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Method for preparing dicyclopentadiene and dimethylcyclopentadiene

A technology of dimethylcyclopentadiene and dicyclopentadiene, which is applied in chemical instruments and methods, organic chemistry, hydrocarbons, etc., and can solve problems such as low reflux ratio, separation, and multiple theoretical plates in rectification towers. problem, achieve the effect of reducing dimerization reaction, increasing product yield, and avoiding the formation of polymers

Inactive Publication Date: 2012-04-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling points of these C6 and C7 components are relatively close to MCPD, and in order to reduce the occurrence of dimerization, the rectification process is required to operate at a lower reflux ratio, and the rectification column should not use more theoretical plates. MCPD cannot be well separated from C6 and C7 components. Existing methods are difficult to obtain high-purity MCPD, and its purity is usually up to 95wt.%, so it is necessary to use DMCPD and C6 and C7 components after MCPD dimerization Purify the product by rectifying the boiling point difference

Method used

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  • Method for preparing dicyclopentadiene and dimethylcyclopentadiene
  • Method for preparing dicyclopentadiene and dimethylcyclopentadiene
  • Method for preparing dicyclopentadiene and dimethylcyclopentadiene

Examples

Experimental program
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Effect test

Embodiment 1～10

[0024] The technological process of embodiment 1~10 sees attached figure 2 , the raw material C9~C10 fraction W1 first enters the rectification tower 1 for vacuum distillation separation, the theoretical plate number of the rectification tower 1 is 25, the top of the tower is enriched with DCPD material W2, and the bottom of the tower is enriched with DMCPD material W3. The top material W2 of the rectification tower 1 enters the depolymerization rectification tower 2 for depolymerization rectification. The theoretical plate number of the depolymerization rectification tower 2 is 15, and the CPD finished product W4 is obtained at the top of the tower, and the heavy component impurities are regularly discharged from the tower reactor W5. The tower still material W3 of rectification tower 1 enters depolymerization rectification tower 3 to carry out depolymerization rectification, and the theoretical plate number of depolymerization rectification tower 3 is 20, and the CPD finis...

Embodiment 11～16

[0043] Equal amounts of CPD and MCPD obtained in Examples 1 to 10 were mixed respectively to obtain CPD raw materials with a purity of 99.0% and MCPD raw materials with a purity of 98.6%. DCPD and DMCPD were then prepared by thermal dimerization in a batch reactor with an effective volume of 2L using a single-stage reaction batch process. Compared with the multi-stage reaction that is heated step by step, the single-stage reaction requires a longer reaction time, but the process is relatively simple. The raw materials are fed according to 80% of the effective volume of the reactor, and the specific thermal dimerization process operating conditions of each embodiment are shown in Table 6. After the reaction, the product composition was analyzed by gas chromatography, and the thermal dimerization product yield and product composition are shown in Table 7 and Table 8.

[0044] The product yield of DCPD or DMCPD is defined as:

[0045]

[0046] Table 6.

[0047]

[0048] ...

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Abstract

The invention relates to a method for preparing dicyclopentadiene and dimethylcyclopentadiene. The method adopts C9-C19 fractions of byproducts of ethylene cracked from petroleum as raw materials. The method comprises the following processes: 1, the raw materials are subjected to reduced pressure rectification separation in a rectification tower, a concentrated dicyclopentadiene material is obtained from the tower top, and a concentrated dimethylcyclopentadiene material is obtained from the tower bottom; 2, the tower top material obtained in process 1 enters a depolymerization rectification tower for depolymerization rectification, and cyclopentadiene is obtained from the tower top; 3, the tower bottom material obtained in the process 1 enters the depolymerization rectification tower for depolymerization rectification, cyclopentadiene is obtained from the tower top, and methylcyclopentadiene is obtained from the lateral line; 4, cyclopentadiene obtained in process 2 and cyclopentadiene obtained in process 3 undergo a thermal dimerization reaction to obtain dicyclopentadiene; and 5, methylcyclopentadiene obtained in the process 3 undergoes the thermal dimerization reaction to obtain dimethylcyclopentadiene. The method of the invention has the following advantages: dimerization reactions in the depolymerization product rectification separation process are substantially reduced; and high purity methylcyclopentadiene can be directly obtained after the depolymerization product separation, so the refinement and the purification of above depolymerized products are avoided.

Description

technical field [0001] The present invention relates to the preparation method of dicyclopentadiene and dimethyl cyclopentadiene, in particular to the preparation of dicyclopentadiene and dicyclopentadiene through processes such as depolymerization, separation and thermal dimerization of C9-C10 fractions produced by petroleum cracking to produce ethylene. Dimethylcyclopentadiene method. Background technique [0002] When petroleum is cracked to produce ethylene, a considerable amount of raffinate is obtained after the cracking raw material is separated from light fractions below C8, that is, C9-C10 fractions. This fraction mainly contains dicyclopentadiene (DCPD), dimethylcyclopentadiene (DMCPD) and a small amount of dimer of cyclopentadiene and methylcyclopentadiene. The total content of the three is about About 40-65wt%. The depolymerization products cyclopentadiene (CPD) and methylcyclopentadiene (MCPD) of these three dimers have a wide range of uses in the field of che...

Claims

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Application Information

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IPC IPC(8): C07C13/61C07C2/44C07C7/04
Inventor 郭世卓许惠明黄勇孙春水谢家明周飞
Owner CHINA PETROLEUM & CHEM CORP
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