Refining process of uracil by sulfuric acid method

A technology of uracil and sulfuric acid method, which is applied in the refining process of uracil by sulfuric acid method, can solve the problems of not meeting high-end applications and export-level requirements, low product yield, and impact on purity, so as to increase product competitiveness, The effect of high product purity and simple operation

Pending Publication Date: 2021-07-16
甘肃堡昌化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many ways to prepare uracil in the prior art, and industrial production mainly focuses on producing uracil with oleum, urea and malic acid as raw materials. This method has mature technology, simple operation, and easy to obtain raw materials, but the product yield The rate is not high, about 60%, and the purity is easily affected by impurities such as sulfate and chloride, about 98-99%, which can only meet the needs of low-end uses, not high-end uses and export-level needs, and the added value is low

Method used

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  • Refining process of uracil by sulfuric acid method

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Embodiment 1

[0019] Present embodiment provides a kind of sulfuric acid method uracil refining method, and its steps comprise:

[0020] Step 1: Add 3,000 kg of pure water, 500 kg of crude uracil, and 25 kg of 200-mesh activated carbon powder into an acid-resistant reactor with a capacity of 5 tons. Under stirring conditions, the water bath is heated to 50°C, and the crude uracil is completely dissolved. Gradually drop liquid caustic soda to adjust pH to 7. The mixed solution is heated to 90°C for filtration, the filter cake is activated carbon, and the filtrate is pumped into a crystallization kettle with a capacity of 5 tons to cool down in a water bath.

[0021] Step 2: Cool the filtrate to 18°C ​​and gradually put it into the suction filtration tank, turn on the vacuum pump for negative pressure suction filtration, turn off the vacuum after the suction filtration, and inject pure water into the suction filtration tank to the liquid level of 2 / 3 of the suction filtration tank, Rotate th...

Embodiment 2

[0024] Present embodiment provides a kind of sulfuric acid method uracil refining method, and its steps comprise:

[0025] Step 1: Add 3,000 kg of pure water, 450 kg of crude uracil, and 20 kg of 150-mesh activated carbon powder into an acid-resistant reactor with a capacity of 5 tons. Under stirring conditions, the water bath is heated to 48°C, and the crude uracil is completely dissolved. Gradually drop liquid caustic soda to adjust pH to 7. The mixed solution is heated to 88°C for filtration, the filter cake is activated carbon, and the filtrate is pumped into a crystallization kettle with a capacity of 5 tons to cool down in a water bath.

[0026] Step 2: Cool the filtrate to 19°C and gradually put it into the suction filtration tank, turn on the vacuum pump for negative pressure suction filtration, turn off the vacuum after the suction filtration, inject pure water into the suction filtration tank to the liquid level of 2 / 3 of the suction filtration tank, Rotate the stir...

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Abstract

The invention belongs to the technical field of mold locking machine equipment, and particularly relates to a process for refining uracil by a sulfuric acid method, which comprises the following steps: adding a uracil crude product, water and activated carbon powder into a refining kettle, heating the mixture in a water bath under a stirring condition to completely dissolve the uracil crude product, gradually dropwise adding liquid caustic soda to adjust the pH value to 7, and cooling the mixture to room temperature; then heating the mixed solution to 85-90 DEG C for filtering out activated carbon and cooling the filtrate to 15-18 DEG C or below for crystallization. The method is applied to deep refining of a sulfuric acid method uracil crude product, the obtained high-purity uracil can meet the high-end application requirement, the export requirements that the main grade is larger than or equal to 99.9% and the sulfate is smaller than or equal to 0.03% are met, wherein the product competitiveness can be greatly improved. The method is simple in process and remarkable in economic benefit, and solves the problems that in the prior art, the yield of a uracil preparation product is not high and is about 60%, the purity is easily influenced by sulfate, chloride and other impurities and is about 98-99%, only low-end application requirements can be met, high-end application and export-grade requirements cannot be met, and the additional value is low.

Description

technical field [0001] The invention relates to the technical field of clamping machine equipment, in particular to a refining process of sulfuric acid uracil. Background technique [0002] Uracil is a white or off-white crystalline powder with a molecular formula of C4H4N2O2. It is one of the four bases that make up RNA. It is an important intermediate of fine chemical industry, pesticide and medicine, especially in the field of medicine, it is an important intermediate for the synthesis of anti-tumor drug 5-fluorouracil and its derivative drugs such as tegafur, bisfurfururacil, doxifluridine, The application is very extensive. [0003] There are many ways to prepare uracil in the prior art, and industrial production mainly focuses on producing uracil with oleum, urea and malic acid as raw materials. This method has mature technology, simple operation, and easy to obtain raw materials, but the product yield The rate is not high, about 60%, and the purity is easily affecte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/54
CPCC07D239/54
Inventor 马旻锐马登旭柳成喜张学欢吕勤孟存江
Owner 甘肃堡昌化工有限公司
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