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Post-treatment method of cyclododecatriene reaction liquid

A cyclododecatriene and reaction liquid technology, applied in chemical instruments and methods, purification/separation of hydrocarbons and hydrocarbons, etc., can solve the complex quenching process, low quenching efficiency and unstable operation of the separation system and other problems, to achieve the effect of saving the reaction process, good stability and stable composition

Active Publication Date: 2021-03-19
WANHUA CHEM GRP
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AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a post-treatment method for cyclododecatriene reaction liquid, which adopts the compounding method of mercaptan quenching agent and basic quenching auxiliary agent to solve the problem of low quenching efficiency in the quenching process. The quenching process is complex and the separation system is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 1g of ammonia gas in 5g of ethanethiol, mix and stir until a uniform state is prepared to obtain a quencher, take 0.6g of quencher and add it to 1000g of unquenched CDT reaction solution, stir evenly to obtain a reaction solution mixture, control the reaction solution The reaction temperature of the mixture is 50°C, and it is aged for 0.5h to obtain the quenched CDT reaction solution. The quenching effect evaluation experiment is further carried out. The quenched reaction solution is heated to 150°C and kept for 24h. The loss rate of CDT is obtained by gas phase detection. was 0.22%.

Embodiment 2

[0032]Dissolve 10g of sodium ethoxide in 10g of ethanethiol, mix and stir until a uniform state is prepared to obtain a quencher, take 2g of quencher and add it to 1000g of unquenched CDT reaction solution, stir evenly to obtain a reaction solution mixture, control the reaction solution mixture The reaction temperature is 60°C, and the aging time is 0.7h, and the quenched CDT reaction solution is obtained. The quenching effect evaluation experiment is further carried out. The quenched reaction solution is heated to 150°C and kept for 24h. The loss rate of CDT obtained by gas phase detection is 0.21%.

Embodiment 3

[0034] Dissolve 5g of sodium ethoxide in 8g of ethanedithiol, mix and stir until a uniform state is prepared to obtain a quencher, take 1.3g of quencher and add it to 1000g of unquenched CDT reaction solution, stir evenly to obtain a reaction solution mixture, and control the reaction The reaction temperature of the liquid mixture is 70°C, and it is aged for 0.8h to obtain the quenched CDT reaction liquid. The quenching effect evaluation experiment is further carried out. The quenched reaction liquid is heated to 150°C and kept for 24h. The loss of CDT is obtained by gas phase detection. The rate is 0.12%.

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Abstract

The invention relates to a post-treatment method of a cyclododecatriene reaction liquid. The method comprises the following steps: mixing a mercaptan compound with an alkaline assistant to obtain a quenching agent, mixing and quenching the quenching agent with a CDT reaction solution, and finally performing separating and recovering. After-treatment is carried out in a quenching mode, the productstability is good, the phenomenon of impurity increase is avoided, and stable and continuous operation can be realized.

Description

technical field [0001] The invention relates to the field of reaction liquid post-treatment technology, in particular to a post-treatment method of a reaction liquid containing cyclododecatriene and an active catalyst. Background technique [0002] Cyclododecatriene, English name cyclododecatriene, referred to as CDT, is an important source of raw materials for orthodox dodecane compounds, which can be used in long-chain nylon (especially nylon 12, nylon 612), flame retardants and spices and other fields. [0003] CDT is obtained by using butadiene as a raw material and performing a polymerization reaction under the action of a homogeneous Ziegler-Natta catalyst (Ziegler-Nattacatalyst). This catalytic process has been proved to be a butadiene cyclopolymerization process catalyzed by Ti active compounds. The related research is in Titanium-catalyzed cyclotrimerization of butadiene Part III. Et x AlCl 3-x (x = 1-2) systems, Journal of Molecular catalysis, 1991 (70), 9-28 and ...

Claims

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Application Information

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IPC IPC(8): C07C7/152C07C13/277
CPCC07C7/152C07C2601/20C07C13/277
Inventor 付松王静陈雁玲黎源李俊平冯民昌崔纯燹李源明董洋
Owner WANHUA CHEM GRP
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