Method for continuously synthesizing 1, 5, 9-cyclododecatriene

A cyclododecatriene and butadiene technology, applied in chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of time-consuming, efficiency, low yield, reaction fluctuation, etc. High yield and purity, shortened reaction time, and reduced polymerization by-products

Inactive Publication Date: 2013-12-04
李翔
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the efficiency and yield are low, and it is not suitable for industrialized implementation
At the same time, the concentration change of the catalyst also has an adverse effect on the selectivity of the reaction, thereby affecting the yield and quality of the product.
[0010] In addition, after one unit operation of the batch reaction is completed, a series of complex operations such as equipment replacement and catalyst addition take a lot of time
More importantly, batch reaction is an unstable operation, which is not conducive to the implementation of industrial automation control, so it will inevitably bring about fluctuations in reaction and instability in product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Example 1: In a four-stage stirring cascade reaction system, each reactor has a volume of 20 liters, and the cyclo-oligomerization reaction of 1,3-butadiene is carried out. The reaction temperature is kept at 60-63° C. through jacket cooling, and the reactor pressure is adjusted to 0.01-0.12 mpa. The relevant parameters of the four-stage reactor are;

[0074] The pressure relationship of the cascade reaction is: P 1 2 3 4 ;

[0075] The catalyst concentration relationship for the cascade reaction is: C 1 >C 2 > C 3 > C 4 ;

[0076] The 1,3-butadiene reaction amount relationship of the cascade reaction is: V 1 > V 2 > V 3 > V 4 ;

[0077] The temperature relationship of the cascade reaction is: T 1 = T 2 = T 3 = T 4 .

[0078] in:

[0079] P—the pressure of each reactor in the cascade reaction;

[0080] C—the concentration of each reactor catalyst in the cascade reaction;

[0081] V—each reactor 1,3-butadiene conversion amount in the cascad...

Embodiment 2

[0097] Embodiment 2: basic and example 1 described process and operating condition, and to the add-on of 1st grade reactor catalyzer doubles, promptly the catalyst system concentration in the system doubles, and repeats the operation like embodiment 1, The reaction was completed in 18 hours.

[0098] The reaction product weight of the whole system: 43kg;

[0099] Catalyst efficiency: 20000g product / g titanium;

[0100] The end reactor reaction product measurement result is:

[0101] 1, 3-butadiene conversion rate: > 99.2%;

[0102] CDT selectivity: > 88.95%;

[0103] Anti, trans, cis-CDT selectivity: > 87.58%;

[0104] C 8 Foreign body selectivity: < 0.82%;

[0105] C 16 Above and polybutadiene selectivity: < 11.1%;

[0106] CDT purity after rectification treatment: ≥ 99.5%.

[0107] The composition of CDT isomers is:

[0108] Anti, trans, cis-CDT: 98.4%;

[0109] Anti, anti, anti-CDT: 1.3%;

[0110] Cis, cis, trans-CDT: 0.3%.

Embodiment 3

[0111] Embodiment 3: basically with the process described in example 1 and increase 1.5 times to the add-on of first-stage reactor catalyst, promptly the catalyst system concentration in the system increases 1.5 times, and repeat the operation like embodiment 1, reaction finishes in 18 hours .

[0112] The reaction product weight of the whole system: 44kg;

[0113] Catalyst efficiency: 20000g product / g titanium;

[0114] The end reactor reaction product measurement result is:

[0115] Conversion rate of 1,3-butadiene: > 99%;

[0116] CDT selectivity: > 88.42%;

[0117]Anti, trans, cis-CDT selectivity: > 87.1%;

[0118] C 8 Foreign body selectivity: < 1.2%;

[0119] C 16 Above and polybutadiene selectivity: < 11.9%;

[0120] CDT purity after rectification treatment: ≥ 99.5%.

[0121] The composition of CDT isomers is:

[0122] Anti, trans, cis-CDT: 98.3%;

[0123] Anti, anti, anti-CDT: 1.3%;

[0124] Cis, cis, trans-CDT: 0.3%.

[0125] 1,5,9-Cyclododecatriene has t...

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PUM

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Abstract

The invention provides a method for continuously synthesizing 1, 5, 9-cyclododecatriene. The method is completed through the processes of preparation of a homogeneous phase complex catalyst system, cascade reaction, catalyst deactivation processing, refining processing of a reaction product and follow-up processing of the reaction product. According to the method, 1, 3-butadiene can continuously react in a cascade reaction system and can be smoothly and efficiently converted into the 1, 5, 9-cyclododecatriene in an energy-saving manner, especially an effect of converting the 1, 3-butadiene into trans, trans, cis-1, 5, 9-cyclododecatriene isomers in a high-selectivity manner is relatively obvious. According to the method, the reaction time is shortened, the reaction cost is reduced, and the process efficiency is improved.

Description

technical field [0001] The invention relates to polyolefin production technology in the field of chemical industry. The present invention continuously synthesizes 1,5,9-cyclododecane in the form of cascade reaction under the conditions of Ziegler-Natta type catalytic system to continuously cyclize and oligomerize 1,3-butadiene. Triene method. Background technique [0002] 1,5,9-Cyclododecatriene, code-named CDT, can be used for the preparation of polyester, polyamide and plasticizers, as well as for the production of polyamide synthetic fibers, cold-resistant plasticizers, artificial rubber, flavoring agents, environmental Oxygen resin crosslinking agent, spices, fire-resistant additives, etc., is an important industrial raw material. [0003] At present, some patents and documents in this field have disclosed some methods and tests for preparing CDT using 1,3-butadiene as a raw material. [0004] For example, FR-A1393071 describes a method for preparing CDT using a compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/277C07C2/46B01J31/22
Inventor 李翔李明泉于桂华邹鹏博姜德龙
Owner 李翔
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