Preparation method of acetyl diammonium phosphate

A technology of acetyl phosphate diammonium salt and phosphoric acid, which is applied in the field of medicine, can solve problems such as hidden dangers, safety, and contamination at the entrance, and achieve the effects of being suitable for industrial production, reducing equipment requirements, and moderate reaction temperature

Inactive Publication Date: 2015-08-26
ZHEJIANG HISUN PHARMA CO LTD
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  • Abstract
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Problems solved by technology

[0005] The disadvantages of this method are: (1) the raw material ketene is gas, which is stored in a compressed steel cylinder, and there is a safety hazard during use; (2) impurities such as diacetyl phosphoric acid and triacetyl phosphoric acid are easily produced during the gas reaction process of ketene , (3) the raw material anhydrous ammonia gas is stored in compressed steel cylinders, which is very inconvenient during industrialized transportation and storage, and has potential safety hazards. The gas addition rate is difficult to control, and it is easy to form a fouling plug at the inlet, and the excessive ammonia gas easily degrades the product, and the obtained product acetyl phosphate diammonium salt has low purity and yield
[0007] The preparation method of acetyl phosphate diammonium salt disclosed in the above-mentioned prior art is not suitable for suitability for industrialized production, therefore, be badly in need of a kind of operation simple, mild condition, the preparation method of acetyl phosphate diammonium salt with low cost, in order to solve acetyl phosphate diammonium salt Many problems existing in the process of industrial production of ammonium salt

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  • Preparation method of acetyl diammonium phosphate
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Experimental program
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Effect test

Embodiment 1

[0029] In a 1L four-neck flask, add 80ml of ethyl acetate, add 54ml (0.79mol) of 85% industrial phosphoric acid under ice-water bath conditions, stir well, then slowly add 150ml (1.58mol) of acetic anhydride, and control the reaction temperature at 15°C. After the addition, the reaction was incubated for 0.5 hours. After the reaction, slowly add 118ml (1.74mol) of 28% concentrated ammonia water to keep the reaction internal temperature at 10°C. After the addition, keep stirring for 2 hours, filter, and dry to obtain 123g of acetyl phosphate diammonium salt solid (purity 98.3% ), the product yield is 90%.

Embodiment 2

[0031] In a 2L four-neck flask, add 320ml of ethyl acetate, add 108ml (1.58mol) of 85% industrial phosphoric acid under ice-water bath conditions, stir evenly, then slowly add 300ml (3.16mol) of acetic anhydride, and control the reaction temperature at 15°C. After the addition, the reaction was incubated for 0.5 hours. After the reaction, slowly add 28% concentrated ammonia water 257ml (3.8mol), keep the reaction temperature at 5°C, after the addition, keep stirring for 1.5h, filter, and dry to obtain 254g of acetyl phosphate diammonium salt solid (purity 98.5 %), product yield 93%.

Embodiment 3

[0033] In a 0.5L four-neck flask, add 40ml of acetonitrile, add 38.5g (0.39mol) of 100% industrial phosphoric acid under ice-water bath conditions, stir evenly, then slowly add 68ml (0.72mol) of acetic anhydride, and control the reaction temperature at 20°C. After the addition, the reaction was incubated for 0.5 hours. After the reaction is over, slowly add 28% concentrated ammonia water 58ml (0.86mol) to keep the reaction temperature at 5°C. After the addition, keep stirring for 2 hours, filter, and dry to obtain acetyl phosphate diammonium salt solid 59.7g (purity 98.2 %), product yield 87%.

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Abstract

The invention relates to an improved preparation method of acetyl diammonium phosphate. According to the improved preparation method, phosphoric acid is reacted with acetic anhydride firstly so as to obtain acetyl phosphate, and then ammonium hydroxide is added so as to obtain acetyl diammonium phosphate. The improved preparation method is simple in operation, high in yield, and low in cost, and is especially suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of acetyl phosphate diammonium salt. Background technique [0002] Acetyl phosphate (ACP), as a high-energy phosphate, is widely used in the field of biocatalysis. However, due to the poor stability of acetyl phosphate, it is rapidly degraded into phosphoric acid and acetic acid at room temperature, and it is usually made into acetyl phosphate in practical applications. Compared with acetyl phosphate, acetyl phosphate has the advantages of good stability, low transportation and storage costs, and convenient use. Commonly used acetyl phosphates include dilithium acetyl phosphate, disodium acetyl phosphate and diammonium acetyl phosphate. Among them, the production cost of dilithium salt is high, and disodium salt is relatively hygroscopic, which are not suitable for industrial production. Only diammonium acetyl phosphate is widely used. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 温伟江傅德进杨勇杨仲毅杨元明黄强马辉杨峰晨
Owner ZHEJIANG HISUN PHARMA CO LTD
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