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Pretreatment method of reaction system for directly preparing olefin from synthesis gas

A reaction system and pretreatment technology, applied in chemical instruments and methods, hydrocarbon production from carbon oxides, hydrocarbons, etc., can solve the problems of low olefin selectivity and high operating cost of industrial devices

Pending Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problems in the prior art that the side reaction of methanation of syngas leads to low selectivity of olefins in the reaction of syngas to olefins and the high operating cost of industrial devices, the present invention provides a pretreatment method for the reaction system of direct synthesis gas to olefins , the method is simple and easy to operate in industrial applications, can effectively passivate the metal wall of the reactor, avoid the methanation side reaction of the syngas, and reduce the operating cost of the device. Purging enhances the economical operation of the device. In addition, it does not affect the subsequent products and does not require additional cumbersome steps such as product separation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a set of catalyst-filled synthesis gas direct-to-light olefin reactors (14Cr1MoR material), the method of the present invention is used to carry out in-situ presulfurization and passivation of the reaction system:

[0027] First, load the catalyst in the reactor according to the conventional method, the catalyst is AlPO with a mass ratio of 1.1:1 4 -18 and ZnCr 1.25 al 0.15 .

[0028] After loading the catalyst, the synthesis gas to olefins reaction system is purged with nitrogen with a volume purity greater than 99.5% until the oxygen content in the gas is less than 1.0%. Stop feeding nitrogen, feed synthesis gas with hydrogen / carbon monoxide volume ratio of 2 as reducing gas, and space velocity is 3000h -1 , to 300°C at a rate of 10°C / h. Continue to feed synthesis gas as a reducing gas, and start to inject dimethyl disulfide into the reactor to mix into a reducing gas containing sulfide, wherein the content of dimethyl disulfide is 120ppm in terms of sulfur, an...

Embodiment 2

[0031] Reactor and the catalyst of packing are the same as embodiment 1.

[0032] After loading the catalyst, the synthesis gas to olefins reaction system is purged with nitrogen with a volume purity greater than 99.5% until the oxygen content in the gas is less than 1.0%. Stop feeding nitrogen. Feed synthesis gas with hydrogen / carbon monoxide volume ratio of 2 as reducing gas, and the space velocity is 2000h -1 , the temperature was raised to 250°C at a rate of 15°C / h. Continue to feed synthesis gas as a reducing gas, and start injecting dimethyl disulfide into the reactor to mix into a reducing gas containing sulfide, wherein the content of dimethyl disulfide is 150ppm in terms of sulfur, and continue to heat up . When the temperature of the reactor reaches 410° C., the injection of dimethyl disulfide is stopped after three hours of constant temperature, and the pretreatment is completed.

[0033] Continue to feed synthesis gas as raw material, start gas circulation, the...

Embodiment 3

[0035] In a set of catalyst-filled synthetic gas direct-to-light olefin reactors (1Cr18Ni9Ti stainless steel), the method of the present invention is used to carry out in-situ presulfidation passivation to the reaction system;

[0036] First, load the catalyst in the reactor according to the conventional method, the catalyst is AlPO with a mass ratio of 1:1.2 4 -34 and ZnCr 1.1 .

[0037] After loading the catalyst, the synthesis gas to olefins reaction system is purged with nitrogen with a volume purity greater than 99.5% until the oxygen content in the gas is less than 1.0%. Stop feeding nitrogen. Feed synthesis gas with hydrogen / carbon monoxide volume ratio of 1.5 as reducing gas, and the space velocity is 1500h -1 , to 200°C at a rate of 5°C / h. Continue to feed synthesis gas as reducing gas, and start to inject carbon disulfide into the reactor to mix into reducing gas containing sulfide, wherein the content of carbon disulfide is 60ppm in terms of sulfur, and continue...

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Abstract

The invention provides a pretreatment method of a reaction system for directly preparing olefin from synthesis gas. The method comprises the following steps: introducing inert gas into a reactor filled with a catalyst for purging, introducing reducing gas instead of the inert gas, raising the temperature to 200-480 DEG C, introducing the reducing gas containing sulfide into the system at the temperature, and finishing pretreatment after 1-40 hours. The method can effectively passivate the metal wall of a reaction device, inhibit methanation side reaction of raw materials under high-temperature and high-pressure conditions, and improve the operation benefits of the device.

Description

technical field [0001] The invention relates to a pretreatment method before synthesis gas reaction, in particular to a pretreatment method for a synthesis gas direct-to-olefins reaction system. Background technique [0002] In recent years, China's coal chemical industry has developed rapidly, and coal-to-olefin technology has risen rapidly as one of the important routes. Dalian Institute of Chemical Physics took the lead in successfully completing the industrialization experiment of methanol from coal through syngas in 2006. As of 2018, its DMTO technology has achieved the technical implementation license of 13.13 million tons of olefins per year, and has put into production 6.46 million tons of olefins per year. In 2010, the SMTO technology of Sinopec Shanghai Research Institute was successfully put into operation in Zhongyuan Petrochemical's 200,000-ton olefin / year industrial plant. At present, Sinopec uses its own SMTO technology to plan and deploy at least 5 coal-to-ol...

Claims

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Application Information

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IPC IPC(8): C07C11/04C07C11/06C07C1/04
CPCC07C1/04C07C1/047C07C2527/188C07C11/04C07C11/06
Inventor 周海波苏俊杰刘苏王仰东焦文千刘畅张琳
Owner CHINA PETROLEUM & CHEM CORP