Method for preparing catalyst, catalyst prepared by using method, and method for preparing glycerol monomethyl ether by using catalyst

A technology of catalyst and monomethyl ether, which is applied in the field of catalyst preparation, can solve the problems of rapid catalyst deactivation, poor temperature resistance, and easy loss, and achieve the effects of reducing tar selectivity, good temperature resistance, and convenient operation

Active Publication Date: 2018-11-23
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst reported in the patent has the problems of poor temperature resistance and easy loss, and the catalyst deactivates quickly. Therefore, it is necessary to prepare a catalyst with stable performance and good activity for the production of glycerol monomethyl ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Weigh 100g of ethyl orthosilicate, dissolve it in 50ml of ethanol, and make solution A; weigh 2g of cesium carbonate, dissolve it in 100ml of deionized water, and get saline solution B. Under the condition of stirring, slowly add A to B dropwise, after the dropwise addition, continue to stir at 70°C for 30 minutes, add ammonia water with a solubility of 28%, and adjust the pH value to 8. Continue to stir to increase the temperature to 90°C, and age for 3 hours under stirring. The slurry was spray-dried to obtain powder C.

[0059] Weigh 30g of silica sol with a solid content of 40%, fully mix it with powder C to form a wet mass, prepare strips with a diameter of 3mm by extrusion, dry at 60°C, and bake at 300°C for 6h to obtain carrier D.

[0060] Weigh 3.78 g of tetraethyl orthosilicate, add ethanol to configure a solution with a total volume of 40 ml. The solution was added dropwise to the carrier D, placed in a reaction kettle for overnight impregnation, and continu...

Embodiment 2

[0064] Weigh 100g of tetraethyl orthosilicate, dissolve it in 50ml of ethanol, and make solution A; weigh 5g of cesium carbonate, dissolve it in 100ml of deionized water, and obtain saline solution B. Under the condition of stirring, slowly add A to B dropwise, after the dropwise addition, continue to stir at 70°C for 30 minutes, add ammonia water with a solubility of 28%, and adjust the pH value to 8. Continue to stir to increase the temperature to 90°C, and age for 3 hours under stirring. The slurry was spray-dried to obtain powder C.

[0065] Weigh 40g of silica sol with a solid content of 30%, fully mix it with powder C to form a wet mass, prepare strips with a diameter of 3mm by extrusion, dry at 60°C, and bake at 300°C for 6h to obtain carrier D.

[0066] Weigh 8.16 g of tetraethyl orthosilicate, add ethanol to configure a solution with a total volume of 40 ml. The solution was added dropwise to the carrier D, placed in the reaction kettle for overnight impregnation, a...

Embodiment 3

[0070] Catalyst preparation method is with example one, and wherein cesium carbonate is 7.5g.

[0071] Take the above catalyst and crush it, screen 5g of 20-40 mesh catalyst particles, fill it into a fixed-bed reactor with an inner diameter of 12mm, replace it with nitrogen three times, adjust the pressure to 0.5MPa, and make the system airtight for 3 hours. After the tightness is passed, the temperature is raised to 180°C. Use the metering pump to feed the configured raw materials to start the etherification reaction, and the feed rate is 0.5h -1 . Wherein: raw material is the mixed solution of methanol (97wt%) and glycerol (90wt%) molar ratio 3: 1, gas chromatography analysis, glycerol conversion rate 25%, glycerol monomethyl ether selectivity 100%.

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Abstract

The invention relates to a method for preparing a catalyst, the catalyst prepared by using the method, and a method for preparing glycerol monomethyl ether by using the catalyst. The method for preparing the catalyst comprises the following steps: (1) separately preparing an ethanol solution of tetraalkyl silicate and an aqueous solution of Cs salt; (2) mixing the two solutions, stirring and adjusting the pH value of the mixed solution to be alkaline, and aging; (3) spray-drying the aged material to obtain silica gel powder; (4) thoroughly mixing silica sol with the silica gel powder, extruding and molding, drying and calcining to obtain a silicon oxide carrier; (5) impregnating the silicon oxide carrier with the ethanol solution of the tetraalkyl silicate, and then treating with low pressure steam to obtain a catalyst carrier; (6) impregnating the catalyst carrier with an aqueous solution of phosphotungstic acid, drying and calcining to obtain the supported catalyst. The catalyst is good in temperature resistance, can effectively improve glycerol conversion rate and glycerol monomethyl ether selectivity, can continuously react, and is convenient to operate and high in stability.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, a catalyst prepared by the method and a method for preparing glycerol monomethyl ether by utilizing glycerin and methanol using the catalyst. Background technique [0002] As biodiesel has received more and more attention and applications, the related facilities used to manufacture biodiesel have also been greatly expanded worldwide, and with the increase in the amount of biodiesel, the amount of its by-product glycerol has also increased. Leading to excess production, prices fell sharply. Therefore, the use of glycerol to produce other chemicals and chemical additives has important practical significance. [0003] Unsaturated polyester resin is a kind of thermosetting resin, which can be cured into an insoluble and infusible high molecular network polymer under the action of heat or initiator. However, the mechanical strength of this polymer is very low, and it cannot meet the requirements ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188C07C41/09C07C43/13
CPCB01J27/188B01J35/008C07C41/09C07C43/13
Inventor 张英伟秦少鹏刘全遥王耀红潘小君
Owner BEIJING RISUN TECH CO LTD
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