Catalyst and method preparing dimethyl carbonate by using catalyst

The technology of a catalyst and a supported catalyst, which is applied in the preparation of processes and catalysts, and the preparation of various metal salt-supported catalysts, can solve the problem that the yield of dimethyl carbonate is less than 2%, the process is complicated, the operation is difficult, etc. problem, to achieve the effect of flexible process, simple preparation method and good stability

Inactive Publication Date: 2016-01-20
SICHUAN LUTIANHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under the action of alkali metal compound catalyst, the yield of dimethyl carbonate is less than 2%
JP10-109960 uses a series of alkali metal monoesters and compound catalysts. Among them, the yield of dimethyl carbonate under the action of LiH can reach up to 36.4%, but this reaction needs to be carried out in a two-end reactor equipped with a distillation column. complex, difficult to operate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 9.696g of ferric nitrate and 28.559g of zinc nitrate in 200mL of distilled water to prepare a metal salt solution containing zinc and iron. Slowly add the solution to an equal volume of silica gel. After the addition, let it stand for 24 hours. It is dried in a drying oven at about ℃, and then calcined in a high-temperature muffle furnace at 600°C-700°C for 4 hours to prepare a zinc-iron composite supported catalyst.

[0031] Add 9 g of urea, 46 g of 1,2-propanediol, and 5.5 g of the above-mentioned catalyst into a 250 mL four-necked flask. The four-necked flask is equipped with a thermometer, a reflux condenser, a stirrer and a nitrogen inlet. Heating to reflux for reaction, the reaction temperature is controlled at 170° C. to 180° C., and the reaction is carried out for 3.5 hours. The composition of the reaction product is analyzed and detected by gas chromatography. The yield of propylene carbonate was 93.5%.

[0032] Choose the above-mentioned zinc, iron c...

Embodiment 2

[0034]Dissolve 7.77g of magnesium nitrate and 36.00g of zinc nitrate in 200mL of distilled water to prepare a metal salt solution containing zinc and magnesium. Slowly add the solution dropwise to an equal volume of silica gel. It is dried in a drying oven at about 600°C, and then calcined in a high-temperature muffle furnace at 600°C-700°C for 4 hours to prepare a zinc-magnesium composite supported catalyst.

[0035] Add 9 g of urea, 46 g of 1,2-propanediol, and 5.5 g of the above-mentioned catalyst into a 250 mL four-necked flask. The four-necked flask is equipped with a thermometer, a reflux condenser, a stirrer and a nitrogen inlet. Heating to reflux for reaction, the reaction temperature is controlled at 170° C. to 180° C., and the reaction is carried out for 3.5 hours. The composition of the reaction product is analyzed and detected by gas chromatography. The yield of propylene carbonate was 93%.

[0036] Select the above-mentioned compound zinc and magnesium composite ...

Embodiment 3

[0038] Dissolve 25.64g of magnesium nitrate and 37.513g of aluminum nitrate in 200mL of distilled water to prepare a metal salt solution containing magnesium and aluminum. Slowly add the solution dropwise to an equal volume of silica gel. It is dried in a drying oven at about ℃, and then calcined in a high-temperature muffle furnace at 600°C-700°C for 4 hours to prepare a magnesium-aluminum composite supported catalyst.

[0039] Add 9 g of urea, 46 g of 1,2-propanediol, and 5.5 g of the above-mentioned catalyst into a 250 mL four-necked flask. The four-necked flask is equipped with a thermometer, a reflux condenser, a stirrer and a nitrogen inlet. Heating to reflux for reaction, the reaction temperature is controlled at 170° C. to 180° C., and the reaction is carried out for 3.5 hours. The composition of the reaction product is analyzed and detected by gas chromatography. The yield of propylene carbonate was 92.5%.

[0040] Choose above-mentioned magnesium, aluminum composite...

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PUM

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Abstract

The invention discloses a catalyst and a method preparing dimethyl carbonate by using the catalyst. The method comprises two steps: step 1, with urea and aliphatic dihydric alcohol as raw materials, reacting urea with aliphatic dihydric alcohol under the action of the catalyst to synthesize ethylene carbonate or propylene carbonate, wherein reaction conditions are that reaction temperature is 100 to 200 DEG C and 0.5 to 5 mL of nitrogen is introduced into a reaction system per minute; and step 2, subjecting ethylene carbonate or propylene carbonate and methanol to ester interchange so as to synthesize dimethyl carbonate, wherein a reaction condition is that reaction temperature is 60 to 170 DEG C, and the catalyst is a supported catalyst prepared by preparing a solution with a certain concentration from a metal salt or metal oxide and then impregnating a same-volume carrier with the solution. The technical characteristics of the invention are that reaction conditions are mild; reaction is carried out at normal pressure; and the catalyst is easy to separate and recycle, can be repeatedly used and poses no corrosion to equipment and no environmental pollution.

Description

technical field [0001] The invention relates to a process for synthesizing dimethyl carbonate by urea alcoholysis and a preparation method of the catalyst thereof, in particular to a process for synthesizing dimethyl carbonate by urea alcoholysis using aliphatic dihydric alcohol as a circulating agent and a preparation method for the catalyst thereof . In particular, it relates to a preparation method of various metal salt-type material-loaded catalysts used in the synthesis of dimethyl carbonate by urea alcoholysis. technical background [0002] Dimethyl carbonate (DMC) has the characteristics of non-toxicity, fast evaporation, and good compatibility with other solvents. Western Europe has listed it as a non-toxic chemical, and vigorously develops its application as a solvent, such as a solvent for paints and coatings, a solvent for high-energy batteries, an adhesive for glue, and a solvent for medical production. It can also be used as a spray . It is used as raw materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/06B01J21/14B01J23/02C07C69/96C07C68/06
CPCY02P20/584
Inventor 李勇罗光碧蒋弟勇汪国瑜
Owner SICHUAN LUTIANHUA
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