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Preparation method of chlorinated paraffin

A technology for chlorinated paraffin and paraffin, which is applied in the field of preparation of chlorinated paraffin, and can solve the problems of high toxicity to aquatic organisms, restricting the use of short-chain chlorinated paraffin, and the like

Inactive Publication Date: 2014-01-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recent studies have found that short-chain chlorinated paraffins are highly toxic to aquatic organisms, and have environmental persistence and bioaccumulation (Environment.Sci.Technol.2008, 42, 1045; Clean-Soil Air Water 2010, 38, 57), Stockholm The Convention proposes to restrict the use of short-chain chlorinated paraffins

Method used

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  • Preparation method of chlorinated paraffin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Preparation of chlorinated paraffin-52 by thermal chlorination method

[0018] The solid paraffin was heated to 55°C and melted into liquid and then pumped into three 600ml tubular chlorination reaction flasks. Each chlorination reaction flask added 250 grams of paraffin wax. Connect the reaction device according to the reaction process. Place 3 chlorination reaction flasks in a 75°C water bath, and pass chlorine gas (70-80mL / min) for chlorination reaction. After the reaction is initiated within 15 minutes, the chlorine flow rate is adjusted to 160-200 mL / min for reaction. During the reaction process, take the reaction solution by weighing and measuring the density (density≥1.25g / mL) to judge the degree of chlorination. When the chlorination reaction proceeded for 47 hours, the chlorination degree reached 52%, and the introduction of chlorine gas was stopped. After the temperature was lowered to room temperature, nitrogen gas was introduced to blow out the re...

Embodiment 2

[0019] Example 2: Preparation of chlorinated paraffin-52 by thermal chlorination method

[0020] The reaction steps are the same as in Example 1, and the difference from Example 1 is that the reaction temperature is 60°C. The reaction time was 48 hours, the specific gravity of the reaction liquid sample did not reach 1.25g / mL, and the degree of chlorination did not reach the 52% standard. The chlorination reaction is slower at 60°C.

Embodiment 3

[0021] Example 3: Preparation of chlorinated paraffin-52 by thermal chlorination method

[0022] The reaction steps are the same as in Example 1, and the difference from Example 1 is that the reaction temperature is 85°C. After 47 hours of chlorination, the specific gravity of the reaction solution sample reached 1.25g / mL, and the degree of chlorination reached 52%. There is no significant difference between 85°C and 75°C reaction.

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Abstract

The invention provides a preparation method of chlorinated paraffin. Paraffin and liquid chlorine are used as raw materials and an azoic compound is used as a catalyst to prepare the chlorinated paraffin through catalytic chlorination. Compared with the current thermal chlorination method, the preparation method has the advantages that the reaction rate is obviously improved and the production cycle is shortened; the long-chain paraffin alkane does not have obvious carbon chain crack phenomenon in the chlorination process; the content of the short-chain chlorinated paraffin in the product can be well controlled by adopting the preparation method provided by the invention. The method is simple in process, easy to operate, and suitable for industrialized production of the chlorinated paraffin.

Description

Technical field [0001] The invention relates to a preparation method of chlorinated paraffin. In the tubular reactor, by adding a free radical initiator, a chlorinated paraffin product with low short-chain chlorinated paraffin content is efficiently prepared. The method has simple process, high efficiency and meets environmental protection requirements. technical background [0002] Chlorinated paraffins are a group of synthetic chlorinated alkane derivatives, mainly used as flame retardants for textiles, rubber and plastics, leather treatment agents, plasticizers for paints and other coatings, and oil additives for metal processing. my country is the country with the largest production of chlorinated paraffins in the world, and there is also a large demand. The industrial production of chlorinated paraffin is also one of the main means to balance the chlorine production in the chlor-alkali industry. Chlorinated paraffins are divided into many types of products according to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G73/38
Inventor 余正坤赫巍
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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