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Preparing method for high purity propargyl n-butyl carbamate

A technology of propargyl n-butyl carbamate and n-butyl isocyanate, which is applied in the field of synthesis of organic compounds, can solve problems such as the industrial production of propargyl n-butyl carbamate that has not yet been seen, and achieve low cost and method Simple, high-yield results

Active Publication Date: 2007-08-15
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Propargyl n-butyl carbamate (abbreviated as PBC) is a precursor of a new type of high-efficiency fungicide iodopropargyl n-butyl carbamate (abbreviated as IPBC), which is increasingly widely used. A report on the industrial production of n-butylcarbamate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Using two metering pumps, the n-butyl isocyanate and propargyl alcohol liquids are sent to the vaporizer at 63.4kg / h and 36.6kg / h respectively to be heated and vaporized, and then enter the porous fixed-bed reactor, and the shell-side cooling of the fixed-bed reactor is adjusted. The water flow rate controls the reaction temperature to 115-130° C., and reacts for 40 minutes to obtain 100 kg / h of liquid crude propargyl butyl carbamate. Under the absolute vacuum pressure of 50KPa and 160°C, the propargyl n-butyl carbamate is passed through the polymer membrane in the gas phase, so that the propargyl n-butyl carbamate can pass through selectively, and the slight excess of the reactant Propargyl alcohol is enriched and collected and returned to the system for reuse. The propargyl n-butyl carbamate obtained through the polymer film is decolorized by attapulgite at 20°C to obtain a high-quality propargyl n-butyl carbamate with a content of 99.1%, a yield of 99.5%, and an appe...

Embodiment 2

[0020] Using two metering pumps, the n-butyl isocyanate and propargyl alcohol liquids are sent to the vaporizer at 63.4kg / h and 36.6kg / h respectively to be heated and vaporized, and then enter the porous fixed-bed reactor, and the shell-side cooling of the fixed-bed reactor is adjusted. The water flow rate was used to control the reaction temperature to 115-130° C., and the reaction was carried out for 60 minutes to obtain 101.1 kg / h of liquid crude propargyl butyl carbamate. Under vacuum absolute pressure 20KPa and 130°C, propargyl n-butyl carbamate passes through the polymer membrane in the gas phase, so that propargyl n-butyl carbamate can pass through selectively, and a slight excess of reactants Propargyl alcohol is enriched and collected and returned to the system for reuse. The propargyl n-butyl carbamate obtained through the polymer membrane is decolorized by an ion exchange resin at 30°C to obtain a high-quality propargyl n-butyl carbamate with a content of 95.8%, a y...

Embodiment 3

[0022] Using two metering pumps, send the n-butyl isocyanate and propargyl alcohol liquids into the vaporizer at 63.4kg / h and 37.7kg / h respectively for heating and vaporization, and then enter the porous fixed bed reactor, and cool down by adjusting the shell side of the fixed bed reactor The water flow rate was used to control the reaction temperature to 130-145° C., and the reaction was carried out for 40 minutes to obtain 101.1 kg / h of liquid crude propargyl butyl carbamate. Under the absolute vacuum pressure of 60KPa and 170°C, the propargyl n-butyl carbamate is passed through the polymer membrane in the gas phase, so that the propargyl n-butyl carbamate can pass through selectively, and the slight excess reactant Propargyl alcohol is enriched and collected and returned to the system for reuse. The propargyl n-butyl carbamate obtained through the polymer membrane is decolorized by activated carbon at 30°C to obtain the high-quality propargyl n-butyl carbamate, the content ...

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PUM

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Abstract

The invention discloses a making method of high-purity propargyl n-butyl carbamic acid ester, which comprises the following steps: reacting trace propargyl alcohol and n-butyl isocyanate in the gas-phased condition to make rough product; making propargyl n-butyl carbamic acid ester pass macromolecular film to do selectivity passage in the vacuum; enriching micro-excessive propargyl alcohol to collect; returning into system to use; decoloring propargyl n-butyl carbamic acid ester under normal temperature.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing propargyl n-butyl carbamate. Background technique [0002] Propargyl n-butyl carbamate (abbreviated as PBC) is a precursor of a new type of high-efficiency fungicide iodopropargyl n-butyl carbamate (abbreviated as IPBC), which is increasingly widely used. A report on the industrial production of n-butyl carbamate. [0003] In CN92113788.5, under nitrogen saturation, n-butyl bromide, propynyl alcohol, potassium cyanide and tetrabutylammonium bromide in acetonitrile solvent are concentrated and purified to obtain PBC, and the yield is about 53%. Another method PBC was obtained by reaction concentration and purification with potassium cyanide, n-butyl bromide and propynyl alcohol in DMF solvent, and the yield was 33.8%. In CN94104163.8, di(C1-C3) alkyl carbonate and propynyl alcohol are used to react to generate dipropargyl carbonate, and the...

Claims

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Application Information

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IPC IPC(8): C07C269/02C07C271/12
Inventor 姜育田安礼如王海超
Owner JIANGSU ANPON ELECTROCHEM
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