Method for preparing 3-iodo-2-propynyI butyl carbamate

A technology of substituting propargyl n-butyl carbamate and propargyl n-butyl carbamate, which is applied in the field of synthesis of organic compounds, can solve problems such as low purity of IPBC products, high product prices, and difficult control. problems, to achieve the effect of inhibiting the formation of polyiodides, reducing the occurrence of side reactions, and controlling the reaction temperature

Inactive Publication Date: 2009-01-07
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

IPBC series products have been used in many industries in our country, because the production of its main agent IPBC is completely monopolized by foreign countries, and the product price is expensive
[0003] The purity of the IPBC products produced by the existing patented methods is not too high. In US20050033083, sodium iodide is used as the iodide agent and reacted in the water phase at 0-11°C. This method uses sodium iodide, which is not ideal in terms of cost
In US5693849, iodine is used as the iodination agent, reacted in the water phase at 6-17°C, and the surfactant is added, and the iodine is added in three batches. This method is difficult to control and has poor repeatability.
In EP0014032, iodine is used as the iodine agent, reacted in a mixed solution of ethanol and water, after the reaction, the reaction solution is neutralized, extracted with toluene, and then the toluene is removed under vacuum to obtain the product. This method does not describe IPBC The purity of the product, but we have repeatedly tested, the product purity of this method is low, and the color of the product is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under the condition of 5°C and stirring, dissolve 10,000 kg of iodine in 50,000 kg of ethanol to make an iodine solution, and make a mixed solution with 12,000 kg of propargyl n-butyl carbamate, 12,500 kg of 30% liquid caustic soda and 25,000 kg of water (the mol ratio of propargyl n-butylcarbamate and alkali is 1: 1.24), prepare 35000 kilograms of chlorine-containing 8% sodium hypochlorite solutions.

[0022] Reactors numbered 1#, 2#, 3#, 4#, and 5# are connected to each other through pipes from low to high. Among them, 3# and 5# reactors are 3000L and there are rotating discs in the kettles. 2#, 4 #Reaction kettles are 6300L and 5000L respectively, and there are overflow pipes and liquid agitators in the kettles, and the 1# reaction kettle is 6300L.

[0023] In 1#, 2#, 3#, 4#, 5# reactor temperature is controlled at 5°C~10°C, -5°C~5°C, 0°C~5°C, 0°C~5°C, 0°C~5°C Under the condition of ℃, with 800 kg / hour of iodine solution, propargyl n-butyl carbamate mixed solution i...

Embodiment 2

[0025] Under the condition of 0℃ and stirring, dissolve 10,000 kg of iodine in 65,000 kg of methanol to make an iodine solution, and make a mixed solution with 12,000 kg of propargyl n-butyl carbamate, 11,500 kg of 30% liquid alkali and 26,000 kg of water (the mol ratio of propargyl n-butylcarbamate and alkali is 1: 1.14), prepare 35000 kilograms of chlorine-containing 11% sodium hypochlorite solutions.

[0026] Reactors numbered 1#, 2#, 3#, 4#, and 5# are connected to each other through pipes from low to high. Among them, 3# and 5# reactors are 3000L and there are rotating discs in the kettles. 2#, 4 #Reaction kettles are 6300L and 5000L respectively, and there are overflow pipes and liquid agitators in the kettles, and the 1# reaction kettle is 6300L.

[0027] In 1#, 2#, 3#, 4#, 5# reactor temperature is controlled at 10°C ~ 15°C, -5°C ~ 0°C, -5°C ~ 0°C, -5°C ~ 5°C, -5°C Under the condition of ℃~0℃, the iodine solution is continuously sent into the 5# kettle spinner at 1000...

Embodiment 3

[0029] Under the temperature of -15°C and stirring conditions, dissolve 10,000 kg of iodine in 50,000 kg of toluene to make an iodine solution, and mix 12,000 kg of propargyl n-butyl carbamate, 12,000 kg of 30% liquid alkali and 25,500 kg of water Liquid (the mol ratio of propargyl n-butylcarbamate and alkali is 1: 1.19), prepare 35000 kilograms of chlorine-containing 11% sodium hypochlorite solution.

[0030] Reactors numbered 1#, 2#, 3#, 4#, and 5# are connected to each other through pipes from low to high. Among them, 3# and 5# reactors are 3000L and there are rotating discs in the kettles. 2#, 4 #Reaction kettles are 6300L and 5000L respectively, and there are overflow pipes and liquid agitators in the kettles, and the 1# reaction kettle is 6300L.

[0031] In 1#, 2#, 3#, 4#, 5# reactor temperature is controlled at 5°C~10°C, -15°C~-5°C, -10°C~-5°C, -15°C~-5°C , Under the condition of -10°C~-5°C, the iodine solution is continuously fed into the 5# kettle spinner at a rate o...

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PUM

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Abstract

The invention discloses a method for preparing iodopropargyl n-butyl carbamate, which comprises the following steps: a mode 1 reaction kettle, a mode 2 reaction kettle, a mode 3 reaction kettle, a mode 4 reaction kettle and a mode 5 reaction kettle are connected in series, wherein, projecting discs are arranged in the mode 3 reaction kettle and the mode 5 reaction kettle; return tubes and liquid stirrers are arranged in the mode 2 reaction kettle and the mode 4 reaction kettle; the mixed liquid composed of iodine solution and propargyl n-butyl carbamate is continuously charged into the projecting disc of the mode 5 reaction kettle, reaction liquid flows from the bottom of the mode 5 reaction kettle into the mode 4 reaction kettle continuously and flows from the return tube of the mode 4 reaction kettle into the projecting disc of the mode 3 reaction kettle continuously, and chloros water solution is continuously charged into the projecting disc of the mode 3 reaction kettle at the same time; the reaction liquid flows from the bottom of the mode 3 reaction kettle into the mode 2 reaction kettle continuously, and the return tube of the mode 2 reaction kettle into the mode 1 reaction kettle continuously; iodopropargyl n-butyl carbamate, the purity quotient of which is more than 99.0 percent, is obtained through washing, filtering and drying after the solvent is removed from the reaction liquid under the vacuum condition in the mode 1 reaction kettle. The product obtained by adopting the method has high purity quotient, large industrialization production is easy to be realized, the secondary reaction can be effectively reduced, and the utility ratio of iodine can be increased.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for preparing iodopropargyl n-butylcarbamate. Background technique [0002] Iodopropargyl n-butyl carbamate (IPBC for short) is the main component of the latest international environment-friendly microorganism (fungus, algae, etc.) , with the characteristics of safety, high efficiency, and environmental protection, and is environmentally friendly and safe. IPBC series products have been widely used by developed countries such as Europe and the United States in the fields of wood anti-corrosion, paint anti-mildew, and daily chemical products for anti-dandruff and anti-itch after being launched in the United States. If used in wood anti-corrosion, it can completely replace formaldehyde and copper chromium arsenic (CCA ) and other high-toxic wood preservatives as the main components to realize the greening of wood preservatives. IPBC series products have been...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/06C07C271/12
Inventor 郑坚姜育田安礼如赵卫东吴学勤李前永
Owner JIANGSU ANPON ELECTROCHEM
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