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Method for synthesizing dimethyl carbonate by using urea and methanol and adopting heterogeneous catalyst

A heterogeneous catalyst, dimethyl carbonate technology, applied in the preparation of carbonate/haloformate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of harsh reaction conditions, high price of raw gas, and product Solve problems such as difficult separation, and achieve the effect of safe reaction process, low raw material cost and simple process

Inactive Publication Date: 2003-07-09
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst used in the methanol oxidative carbonylation method uses CuCl as the main active component, which is highly corrosive to equipment, has a short catalyst life, and has the characteristics of high feed gas price and CO toxicity.
The problem with the transesterification method is that the main research at home and abroad is mostly focused on the homogeneous batch reaction, the catalyst life is short, the reaction conditions are harsh, and various organic solvents need to be added during the reaction process, which brings great difficulties to the subsequent separation of the product. difficulties, virtually increased equipment investment costs and production energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Choose calcium carbonate as the precursor salt, weigh a certain amount of calcium carbonate in a high-temperature furnace, and calcinate the catalyst at 900°C, 0.1MPa, and air atmosphere for 2 hours to obtain a solid calcium oxide catalyst. Weigh 15 grams of urea, measure 20 milliliters of methanol, the molar ratio of methanol to urea is 2:1, put them into an autoclave, add 2 grams of CaO catalyst, rapidly heat from room temperature to 140 °C under magnetic stirring, keep for 3 hours, and then Heating to 190°C, constant temperature reaction for 5 hours, after the temperature dropped to room temperature, the reaction product was analyzed by gas chromatography, the results are listed in Table 1.

Embodiment 2

[0021] Choose calcium carbonate as the precursor salt, weigh a certain amount of calcium carbonate in a high-temperature furnace, and calcinate the catalyst at 900°C, 0.1MPa, and nitrogen atmosphere for 2 hours to obtain a solid calcium oxide catalyst. Weigh 15 grams of urea, measure 40 milliliters of methanol, the molar ratio of methanol to urea is 4:1, put them into an autoclave, and add 3 grams of CaO catalyst, rapidly heat from room temperature to 140 ° C under magnetic stirring, keep for 3 hours, and then Heating to 190°C, constant temperature reaction for 12 hours, after the temperature dropped to room temperature, the reaction product was analyzed by gas chromatography, the results are listed in Table 1.

Embodiment 3

[0023] Calcium carbonate was selected as the precursor salt, a certain amount of calcium carbonate was weighed in a high-temperature furnace, and the catalyst was calcined at 900° C., 0.1 MPa, and nitrogen atmosphere for 6 hours to obtain a solid calcium oxide catalyst. Weigh 7.5 grams of urea, measure 30 milliliters of methanol, the molar ratio of methanol to urea is about 8:1, put it into an autoclave, and add 4 grams of CaO catalyst, rapidly heat from room temperature to 150 ° C under magnetic stirring, and keep for 2 hours, Then heated to 220° C. and reacted at constant temperature for 6 hours. After the temperature dropped to room temperature, the reaction product was analyzed by gas chromatography. The results are listed in Table 1.

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Abstract

The method for synthesizing dimethyl carbonate by using urea and methanol and adopting heterogeneous catalyst includes the following steps: under the condition of 600-1300 deg.c 10X10 to the power 5-1X10 to the power 5 pa and air or oxygen gas atmosphere calcining carbonate or hydroxide of alkali metal and alkaline earth metal for 1-10 hr. to obtain catalyst, adding urea and methanol into high-pressure reaction still, and adding catalyst, heating to 120-180 deg.c under the condition of magnetic stirring, low-temp. resistion time is 2 hr-10 hr. more heating to 180-240 deg.C, high-temp. reaction time 2 hr-20 hr, cooling to room temp. and making separation so as to obtain the invented roduct.

Description

Technical field: [0001] The invention belongs to a method for synthesizing dimethyl carbonate, in particular to a method for synthesizing dimethyl carbonate by urea and methanol using a heterogeneous catalyst. Background technique: [0002] Dimethyl carbonate (DMC), as a low-toxicity environment-friendly chemical product, has been widely used in the fields of preparing high-performance resins, solvents, dye intermediates, pharmaceutical additives, food preservatives, lubricating oil additives, etc. applications have drawn increasing attention. In recent years, a large number of patents on the production and application of dimethyl carbonate have been published at home and abroad, and a certain scale of industrial production has been achieved. At present, the industrial production methods of dimethyl carbonate mainly include phosgene method, methanol oxidative carbonylation method and transesterification method. Among them, the phosgene method has been gradually eliminated ...

Claims

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Application Information

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IPC IPC(8): C07C68/00C07C69/96
Inventor 孙予罕魏伟杨金海魏彤王谋华陈兰光褚衍来吴炎增
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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