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Process for synthesis of n-octylamine using loop reactor

A loop reactor, n-octylamine technology, applied in chemical instruments and methods, ammonia-carboxylic acid reaction preparation, preparation of organic compounds, etc., can solve problems such as restricting industrialization, high reaction temperature, and increasing energy consumption.

Pending Publication Date: 2020-12-25
重庆合汇制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high reaction temperature of this method, the corrosion of fatty acids on equipment is greatly affected by the temperature, and the corrosion peak appears at 280 ° C. At the same time, the boiling point of octanoic acid, high temperature is likely to cause material entrainment, increase energy consumption, increase production costs, and seriously restrict the industrialization of this process.

Method used

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  • Process for synthesis of n-octylamine using loop reactor
  • Process for synthesis of n-octylamine using loop reactor
  • Process for synthesis of n-octylamine using loop reactor

Examples

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preparation example Construction

[0051] Dodecylbenzenesulfonate is obtained by the following preparation method: 1) the metered n-octanoic acid and dodecylbenzenesulfonic acid are dropped into at one time from the feeding port of the raw material preparation tank; Raise the temperature to 60°C, stir and keep warm for 30min, so that n-octanoic acid and dodecylbenzenesulfonic acid are evenly mixed; 3) put the measured metal oxide into the feed port of the raw material preparation tank, and stir for 2h; 4) After the reaction, 60 Keep warm at -80°C for standby; the molar ratio between dodecylbenzenesulfonic acid and metal oxide is 1:1.2; n-octanoic acid is used as a diluent, and the input amount is equal to the input amount of alkylbenzenesulfonic acid; metal oxide The material is selected according to the specific dodecyl sulfonate used in the embodiment, for example, when a single metal ion alkylbenzene sulfonate such as zinc dodecylbenzene sulfonate is used in the embodiment, the selected The metal oxide is Zn...

Embodiment 1

[0054]Feed 18t of n-octanoic acid into the loop reactor, then add 360kg of zinc dodecylbenzenesulfonate as a catalyst, replace it with nitrogen, feed liquid ammonia, start the reaction circulation pump, raise the temperature to 150°C, and keep it for 2 hours , continue to heat up to about 200°C, and react at 0.8MPa for 12 hours. After the reaction is completed and cooled, the discharge material enters the distillation tower for vacuum distillation; octanonitrile distillate can reach 99%, and its octanoic acid conversion rate is 97-99%. , the selectivity reaches 90-98%, and the distillation yield of octylnitrile reaches 97%. Feed the octonitrile distillate into the loop reactor, in the presence of 324kg Raney nickel catalyst, feed the hydrogen with a purity of 99%, 300kg liquid ammonia as a reaction inhibitor, the total pressure is at 4.0MPa, and the temperature is at 150°C Under the conditions, the reaction was carried out for 6 hours. After the reaction was completed, the cru...

Embodiment 2

[0056] Feed 18t of n-octanoic acid into the loop reactor, then add 360kg of aluminum dodecylbenzenesulfonate as a catalyst, replace it with nitrogen, feed liquid ammonia, start the reaction circulation pump, raise the temperature to 150°C, and keep it for 2 hours , continue to heat up to about 200°C, and react at 0.8MPa for 12 hours. After the reaction is completed and cooled, the discharge material enters the distillation tower for vacuum distillation; octanonitrile distillate can reach 99%, and its octanoic acid conversion rate is 97-99%. , the selectivity reaches 90-98%, and the distillation yield of octylnitrile reaches 97%. Feed the octonitrile distillate into the loop reactor, in the presence of 324kg Raney nickel catalyst, feed the hydrogen with a purity of 99%, 300kg liquid ammonia as a reaction inhibitor, the total pressure is at 4.0MPa, and the temperature is at 150°C Under the conditions, the reaction was carried out for 6 hours. After the end, a crude product was o...

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Abstract

The invention relates to the technical field of n-octylamine synthesis, in particular to a method for synthesizing n-octylamine by using a loop reactor. The invention relates to a method for synthesizing n-octylamine by using a loop reactor, which comprises the following step of: reacting n-caprylic acid, liquid ammonia and hydrogen serving as raw materials in the loop reactor. By adopting a special ammoniation catalyst, the ammoniation reaction temperature is remarkably reduced, so that corrosion to a pipeline is effectively prevented; in addition, the method is high in conversion rate, goodin selectivity, low in reaction temperature, small in corrosion to equipment, low in raw material cost, small in three-waste pollution and suitable for industrial production of n-octylamine.

Description

technical field [0001] The invention relates to the technical field of n-octylamine synthesis, in particular to a method for synthesizing n-octylamine using a loop reactor. Background technique [0002] N-octylamine is an organic chemical product and the main raw material for the synthesis of medicines, pesticides, and pesticide intermediates. It is widely used in slow-release agents, lubricant additives, bactericides, and surfactants. At present, domestic consumption mainly depends on imports. [0003] In the prior art, the synthetic method of n-octylamine mainly contains following several kinds: [0004] Method 1: heating and catalytic synthesis of octane chloride and ammonia in ethanol solution, this method has the disadvantages of poor selectivity, a large amount of chlorides are generated at the same time, the treatment of three wastes is difficult, and the generation cost is high. [0005] Method 2: Chinese patent CN200610154969.X reports that under high temperature ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/07C07C253/22C07C255/03B01J31/02
CPCC07C209/48C07C253/22B01J31/0225C07C211/07C07C255/03
Inventor 梅金龙李爽陈亮刘琛
Owner 重庆合汇制药有限公司
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