Method using carbon dioxide and 1, 2-propylene glycol to synthesize propylene carbonate

A technology of propylene carbonate and carbon dioxide, which is applied in the direction of organic chemistry, can solve the problems of low yield of propylene carbonate and harsh reaction conditions, etc., and achieve the effect of simple reaction system, easy handling, and promotion of equilibrium shift to the right

Active Publication Date: 2014-07-16
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The synthesis of propylene carbonate from carbon dioxide and 1,2-propanediol is limited by thermodynamics and the reaction conditions are relatively harsh. The yield of propylene carbonate reported so far is generally low (< 28.0%)

Method used

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  • Method using carbon dioxide and 1, 2-propylene glycol to synthesize propylene carbonate
  • Method using carbon dioxide and 1, 2-propylene glycol to synthesize propylene carbonate
  • Method using carbon dioxide and 1, 2-propylene glycol to synthesize propylene carbonate

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Embodiment 1

[0034] A method for synthesizing propylene carbonate by carbon dioxide and 1,2-propylene glycol, the steps are as follows:

[0035] 1) Add 0.3804 g of 1,2-propanediol (5 mmol), 0.0814 g of cesium carbonate (0.25 mmol), and 0.1742 g of propylene oxide (3 mmol) into the glass sleeve of a 25 mL autoclave. into 3 MPa carbon dioxide, at 100 o Stir at C for 20 min;

[0036] 2) After the temperature is stabilized, adjust the carbon dioxide pressure to 10 MPa, at 100 o Reaction at C for 12 h;

[0037] 3) After the reaction is over, the reactor is naturally cooled to 22 o C, then placed in an ice-water bath, cooled to 0 o C; Slowly release carbon dioxide to produce propylene carbonate.

[0038] After extraction with 10 mL of ether, an internal standard was added, and a small amount of sample was taken for gas chromatography analysis. The internal standard yield of propylene carbonate was 26.7%.

Embodiment 2

[0040] A method for synthesizing propylene carbonate by carbon dioxide and 1,2-propanediol, used reactant 1,2-propanediol and catalyst and reaction conditions, preparation steps are the same as in Example 1, except that 0.1322 g of ethylene oxide is used (3 mmol) to replace the dehydrating agent propylene oxide. After extraction with 10 mL of ether, an internal standard was added, and a small amount of sample was taken for gas chromatographic analysis. The internal standard yield of propylene carbonate was 23.9%, the molar weight of ethylene carbonate was 0.12 mmol, and the yield relative to ethylene oxide was 4.0 %.

Embodiment 3

[0041] Embodiment 3: a group of tests

[0042] A method for synthesizing propylene carbonate from carbon dioxide and 1,2-propanediol, the reactant 1,2-propanediol and dehydrating agent and reaction conditions, preparation steps are the same as in Example 1, except that different basic catalysts are used to replace cesium carbonate. After extraction with 10 mL of ether, an internal standard was added, and a small amount of sample was taken for gas chromatography analysis. The internal standard yield of propylene carbonate is shown in Table 1.

[0043] Table 1 Synthesis of propylene carbonate catalyzed by different basic catalysts

[0044] serial number catalyst Dehydrating agent Yield / % 1 Cs 2 CO 3 PO 26.7 2 K 2 CO 3 PO 12.1 3 Na 2 CO 3 PO 3.4 4 CaO PO 4.1 5 MgO PO 1.2 6 Na 2 o PO 3.5 7 MgCO 3 PO 0.8 8 NaOAc PO 2.3 9 Na 3 PO 4 PO 0.6 10 NaHCO 3 PO 1.8 11...

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Abstract

The invention relates to a method using carbon dioxide and 1, 2-propylene glycol to synthesize propylene carbonate. The method comprises the following steps: 1) adding 1, 2-propylene glycol, a dehydrating agent and a basic catalyst into a glass sleeve of an autoclave, inflating 0.1-3MPa of carbon dioxide, and stirring for 20 minutes at 60-220 DEG C; 2) after the temperature is stable, adjusting the pressure of carbon dioxide to 0.5-20MPa, and reacting for 2-24 hours at 60-220 DEG C; 3) after a reaction kettle is naturally cooled to 18-25 DEG C, putting the reaction kettle in an ice-water bath to be cooled to 0 DEG C, and finally obtaining the propylene carbonate; and also, adding polyethylene glycol-800 in the step 1) at the same time. The method has the advantages that the method utilizes epoxypropane as the dehydrating agent to greatly increase the yield of the propylene carbonate, the epoxypropane is converted into a raw material, namely 1, 2-propylene glycol and can be recycled after reaction, and no by-product is generated; and the preparation process is simple and is easily implemented.

Description

technical field [0001] The invention relates to a method for synthesizing propylene carbonate, in particular to a method for synthesizing propylene carbonate from carbon dioxide and 1,2-propylene glycol. Background technique [0002] With the development of human society and economy, the consumption of energy is increasing day by day, and the emission of carbon dioxide into the atmosphere is also increasing, which brings adverse effects on the environment and human life. At the same time, industrial development will inevitably lead to increasing scarcity and shortage of energy and basic chemical resources. Carbon dioxide is not only the main greenhouse gas, but also the most widely distributed and abundant carbon resource on the earth. In recent years, with the deepening of research on carbon dioxide, the use of carbon dioxide as a renewable carbon resource for the synthesis of high value-added chemical products has gradually become a research hotspot. Whether from the pe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36
Inventor 刁振凤何良年於兵张洪学
Owner NANKAI UNIV
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