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Solvent-free heating-free method for synthesizing potassium diformate

A potassium diformate, heating-free technology, applied in carboxylate preparation, organic chemistry, etc., can solve the problems of control of unfavorable reaction intensity, increase of production cost, increase of energy consumption, etc., and achieve economic feasibility and production efficiency Improve and reduce the effect of raw material loss

Inactive Publication Date: 2008-02-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The U.S. invention patent US6137005 discloses a process for preparing potassium diformate by the reaction of formic acid and potassium formate. This method can obtain potassium diformate with a higher yield, but the price of potassium formate, one of the raw materials used, is high, which increases the cost of the method. production cost
Chinese patent CN1428325A discloses a method of directly reacting potassium carbonate or potassium hydroxide with formic acid in a special reactor to prepare potassium diformate. Bottom feeding not only increases energy consumption, but also is not conducive to the control of reaction intensity
Chinese patent CN1704394A discloses a process for preparing potassium diformate by reacting formic acid aqueous solution with potassium carbonate or potassium hydroxide aqueous solution. The disadvantages of this process are large water consumption, evaporation and concentration, high energy consumption, and increased production cost.
Chinese patent CN1844074A also discloses a preparation method of potassium diformate. Potassium diformate is obtained by the reaction of formic acid aqueous solution and solid potassium oxide. This method has simple process, less water consumption, and reduces energy consumption, but there is also the price of raw material potassium oxide. high problem
However, the reaction time of this process is long and the process is complicated, which requires additional separation steps of the process product methanol, which greatly increases equipment investment and energy consumption.

Method used

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  • Solvent-free heating-free method for synthesizing potassium diformate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: 11.0 mL of 88.0% formic acid was added to a 50 mL three-necked round-bottomed flask, and at room temperature and under magnetic stirring, 7.78 g of solid flake potassium hydroxide (82%) was slowly added. With the addition of potassium hydroxide, the temperature gradually increased. When the temperature reaches 80°C, slow down the feeding rate, and keep the temperature at 80±1°C by controlling the feeding rate. After the addition, the stirring reaction was continued at room temperature, and the stirring was stopped when the temperature dropped to 45°C. The reaction product was cooled and crystallized at room temperature, and dried in a 60°C electric constant temperature drying oven. After drying, the product was ground to obtain 14.6 g of potassium diformate, with a product yield of 98.7%.

[0017] The infrared spectrogram of gained potassium diformate product is shown in Figure 1, and among the figure absorption peak and the corresponding peak of potassium d...

Embodiment 2

[0018] Embodiment 2: adopt the raw material ratio in the embodiment 1, when the temperature reaches 70 ℃ during the feeding process, slow down the feeding speed, keep the temperature at 70 ± 1 ℃ by controlling the feeding speed. After the addition, the stirring reaction was continued at room temperature, and the stirring was stopped when the temperature dropped to 20°C. The rest of the conditions and steps are the same as in Example 1, finally obtaining 14.1 g of potassium diformate, and the product yield is 95.3%.

Embodiment 3

[0019] Embodiment 3: adopt the raw material ratio in the embodiment 1, when the temperature reaches 70 ℃ during the feeding process, slow down the feeding speed, keep the temperature at 70 ± 1 ℃ by controlling the feeding speed. After the addition, the stirring reaction was continued at room temperature, and the stirring was stopped when the temperature dropped to 50°C. All the other conditions and steps are the same as in Example 1, finally obtaining 14.5 g of potassium diformate, and the product yield is 98.0%.

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Abstract

A non-solvent and non-heating method for synthesizing potassium diformate relates to a compound preparation method, which is a one-step potassium diformate synthesis method that takes potassium hydroxide and formic acid as raw materials and requires no solvent and no heating. A normal atmospheric pressure refluxing reaction method is adopted, and the solid potassium hydroxide is added into the formic acid by a molar ratio of 1:2.0-3.0 between the solid potassium hydroxide and the formic acid; the reaction temperature is kept between 50-90 DEG C when the materials are added; the reaction continues when the materials adding stops and is not stopped until the temperature falls to 20-50 DEG C; the reaction product is cooled and crystallized at room temperature, and the crystallized product is dried at a temperature of 50-60 DEG C and finely grinded, then the potassium diformate is acquired. No heating is required in the reaction, thereby the reaction intensity is well controlled while the reaction heat is fully utilized; the product is synthesized without solvent, thereby saving the evaporating and concentrating processes, shortening the production period and improving the production efficiency; the yield of the potassium diformate is as high as 99 percent or over. The method is suitable for large scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a method for synthesizing potassium diformate by using potassium hydroxide and formic acid as raw materials. Background technique [0002] Potassium diformate is a new type of feed additive used as an alternative to antibiotic growth promoters. It is the first new green feed additive approved by the European Union in 2001 to replace antibiotic growth promoters, and the Ministry of Agriculture of China also approved its promotion and use in feed in 2005. Studies have shown that potassium diformate is added to the feed as an acidifier, which can effectively inhibit harmful bacteria, improve the microbial flora in animals, and enhance the immune function of animals; improve enzyme activity and nutrient digestibility; improve the palatability of feed, effectively Improve animal daily gain, feed conversion rate, and reduce disease. The European Union has completely banned the us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/06C07C51/41
Inventor 李清彪林文爽孙道华王惠璇黄加乐洪金庆叶美玲陈翠雪郑进宝王远鹏
Owner XIAMEN UNIV
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