Method for high-value resource utilization of isobutene with low polymerization degree

A low-polymerization technology of isobutylene, which is applied in the field of converting low-polymerization isobutylene into multi-carbon mercaptans, achieves the effects of wide sources, environmental protection prices, and few by-products

Inactive Publication Date: 2021-06-25
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, synthesizing a certain amount of isobutylene with a low degree of polymerization into a series of carbon mercaptan products that are urgently needed in my country and have high added value will become a very promising way for high-value resource utilization of butene with a low degree of polymerization. There is no relevant report yet.

Method used

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  • Method for high-value resource utilization of isobutene with low polymerization degree
  • Method for high-value resource utilization of isobutene with low polymerization degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 316 stainless steel reactor with an inner diameter of 16mm and a length of 354mm, 30mL of dry Amberlyst 35 resin was loaded, and the catalyst was treated in situ under nitrogen, room pressure, and 110°C overnight; hydrogen sulfide was passed through a mass flow meter at 60mL / min Controlled feed into the reactor, triisobutene is passed into the reactor through a high-efficiency liquid phase pump at 3mL / h, hydrogen sulfide and triisobutene are fully mixed and reacted with Amberlyst35 resin, the reaction pressure is 1.0Mpa, and the reaction temperature is 5°C; After 4 hours, the sampling analysis showed that the conversion rate of triisobutene was 71.01%. The selectivity of tert-butyl mercaptan in the product was 12.8%, the selectivity of tert-octyl mercaptan was 21.6%, and the selectivity of tert-dodecyl mercaptan was 65.6%. Other thiols are generated; the reaction product chromatographic analysis spectrum is shown in figure 1 .

Embodiment 2

[0031] The reactor parameters were the same as those in Example 1, and the catalyst was also 30 mL of dry Amberlyst35 resin. The catalyst was treated in situ under nitrogen, room pressure, and 110° C. overnight, and hydrogen sulfide was controlled to flow into the reactor at 60 mL / min through a mass flow meter. Isobutene was fed into the reactor through a high-efficiency liquid phase pump at 12mL / h. After the hydrogen sulfide and triisobutene were fully mixed, they were contacted with Amberlyst35 resin for reaction. The selectivity of tert-butyl mercaptan in the product is 9.01%, the selectivity of tert-octyl mercaptan is 14.78%, the selectivity of tert-dodecyl mercaptan is 76.21%, no other mercaptans are generated, and the online reaction is 200h The catalyst showed no obvious signs of deactivation.

Embodiment 3

[0033] The reactor parameters are the same as those in Example 1. The catalyst is also 30 mL of dry Amberlyst35 resin. The catalyst is treated in situ under nitrogen, room pressure, and 110° C. overnight, and hydrogen sulfide is passed into the reactor at a rate of 65 mL / min through a mass flow meter. Diisobutene is fed into the reactor through a high-efficiency liquid phase pump at 15mL / h. After the hydrogen sulfide and diisobutene are fully mixed, they are contacted with Amberlyst35 resin for reaction. The rate is 93.6%, the selectivity of triisobutene in the product is 8.8%, the selectivity of tert-octyl mercaptan is 88.4%, the selectivity of tert-dodecyl mercaptan is 2.8%, and no other by-products are generated.

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Abstract

.The invention discloses a method for high-value resource utilization of low-polymerization-degree isobutene, which comprises the following steps of: fully mixing the low-polymerization-degree isobutene with hydrogen sulfide, fully contacting with a pretreated catalyst, reacting at the pressure of 0.2-1.5 Mpa and the temperature of 5-200 DEG C, condensing after the reaction is finished, carrying out gas-liquid separation, and rectifying and separating liquid to obtain a mercaptan product. The gas returns to the reaction for recycling or is absorbed by alkali liquor and absolute ethyl alcohol solution; According to the method, the problems that in the prior art, low-polymerization-degree isobutene downstream products are few in variety and difficult to realize high-value resource utilization and products in the mercaptan market in China are in shortage are effectively solved, and the low-polymerization-degree isobutene can be converted into corresponding series of mercaptan products such as tert-butyl mercaptan, tert-octyl mercaptan and tert-dodecyl mercaptan in one step. The method has the advantages of good catalyst stability and good economic benefits and social benefits.

Description

technical field [0001] The invention relates to a process and method for converting isobutene with a low degree of polymerization into multi-carbon mercaptans. Background technique [0002] Isobutene with a low degree of polymerization is mainly diisobutene, triisobutene and tetraisobutene. For isobutene, it is currently mainly used to produce methyl tert-butyl ether (MTBE) with low added value. Due to the promotion of ethanol gasoline, MTBE will not be able to adjust If gasoline is used, its production capacity will be greatly reduced, and the rational utilization of isobutene as a raw material for MTBE will become a new problem. However, there are few downstream products of diisobutene, triisobutene and tetraisobutene. At present, with the development of isobutene polymerization technology and other chemical separation technologies, the output of isobutene with low polymerization degree in my country has been greatly increased, and some of them are used as gasoline conditi...

Claims

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Application Information

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IPC IPC(8): C07C319/04C07C321/04
CPCC07C319/04C07C321/04
Inventor 罗永明朱松山陆继长冯斯佑李英豪邓维华方键
Owner KUNMING UNIV OF SCI & TECH
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