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A kind of preparation method of environment-friendly, high-efficiency vulcanization crosslinking agent 1,6-bis(n,n-dibenzylcarbamoyldithio)hexane

A technology of dibenzylcarbamoyl disulfide and dibenzylcarbamoyl, which is applied in the field of synthesis of rubber additives, can solve the problems of difficult metathesis reaction, unpleasant and toxic smell, slow reaction speed, etc., and achieve high purity, The effect of high yield and easy reaction

Active Publication Date: 2017-06-30
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wherein Germany contains formaldehyde, toluene and weak alkaline environment as reaction conditions, with water as solvent, synthetic product, but this preparation method has following shortcoming: 1. can produce a large amount of waste water containing formaldehyde, containing a small amount of toluene, and difficult It smells toxic and is difficult to handle; 2. The reaction speed is slow and the reaction time required is long
In addition, in China, dioxane, dichloromethane, and toluene are used as solvents to synthesize products, but the preparation method has the following disadvantages: the two raw materials are salts that are difficult to dissolve in organic solvents, and in the heterogeneous phase system, so this metathesis reaction is difficult to carry out, and the required reaction time is too long

Method used

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  • A kind of preparation method of environment-friendly, high-efficiency vulcanization crosslinking agent 1,6-bis(n,n-dibenzylcarbamoyldithio)hexane
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Examples

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Effect test

Embodiment 1

[0028] A kind of preparation method of environment-friendly, efficient vulcanization cross-linking agent 1,6-bis(N,N-dibenzylcarbamoyldithio)hexane, the steps are as follows:

[0029] (1) Put 39.4g of dibenzylamine, 8.4g of sodium hydroxide and 190g of ethanol into a 1000mL three-neck flask, stir at 20°C for 20min, weigh 16g of carbon disulfide in a constant pressure dropping funnel, and add carbon disulfide dropwise to the flask within 30min. In the three-necked flask, stirring was continued at 20°C for 3 hours, and an ethanol solution containing sodium dibenzyl dithiocarbamate was obtained after the reaction was completed.

[0030] (2) Weigh 14.7g of 1,6-dichlorohexane and 0.2g of KI into the flask, connect the condenser, heat up the system to reflux with a heating mantle, stir for 4 hours under reflux, and cool down to room temperature after the reaction , suction filtration to obtain a white filter cake, put the filter cake into a 500mL beaker, add about 150g of water, sti...

Embodiment 2

[0033] A kind of preparation method of environment-friendly, high-efficiency vulcanization cross-linking agent 1,6-bis(N,N-dibenzylcarbamoyldithio)hexane, the same as Example 1, the difference is:

[0034] Step (1) The reaction temperature is 30° C. to obtain an ethanol solution containing sodium dibenzyl dithiocarbamate.

[0035] Step (2) The filter cake was dried to obtain 60.5 g of white solid 1,6-bis(N,N-dibenzylcarbamoyl-thio)hexane with a total yield of 91%.

[0036] Step (3) obtains 27.4 g of 1,6-di(N,N-dibenzylcarbamoyldithio)hexane product with a content of 97%, and the yield is 94%. The melting point of the final product is 90° C., and the ash content (750°C / 2h) is 0.1%.

Embodiment 3

[0038] A kind of preparation method of environment-friendly, high-efficiency vulcanization cross-linking agent 1,6-bis(N,N-dibenzylcarbamoyldithio)hexane, the same as Example 1, the difference is:

[0039] Step (1) The reaction temperature is 10° C. to obtain an ethanol solution containing sodium dibenzyl dithiocarbamate.

[0040] Step (2) The filter cake was dried to obtain 60 g of white solid 1,6-bis(N,N-dibenzylcarbamoyl-thio)hexane with a total yield of 90.2%.

[0041] Step (3) obtains 27.5 g of 1,6-di(N,N-dibenzylcarbamoyldithio)hexane product with a content of 97%, and the yield is 94.3%. The melting point of the final product is 90° C., and the ash content (750°C / 2h) is 0.1%.

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Abstract

The invention relates to a preparation method of an environment-friendly and efficient sulfurization crosslinking agent 1,6-bis(N,N-dibenzyl carbamyl disulfide) hexane. The preparation method comprises steps as follows: sodium dibenzyldithiocarbamate is synthesized firstly and then reacts with 1,6-dichlorohexane, 1,6-bis(N,N-dibenzyl carbamyl sulfide) hexane is generated, the composition reacts with sulfur, and a product, namely, 1,6-bis(N,N-dibenzyl carbamyl disulfide) hexane is generated. The prepared product contains little inorganic salt and has high purity; the preparation method is simple, practicable and environment-friendly, little waste water is produced in the preparation process, and environmental pollution is reduced.

Description

technical field [0001] The invention relates to a preparation method of 1,6-bis(N,N-dibenzylcarbamoyldisulfide)hexane, an environment-friendly and highly efficient vulcanization crosslinking agent, and belongs to the field of synthetic technology of rubber additives. Background technique [0002] Natural rubber will undergo vulcanization reversion during high temperature or long-term vulcanization. Reversion will reduce the crosslinking density of the vulcanized rubber, thereby reducing the mechanical properties and dynamic properties of the vulcanized rubber. 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane is a new type of high-efficiency composite crosslinking agent, which not only has the function of vulcanization accelerator, but also has the effect of anti-reversion. The cross-links formed by it have the stability of monosulfide bonds and disulfide bonds, and at the same time have the flexibility similar to polysulfide cross-links. During the vulcanization process, a sta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/20C07C333/24
CPCC07C333/16C07C333/20C07C333/24
Inventor 张琳李剑波张朋龙崔亭亭
Owner SHANDONG YANGGU HUATAI CHEM
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