Method for preparing high-quality DRCP

A cloned, high-quality technology, applied in the field of chemical engineering, can solve the problems of short reaction time, high reaction temperature, limited product application, etc., and achieve the effect of simple and easy method, easy industrialization, and load reduction.

Active Publication Date: 2012-03-14
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a short reaction time and a high yield, but the reaction uses a composite solvent, and toluene is used for washing after the reaction. There are many types of solvents, the recovery system is complicated, and the reaction temperature is high, which is easy to affect the color of the product, which limits the whiteness of the product. application of materials

Method used

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  • Method for preparing high-quality DRCP

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 118.6 grams (0.43 moles) of hexachlorocyclopentadiene and 70 grams of tetrachloroethane into a 250 mL four-neck flask equipped with a stirrer and a thermometer, raise the temperature to 140°C and add 21.6 grams (0.2 moles) of cyclooctadiene dropwise After dropping, the temperature is controlled at 150-160°C, and the temperature is kept at 150-160°C, and the temperature is kept for 5 hours. The cyclooctadiene peak disappears according to the gas spectrometry, the temperature is lowered, filtered, the solid is rinsed with xylene, and dried to obtain 122.8 grams of clones with a whiteness of 98 and a yield of 94. %.

Embodiment 2

[0019] Add 112.5 grams (0.41 moles) of hexachlorocyclopentadiene and 70 grams of cyclohexane into the autoclave, raise the temperature to 140°C, add 21.6 grams (0.2 moles) of cyclooctadiene dropwise, and control the temperature at 160-170°C after dropping. Keep warm for 5 hours, cool down, filter, rinse the solid with toluene, and dry to obtain 128.4 g of clones with a whiteness of 98.5 and a yield of 98.5%.

Embodiment 3

[0021] Add 112.5 grams (0.41 moles) of hexachlorocyclopentadiene and 70 grams of dichloroethane into the autoclave, raise the temperature to 140°C, add 21.6 grams (0.2 moles) of cyclooctadiene dropwise, and control the temperature at 160-170°C after dropping , keep warm for 4 hours, cool down, filter, rinse the solid with dichloroethane, and dry to obtain 127.1 grams of clones, with a whiteness of 98.1 and a yield of 97.4%.

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Abstract

The invention discloses a method for preparing high-quality DRCP, which is characterized in that hexachlorocyclopentadiene and cyclooctadiene are insulated and react for 3-10h in a solvent under 140-180 DEG C, wherein the molar ratio of hexachlorocyclopentadiene to cyclooctadiene is 2.0-2.5:1; the solvent is single and is alkane or halohydrocarbon; and the mass of the solvent is 30-60% of the total mass of hexachlorocyclopentadiene and cyclooctadiene. The method is simple and practicable and easy for industrialization, and the single solvent is convenient for recycling the subsequent solvent,thus reducing the load of subsequent processing. The high-quality DRCP obtained by the method of the invention has chromaticity being more than 98 and yield up to 98.5%.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a preparation method of a chlorine-based flame retardant declone. Background technique [0002] Dechlorane [bis(hexachlorocyclopentadiene) cyclooctane] is also called Dechlorane Plus, English name Dechlorane Plus, CASNo.13560-88-9, white powder, melting point 350°C, density 1.8-2.0g / cm 3 , chlorine content 65.08%, scientific name 1, 2, 3, 4, 7, 8, 9, 10, 13, 13, 14, 14-dodecachloro-1, 4, 4a, 5, 6, 6a, 7,10,10,11,12,12a-Dodecahydro-1,4,7,10-Dimethylidene diphenylcyclooctane, containing alicyclic chlorine, the structural formula is as follows: [0003] [0004] It is an additive flame retardant with excellent flame retardancy, thermal stability, electrical insulation and coloring properties, low smoke generation, inert filler performance, no reactivity, no plasticizing effect, hydrophobic . Widely used in the flame retardant modification of nylon 66, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C23/46C07C17/30
Inventor 陈灿银宋静德许军单江
Owner JIANGSU ANPON ELECTROCHEM
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