Loading silver catalyst for preparing anhydrous formaldehyde by direct dehydrogenation of methanol and its manufacturing method

An anhydrous formaldehyde and silver catalyst technology, applied in the chemical industry, can solve the problems of low selectivity of the catalyst to formaldehyde, no industrial application value, industrial application limitation, etc., and achieves convenient large-scale industrial production, insensitive reaction parameters, and easy production. control effect

Inactive Publication Date: 2004-10-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing patent reports have catalysts composed of copper, silver, and silicon (Special Publication No. 41-11853), molten zinc, potassium, indium or aluminum or alloys of these metals (Special Publication No. 47-19251), carbon-containing molten Zinc or zinc-containing alloys (Japanese Patent Opening No. 48-97808) and catalysts composed of copper, zinc, and selenium (Japanese Patent No. 52-215), etc., but most of the catalysts obtained by these methods have short life, low reactivity, and no industrial Value
And the catalyzer (patent open clear 51-1407) that is made up of copper, zinc, sulfur and the catalyzer that is made up of copper, zinc supply gaseous sulfide and carry out methan...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: take by weighing 0.014g silver nitrate and be dissolved in 100ml water, add 0.56g Mg(NO 3 ) 2 ·6H 2 O, put it into a 250ml three-necked bottle after dissolving, add 33ml tetraethyl orthosilicate drop by drop, and at the same time vigorously electromagnetically stir, keep the oil bath temperature at 50°C, add 50ml of gelling agent ~ isopropanol, put it under reflux Condenser, after stirring for one hour, slowly add 0.3mol / l Al(NO 3 ) 3 The solution was 15ml, and the stirring was stopped after the sol solidified, the temperature was raised to 100°C, and the solvent was evaporated for 12 hours. Transfer to a crucible, bake with an infrared lamp for 24 hours, then transfer to a muffle furnace and bake at 700°C for 6 hours, and pulverize to 40-60 meshes to obtain 1#Ag-SiO 2 -MgO-Al 2 o 3 catalyst.

Embodiment 2

[0019] Embodiment 2: take by weighing 0.83g silver nitrate and be dissolved in 100ml water, add 2.83g Mg(NO 3 ) 2 ·6H 2 O, use 50ml ethanol as the gelling agent instead, and add a few drops of 1mol / l HNO 3 Auxiliary gelation, change the oil bath temperature to 70°C, add 0.3mol / l Al(NO 3 ) 3 Solution 25ml, the calcination temperature is raised to 1000 ° C, the rest is the same as Example 1, and 2#Ag-SiO can be obtained 2 -MgO-Al 2 o 3 catalyst.

Embodiment 3

[0020] Embodiment 3: take by weighing 1.86g silver nitrate and be dissolved in 100ml water, add 11.30g Mg(NO 3 ) 2 ·6H 2 O, put it into a 250ml three-necked bottle after dissolving, add 33ml tetraethyl orthosilicate at one time, and at the same time vigorously electromagnetically stir to maintain the temperature of the oil bath at 100°C, and add 50ml of gelling agent ~ isopropanol, put it under reflux Condenser, after stirring for three hours, slowly add 0.3mol / l Al(NO 3 ) 3 The solution was 30ml, and the stirring was stopped after the sol solidified, the temperature was raised to 90°C, and the solvent was evaporated for 24 hours. Transfer to a crucible, bake with an infrared lamp for 24 hours, then transfer to a muffle furnace and bake at 1300°C for 10 hours, and pulverize to 40-60 meshes to obtain 3#Ag-SiO 2 -MgO-Al 2 o 3 catalyst.

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PUM

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Abstract

A Ag-carried catalyst for preparing the anhyrous formaldehyde by derect dehydrogenation of methanol is prepared by sol-gel method, which includes such steps as mixing ethyl silicate with the solution of soluble Mg salt and Al salt in water or alcohol, dropping their mixture in the aqueous solution of inorganic Ag salt, gelatinizing while adding the solution of soluble Al salt for increasing the activity and selectivity of product, ageing, drying and calcining. Its advantages are high transform rate of methanol and selectivity of formaldehyde (up to 100%) and low cost.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a silver-loaded catalyst used for direct dehydrogenation of methanol to prepare anhydrous formaldehyde and a preparation method thereof. Background technique [0002] As a very important basic chemical raw material, formaldehyde is widely used in the production of chemical products such as acetal resin, urea-formaldehyde resin and phenolic resin, pentaerythritol and hexamethamine. Formaldehyde is usually produced by methanol oxidative dehydrogenation method, which can be obtained of formaldehyde solution. With the development of modern industry, the demand for anhydrous formaldehyde is increasing day by day. Basically, anhydrous formaldehyde is prepared by removing water from commercial formaldehyde through rectification and extraction. This process consumes a lot of energy and is not economical. At present, the most researched production scheme is the prod...

Claims

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Application Information

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IPC IPC(8): B01J23/66C07C45/29C07C47/055
Inventor 戴维林任丽萍曹勇范康年
Owner FUDAN UNIV
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