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Carried siver catalyst for preparing anhydrous formaldehyde and its preparing process

An anhydrous formaldehyde, catalyst technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of no industrial application value, limited industrial application, no industrial prospect, etc. The effect of large-scale industrial production, insensitive reaction parameters, and easy production control

Inactive Publication Date: 2003-01-15
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The key technical part in this method of producing anhydrous formaldehyde by direct dehydrogenation of methanol is the catalyst used. Existing patent reports have a catalyst composed of copper, silver and silicon (Special Publication No. 41-11853), molten zinc , potassium, indium or aluminum or alloys of these metals (Japanese Patent Publication No. 47-19251), molten zinc containing carbon or alloys containing zinc (Japanese Patent Publication No. 48-97808), and catalysts composed of copper, zinc and selenium (Japanese Patent No. 48-97808) Kaizhao 52-215), etc., but these methods have various shortcomings such as short catalyst life and low reactivity, and have no industrial application value
In addition, using a catalyst composed of copper, zinc, and sulfur (Japanese Patent Application No. 51-1407) and a catalyst composed of copper and zinc to supply gaseous sulfides to carry out methanol dehydrogenation (Japanese Patent Application No. 51-76209), in the reaction Sulfur is mixed in the product or exhaust gas. This kind of catalyst that is not friendly to the environment has no industrial prospects
The use of a kind of sodium-containing catalyst makes the formaldehyde yield increase to 70% (Appl.Catal.2001(213) 203), but its industrial application is limited due to problems such as reaction temperature and catalyst life and regeneration

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: take by weighing 0.75g silver nitrate and be dissolved in 100mL water, add 5.56g 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 70°C, add 50mL of gelling agent ~ isopropanol, put it under reflux Condenser tube, after stirring for three hours, the sol solidified, stopped stirring, raised the temperature to 100°C, and evaporated the solvent 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 crush it to 40-60 meshes to obtain Ag-SiO with a silver content of 5%. 2 -MgO catalyst, denoted as 1# catalyst.

Embodiment 2

[0019] Embodiment 2: take by weighing 1.5g silver nitrate and be dissolved in 100mL water, add 5.56g Mg(NO 3 ) 2 ·6H 2 O, put it into a 250mL three-neck 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 75°C, add 50mL of gelling agent ~ ethanol, and install a reflux condenser After stirring for six hours, the sol was solidified, the stirring was stopped, 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 for 10 hours at 650°C, and grind to 40-60 meshes to obtain Ag-SiO with a silver content of 10%. 2 -MgO catalyst, denoted as 2# catalyst.

Embodiment 3

[0020] Embodiment 3: take by weighing 2.25g silver nitrate and be dissolved in 100mL water, add 5.56g Mg(NO 3 ) 2 ·6H 2 Dissolve O, use 50mL ethanol as the gelling agent, and add a few drops of 1mol / L HNO 3 Auxiliary gelation, the same as example 2, Ag-SiO with a silver content of 15% can be obtained 2 -MgO catalyst, denoted as 3# catalyst.

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PUM

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Abstract

A carried silver catalyst for preparing anhydrous formaldehyde by directly dehydrogenating methanol is prepared by sol-gel method, which includes such steps as mixing ethyl n-silicate with the solution containing soluble Mg salt, dropping it in aqueous solution of inorganosilver salt, generating colloid, aging, drying and calcining. Its advantages are high activity, long service life and low cost.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of a novel loaded silver catalyst used for directly dehydrogenating methanol to produce anhydrous formaldehyde. Background technique [0002] Formaldehyde is an important basic raw material in the chemical industry, and is widely used in the production of chemical products such as acetal resin, urea-formaldehyde resin, phenolic resin, pentaerythritol, and urotropine, as well as intermediate products of pharmaceuticals and pesticides. In these fields, most of the formaldehyde products used are anhydrous formaldehyde. To produce anhydrous formaldehyde, it is necessary to carry out rectification operation on commercial formaldehyde containing water. This not only needs to invest in considerable equipment and operating costs, but also because the formaldehyde aqueous solution has a negative deviation of a certain value relative to the ideal solution, res...

Claims

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Application Information

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IPC IPC(8): B01J23/50B01J23/66B01J37/03C07C47/055
Inventor 戴维林任丽萍曹勇范康年
Owner FUDAN UNIV
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