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A method for continuous production of cyclododecatriene

A technology for cyclododecatriene and butadiene, which is applied in the field of continuous production of cyclododecatriene, can solve the problems of long residence time, low catalytic efficiency, unreasonable quenching process, etc. Stable operation and avoid catalyst deactivation effect

Active Publication Date: 2022-02-18
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to provide a method for continuous production of cyclododecatriene, which uses an organometallic compound to be mixed with raw material butadiene in advance to achieve the purpose of eliminating active hydrogen impurities in the raw material of butadiene. It is added to the aging reaction, and the aging reaction solution is quenched by polyene polyamine compound, which solves the problems of low catalytic efficiency, long residence time, unreasonable quenching process, etc.

Method used

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  • A method for continuous production of cyclododecatriene
  • A method for continuous production of cyclododecatriene
  • A method for continuous production of cyclododecatriene

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Experimental program
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Effect test

Embodiment 1

[0070] Step 1, Catalyst Preparation: Catalyst Preparation Reactor A is a three-pot reactor in series, and the catalyst raw material is fed from the first pot. The composition is shown in Table 1.

[0071] Table 1. Catalyst feed amount

[0072]

[0073] Control the liquid level to ensure the residence time The jacket controls the temperature at 30°C and the residence time is 10min.

[0074] Step 2, butadiene impurity removal: add butadiene: 300kg / h and trimethylaluminum: 30g / h to impurity removal stirred tank B, mixing temperature 15°C, control residence time 2min, discharge into polymerization reaction kettle C.

[0075] Step 3, reaction: The catalyst solution obtained in step 1 and the butadiene stream after removal of impurities obtained in step 2 enter the polymerization reactor C at a total rate of 485.6 kg / h, the reaction temperature is 100° C., and the residence time is 100 min.

[0076] Step 4, aging: the reaction solution 4 is discharged from the reactor into the ...

Embodiment 2

[0092] Step 1, Catalyst preparation: Catalyst preparation reactor A is a three-pot reactor in series, and the catalyst raw material is fed from the first pot. The composition is shown in Table 4.

[0093] Table 4. Catalyst feed amount

[0094]

[0095] Control the liquid level to ensure the residence time The jacket controls the temperature at 60°C and the residence time is 5min.

[0096] Step 2, butadiene impurity removal: add butadiene 202kg / h and trimethylaluminum 4g / h to the impurity removal stirring reactor B, mix at 0°C, control the residence time for 5min, and discharge the material into the polymerization reactor c.

[0097] Step 3, reaction: the catalyst solution obtained in step 1 and the butadiene stream 12 after removal of impurities obtained in step 2 enter a three-pot series polymerization reactor at a total rate of 388 kg / h, with a reaction temperature of 90° C. and a residence time of 200 min.

[0098] Step 4, aging: the reaction liquid 4 is discharged fro...

Embodiment 3

[0105] Step 1, Catalyst preparation: Catalyst preparation reactor A is a three-pot reactor in series, and the catalyst raw material is fed from the first pot. The composition is shown in Table 6.

[0106] Table 6. Catalyst feed amount of embodiment 3

[0107]

[0108] Control the liquid level to ensure the residence time The jacket controls the temperature at 20°C and the residence time is 60min.

[0109] Step 2, butadiene impurity removal: add butadiene 252kg / h and triisobutylaluminum 10g / h to the impurity removal stirring impurity removal kettle B, the mixing temperature is 10°C, the residence time is controlled for 1min, and the material is discharged into the polymerization Reactor C.

[0110] Step 3, reaction: a total of 439 kg / h of the catalyst solution obtained in step 1 and the butadiene obtained in step 2 entered the three-pot series polymerization reactor C with a reaction temperature of 150° C. and a residence time of 30 min.

[0111] Step 4, Aging: The reactio...

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Abstract

The present invention relates to a method for the continuous production of cyclododecatriene. Including: (1) butadiene is mixed with an organometallic compound to obtain a butadiene-containing material stream, and under the action of a catalyst solution, the butadiene-containing material stream undergoes butadiene cyclotrimerization in a polymerization reactor reaction to obtain a reaction solution containing cyclododecatriene; (2) the reaction solution containing cyclododecatriene enters the aging reactor with another part of the catalyst solution to react; (3) the reaction solution obtained by the aging reactor Enter the quenching reactor, use polyene polyamines as quenching agents to quench the reaction, and obtain the quenched reaction solution containing cyclododecatriene. The present invention firstly pretreats butadiene, so that the polymerization reaction process is not affected by the impurities brought in by the raw materials, and the catalyst efficiency is increased; at the same time, the catalyst quenching agent is used to quench the reaction, which simplifies the post-treatment process and improves the production efficiency. efficiency.

Description

technical field [0001] The invention relates to a method for continuously producing cyclododecatriene, which belongs to the field of organic chemical preparation. Background technique [0002] Cyclododecatriene, English name cyclododecatriene, referred to as CDT, is an important source of raw materials for ortho-12-carbon compounds. Its downstream applications include long-chain nylon (especially nylon 12 and nylon 612), flame retardants, and spices. [0003] CDT is obtained by using butadiene as a raw material and reacting 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(II) active compounds. complexes in TiCl 4 -Et x AlCl 3-x (x=1-2) systems, Journal of Molecular catalysis, 1991(70), 9-28 and Studies of the cyclotrimerization of butadiene and butyne-2 in the presence of catalytic systems containing titanium(II) arene complexes, Journal o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/46C07C7/00C07C7/04C07C7/148C07C13/277C07C7/173C07C11/167
Inventor 张彦雨陈海波边新建黎源吴训锟黎晓峰张文立王文
Owner WANHUA CHEM GRP CO LTD
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