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Electrochemical synthesis method for preparing 1, 1, 4, 4-tetramethoxy-2-butene

A technology of tetramethoxy and synthetic method, which is applied in the field of electrochemical synthesis for the preparation of 1,1,4,4-tetramethoxy-2-butene, which can solve the problems of excessive three wastes, long process, and equipment corrosion , to achieve the effects of process simplification, high molecular utilization and short synthetic route

Active Publication Date: 2022-03-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above methods all face the problems of long process, different degrees of equipment corrosion, difficulty in product recycling and more three wastes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take a piece of isostatic graphite catalytic electrode (30mm*20mm*1mm) and add anhydrous methanol to ultrasonic for 10 minutes, take it out and put it in deionized water to continue ultrasonic for 10 minutes, then put it in an oven to dry for later use.

[0034] Weigh 3g of tin nitrate, 1g of zirconium nitrate, 0.5g of sodium citrate, and 1g of sodium hydrogenphosphite and add them into deionized water to prepare 200g of electrodeposition electrolyte. The isostatic graphite is used as the anode, and the platinum electrode is used as the cathode, and the reaction is performed under a constant voltage of 3V for 30min. The graphite electrode was taken out, washed three times with deionized water, put into a muffle furnace, and calcined at 450° C. for 2 hours to obtain a catalytic anode.

[0035] Select the prepared catalytic electrode as the anode, foam copper as the cathode, weigh 24g of methanol, 24g of furan, and 12g of sodium bromide, mix them into an electrolyte, and ...

Embodiment 2

[0037] Take a piece of isostatic graphite electrode (30mm*20mm*1mm) and add anhydrous methanol to ultrasonic for 10 minutes, take it out and put it in deionized water to continue ultrasonic for 10 minutes, then put it in an oven to dry for later use.

[0038] Weigh 5g of iridium nitrate, 5g of cerium nitrate, 1.5g of sodium citrate, and 1.5g of sodium hydrogenphosphite and add them into deionized water to prepare 200g of electrodeposition electrolyte. The isostatic graphite is used as the anode, and the platinum electrode is used as the cathode, and the reaction is performed under a constant voltage of 3V for 30min. The graphite electrode was taken out, washed three times with deionized water, put into a muffle furnace, and calcined at 450° C. for 2 hours to obtain a catalytic anode.

[0039] Select the prepared catalytic electrode as the anode, foam nickel as the cathode, weigh 100g of methanol, 24g of furan, and 6g of potassium bromide, mix them into an electrolyte, and pour...

Embodiment 3

[0041] Take a piece of isostatic graphite electrode (30mm*20mm*1mm) and add anhydrous methanol to ultrasonic for 10 minutes, take it out and put it in deionized water to continue ultrasonic for 10 minutes, then put it in an oven to dry for later use.

[0042] Weigh 15g of lead nitrate, 5g of copper nitrate, 3.5g of sodium citrate, and 3.5g of sodium hydrogenphosphite and add them into deionized water to prepare 200g of electrodeposition electrolyte. The isostatic graphite is used as the anode, and the platinum electrode is used as the cathode, and the reaction is performed under a constant voltage of 3V for 30min. The graphite electrode was taken out, washed three times with deionized water, put into a muffle furnace, and calcined at 450° C. for 2 hours to obtain a catalytic anode.

[0043]Select the prepared catalytic electrode as the anode, graphite as the cathode, weigh 150g methanol, 24g furan, 2g tetramethyl sodium bromide, mix and make electrolyte, pour it into a single-...

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PUM

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Abstract

The invention relates to an electrochemical synthesis method for preparing 1, 1, 4, 4-tetramethoxy-2-butene, in particular to a method for synthesizing 1, 1, 4, 4-tetramethoxy-2-butene by taking furan as a raw material through a one-step method. The method comprises the following steps: (1) mixing furan, methanol and bromine salt to prepare an electrolyte; and (2) the electrolyte is introduced into a diaphragm-free single-chamber electrolytic cell for an electrolytic reaction, and the 1, 1, 4, 4-tetramethoxy-2-butene is prepared. The process for preparing the 1, 1, 4, 4-tetramethoxy-2-butene is relatively simplified, halogen is recycled in the process, the three wastes are extremely few, and the obtained by-product still has relatively high economic value.

Description

technical field [0001] The invention belongs to the field of electrochemical synthesis, in particular to an electrochemical synthesis method for preparing 1,1,4,4-tetramethoxy-2-butene. [0002] technical background [0003] 1,1,4,4-Tetramethoxy-2-butene is one of the key raw materials for the preparation of synthetic carotenoids, for the synthesis of β-carotene, canthaxanthin, astaxanthin, lutein, tomato Red pigment and other substances are of great significance. [0004] The traditional method of synthesizing 1,1,4,4-tetramethoxy-2-butene is to prepare 2,5-dimethoxy-2,5-dihydrofuran by acetalization. For example, German patent DE 19946816 discloses the preparation of 1,1,4,4-tetramethyl by reacting 2,5-dimethoxy-2,5-dihydrofuran with methanol under the catalysis of a solid catalyst with an acidic center Oxygen-2-butene; U.S. Patent No. 5,338,888 discloses a method of using an inorganic strong acid or an organic strong acid as a catalyst to prepare 1,5-dimethoxy-2,5-dihydr...

Claims

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Application Information

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IPC IPC(8): C25B3/07C25B9/60
CPCC25B3/07C25B9/60
Inventor 栾谨鑫黎源张永振王未振
Owner WANHUA CHEM GRP CO LTD
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