Method for preparation of methyl ethyl carbonate with co-precipitation catalyst

A kind of technology of methyl ethyl carbonate and dimethyl carbonate, applied in the field of co-precipitation catalyst for preparing methyl ethyl carbonate

Inactive Publication Date: 2017-12-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, the catalyzers mentioned above all have certain defects in the process of cataly

Method used

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  • Method for preparation of methyl ethyl carbonate with co-precipitation catalyst
  • Method for preparation of methyl ethyl carbonate with co-precipitation catalyst
  • Method for preparation of methyl ethyl carbonate with co-precipitation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Embodiment 1: the prepared Al with composite pore structure 2 o 3 -SiO 2 200 g of the carrier was placed in a muffle furnace and calcined at 500 °C for 4 hours to remove Al 2 o 3 -SiO 2 Adsorbed water; take 0.75 mol (238.5 g) Mg(NO 3 ) 2 ·6H 2 O, 0.20 mol (26.7 g) AlCl 3 , 0.02 mol (11.32 g) La 2 (SO 4 ) 3 Dissolve in 2000 mL deionized water to prepare a mixed solution of magnesium nitrate, aluminum chloride and lanthanum sulfate, and prepare 3 mol / L KOH and NaHCO 3 The mixed lye, the roasted Al 2 o 3 -SiO 2 Mix 200 g of the carrier with 2000 mL of deionized water, stir vigorously to make it evenly mixed with the water, and heat the solution containing the carrier to 70 °C in a water bath. Under vigorous stirring, in solution, drop the mixed solution of magnesium nitrate, aluminum chloride, lanthanum sulfate and lye simultaneously, control the rate of addition of magnesium nitrate, aluminum chloride and lanthanum sulfate mixed solution to be 3 ml / s, guaran...

Embodiment 2

[0079] Embodiment 2: get 0.75 mol (238.5 g) Mg(NO 3 ) 2 ·6H 2 O, 0.20 mol (26.7 g) AlCl 3 , 0.02 mol (11.32g) La 2 (SO 4 ) 3 , replace the precipitant with NaOH (1#), KOH (2#), NH 3 ·H 2 O(3#), KOH and NaHCO 3 The mixed alkali (4#), NaOH and NH 3 ·H 2 Mixed base of O (5#), KOH and NH 3 ·H 2 The mixed base of O (6#), the catalyst carrier is Al 2 o 3 -SiO 2 , the precipitation temperature is 70 ℃, the precipitation pH is 11, and the aging time is 20 h. Using the similar preparation method in Example 1, the MgO loading is 15 wt%, and the Al 2 o 3 The load is 5%, La 2 o 3 The load is 3%, the supported catalyst with different precipitants is 15% MgO-5%Al 2 o 3 -3% La 2 o 3 / Al 2 o 3 -SiO 2 .

[0080] In the fixed-bed reactor, 15% MgO-5% Al prepared by precipitation with different precipitants were loaded respectively 2 o 3 -3%La 2 o 3 / Al 2 o 3 -SiO 2 Catalyst 50 g each, using a constant flow pump to pump dimethyl carbonate and ethanol into the react...

Embodiment 3

[0084] Embodiment 3: get 0.75 mol (238.5 g) Mg(NO 3 ) 2 ·6H 2 O, 0.20 mol (26.7 g) AlCl 3 , 0.02 mol (11.32g) La 2 (SO 4 ) 3 , the precipitation temperature is 25°C, 40°C, 50°C, 60°C, 70°C, 80°C, 90°C, and the catalyst carrier is Al 2 o 3 -SiO 2 , the precipitants are KOH and NaHCO 3 The mixed alkali, the precipitation pH is 11, and the aging time is 20 h. Using the similar preparation method in Example 1, it can be prepared that the MgO loading is 15 wt%, and the Al 2 o 3 The load is 5%, La 2 o 3 Supported catalysts with 3% loading and different precipitation temperatures 15% MgO-5%Al 2 o 3 -3% La 2 o 3 / Al 2 o 3 -SiO 2 . In the fixed-bed reactor, 15% MgO-5% Al prepared with different precipitation temperatures were loaded respectively 2 o 3 -3% La 2 o 3 / Al 2 o 3 -SiO 2 Catalyst 50 g each, using a constant flow pump to pump dimethyl carbonate and ethanol into the reactor according to the molar ratio of 1:1, the space velocity is 30 h -1 , normal pr...

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Abstract

The invention relates to a preparation method of chemical raw materials, in particular to a method for preparation of methyl ethyl carbonate with a co-precipitation catalyst. The method adopts coprecipitation technique to carry one or more of the active components Al2O3, CaO, La2O3, Fe2O3, Mn2O3, Cs2O, MgO, BaO, SrO and K2O, wherein Y is one or more oxides of Si and Al, and Z is one or more oxides of Si, Al and Ti. The invention has the advantages that: macropore can significantly improve the mass transfer effect, and micropore can significantly increase the specific surface area of the carrier and improve the dispersity of the active center. Magnesium nitrate, aluminum chloride and lanthanum sulfate are adopted as the active components and are mixed with a precursor to obtain the 15%MgO-5%Al2O3-3%La2O3/Al2O3-SiO2 catalyst, which can be applied to dimethyl carbonate and ethanol ester exchange fixed bed continuous reaction. The catalyst active center metal oxide prepared by precipitation method has smaller crystal grains, higher dispersity and surface area, and the prepared catalyst has catalytic effect superior to the catalyst prepared by impregnation method.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing ethyl methyl carbonate with a co-precipitation catalyst. Background technique [0002] Methyl Ethyl Carbonate (MEC for short), molecular formula: C 4 h 8 o 3 , colorless transparent liquid, density 1.01 g / mL, melting point -55 ° C, boiling point 107 ° C, flammable, can be mixed with organic solvents such as alcohols, ketones, esters in any proportion, is an excellent solvent, ethyl methyl carbonate is due to Its molecular structure has methyl and ethyl groups at the same time, so it has the characteristics of dimethyl carbonate and diethyl carbonate, and can be used as some special organic synthesis reagents, and it is also a solvent for special fragrances. Due to the low viscosity, large dielectric constant and strong solubility of lithium salts, ethyl methyl carbonate is an excellent lithium-ion battery electrolyte solvent, which can imp...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96B01J23/10B01J29/08B01J35/10
CPCB01J23/002B01J23/10B01J29/088B01J35/10B01J35/1004B01J2229/18B01J2523/00C07C68/06C07C69/96B01J2523/22B01J2523/31B01J2523/3706B01J2523/41Y02P20/50
Inventor 张志刚陈飞姚杰石磊王岩张冬喜王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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