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Preparation method of high-purity ethylidene norbornene (ENB)

A high-purity ethylidene norbornene technology, which is applied in the direction of depolymerization to hydrocarbons, isomerization to hydrocarbons, and organic chemistry. VNB dimerization mode and process control, and the use of by-products are not mentioned, so as to improve the comprehensive utilization rate, overcome a large number of losses, and reduce the cost.

Active Publication Date: 2014-01-01
HENGHE MATERIALS & SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method does not describe the dimerization mode and process control of VNB in ​​detail.
[0012] The preparation methods of ethylene norbornene and its intermediates disclosed in the above-mentioned patents did not describe in detail the dimerization method of VNB and the refining method of ENB in ​​the whole preparation process of ethylene norbornene, nor mentioned the rest of the production process. By-product utilization

Method used

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  • Preparation method of high-purity ethylidene norbornene (ENB)
  • Preparation method of high-purity ethylidene norbornene (ENB)
  • Preparation method of high-purity ethylidene norbornene (ENB)

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Experimental program
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Effect test

Embodiment 1

[0058] The distillate of cracked C9 bicyclic section enters the depolymerization kettle R1, the depolymerization temperature is 220°C, the system operating pressure is 0.08MPa (G), and the residence time is 1.5h; the generated F2 material enters the CPD refining tower T1, and the top of the refining tower 40°C, the temperature of the tower kettle is 140°C, the system pressure is 0.05MPa(G), and the reflux ratio is 2. The high-purity CPD obtained at the top of the tower is mixed with isooctane at a mass ratio of 1:1, and the mixed The material and BD are mixed according to the mass ratio of 2:1, and then 1000ppm of polymerization inhibitor is added, and enter the dimerization reactor, and the temperature is controlled by the intercooler E2 at 130°C, and the temperature is kept at 3MPa (G) for 200min to form a reaction mixture from dimerization The bottom discharge of reactor R5. The obtained mixture enters the rectification tower T2 after being cooled by the cooler E3. The oper...

Embodiment 2

[0063] The distillate of cracked C9 bicyclic section enters the depolymerization kettle R1, the depolymerization temperature is 220°C, the system operating pressure is 0.08MPa (G), and the residence time is 1.5h; the generated F2 material enters the CPD refining tower T1, and the top of the refining tower 40°C, the temperature of the tower kettle is 140°C, the system pressure is 0.05MPa(G), and the reflux ratio is 2. The high-purity CPD obtained at the top of the tower is mixed with isooctane at a mass ratio of 2:1, and the mixed The material and BD are mixed according to the mass ratio of 3:2. After adding 1000ppm of polymerization inhibitor, it enters the dimerization reactor, and the temperature is controlled by the intercooler E2 at 130°C, and the temperature is kept at 3MPa (G) for 200min to form a reaction mixture from dimerization The bottom discharge of reactor R5. The obtained mixture enters the rectification tower T2 after being cooled by the cooler E3. The operating...

Embodiment 3

[0066]The distillate of cracked C9 bicyclic section enters the depolymerization kettle R1, the depolymerization temperature is 220°C, the system operating pressure is 0.08MPa (G), and the residence time is 1.5h; the generated F2 material enters the CPD refining tower T1, and the top of the refining tower 40°C, the temperature of the tower kettle is 140°C, the system pressure is 0.05MPa(G), and the reflux ratio is 2. The high-purity CPD obtained at the top of the tower is mixed with isooctane at a mass ratio of 1:1, and the mixed The material is mixed with BD according to the mass ratio of 2:1, after adding 1500ppm of polymerization inhibitor, it enters the dimerization reactor, and the temperature is controlled by the intercooler E2 at 130°C, and the temperature is kept at 3MPa (G) for 200min to form a reaction mixture from dimerization The bottom discharge of reactor R5. The obtained mixture enters the rectification tower T2 after being cooled by the cooler E3. The operating ...

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Abstract

The invention relates to a preparation method of high-purity ethylidene norbornene (ENB), which comprises the following steps: 1) preparing cyclopentadiene (CPD) from cracked C9 bicyclic section distillate; 2) reacting the CPD and 1,3-butadiene (BD) in a non-dead-volume cascade tubular reactor to generate 5-vinyl-2-norbornene (VNB); 3) separating the crude VNB to obtain refined VNB, collecting the unreacted BD, CPD and circulating solvent, and returning to the front of the tubular reactor, thereby forming a circulating loop; and 4) dehydrating the refined VNB obtained in the step 3), carrying out isomerization reaction to obtain crude ENB, and removing light and heavy components from the crude ENB by a refining tower to obtain the high-purity ENB. The method has the advantages of simple and reliable process route and low facility request, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of ethylidene norbornene preparation, in particular to a preparation method of high-purity ethylidene norbornene. Background technique [0002] Ethylidene norbornene can be copolymerized with ethylene and propylene to produce ethylene-propylene rubber. As the third monomer of ethylene-propylene rubber, it not only endows ethylene-propylene rubber with vulcanizability, but also has high reactivity, fast vulcanization speed, and small secondary reaction. . The obtained ethylene-propylene rubber also has properties such as discharge resistance, water vapor resistance, ozone resistance, and chemical resistance (solvent, acid, alkali, etc.), and can be used for building materials such as rubber products around the engine, waterproof boards, and impact-resistant plastics. modified material. Due to the above-mentioned advantages of ethylidene norbornene as the third monomer of ethylene-propylene rubber, the selection rate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/43C07C5/25C07C13/15C07C4/22C08F240/00
Inventor 李来福孙向东王斌彭振博李爱元
Owner HENGHE MATERIALS & SCI TECH CO LTD
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