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Continuous preparation method of propylene glycol monobutyl ether

A technology of propylene glycol butyl ether and butanol, which is used in ether preparation, chemical instruments and methods, and alkylene oxide preparation of ether, etc. Effect

Inactive Publication Date: 2016-06-15
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, it also overcomes the problems of low conversion rate of raw materials in previous catalytic reactions, rapid reduction in catalyst activity, and excessive waste water.

Method used

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  • Continuous preparation method of propylene glycol monobutyl ether
  • Continuous preparation method of propylene glycol monobutyl ether
  • Continuous preparation method of propylene glycol monobutyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] First wrap the jacketed Add solid base NH(CH 2 ) 2 NH 2 / MCM-41, the tubular reactor is composed of a three-stage heating tubular furnace, wherein the ratio of the solid base catalyst filling to the inner volume of the tubular reactor is 0.60:1; the raw material butanol and propylene oxide are mixed according to the mass ratio The ratio of 2.55:1 is pumped into the mixer by the metering pump, heated and vaporized by the preheater heating furnace, and enters the tubular reactor for reaction. The mixed gas generated by the reaction enters the collector after being condensed by the condenser, and the output content at the bottom of the collector is ≥62.0 The crude product of propylene glycol butyl ether in wt%; the crude product of propylene glycol butyl ether extracted from the bottom of the collector above 50.0% is added to the side line rectification tower, and after vacuum distillation, the side line discharge of the side line rectification tower has a content ≥ 99....

Embodiment 2

[0041] The pressure of the tubular reactor was changed, and the gas phase catalytic reaction was carried out under the same conditions as step (1) in the embodiment (1). Control the mass ratio of butanol / propylene oxide in the tubular reactor to 2.55:1, the ratio of solid base catalyst filling to the inner volume of the tubular reactor to 0.6:1, and the space velocity ratio to 0.65h -1 , the reaction temperature is 140.5°C, and the influence of pressure on the purity of the crude product of propylene glycol butyl ether and the conversion rate of propylene oxide is shown in figure 2 As shown, when the pressure was at 0.12-0.18MPa, the purity of the crude product of propylene glycol butyl ether and the conversion rate of propylene oxide increased, and when the pressure continued to increase, the purity of the crude product of propylene glycol butyl ether and the conversion rate of propylene oxide decreased to some extent. Its main reason is because propylene glycol butyl ether ...

Embodiment 3

[0043] Change the reaction temperature of tubular reactor, adopt the same condition as step (1) in the embodiment (1) to carry out gas-phase catalytic reaction, control the mass ratio of butanol / propylene oxide in the tubular reactor to be 2.55: 1, catalyst The ratio of the filling amount to the inner volume of the tubular reactor is 0.6:1, and the space velocity ratio is 0.65h -1 , the reaction pressure is 0.18MPa, and the influence of temperature on the crude product purity and propylene oxide conversion rate of propylene glycol butyl ether is shown in image 3 As shown, when the temperature is 120.0-140.5°C, the purity of the crude product of propylene glycol butyl ether and the conversion rate of propylene oxide increase, and when the temperature continues to increase, the purity of the crude product of propylene glycol butyl ether and the conversion rate of propylene oxide decrease. Its main reason is because propylene glycol butyl ether generates derivative product and r...

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Abstract

The invention discloses a continuous preparation method of propylene glycol monobutyl ether. The method comprises the following steps: carrying out gas-phase catalytic reaction on butanol and epoxypropane in a tubular reactor by using a solid alkali NH(CH2)2NH2 / MCM-41 as a catalyst, and carrying out rectification separation on the obtained reaction product to obtain the propylene glycol monobutyl ether. The preparation method can implement continuous operation; the conversion rate of epoxypropane into propylene glycol monobutyl ether can reach 97.10% or above; the purity of the finally prepared propylene glycol monobutyl ether can reach 99.0 wt% or above; and the recovered butanol can be recycled. After the solid alkali catalyst NH(CH2)2NH2 / MCM-41 is continuously used for 180 hours, the epoxypropane conversion rate is only lowered by 0.29%. The technique solves the problems of low raw material conversion rate, high catalyst activity reduction speed, abundant wastewater and the like in the past catalytic reaction.

Description

technical field [0001] The invention relates to a preparation method of propylene glycol butyl ether, in particular to a continuous preparation method of propylene glycol butyl ether. Background technique [0002] Propylene glycol ether is mainly used in solvents, engine fuel additives, antifreeze, brake fluid, chemical intermediates, etc. The consumption growth of glycol ether in the world is mainly in Europe. Compared with glycol ether, the consumption growth rate of propylene glycol ether is relatively fast. my country's propylene glycol ether is mainly used in the fields of coatings, inks, cleaning agents and pesticides. In the future, the main driving force for the consumption of propylene glycol ether in my country will be the paint and ink industry. In the field of automobile brake fluid and antifreeze fluid, propylene glycol ether may also replace part of ethylene glycol ether, and there is a certain potential market. [0003] At present, there are mainly two ways ...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C41/42C07C43/13B01J31/26
CPCC07C41/03C07C41/42B01J31/26B01J2231/48C07C43/13
Inventor 顾正桂朱俊健
Owner NANJING NORMAL UNIVERSITY