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Preparation method for styrenated diphenylamine antioxidant

A technology of styrenated diphenylamine and antioxidant, which is applied in the field of preparation of styrenated diphenylamine antioxidant, can solve the problems of not being able to meet environmental protection and high temperature performance, and achieve stable activity, simple device structure, and easy preparation Effect

Inactive Publication Date: 2015-07-01
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The antioxidant zinc dialkyldithiophosphate (ZDDP) in general engine oil can no longer meet the requirements of environmental protection and high temperature performance, so it is necessary to develop new high temperature antioxidants

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 200g of diphenylamine (purity 99.8%) and 9.8g of acid-treated activated clay into a 1L reactor equipped with a stirrer, dropping device and nitrogen replacement device, and start heating to 50-60 °C, after the diphenylamine is completely dissolved, start stirring and raise the temperature to 175 °C. 360g of styrene was continuously added dropwise into the above reactor through the feeding device over 2h, and the reaction temperature was maintained at 175°C, and the system was kept at this temperature to continue the reaction for 2.5h. The above reaction product was diluted with toluene and then filtered to remove the catalyst to obtain an intermediate sample. The intermediate sample is subjected to atmospheric pressure distillation to remove toluene, and reduced pressure distillation to remove a small amount of diphenylamine to obtain a styrenated diphenylamine product.

Embodiment 2

[0011] Add 300g of diphenylamine (99.8% purity) and 15g of acid-treated activated clay into a 1L reactor equipped with a stirrer, dropping device and nitrogen replacement device, and start heating to 60-80°C after turning on the nitrogen replacement for 3 times After the diphenylamine is completely dissolved, start stirring and raise the temperature to 180°C. 380g of styrene was continuously added dropwise into the above reactor through the feeding device over 2h, and the reaction temperature was maintained at 170°C, and the reaction was continued at this temperature for 3h. The above reaction product was diluted with toluene and then filtered to remove the catalyst to obtain an intermediate sample. The intermediate sample is subjected to atmospheric pressure distillation to remove toluene, and reduced pressure distillation to remove a small amount of diphenylamine to obtain a styrenated diphenylamine product.

Embodiment 3

[0013] Add 100g of diphenylamine (purity 99.8%), 8g of acid-treated activated clay in a 1L reactor equipped with a stirrer, a dropping device and a nitrogen replacement device, start heating to 70°C after opening the nitrogen replacement for 3 times, and wait for After the diphenylamine was completely dissolved, the stirring was started and the temperature was raised to 160°C. 150g of styrene was continuously added dropwise into the above reactor through the feeding device over 2.5h, and the reaction temperature was maintained at 180°C, and the reaction was continued at this temperature for 2h. The above reaction product was diluted with toluene and then filtered to remove the catalyst to obtain an intermediate sample. The intermediate sample is subjected to atmospheric pressure distillation to remove toluene, and reduced pressure distillation to remove a small amount of diphenylamine to obtain a styrenated diphenylamine product.

[0014] In summary, the preparation method of...

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PUM

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Abstract

The invention relates to a preparation method for a styrenated diphenylamine antioxidant. The preparation method comprises the following steps: reacting polydiphenylamine with styrene by taking active white soil subjected to acidy treatment as a catalyst to generate a styrenated diphenylamine mixture; removing diphenylamine and styrene which are not completely reacted through distillation to obtain distillation raffinate, namely the styrenated diphenylamine antioxidant.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a preparation method of a styrenated diphenylamine antioxidant. Background technique [0002] At present, whether it is aerospace lubricants, engine lubricants, or industrial lubricants (such as high-temperature chain oil, compressor oil, heat transfer oil, etc.), high-performance antioxidants are required, and this requirement is Getting harsher. The antioxidant zinc dialkyldithiophosphate (ZDDP) in general engine oil can no longer meet the requirements of environmental protection and high-temperature performance, so it is necessary to develop new high-temperature antioxidants. The above requirements can be met by styrenated diphenylamine antioxidants. Styrenated diphenylamine is suitable for black and light-colored rubber products. It can replace anti-aging agents SP, BLE, anti-aging agents A, D, and RD in equal amounts. It has good protection against thermal-oxidative aging...

Claims

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Application Information

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IPC IPC(8): C07C209/60C07C211/55
Inventor 曹宏生韩大波徐小亮
Owner JIANGSU FEIYA CHEM IND
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