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Regeneration method of olefin epoxidation catalyst and application thereof

A catalyst and epoxidation technology, applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of poor strength of Ti-SiO composite oxide, Problems such as high energy consumption and rapid catalyst deactivation in high-temperature roasting achieve the effect of complete regeneration, lower regeneration cost, and simple and easy-to-control process

Active Publication Date: 2018-12-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patents such as CN100398528C, EPA0934116, EPA1371414, and WO-A2005 / 000827 report washing and regenerating catalysts with solvents such as methanol, but the regeneration is not complete, and there is a problem that the regenerated catalyst deactivates faster than the fresh catalyst
If the titanium-silicon molecular sieve catalyst is roasted and regenerated at high temperature with reference to the patent CN103182323B, there will be Ti-SiO 2 The strength of the composite oxide becomes poor, and it will be pulverized during use. At the same time, the energy consumption of high-temperature roasting is also high.

Method used

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  • Regeneration method of olefin epoxidation catalyst and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Take 100g deactivated Ti-SiO 2 The composite oxide catalyst was loaded into the reactor, and the back pressure of the reactor was set to 5MPa, and the high-pressure N 2 Make the system pressure reach 5MPa.

[0050]Configure 6000g of tetrahydrofuran and liquid ammonia mixed solution (tetrahydrofuran 4800g, liquid ammonia 1200g), turn on the high-pressure pump to pump the mixed solution of tetrahydrofuran and liquid ammonia into the reactor, and establish the circulation of the mixed solution of tetrahydrofuran and liquid ammonia; turn on microwave heating to make the system temperature reach 90 °C, cycle washing for 15h.

[0051] Stop the pump to mix the solution, reduce the system pressure to normal pressure, and use N 2 Purge reactor, N 2 The line speed is 1.5m / s, and the purging is 4h.

[0052] The temperature was raised to 120°C by microwave heating, the vacuum pump was turned on, the system pressure was evacuated to 200 Pa and kept for 3 hours, and the regenerat...

Embodiment 2

[0055] Take 100g deactivated Ti-SiO 2 The composite oxide catalyst was loaded into the reactor, and the back pressure of the reactor was set at 7MPa. 2 Make the system pressure reach 7MPa.

[0056] Configure 8000g tetrahydrofuran and liquid ammonia mixed solution (tetrahydrofuran 7000g, liquid ammonia 1000g), turn on the high-pressure pump to pump the mixed solution of tetrahydrofuran and liquid ammonia into the reactor, and establish the circulation of the mixed solution of tetrahydrofuran and liquid ammonia; turn on microwave heating to make the system temperature reach 110 °C, cycle washing for 24h.

[0057] Stop the pump to mix the solution, reduce the system pressure to normal pressure, and use N 2 Purge reactor, N 2 The line speed is 4m / s, and the purge is 3h.

[0058] The temperature was raised to 150°C by microwave heating, the vacuum pump was turned on, the system pressure was evacuated to 500 Pa and kept for 4 hours, and the regeneration of the catalyst was compl...

Embodiment 3

[0061] Take 100g deactivated Ti-SiO 2 The composite oxide catalyst was loaded into the reactor, and the back pressure of the reactor was set to 8MPa, and the high-pressure N 2 Make the system pressure reach 8MPa.

[0062] Configure 9000g of tetrahydrofuran and liquid ammonia mixed solution (tetrahydrofuran 8000g, liquid ammonia 1000g), turn on the high-pressure pump to pump the mixed solution of tetrahydrofuran and liquid ammonia into the reactor, and establish the circulation of the mixed solution of tetrahydrofuran and liquid ammonia; turn on microwave heating to make the system temperature reach 120 ℃, cycle washing for 30h.

[0063] Stop the pump to mix the solution, reduce the system pressure to normal pressure, and use N 2 Purge reactor, N 2 The line speed is 9m / s, and the purging is 5h.

[0064] The temperature was raised to 150°C by microwave heating, the vacuum pump was turned on, the system pressure was evacuated to 900 Pa and kept for 5 hours, and the regenerati...

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Abstract

The invention discloses a regeneration method of an olefin epoxidation catalyst. The regeneration method comprises the following steps: under the conditions of high pressure N2 and microwave heating,pumping a mixed solution of tetrahydrofuran and liquid ammonia into a reactor containing a Ti-SiO2 compound oxide catalyst needing to be regenerated for circulative washing; then blowing the mixed solution of the tetrahydrofuran and the liquid ammonia by using N2, and carrying out vacuum drying to complete the regeneration of the catalyst. When the regenerated catalyst is applied to the chemical process of preparing epoxy propane through propylene epoxidation; all performance indexes of the regenerated catalyst reach the level of a fresh catalyst and the average selectivity of the epoxy propane is greater than 94 percent.

Description

technical field [0001] The invention belongs to the field of catalyst regeneration, and in particular relates to a regeneration method and application of an olefin epoxidation catalyst. Background technique [0002] The ethylbenzene co-oxidation process (PO / SM) using ethylbenzene hydroperoxide (EBHP) as the oxidant and the CHP process using cumene hydroperoxide (CHP) as the oxidant are two important processes for the production of propylene oxide (PO). Process; these two processes overcome the shortcomings of the chlorohydrin method, such as large corrosion and large amount of sewage, and have the advantages of low product cost and less environmental pollution. The catalyst used in these two processes is Ti-SiO 2 Composite oxide, the service life of the catalyst is ≤1 year; the main reason for catalyst deactivation is: macromolecular organic matter covers the active center and blocks the pores. [0003] Patents such as CN100398528C, EPA0934116, EPA1371414, and WO-A2005 / 000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/20B01J21/08B01J38/04B01J38/48B01J38/58B01J38/66C07D303/04C07D301/19
CPCB01J21/08B01J21/20B01J23/002B01J38/04B01J38/48B01J38/58B01J38/66C07D301/19C07D303/04Y02P20/52Y02P20/584
Inventor 王磊王同济叶飞孙康崔娇英初乃波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD