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Preparation method of propylene carbonate

A technology of propylene carbonate and propylene glycol is applied in the field of industrial synthesis of urea and propylene glycol to prepare propylene carbonate, and achieves the effects of high product yield, easy operation and fast reaction rate

Inactive Publication Date: 2015-10-07
何肖凤
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alcoholysis of urea and propylene glycol (PG) to synthesize PC is a route currently being researched and explored at home and abroad. This process has the advantages of mild reaction conditions, safe operation, safe raw materials, and small negative impact on the environment. However, the current research on this method relatively few

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Preparation of catalyst:

[0015] Magnesium oxide-zinc oxide composite rare earth oxide (preferably lanthanum oxide, cerium oxide) catalyst:

[0016] Prepared by co-precipitation method, 1mol / L Mg(NO 3 ) 2 and 1mol / L Zn(NO 3 ) 2 Mix the solution, stir and heat up to 45°C, slowly add 1mol / L Na 2 CO 3 Solution, control the time for about 30 minutes, adjust the pH value to 8-9, keep aging at 45°C for 2h, let stand, filter, wash, and dry at 110°C for 12h. Using the impregnation method, impregnate 1mol / L lanthanum nitrate and cerium nitrate on the dried catalyst for 12 hours, dry at 110°C for 3h, and bake at 500°C for 3h. Wherein the molar ratio of Mg:Zn is 2:1. The mass percentage of rare earth oxide is 0.5%;

[0017] 2. Preparation of propylene carbonate:

[0018] The molar ratio of urea to 1,2-propanediol is 1:3.5-4.5, on the magnesium oxide-zinc oxide composite rare earth oxide catalyst (the amount of catalyst is 2wt% dimethyl ether), the reaction temperature...

Embodiment 2

[0020] 1. Preparation of catalyst

[0021] Magnesium oxide-zinc oxide composite rare earth oxide (preferably lanthanum oxide, cerium oxide) catalyst:

[0022] Prepared by co-precipitation method, 1mol / L Mg(NO 3 ) 2 and 1mol / L Zn(NO 3 ) 2 Mix the solution, stir and heat up to 50°C, slowly add 1mol / L Na 2 CO 3 Solution, control the time for about 30 minutes, adjust the pH value to 8-9, keep aging at 50°C for 2h, let stand, filter, wash, and dry at 110°C for 12h. Using the impregnation method, impregnate 1mol / L lanthanum nitrate and cerium nitrate on the dried catalyst for 12 hours, dry at 110°C for 3h, and bake at 550°C for 3h. Wherein the molar ratio of Mg:Zn is 2:1. The mass percentage of rare earth oxide is 0.5%;

[0023] 2. Preparation of propylene carbonate:

[0024] The molar ratio of urea to 1,2-propanediol is 1:3.5-4.5, on the magnesium oxide-zinc oxide composite rare earth oxide catalyst (the catalyst dosage is 1.5wt% of dimethyl ether), the reaction temperatur...

Embodiment 3

[0026] 1. Preparation of catalyst

[0027] Magnesium oxide-zinc compound rare earth oxide (preferably lanthanum oxide, cerium oxide) catalyst:

[0028] Prepared by co-precipitation method, 1mol / L Mg(NO 3 ) 2 and 1mol / L Zn(NO 3 ) 2 Mix the solution, stir and heat up to 65°C, slowly add 1mol / L Na 2 CO 3 Solution, control the time for about 30 minutes, adjust the pH value to 7-8, keep aging at 65°C for 2h, let stand, filter, wash, and dry at 110°C for 12h. Using the impregnation method, impregnate 1mol / L lanthanum nitrate and cerium nitrate on the dried catalyst for 12 hours, dry at 110°C for 3h, and bake at 600°C for 3h. Wherein the molar ratio of Mg:Zn is 2:1. The mass percentage of rare earth oxide is 0.5%;

[0029] 2. Preparation of propylene carbonate:

[0030] The molar ratio of urea to 1,2-propanediol is 1:3.5-4.5, on the magnesium oxide-zinc oxide composite rare earth oxide catalyst (the amount of catalyst is 2.5wt% of dimethyl ether), the reaction temperature is...

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Abstract

The invention discloses a preparation method of propylene carbonate. The preparation method is characterized by comprising the following steps: adding urea and 1,2-propylene glycol at a molar ratio of 1:(1-6) into a high-pressure kettle, and conducting a reaction on a magnesium oxide-zinc oxide composite rare earth oxide catalyst, wherein the catalyst dosage is 1-3wt% of the urea; stirring for heating, wherein the reaction temperature is 120-180 DEG C, and the reaction time is 0.5-4h; after the reaction, stopping stirring, and cooling to room temperature; and distilling the kettle liquid and separating to obtain the product propylene carbonate. The preparation method disclosed by the invention has the following advantages: the technology of directly generating propylene carbonate from urea and propylene glycol is simple, and industrial production is easy to realize; the preparation process has high reaction speed and high conversion rate and product yield; the adopted raw materials are cheap, the operation is simple and safe, and thus the preparation method has a remarkable value in industrial application; and the prepared propylene carbonate is nontoxic and biodegradable and has good usability and wide application range.

Description

technical field [0001] The invention relates to the preparation of propylene carbonate, in particular to the industrial synthesis of urea and propylene glycol to prepare propylene carbonate. Background technique [0002] Organic carbonate is a kind of chemical substance with low toxicity, little pollution and wide application. According to the structure, it can be divided into two types: cyclic carbonate and linear carbonate diester. Propylene carbonate (referred to as PC) is one of the most widely used cyclic carbonates. It is a high-boiling point and high-polarity organic solvent and fine chemical synthesis intermediate with excellent performance. Because PC has great affinity to carbon dioxide, hydrogen sulfide and some organic sulfur, but has little solubility to hydrogen, nitrogen, carbon monoxide, methane, oxygen, etc., it can be used to absorb carbon dioxide and hydrogen sulfide in natural gas and synthetic ammonia raw material gas gas. Propylene carbonate is a stab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36B01J23/10
CPCC07D317/36B01J23/002B01J23/10B01J2523/00B01J2523/22B01J2523/27B01J2523/3706B01J2523/3712
Inventor 何肖凤
Owner 何肖凤
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