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Method for solving oxidation material rushing-out in preparation for oxalic acid by virtue of starch

A technology of oxalic acid and starch, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve problems such as potential safety hazards, and achieve the effects of high safety, low input cost, and no impact on the cost of oxalic acid

Inactive Publication Date: 2013-02-13
HUBEI YITAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to address the above-mentioned deficiencies in the potential safety hazards in the process of preparing oxalic acid by nitric acid oxidation of starch, by introducing a kind of initiator-sodium nitrite, to provide a method that can quickly and steadily drive nitric acid and monosaccharide A simple and safe method for solving the oxidation punching material in the preparation of oxalic acid from starch

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 100ml of an acidic solution with a concentration of 50% by mass into a 500ml three-neck flask, raise the temperature to 60°C, slowly add 100g of starch, hydrolyze for 2 hours, and prepare a monosaccharide solution for later use.

[0024] Add 100ml vitriol oil, 0.1g catalyst (V 2 o 5 ) Stir evenly, raise the temperature to 60°C, then add 0.5g of initiator—sodium nitrite, and start to drop nitric acid solution at the same time, triggering the reaction, the temperature in the reaction bottle rises steadily, and a small amount of yellow gas is produced. Immediately start to drop the monosaccharide solution into the four-necked reaction bottle, the oxidation reaction starts, and keep the oxidation reaction at about 65°C. Continuously add nitric acid and monosaccharide solution dropwise until the reaction is complete, keep warm for 2 hours, drop to room temperature to crystallize, centrifuge to obtain oxalic acid.

[0025] Observing the oxidation reaction phenomenon, th...

Embodiment 2

[0027] Add 100ml of an acidic solution with a mass percentage concentration of 50% into a 500ml three-neck flask, raise the temperature to 60°C, slowly add 100g of starch, hydrolyze for 2 hours, and prepare a monosaccharide solution for later use.

[0028] Add the 200ml oxalic acid crude product centrifugal mother liquor that obtains in the embodiment 1 in the 500ml four-neck flask that has been installed, add 10ml vitriol oil, 0.1g catalyzer (V 2 o 5 ) Stir evenly, raise the temperature to 65°C, then add 0.8g of initiator—sodium nitrite, and start to drop nitric acid solution at the same time, triggering the reaction, the temperature in the reaction bottle rises steadily, and a small amount of yellow gas is produced. Immediately start to drop the monosaccharide solution into the four-necked reaction bottle, the oxidation reaction starts, and keep the oxidation reaction at about 65°C. Continuously add nitric acid and monosaccharide solution dropwise until the reaction is comp...

Embodiment 3

[0031] Add 100ml of 50% acidic solution to a 500ml three-neck flask, raise the temperature to 60°C, slowly add 100g of starch, hydrolyze for 2 hours, and prepare a monosaccharide solution for later use.

[0032] In the four-necked flask of installed 500ml, add the 200ml oxalic acid crude product centrifugal mother liquor that obtains among the embodiment 2, add 10ml vitriol oil, 0.1g catalyzer (V 2 o 5 ) Stir evenly, raise the temperature to 65°C, then add 1g of initiator—sodium nitrite, and start to drop nitric acid solution at the same time, triggering the reaction, the temperature in the reaction bottle rises rapidly, and a large amount of yellow gas is produced. Immediately start to drop the monosaccharide solution into the four-necked reaction bottle, the oxidation reaction starts, and keep the oxidation reaction at about 65°C. Continuously add nitric acid and monosaccharide solution dropwise until the reaction is complete, keep warm for 2 hours, drop to room temperature...

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Abstract

The invention discloses a method for solving oxidation material rushing-out in preparation for oxalic acid by virtue of starch, comprising the following steps of: (1) hydrolyzing the starch in an acidic condition to prepare a monosaccharide liquid; (2) adding an oxalic acid crude product centrifugal mother liquid in a reaction container with an added amount which is 1 / 3-1 / 2 of the whole reaction volume, replenishing concentrated sulphuric acid in a volume which is 5-20% of the total volume of the monosaccharide liquid and a catalyst simultaneously, and then adding an initiator; and adjusting the temperature of the reaction system to be above 50 DEG C, and adding nitric acid in a volume by volume concentration of 50-90%; and (3) immediately adding the monosaccharide liquid obtained in the step (1) after the nitric acid and the initiator start to react, and enabling the nitric acid and saccharides to start to react, so as to generate the oxalic acid. The method disclosed by the invention has the beneficial effects that the material rushing-out phenomenon generated by the directly serious initiation of monosaccharides and the nitric acid during an initiation process in the starting phase of the traditional preparation for oxalic acid by virtue of a starch-nitric acid oxidation process is avoided, and the production potential safety hazards brought by the material rushing-out phenomenon aforementioned are thoroughly solved; and moreover, the method is extremely low in investment cost without influence on the cost of the oxalic acid, high in safety, convenient to operate and extremely easy to popularize.

Description

【Technical field】 [0001] The invention belongs to the technical field of fine chemical industry, and specifically relates to a method for solving the problem of oxidative punching in the preparation of oxalic acid from starch. 【Background technique】 [0002] Oxalic acid, also known as oxalic acid, is the simplest dibasic acid in nature, usually in the form of dihydrate (H 2 C 2 o 4 2H 2 O), it is an important chemical raw material, widely used in the separation and purification of medicine, dyestuffs, coatings and rare earth metals, and the bleaching of clothing. [0003] Industrially, oxalic acid has a variety of preparation methods: such as sodium formate method, ethylene glycol nitric acid oxidation method, propylene oxidation method, carbon monoxide coupling method, etc., but the most widely used method for preparing oxalic acid in China is carbohydrate nitric acid oxidation method. The main raw material is starch. The main process of preparing oxalic acid by starch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/06C07C51/27
Inventor 王正友陈进
Owner HUBEI YITAI PHARMA
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