Method for preparing perchlorinated cyclopentadienyl

A technology for substituting cyclopentadiene and monocyclopentadiene, which is applied in the field of synthesis of organic compounds, can solve the problems of low content and low yield of perchlorinated cyclopentadiene products, and improve the utilization rate and cost of chlorine gas. The effect of low cost and simple process

Active Publication Date: 2008-12-10
JIANGSU ANPON ELECTROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Generally, the method for synthesizing perchlorocyclopentadiene is to react monocyclopentadiene with chlorine gas in a single reactor, and determine the end point of the reaction by observing the specific gravity of the reaction solution. When the specific gravity of the reaction material is 1.7, stop the reaction to obtain The product is a mixture, the yield is not high, and the product content of perchlorocyclopentadiene is low

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  • Method for preparing perchlorinated cyclopentadienyl
  • Method for preparing perchlorinated cyclopentadienyl

Examples

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example 1

[0029] In a 500L cracking kettle, first add 100Kg of dicyclopentadiene, and slowly raise the temperature of the cracking kettle to 300-350°C through an electric heating package. The diene is added to the cracking tank, and the steam flows into the storage tank after quenching to form monocyclopentadiene. While adding monocyclopentadiene to a 500L tetrachlorination kettle, feed chlorine gas, keep the temperature of the tetrachlorination kettle at 20-40°C, and transfer the unreacted chlorine gas in the tetrachlorination kettle back into the tetrachlorination kettle to participate in the chlorination reaction , when the reflux liquid is slightly yellow through the exhaust gas reflux sight glass, it means that the tetrachloride has reached the end point. 1,2,3,4-tetrachlorocyclopentane is transferred in the octachlorination still, and the octachlorination still has four stages in series, and successively the 1st, 2nd, 3rd, 4th grade octachlorination stills Add 350Kg of 1,2,3,4-te...

example 2

[0031] In a 500L cracking kettle, first add 100Kg of dicyclopentadiene, and slowly raise the temperature of the cracking kettle to 450-500°C through an electric heating package. Diene is added to the cracking tank, and the steam is rapidly cooled to form monocyclopentadiene. While adding monocyclopentadiene to a 500L tetrachlorination kettle, chlorine gas is introduced to keep the temperature of the tetrachlorination kettle at 30-50°C. The unreacted chlorine in the kettle is transferred back into the tetrachlorination kettle to participate in the chlorination reaction. When the reflux liquid is slightly yellow through the tail gas reflux sight glass, it means that the tetrachlorination has reached the end. 1,2,3,4-tetrachlorocyclopentane is transferred in the octachlorination kettle, the octachlorination kettle has three stages in series, successively add 350Kg 1 , 2,3,4-Tetrachlorocyclopentane, keep the temperature at 280-300°C, 220-250°C, 150-180°C respectively, after 8 hour...

example 3

[0033] Slowly raise the temperature of the tubular cracker through an electric heating pack, and at the same time, feed nitrogen into the tubular cracker. When the temperature reaches 150°C, continuously feed dicyclopentadiene through a flow meter at a rate of 140 kg per hour, and turn off the nitrogen at the same time , The steam from the tubular cracker is quenched into monocyclopentadiene. While adding monocyclopentadiene to the 500L tetrachlorination kettle, feed chlorine gas, keep the temperature of the tetrachlorination kettle at 70-80°C, and transfer the unreacted chlorine gas in the tetrachlorination kettle back into the tetrachlorination kettle to participate in the chlorination reaction , when the reflux liquid is slightly yellow through the exhaust gas reflux sight glass, it means that the tetrachloride has reached the end point. 1,2,3,4-tetrachlorocyclopentane is transferred in the octachlorination still, and the octachlorination still has four stages in series, an...

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Abstract

The invention discloses a method for preparing hexachlorocyclopentadiene. The method comprises the following steps of: using dicyclopentadiene as a raw material and carrying out pyrolysis, two-step chlorination, dechlorination, rectification, and deacidification to obtain a product with a purity of more than 98 percent, wherein the chlorination is a serial multi-step reaction which is capable of making an effective use of chlorine and improving the utilization rate of the chlorine. With the use of dicyclopentadiene, the overall yield of the invention can reach more than 90 percent.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for preparing perchlorinated cyclopentadiene. Background technique [0002] Perchlorinated cyclopentadiene is an important pesticide and chemical intermediate, which can be used in the synthesis of pesticides (aldrin, dieldrin, endosulfan, chlordane, mirex), medicine (antipyrine) and polyurethane industries flame retardant. [0003] Perchlorocyclopentadiene is a light yellow or brownish yellow transparent liquid at room temperature with a pungent odor and is nonflammable. The boiling point is 239°C (68-70°C, 1-1.3mmHg), the freezing point is 9.6°C, and the density (d425) is 1.7019×10 3 kg / m 3 , Refractive index (Nd25) 1.563, no flash point, insoluble in water, soluble in ether, carbon tetrachloride and other organic solvents. [0004] Generally, the method for synthesizing perchlorocyclopentadiene is to react monocyclopentadiene with chlorine gas in a si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C23/08C07C17/02C07C17/23
Inventor 姜育田季玉祥刘跃安礼如魏标
Owner JIANGSU ANPON ELECTROCHEM
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