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Preparation method of 2-bromo-2-nitro-1,3-propylene glycol

A technology of propylene glycol and tribromonitromethane, applied in the field of 2-bromo-2-nitro-1, can solve the problems of increased impurities, low utilization rate of bromine, reduced content, etc., and achieves reduction of production cost, realization of cleaning, The effect of increased utilization

Active Publication Date: 2007-01-31
JIANGSU LIANHE CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. If the raw material uses bromine as the bromination agent, the utilization rate of bromine is low, only 45%
[0006] 2. If the raw material uses bromosuccinimide as the brominating agent, the yield can be increased, but at the same time it will increase the cost
[0007] 3. If bromine chloride is used as the bromination agent as the raw material, the utilization rate of bromine can be improved, but the impurities in the product will increase and the content will decrease
[0008] 4. The introduction of solvent ethanol not only increases the actual cost of production, but also increases the investment in equipment such as solvent recovery and treatment devices

Method used

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  • Preparation method of 2-bromo-2-nitro-1,3-propylene glycol

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: the preparation method of 2-bromo-2-nitro-1,3-propanediol

[0032] In a 1-liter reactor, put 1 mole of nitromethane, 50 milliliters of water, and 1.5 moles of bromine, slowly add 3 moles of 30% sodium hydroxide solution and stir for 1 hour, and feed 110 grams of chlorine gas at 30 to 40 ℃, stirred and reacted for 1 hour, and stood to separate layers to separate 310.8 g of tribromopicrin with a purity of 99% and a yield of 98%. 310.8 grams of the bromopicrin reaction solution obtained by the above reaction, 180 grams of formaldehyde, and 131 grams of nitromethane were stirred and reacted for 1 hour. Below 40 ° C, 10% sodium hydroxide solution was slowly added dropwise, and at 30 React at ~40°C for 1 hour, cool, crystallize, filter, and dry to obtain 564.2 g of bronopol finished product with a purity of 99% and a yield of 95%.

Embodiment 2

[0033] Embodiment 2: the preparation method of 2-bromo-2-nitro-1,3-propanediol

[0034] In a 1-liter reactor, put 1 mole of nitromethane, 50 milliliters of water, and 1.5 moles of bromine, slowly add 3 moles of 30% sodium hydroxide solution and stir for 1 hour, and feed 106.5 grams of chlorine gas at 30 to 40 ℃, stirred and reacted for 1 hour, stood to separate layers, and separated 306.7 g of tribromopicrin with a purity of 99% and a yield of 96.7%. 306.7 grams of the bromopicrin reaction solution obtained by the above reaction, 180 grams of formaldehyde, and 131 grams of nitromethane were stirred and reacted for 1 hour. Below 40 ° C, 10% sodium hydroxide solution was slowly added dropwise, and at 30 ~ React at 40°C for 1 hour, cool, crystallize, filter, and dry to obtain 562.6 g of bronopol finished product with a purity of 99% and a yield of 96%.

Embodiment 3

[0035] Embodiment 3: the preparation method of 2-bromo-2-nitro-1,3-propanediol

[0036] In a 1-liter reactor, put 1 mole of nitromethane, 50 milliliters of water, and 1.5 moles of bromine, slowly add 3 moles of 30% sodium hydroxide solution and stir for 1 hour, and feed 110 grams of chlorine gas at 30 to 40 ℃, stirred and reacted for 1 hour, and stood to separate layers to separate 310.8 g of tribromopicrin with a purity of 99% and a yield of 98%. 310.8 grams of the bromopicrin reaction solution obtained by the above reaction, 180 grams of formaldehyde, and 131 grams of nitromethane were stirred and reacted for 1 hour. Below 40 ° C, 10% potassium hydroxide solution was slowly added dropwise. React at 40°C for 1 hour, cool, crystallize, filter, and dry to obtain 569.7 g of bronopol finished product with a purity of 99% and a yield of 94%.

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Abstract

The present invention relates to a preparation method of 2-bromo-2-nitro-1,3-propanediol. Said method includes the following steps: adding nitromethane, bromine and water into a reactor, slowly adding sodium hydroxide aqueous solution, stirring for 0.5-2hr, introducing chlorine gas, stirring to make reaction at 0-70deg.C to obtain nitrobromoform, then stirring the obtained nitrobromoform, formaldehyde and nitromethane for 0.5-2hr, slowly adding aqueous solution of inorganic alkali catalyst at 60deg.C, making reaction for 0.5-2hr at 0-60deg.C, cooling, crystallizing, filtering and drying so as to obtain 2-bromo-3-nitro-1,3-propanediol.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and relates to a preparation method of 2-bromo-2-nitro-1,3-propanediol (bronopol). Background technique [0002] The molecular formula of 2-bromo-2-nitro-1,3-propanediol (bronopol) is C 3 h 6 BrNO 4 , with a molecular weight of 200.0. In 1964, it was developed by Boot Co. Ltd (now AgEvo GmbH) as a cosmetic preservative and medicine, and later as an agricultural fungicide. In 1990, it was developed as a rice seed treatment agent in my country to prevent and control rice spoilage. Seedling disease, used as a cotton seed treatment agent to prevent and control cotton black arm disease or bacterial scab blight caused by cabbage black rot and yellow stem disease, has special effects, and has no phytotoxicity to cotton. It can also be used as an industrial fungicide, such as a fungicide for cooling towers. The structural formula of bronopol is as follows: [0003] [0004] German patent DE1954173...

Claims

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Application Information

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IPC IPC(8): C07C205/26C07C201/12
Inventor 郎玉成
Owner JIANGSU LIANHE CHEM TECH
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