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Preparation method of bi-(2-ethylhexyl)

A technology of ethylhexyl and ethylhexanol, which is applied in the preparation of amino compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of complicated steps and low product yield, and achieve selectivity improvement and process simplification steps, investment reduction and production efficiency effects

Inactive Publication Date: 2012-12-26
张家港市大伟助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Di(2-ethylhexyl)amine is a synthetic intermediate of high-grade lubricating oil extreme pressure anti-wear agent. With the development of domestic high-grade lubricating oil industry, the demand for it increases rapidly; 2-ethylhexanol and Ammonia is used as a raw material. First, 2-ethylhexanonitrile is generated under the action of a catalyst, and 2-ethylhexylamine is obtained through hydrogenation catalysis, and the pure product is obtained through rectification, and then deaminated under the action of a catalyst to generate bis(2-ethylhexylamine). Base hexyl) amine, this method step is numerous and diverse, and product yield is low

Method used

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  • Preparation method of bi-(2-ethylhexyl)

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Embodiment 1

[0018] Weigh 130g of 2-ethylhexanol and 10 grams of activated quaternary Raney nickel catalyst into a 1L autoclave, replace with nitrogen and hydrogen respectively, and then feed 85 grams of anhydrous liquid ammonia, then feed 0.3Mpa hydrogen, Start stirring, raise the temperature to 160-190°C and keep it for 8 hours, lower the temperature to below 100°C, release ammonia and hydrogen to 0.5Mpa, continuously feed hydrogen, keep the reaction pressure and continuously vent, heat up to 190-210°C for reaction 3 hour, cooling and venting to normal pressure, discharging, filtering the catalyst, clear liquid rectification to obtain 109g of product.

Embodiment 2

[0020] Weigh 130g of 2-ethylhexanol and 10 grams of activated binary Raney nickel catalyst into a 1L autoclave, replace with nitrogen and hydrogen respectively, then feed 85 grams of anhydrous liquid ammonia, and then feed 0.3Mpa hydrogen, Start stirring, raise the temperature to 180-210°C and keep it for 10 hours, lower the temperature to below 100°C, release ammonia and hydrogen to 0.5Mpa, continuously feed hydrogen, keep the reaction pressure and continuously vent, heat up to 200-220°C for reaction 4 hour, cooling and venting to normal pressure, discharging, filtering catalyst, clear liquid rectification to obtain product 102g.

Embodiment 3

[0022] Weigh 130g of 2-ethylhexanol and 6g of copper-nickel carrier catalyst (with clay as the carrier) into a 1L autoclave, replace with nitrogen and hydrogen respectively, then feed 85g of anhydrous liquid ammonia, and then feed 0.3MPa hydrogen , start stirring, raise the temperature to 210-240°C and keep it for 12 hours, lower the temperature to below 100°C, release ammonia and hydrogen to 0.5Mpa, continuously feed hydrogen, keep the reaction pressure and continuously vent, heat up to 220-240°C to react After 6 hours, the temperature was lowered and vented to normal pressure, the material was discharged, the catalyst was filtered, and the clear liquid was rectified to obtain 97g of the product.

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Abstract

The invention discloses a preparation method of bi-(2-ethylhexyl), mainly comprising the following steps of: adding 2-ethylhexanol, ammonia, hydrogen and a catalytic agent in a high-pressure reaction kettle and stirring at high speed; carrying out catalysis and amination reaction at the temperature of 120-260 DEG C to prepare a mixture containing2-ethylhexylamine, 2-ethylhexanol and bi-(2-ethylhexyl); continuously carrying out condensation deamination reaction on the mixture in a hydrogen atmosphere to obtain a reactant taking bi-(2-ethylhexyl) ammonia as the main component, wherein the product selectivity is higher than 90 percent, and then rectifying to obtain the bi-(2-ethylhexyl), wherein the purity of the bi-(2-ethylhexyl) is higher than 99 percent. The bi-(2-ethylhexyl) prepared by the method is mainly used for the synthesis of high-grade lubricant oil extreme-pressure antiwear agents.

Description

technical field [0001] The invention relates to a preparation method of di(2-ethylhexyl)amine. Background technique [0002] Di(2-ethylhexyl)amine is a synthetic intermediate of high-grade lubricating oil extreme pressure anti-wear agent. With the development of domestic high-grade lubricating oil industry, the demand for it increases rapidly; 2-ethylhexanol and Ammonia is used as a raw material. First, 2-ethylhexanonitrile is generated under the action of a catalyst, and 2-ethylhexylamine is obtained through hydrogenation catalysis, and the pure product is obtained through rectification, and then deaminated under the action of a catalyst to generate bis(2-ethylhexylamine). Base hexyl) amine, this method step is numerous and diverse, and product yield is low. Contents of the invention [0003] The purpose of the invention is to provide a method for preparing di(2-ethylhexyl)amine with simple process and high product yield. [0004] In order to achieve the above object, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/07C07C209/60C07C209/16
Inventor 黄德周勇新谌建新
Owner 张家港市大伟助剂有限公司