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Method for preparing large granular chloramine T based on cooling crystallization

A technology of cooling crystallization and large particles, which is applied in the field of medicine, can solve the problems of small particle size, and achieve the effects of improved purity, simple operation, and short cycle

Active Publication Date: 2014-05-07
天津普恒康泰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the particle size of the products produced by the existing technology is too small

Method used

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  • Method for preparing large granular chloramine T based on cooling crystallization
  • Method for preparing large granular chloramine T based on cooling crystallization
  • Method for preparing large granular chloramine T based on cooling crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing large particle chloramine T based on cooling crystallization, comprising the following steps:

[0027] (1) Weigh 35g of chloramine T, add it to 140mL ethanol aqueous solution (the volume ratio of ethanol and water in the ethanol aqueous solution is 8:1), heat to 40°C, and stir to dissolve;

[0028] (2) Pour into a jacketed reactor with controllable stirring, stir at 200rpm, cool the solution obtained in step (1) until crystallization is cloudy, and add 0.175g chloramine T crystal to the cloudy solution at 35°C Seed, grow the crystal for 40 minutes, gradually increase the cooling rate, and drop it to 12°C in 3 hours to obtain a crystal suspension;

[0029] (3) Suction filter the crystal suspension obtained in step (2) under reduced pressure, and dry naturally to obtain large particles of chloramine T. The yield is 70%.

[0030] The TG and DSC of the obtained chloramine T crystals are shown in figure 1 , see XRD figure 2 , the crystal morpholog...

Embodiment 2

[0032] A method for preparing large particle chloramine T based on cooling crystallization, comprising the following steps:

[0033] (1) Weigh 30g of chloramine T, add it to 180mL ethanol aqueous solution (the volume ratio of ethanol and water in the ethanol aqueous solution is 6:1), heat to 50°C, and stir to dissolve;

[0034] (2) Pour into a jacketed reactor with controllable stirring, stir at 220rpm, cool the solution obtained in step (1) until crystallization is cloudy, and add 0.3g of chloramine T crystal to the cloudy solution at 35°C Seed, grow the crystal for 30 minutes, gradually increase the cooling rate, and drop it to 10°C in 5 hours to obtain a crystal suspension;

[0035] (3) Filter the crystal suspension obtained in step (2) and dry it naturally to obtain large particles of chloramine T. The yield is 68%.

[0036] The crystal form seen under the microscope of the obtained large particle chloramine T product is as follows image 3 As shown in (b), the TG and D...

Embodiment 3

[0038] A method for preparing large particle chloramine T based on cooling crystallization, comprising the following steps:

[0039] (1) Weigh 25g of chloramine T, add it to 175mL ethanol aqueous solution (the volume ratio of ethanol and water in the ethanol aqueous solution is 5:1), heat to 50°C, and stir to dissolve;

[0040] (2) Pour into a jacketed reactor with controllable stirring, stir at 220rpm, cool the solution obtained in step (1) until crystallization is cloudy, and add 0.5g chloramine T to the cloudy solution at 30°C Seed crystals, grow crystals for 20 minutes, gradually increase the cooling rate, and drop to 8°C in 7 hours to obtain a crystal suspension;

[0041] (3) Filter the crystal suspension obtained in step (2) and dry it naturally to obtain large particles of chloramine T. Yield 72%.

[0042] The crystal form seen under the microscope of the obtained large particle chloramine T product is as follows image 3 As shown in (c), the TG and DSC of the obtain...

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Abstract

The invention discloses a method for preparing large granular chloramine T based on cooling crystallization. The method comprises the following steps: (1) adding a chloramine T crude product to ethanol water, heating, stirring ad dissolving; (2) under a stirring condition, cooling the solution obtained in the step (1) till devitrifying and getting turbid, adding chloramine T seed crystals, growing the grain, and cooling to 8-12 DEG C, thus obtaining crystallization suspension liquid; and (3) filtering the crystallization suspension liquid obtained in the step (2), and drying so as to obtain the large granular chloramine T. The method is simple to operate; conditions are easy to control; the obtained product is short in period and relatively high in purity; the prepared chloramine T crystal product is large in particle, uniform in particle size and high in yield, and the appearance of the crystal is complete.

Description

technical field [0001] The invention relates to a method for preparing large-grain chloramine T based on cooling crystallization, which belongs to the production field of chloramine T in the fields of medicine, chemical printing and dyeing and food. Background technique [0002] Chloramine T, the chemical name is p-toluenesulfonyl chloride sodium, and its structural formula is as follows: [0003] [0004] The shape is white crystalline powder, with a slight smell of chlorine, not bitter, decomposes slowly in the air, the available chlorine only decreases by 0.1% in one year, and gradually loses chlorine and turns yellow. As a disinfectant, this product is a broad-spectrum bactericidal disinfectant for external use, containing 24-25% available chlorine, relatively stable, and has a killing effect on bacteria, viruses, fungi, and spores. The principle of action is that the solution produces hypochlorous acid and releases chlorine, which has a slow and long-lasting bacteri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/48C07C303/44
Inventor 王占忠卫宏远
Owner 天津普恒康泰科技有限公司
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