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Method for continuously manufacturing potassium diformate

A technology of potassium diformate and formic acid, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, can solve the problem that potassium oxide cannot be directly stored in the air, the source of potassium oxide is small, and it is difficult to industrialize application, etc. It is suitable for large-scale industrial production, the production process is continuous and uninterrupted, and the reaction is mild and controllable.

Active Publication Date: 2016-05-11
BEIJING UNIV OF CHEM TECH +2
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Chinese invention patent CN1844074 introduces the method for preparing potassium diformate with formic acid and potassium oxide as raw materials, but because the source of potassium oxide used in this method is less, the price is high, and potassium oxide cannot be directly stored in the air, resulting in this method High cost and limited industrial application
The U.S. patent of invention US6137005 introduces the method for preparing potassium diformate by the reaction of formic acid and potassium formate. Although the reaction yield of this method is high, the price of potassium formate, the raw material for the reaction, is high, making this method difficult to carry out industrial application.
Chinese patent CN1428325 has introduced the method that solid potassium carbonate reacts with formic acid to synthesize potassium diformate, but the resulting product yield is low, only about 50%
However, the reaction process takes a long time and the process is complicated, and it is necessary to increase the separation steps of the process product methanol, which greatly increases the equipment investment and loss.

Method used

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  • Method for continuously manufacturing potassium diformate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: take by weighing potassium hydroxide solid 15.73g (82%), add distilled water and be prepared into potassium hydroxide solution, get half of former potassium hydroxide solution and put into the first reactor, pass into potassium hydroxide solution 0.04mol carbon dioxide gas forms a mixed solution, and the mol ratio of potassium hydroxide and potassium carbonate in the controlled mixed solution is 1.5. Add 30ml of formic acid (the molar ratio of formic acid to potassium ions is 2.6:1) and the mixed solution into the second reactor and stir the reaction with a transfer pump. The reaction temperature is 60°C. While reacting, the remaining potassium hydroxide solution Continue to pass into the first reactor, and continuously extract the product in the second reactor after about two minutes, and react at a temperature of 60°C for 1 hour. After the reaction is stopped, the product solution is distilled under reduced pressure, and it is left to stand at room temper...

Embodiment 2

[0030] Embodiment 2: adopt the feed ratio of example 1, pass into carbon dioxide gas amount to be 0.05mol, control the molar ratio of potassium hydroxide and potassium carbonate in the mixed solution to be 0.80, the reaction temperature is 55 ℃, and the reaction time is 2.5h. All the other conditions and steps are the same as Example 1, and the product is dried to obtain 25.75 g of potassium diformate, and the product yield is 86.17%.

Embodiment 3

[0031] Embodiment 3: take by weighing potassium hydroxide solid 17.04g, formic acid 30ml (formic acid mol and potassium ion molar ratio is 2.4:1) add distilled water and prepare potassium hydroxide solution, pass into carbon dioxide gas amount and be 0.05mol, hydrogen in the mixed solution The molar ratio of potassium oxide to potassium carbonate was 1, the reaction temperature was 65° C., and the reaction time was 2 hours. The remaining conditions and steps were the same as in Example 1. The product was dried to obtain 27.56 g, with a yield of 86.09%.

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Abstract

The invention provides a method for continuously manufacturing potassium diformate. The method is characterized in that carbon dioxide gas serves as a regulating agent, formic acid and potassium hydroxide serve as raw materials, potassium diformate is synthesized in one step, and no gas is emitted in the whole reaction process. In the production process, solid potassium hydroxide is prepared into a solution, a certain quantity of the potassium hydroxide solution is obtained, and the carbon dioxide gas is introduced into the potassium hydroxide solution to prepare a potassium hydroxide and potassium carbonate mixed solution; potassium ions and formic acid with the molar ratio of 1:(2.0-3.0) are added in the mixed solution, and stirring reaction is conducted; in the reaction process, reaction temperature is kept to be 55-75 DEG C; the carbon dioxide gas generated due to reaction of formic acid and the mixed solution is recycled and reacts with a newly introduced potassium hydroxide solution; the product of the primary reaction is taken out, secondary reaction continues, reaction temperature is kept to be 55-75 DEG C, and secondary reaction lasts for 1-2.5 hours. The whole reaction is mild, controllable and free of emission, continuous production is achieved, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for producing potassium diformate, in particular to a synthesis method in which carbon dioxide gas is used as a regulator to make the whole reaction mild and controllable. Background technique [0002] Potassium diformate is a new type of feed additive. As a substitute for antibiotic growth promoters, potassium diformate was approved by the European Union as early as 2001. It is the first non-antibiotic approved by the European Union to replace antibiotic growth promoters. Feed additives. In order to ensure food safety, since 2006, the European Union will completely prohibit the use of auxin antibiotics in feed as feed additives. Potassium diformate is an acidifying agent. Compared with acidifying agents such as formic acid, potassium diformate is convenient to transport, and has low corrosion and irritation. Studies have found that potassium diformate, as a feed additive, can increase the feed intake of livestock an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/06
CPCC07C51/412C07C53/06
Inventor 张建文翟宝金伟常立顺燕文广盖翠萍
Owner BEIJING UNIV OF CHEM TECH
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