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Preparation method of liquid amine type antioxidant

A kind of amine antioxidant, liquid technology

Inactive Publication Date: 2019-05-10
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method is relatively complicated. Diphenylamine is removed by vacuum distillation and decolorized by activated carbon, which produces a large amount of solid waste and causes potential harm to the environment.
The product prepared by this method has a darker color and more diphenylamine residues, which affects the appearance and performance of the product

Method used

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  • Preparation method of liquid amine type antioxidant
  • Preparation method of liquid amine type antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The present embodiment provides a kind of preparation method of liquid amine antioxidant RF5057, comprises the following steps:

[0021] (1) Add 200g activated clay, 2g p-toluenesulfonic acid and 5g activated alumina to compound in the mixing device, and start the mixing device for half an hour to obtain a uniformly mixed activated clay composite catalyst, which is ready for use.

[0022] Add 130g diphenylamine, 30g activated clay composite catalyst, 90ppm polymerization inhibitor hydroquinone in the stainless steel reaction kettle, feed nitrogen into the reaction kettle, fully replace the air in the kettle, and start heating. At the same time, the vacuum system is turned on, and the vacuum degree in the kettle is controlled at 0.08MPa~0.095MPa. When the temperature reaches about 70°C, the stirring is started at a stirring rate of 300 rpm, and the moisture in the reaction system is removed under vacuum conditions. Gradually raise the temperature to 100°C for half an ho...

Embodiment 2

[0026] The present embodiment provides a kind of preparation method of liquid amine antioxidant RF5057, comprises the following steps:

[0027] (1) Add 200g of activated clay, 1g of p-toluenesulfonic acid and 3g of activated alumina in the mixing device to compound, and start the mixing device for half an hour to obtain a uniformly mixed activated clay composite catalyst, which is ready for use.

[0028] Add 130g diphenylamine, 40g activated clay composite catalyst, 90ppm polymerization inhibitor hydroquinone in the stainless steel reaction kettle, feed nitrogen into the reaction kettle, fully replace the air in the kettle, and start heating. At the same time, the vacuum system is turned on, and the vacuum degree in the kettle is controlled at 0.08MPa~0.095MPa. When the temperature reaches about 70°C, the stirring is started at a stirring rate of 300 rpm, and the moisture in the reaction system is removed under vacuum conditions. Gradually raise the temperature to 100°C for h...

Embodiment 3

[0032] The present embodiment provides a kind of preparation method of liquid amine antioxidant RF5057, comprises the following steps:

[0033] (1) Add 200g of activated clay, 3g of p-toluenesulfonic acid and 1g of activated alumina to the mixing device for compounding, and start the mixing device for half an hour to obtain a uniformly mixed activated clay composite catalyst, which is ready for use.

[0034] Add 130g diphenylamine, 25g activated clay composite catalyst, 75ppm polymerization inhibitor 2,6-dinitro-p-cresol in the stainless steel reaction kettle, feed nitrogen into the reaction kettle, fully replace the air in the kettle, and start heating. At the same time, the vacuum system is turned on, and the vacuum degree in the kettle is controlled at 0.08MPa~0.095MPa. When the temperature reaches about 70°C, the stirring is started, and the stirring rate is 300 rpm, and the moisture in the reaction system is removed under vacuum conditions. Gradually raise the temperature...

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Abstract

The invention discloses a preparation method of a liquid amine type antioxidant. The preparation method includes following steps: proportionally adding diphenylamine, activated clay composite catalystand polymerization inhibitor into a reaction kettle; proportionally adding diisobutylene into the reaction kettle, and rising temperature for alkylation reaction; cooling and filtering a reaction product after reaction in the step (2), and performing reduced pressure distillation on filtered-out mother liquid to remove unreacted olefin to obtain the liquid amine type antioxidant. The activated clay composite catalyst is adopted for alkylation reaction, so that reaction temperature is lowered, reaction time is shortened, generated alkyl diphenylamine RF5057 is little in diphenylamine residue,the antioxidant is shallow in appearance color and free of three wastes after aftertreatment, and the preparation method is an environment-friendly synthesis process.

Description

technical field [0001] The invention belongs to the technical field of lubricating oil additives, and mainly relates to a synthesis method of a lubricating oil antioxidant, in particular to a preparation method of a liquid amine antioxidant. Background technique [0002] Antioxidants are compounds that prevent or delay the oxidation of organic materials. All organic materials have the property of reacting with oxygen in the air, and the substances will change their original properties after the oxidation reaction. Although there are many methods to prevent the oxidation of organic matter in industry, adding antioxidants is still the easiest and most effective method. During use, lubricating oil will inevitably come into contact with oxygen to undergo chemical action, oxidize and deteriorate, generate acidic substances, and cause equipment corrosion. [0003] Amine antioxidants are one of the earliest antioxidants, and they are highly efficient high-temperature antioxidants....

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C211/55C10M133/12C10N30/10C10N30/02
Inventor 王学义范金凤乔庆文
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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