Method for preparing diethoxymethane by solid superacid catalysis

A technology of diethoxymethane and solid superacid, which is applied in chemical instruments and methods, preparation of ethers, and preparation of ethers by exchanging organic parts, etc., can solve problems such as poor selectivity, high equipment cost, and poor catalyst stability, and achieve industrialization Production, good recyclability, good stability effect

Inactive Publication Date: 2021-02-02
艾延
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using organic acid as a catalyst, using kettle reaction to rectify diethoxymethane, the process is simple, easy to operate, and the phenomenon is intuitive, but there are low conversion rate and poor selectivity in the preparation process, and easy to produce monoethoxymethane. The reaction process The product generated in the process cannot be removed in time, and secondary reactions are prone to occur, which brings difficulty to refining and affects product quality and yield.
[0008] Chinese patent CN105622365A discloses a method for preparing diethoxymethane with a supported heteropolyacid catalyst, but the catalyst synthesis method is loaded, the amount of catalyst is large, and the stability of the catalyst is poor, which is not conducive to industrial production
[0009] Chinese patent CN108047006A discloses a method for the preparation of diethoxymethane by solid superacid catalysis, wherein tube bundle reactors and rectification devices are used, the equipment cost is high, the operation is complicated, and it is not conducive to industrial production

Method used

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  • Method for preparing diethoxymethane by solid superacid catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] S1, the active substance of the solid superacid catalyst is H2SO4, and the carrier is SnO 2 -TiO 2 .

[0030] Described H2SO4 / SnO2-TiO solid superacid catalyst preparation method is as follows:

[0031] 1) Evenly mix 200g of tin hydroxide and 250gmol of titanium dioxide powder, 130g of porogen, 35g of binder and 103g of scallop powder, extrude, put into a muffle furnace and bake at 800°C for 5 hours to obtain SnO2- TiO2;

[0032] 2) Take a 0.8mol / L sulfuric acid solution and impregnate it into the channel prepared in step 1) three times in an ultrasonic environment, and the ultrasonic immersion time is 2 hours;

[0033] 3) After the impregnated catalyst precursor was dried in an oven at 100°C for 3 hours, it was put into a muffle furnace and baked at 500°C for 2 hours to prepare a H2SO4 / SnO2-TiO2 solid superacid catalyst.

[0034] S2, using ethanol and dimethoxymethane as raw materials, using the solid superacid prepared in step S1 as a catalyst, first put 1mol of d...

Embodiment 2

[0036] S1, the active substance of the solid superacid catalyst is H2SO4, and the carrier is SnO 2 -TiO 2 .

[0037]Described H2SO4 / SnO2-TiO solid superacid catalyst preparation method is as follows:

[0038] 1) Evenly mix 200g of tin hydroxide and 250gmol of titanium dioxide powder, 130g of porogen, 35g of binder and 103g of scallop powder, extrude, put into a muffle furnace and bake at 800°C for 5 hours to obtain SnO2- TiO2;

[0039] 2) Take a 0.3mol / L sulfuric acid solution and impregnate it into the channel prepared in step 1) twice in an ultrasonic environment, and the ultrasonic immersion time for each time is 5 hours;

[0040] 3) After the impregnated catalyst precursor was dried in an oven at 100°C for 5 hours, it was put into a muffle furnace and baked at 500°C for 3 hours to prepare a H2SO4 / SnO2-TiO2 solid superacid catalyst.

[0041] S2, using ethanol and dimethoxymethane as raw materials, using the solid superacid prepared in step S1 as a catalyst, first put 1m...

Embodiment 3

[0043] S1, the active substance of the solid superacid catalyst is H2SO4, and the carrier is SnO 2 -TiO 2 .

[0044] Described H2SO4 / SnO2-TiO solid superacid catalyst preparation method is as follows:

[0045] 1) Evenly mix 200g of tin hydroxide and 250gmol of titanium dioxide powder, 130g of porogen, 35g of binder and 103g of scallop powder, extrude, put into a muffle furnace and bake at 800°C for 5 hours to obtain SnO2- TiO2;

[0046] 2) Take a 0.3 mol / L sulfuric acid solution and impregnate it three times into the pores prepared in step 1) in an ultrasonic environment, and the ultrasonic immersion time is 4 hours;

[0047] 3) After the impregnated catalyst precursor was dried in an oven at 100°C for 3 hours, it was put into a muffle furnace and baked at 500°C for 2 hours to prepare a H2SO4 / SnO2-TiO2 solid superacid catalyst.

[0048] S2, using ethanol and dimethoxymethane as raw materials, using the solid superacid prepared in step S1 as a catalyst, first put 1mol of di...

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Abstract

The invention relates to a method for preparing diethoxymethane by solid superacid catalysis. The method overcomes the defects of low selectivity of diethoxymethane products and low yield of byproductmethoxyethoxymethane in the prior art through sectional feeding and heating operation and reaction modes, and the selectivity of the products is up to 93% or above, and the raw material conversion rate of dimethoxymethane is 94% or above.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for preparing diethoxymethane by catalyzing a solid superacid. Background technique [0002] Although diethoxymethane (DEM) has only been commercialized in recent years, it has attracted the attention of researchers due to its unique properties. Its typical properties are: suitable operating temperature range; low viscosity, easy to operate and handle; DEM has low solubility in water and water in DEM; it forms a binary azeotrope with water and ethanol, which is beneficial to the purification of the product; and Water is immiscible, easy to separate from water, and has good process economy; it has good stability and is stable under strong alkali and weak acid conditions such as hydroxide, sodium hydride, and Grignard reagent, and is not easy to form peroxide. [0003] These characteristics make DEM have important and extensive application value in organic synthe...

Claims

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Application Information

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IPC IPC(8): C07C41/14C07C43/10B01J27/053
CPCB01J27/053C07C41/14C07C43/10
Inventor 艾延
Owner 艾延
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