Liquid-phase catalyst and method for synthesizing erucyl amide through liquid-phase catalysis of liquid-phase catalyst

A liquid-phase catalyst, erucic acid amide technology, applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low product purity, low yield, long reaction time, etc., and achieve catalytic effect. Good, improve the synthesis conversion rate and yield, the effect of less equipment wear

Pending Publication Date: 2022-03-22
江西威科油脂化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The second object of the present invention is to provide a method for liquid-phase catalytic synthesis of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0020] Example 1:

[0021] Dutyricate 35 g of butyl silicate was added to 250 ml of flask, and the temperature was raised to 42 ° C, then the polyetheter titanate 55g, polyethylene glycol (PEG400) was sequentially added, and then the temperature was raised to 42 ° C, constant temperature agitation. It was mixed for 45min, cooled to room temperature, then filtered, the catalyst finished product was obtained.

[0022] 5 kg of mustard is added to 10 L of the reactor, vacuum, degassed dehydration, and temperature rise to 150 ° C, start to be filled with ammonia gas, ammonia gas flow control at 0.1-0.3L / min, the pressure control in the reactor is 0.28- 0.32 MPa, temperature control in the reactor control 172-175 ° C.

[0023] After 4 h, the catalyst is continuously added to the catalyst 24 g, and the reaction is continuously meta, then the temperature is lowered to 120 ° C, filtered, resulting in the product erlanamide, the product yield is 97.6%, the melting point 81.9 ° C, the acid...

Example Embodiment

[0024] Example 2:

[0025] Dutyry 45 g of butyl silicate was added to 250 ml of flask, in a vacuum state, heated to 48 ° C, then polyated titanate 40g, polyethylene glycol 15g (PEG600), then raised to 48 ° C, constant temperature agitation It was mixed for 50 min, cooled to room temperature, then filtered, the catalyst finished product was obtained.

[0026] 5 kg of mustard is added to 10 L of the reaction kettle, vacuum, degassed dehydration, and temperature rise to 148 ° C, start to be charged with ammonia gas, ammonia flow 0.2-0.4L / min, pressure control in the reactor control 0.30-0.36MPa The temperature control of 170-173 ° C in the reaction kettle.

[0027] After 5 h, the catalyst was continuously added to the catalyst for 3 h, and then the reaction was continued, then the temperature was lowered to 120 ° C, filtered, obtained by 96.8%, and the product yield was 96.8%, the melting point 82.1 ° C, acid value of 0.19 mgKOH / g, iodine Value 76.1gi 2 / 100 g, the total amide c...

Example Embodiment

[0028] Example 3:

[0029] Dutyr silicate 31g was added to 250 ml of flask, and the temperature was raised to 51 ° C in a vacuum, and then polyetheter titanate 51g, polyethylene glycol (PEG200) was added, and the temperature was warmed to 51 ° C, and the constant temperature was stirred for 35 min. Cool to room temperature and then filtered to obtain a catalyst finished product.

[0030] 5 kg of erlalin was added to 10 L of the reaction kettle, evacuated and dehydrated, and heated to 155 ° C, started with ammonia gas, ammonia flow control 0.2-0.5L / min, pressure control in the reactor 0.38-0.45MPa The temperature controls 173-176 ° C in the reactor.

[0031] After 3 h, the catalyst 21 g was continuously added using a metering pump, and the reaction was continued for 5 h, then it was lowered to 130 ° C, filtered, obtained by 97.1%, the product yield was 97.1%, the melting point was 82.6 ° C, the acid value of 0.33 mgKOH / g, iodine Value 75.3gi 2 / 100 g, total amide content of 98...

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Abstract

The invention discloses a liquid-phase catalyst and a method for synthesizing erucyl amide through liquid-phase catalysis of the liquid-phase catalyst. The liquid-phase catalyst is prepared from butyl silicate, polybutyl titanate and polyethylene glycol (PEG200-800). The synthesis method comprises the following steps: A, firstly heating butyl silicate, then adding polybutyl titanate and polyethylene glycol, keeping the temperature, stirring and mixing in a vacuum state, cooling to room temperature, then filtering to obtain a finished product liquid phase catalyst, and sealing and storing; and B, continuously and uniformly adding the liquid-phase catalyst into a reactor (kettle) in which erucic acid and ammonia are subjected to amidation reaction by adopting a metering pump to prepare erucyl amide. Compared with the existing solid catalyst, the reaction temperature and reaction pressure are reduced, the reaction time is shortened, the product yield and quality are improved, the addition amount is small, use is convenient, continuous and uniform addition can be achieved, and continuous synthesis can be achieved; no catalyst solid waste exists, so that the environment-friendly treatment cost is saved.

Description

technical field [0001] The invention relates to the technical field of fatty acid amide synthesis, in particular to a liquid-phase catalyst and a method for synthesizing erucamide through liquid-phase catalysis. Background technique [0002] Erucamide (CAS NO: 112-84-5) is made from erucic acid extracted from natural oil (rapeseed oil) through amidation reaction with ammonia. It is an important fatty acid derivative. The product is environmentally friendly and non-toxic. Its molecular structure contains long carbon chains and polar amide groups. It has very excellent surface properties, especially smooth, lubricating, dispersing, anti-sticking, mold release and anti-scratch effects. Wide range of applications. [0003] The amidation reaction between erucic acid and ammonia belongs to the gas-liquid phase reaction. The gaseous ammonia can only react on the surface of liquid erucic acid when it is dissolved or adsorbed. The solubility is extremely small, and it needs to be c...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C231/02C07C233/09
CPCB01J31/068C07C231/02C07C233/09Y02P20/584
Inventor 吴剑陈淇吴贵岚吴勇圣
Owner 江西威科油脂化学有限公司
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