkane The weight ratio of quasi-like compounds to phenolic compounds is 0.5:95:100.

[0056] 2) The above mixture was heated from room temperature to 65°C, and at this temperature, 50.07 g of phosphorus trichloride was added dropwise for 3 hours, and the molar ratio of phosphorus trichloride to phenolic compound was 1:3.2.

[0057] 3) After the dropwise addition, keep the reaction at 65° C. for 5 hours, then raise the temperature to 158° C., and keep the reaction at this temperature for 10 hours.

[0058] 4) After the reaction was completed, the temperature was lowered to 20° C., stirred for 1 h, and then filtered. The filter cake wa...

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Abstract

The invention provides a preparation method of a phosphite phenolic ester antioxidant additive. The preparation method of the phosphite phenolic ester antioxidant additive comprises the following steps: in the presence of a solvent and a catalyst, reacting a phenolic compound with phosphorus trichloride to obtain the phosphite phenolic ester antioxidant additive, the solvent is a C8-C10 alkane compound, the synthetic route is shown as a formula (I), and R1 is selected from H, CH3 or C(CH3)3; R2 is selected from H, CH3, C (CH3) 3 or CnH2n+1, and n is equal to 5-9. Because the C8-C10 alkane compound has lower polarity, compared with other solvents, the solubility of hydrogen chloride in the reaction solvent is lower; the boiling point of the solvent is higher, so that the whole reaction process can be carried out at higher temperature, thereby being beneficial to enhancing the yield of the antioxidant assistant and the conversion rate of the raw material, and further lowering the dissolution amount of the hydrogen chloride in the reaction system.

Description

technical field [0001] The invention relates to the field of preparation of phosphite phenolic ester antioxidant additives, in particular to a preparation method of phosphite phenolic ester antioxidant additives. Background technique [0002] Aging phenomena such as stickiness, discoloration, and embrittlement of polymer materials will occur during long-term use, which will undoubtedly bring huge losses and inconvenience to national production and people's lives. Adding antioxidant additives is one of the means to delay the aging of materials. At present, there are many kinds of antioxidants, among which phosphite phenolic ester, as an auxiliary antioxidant additive, can be used in combination with hindered phenolic antioxidants and light stabilizers, and has a good synergistic effect. Based on this, its application in polyolefins is becoming more and more extensive, and its synthesis method has always been the focus of researchers. [0003] An existing literature reports ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/145
CPCC07F9/145
Inventor 田军刘阳勾少萍贾梦婧张会京范小鹏熊昌武孙春光李海平
Owner RIANLON (ZHUHAI) NEW MATERIAL CO LTD
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