Method for purifying hexachlorocyclopentadiene

A technology for hexachlorocyclopentadiene and a purification method, which is applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry and other directions, can solve the difficulty of separating crude hexachlorocyclopentadiene products and the inability to obtain high-purity hexachlorocyclopentadiene. cyclopentadiene, large amount of solvent consumption, etc., to avoid product loss, easy operation, and improved economic benefits

Inactive Publication Date: 2013-02-27
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The main production methods of hexachlorocyclopentadiene are chlorine gas method, molten salt method (Lummus method), Lidov method, Prims method and sodium hypochlorite method, but it is difficult to separate the crude product of hexachlorocyclopentadiene obtained by these methods
This method consumes a large amount of solvent, and the conditions are harsh, and the requirements for equipment are relatively high.
[0006] 2. In US3214444, the method of azeotropic distillation is used to remove the halocarbon impurities, so as to avoid the formation of unnecessary maleic anhydride products during the reaction between hexachlorocyclopentadiene and maleic anhydride. The hexachlorocyclopentadiene obtained by this method is suitable for the production of chlorine bridge anhydride or bridge acid, but high purity hexachlorocyclopentadiene cannot be obtained
The purity of the product obtained by this method is relatively low, and the loss is relatively serious

Method used

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  • Method for purifying hexachlorocyclopentadiene

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Embodiment 1

[0030] Weigh 150g of crude hexachlorocyclopentadiene, distill the above liquid under reduced pressure (vacuum degree is 10 mmHg), collect the fraction before 76°C and the fraction at 76-116°C respectively, and then distill the fraction before 76°C under 100°C Stir at constant temperature for 3 hours, distill, collect the fraction at 76-116°C, mix the fractions at 76-116°C obtained from the two distillations, stir at constant temperature at 100°C for 3 hours, then distill under reduced pressure (vacuum degree is 10 mmHg), collect 105 85 g of distillate at -112°C is high-purity hexachlorocyclopentadiene with a purity of 98.7% and a yield of 93.1%.

Embodiment 2

[0032] Weigh 800g of crude hexachlorocyclopentadiene, add 5g of anhydrous magnesium sulfate to remove the contained water, let stand overnight, and filter with suction to obtain a clear oily liquid. Distill the above liquid under reduced pressure (vacuum degree is 14 mmHg), collect the fraction before 78°C and the fraction at 78-117°C respectively, then stir the fraction before 78°C at 100°C for 3.5 hours, and collect 78-117°C by vacuum distillation. For the fraction at 117°C, continue to stir the fraction at 78-117°C obtained by two distillations at 100°C for 3 hours, then distill under reduced pressure (vacuum degree is 14 mmHg), collect 449g of fraction at 106-113°C, which is high-purity six Chlorocyclopentadiene, the purity is 99.2%, and the yield is 92.8%.

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Abstract

The invention discloses a method for purifying hexachlorocyclopentadiene. The method for purifying the hexachlorocyclopentadiene includes the steps: firstly, distilling crude hexachlorocyclopentadiene under reduced pressure and collecting front cut fractions and rear cut fractions of two temperature sections; secondly, continuing constant-temperature stirring of the front cut fractions for 2-8 hours, performing reduced pressure distillation and mixing the front cut fractions with the rear cut fractions; and thirdly, continuing constant-temperature stirring for 2-8 hours and performing reduced pressure distillation to obtain the high-purity hexachlorocyclopentadiene. The method has excellent effects in application, the purity of the hexachlorocyclopentadiene can reach 99%, the yield can reach more than 93%, needed equipment is simple, energy consumption is low, the process is easily controlled, and the method is suitable for industrial application.

Description

technical field [0001] The invention belongs to a method for purifying products, in particular to a method for purifying hexachlorocyclopentadiene as a crude product. Background technique [0002] Hexachlorocyclopentadiene forms aromatic pentachlorocyclopentadiene anion, so it is active and can undergo Diels-Alder reaction with most dienophiles, and the conditions are relatively mild, the temperature is generally between 20-200 °C It can even react with simple alkenes and polycyclic aromatic hydrocarbons (such as naphthalene, anthracene, etc.) that cannot be reacted under normal conditions. Hexachlorocyclopentadiene is mostly used as an intermediate in the production of pesticides. Before the 1960s, it was used to produce organochlorine insecticides and acaricides, such as mirex, aldrin, dieldrin, Chlordane, endosulfan, etc. In addition, hexachlorocyclopentadiene is also used as a flame retardant and curing agent for polyester resins and polyurethane foams. Since there ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C23/08C07C17/383
Inventor 罗仕忠张坡李通徐振新王洪梅胡像锋储伟鲁灵江
Owner SICHUAN UNIV
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