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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 erucamide, which can solve the problems of low yield, low product purity and long reaction time in the prior art.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 35g of butyl silicate to a 250ml flask, raise the temperature to 42°C under vacuum, then add 55g of polybutyl titanate and 10g of polyethylene glycol (PEG400) in turn, then raise the temperature to 42°C, and stir at constant temperature Mix for 45 minutes, cool to room temperature, and then filter to obtain the finished catalyst.

[0022] Add 6kg of erucic acid into a 10L reactor, vacuumize, degas and dehydrate, and raise the temperature to 150°C, start filling ammonia gas, the flow of ammonia gas is controlled at 0.1-0.3L / min, and the pressure in the reactor is controlled at 0.28- 0.32MPa, the temperature in the reactor is controlled at 172-175°C.

[0023] After reacting for 4 hours, use a metering pump to continuously and evenly add 24g of catalyst, continue the reaction for 4 hours, then cool down to 120°C, filter to obtain the product erucamide, the product yield is 97.6%, the melting point is 81.9°C, the acid value is 0.23mgKOH / g, iodine Value 75.9gI 2 / 100g,...

Embodiment 2

[0025] Add 45g of butyl silicate to a 250ml flask, raise the temperature to 48°C under vacuum, then add 40g of polybutyl titanate and 15g of polyethylene glycol (PEG600) in sequence, then raise the temperature to 48°C, and stir at constant temperature Mix for 50 minutes, cool to room temperature, and then filter to obtain the finished catalyst.

[0026] Add 6kg of erucic acid into a 10L reactor, vacuumize, degas and dehydrate, and raise the temperature to 148°C, start filling with ammonia gas, the flow rate of ammonia gas is 0.2-0.4L / min, and the pressure in the reactor is controlled at 0.30-0.36MPa , The temperature in the reactor is controlled at 170-173°C.

[0027] After reacting for 5 hours, use a metering pump to continuously and evenly add 18g of catalyst, continue the reaction for 3 hours, then cool down to 120°C, filter to obtain the product erucamide, the product yield is 96.8%, the melting point is 82.1°C, the acid value is 0.19mgKOH / g, iodine Value 76.1gI 2 / 100g,...

Embodiment 3

[0029] Add 31g of butyl silicate to a 250ml flask, heat up to 51°C under vacuum, then add 51g of polybutyl titanate and 18g of polyethylene glycol (PEG200) in sequence, continue to heat up to 51°C, stir and mix at constant temperature for 35min, Cool to room temperature, and then filter to obtain the finished catalyst.

[0030] Add 6kg of erucic acid into a 10L reactor, vacuumize and degas and dehydrate, and raise the temperature to 155°C, start filling with ammonia gas, control the flow rate of ammonia gas at 0.2-0.5L / min, and control the pressure in the reactor at 0.38-0.45MPa , The temperature in the reactor is controlled at 173-176°C.

[0031] After reacting for 3 hours, use a metering pump to continuously and evenly add 21g of catalyst, continue the reaction for 5 hours, then cool down to 130°C, and filter to obtain the product erucamide, the product yield is 97.1%, the melting point is 82.6°C, the acid value is 0.33mgKOH / g, iodine Value 75.3gI 2 / 100g, the total amide ...

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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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