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In-device regeneration method of inactivated titanium silicalite molecular sieve

A titanium-silicon molecular sieve and catalyst technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst regeneration/reactivation, etc., can solve the problem of difficult catalyst regeneration, and achieve the effect of simple operation

Active Publication Date: 2021-08-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the catalytic system of phenol hydroxylation, it is difficult to regenerate the catalyst by simply relying on solvent washing

Method used

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  • In-device regeneration method of inactivated titanium silicalite molecular sieve
  • In-device regeneration method of inactivated titanium silicalite molecular sieve
  • In-device regeneration method of inactivated titanium silicalite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take a three-neck flask and add 200g of 50% ferrous sulfate solution and 20g of pyridine successively, stir at normal temperature and pressure for 3h, evaporate the solvent to dryness, wash and dry to obtain the metal ligand catalyst II. Elemental analysis results: C64.53%, H5.42%, Fe15.00%, N15.05%. The NMR results are as follows: 1 H NMR (600MHz, CDCl3): δ7.36(8H), 8.59(8H), 8.98(4H).

[0036] The loading amount of catalyst TS-1 in the reactor is 100g. At normal temperature and pressure, 20kg of toluene was injected into the reactor at a rate of 1kg / h to wash the deactivated catalyst.

[0037] After mixing 10 g of catalyst II and 10 kg of tert-butyl hydroperoxide solution (concentration 10%), inject it into the reactor at a speed of 500 g / h at 150° C. to decompose the tar on the deactivated catalyst.

[0038] At normal temperature and pressure, 5 kg of toluene was injected into the reactor at a rate of 100 g / h to clean the small molecule products produced by the de...

Embodiment 2

[0041] Take a three-neck flask and add 6000g of 5% manganese sulfate solution and 60g of pyridine in sequence, stir for 3 hours at normal temperature and pressure, evaporate the solvent to dryness, wash and dry to obtain the metal ligand catalyst II. Elemental analysis results: C 64.69%, H 5.43%, Mn 14.79%, N 15.09%. The NMR results are as follows: 1 H NMR (600MHz, CDCl3): δ7.36(8H), 8.59(8H), 8.98(4H).

[0042] The loading amount of catalyst TS-1 in the reactor is 100g. At normal temperature and pressure, 5 kg of DMF was injected into the reactor at a rate of 100 g / h to wash the deactivated catalyst.

[0043] After mixing 50 g of catalyst II and 5 kg of peracetic acid solution (concentration 15%), inject it into the reactor at a speed of 50 g / h at 60° C. to decompose the tar on the deactivated catalyst.

[0044]At normal temperature and pressure, 20kg of tetrahydrofuran was injected into the reactor at a rate of 1000g / h to clean the small molecule products produced by the ...

Embodiment 3

[0047] Take a three-neck flask and add 800g of 20% cobalt nitrate solution and 20g of pyridine in sequence, stir at normal temperature and pressure for 3 hours, evaporate the solvent to dryness, wash and dry to obtain the metal ligand catalyst II. Elemental analysis results: C 64.00%, H 5.37%, Co 15.70%, N 14.93%. The NMR results are as follows: 1 H NMR (600MHz, CDCl3): δ7.36(8H), 8.59(8H), 8.98(4H).

[0048] The loading amount of catalyst TS-1 in the reactor is 100g. At normal temperature and pressure, 10kg of acetone was injected into the reactor at a rate of 400g / h to wash the deactivated catalyst.

[0049] After mixing 10 g of Catalyst II and 2 kg of hydrogen peroxide solution (concentration 27%), inject it into the reactor at a rate of 300 g / h at 70° C. to decompose the tar on the deactivated catalyst.

[0050] At normal temperature and pressure, 10kg of cumene was injected into the reactor at a rate of 300g / h to clean the small molecule products produced by the decomp...

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Abstract

The invention relates to a method for regenerating an inactivated titanium silicalite molecular sieve (TS-1) catalyst, provides a continuous in-vessel regeneration scheme, and is particularly suitable for phenol hydroxylation reaction. Aiming at the characteristic that the catalyst is easy to adsorb tar and is inactivated in the phenol hydroxylation reaction process, the regeneration of the catalyst is realized by adopting the steps of washing organic matters by a solvent, decomposing tar by peroxide under the action of the catalyst, dissolving small molecules by the solvent and the like. The whole regeneration process is carried out in the reactor, the reaction is continuous, the operation is simple, the complicated catalyst disassembly and assembly processes are avoided, and the performance of the regenerated catalyst can reach the level of a fresh catalyst. The structure of the catalyst for decomposing tar is shown in the specification, wherein M is a transition metal.

Description

technical field [0001] The invention relates to a method for regenerating an inactivated titanium-silicon molecular sieve, and is especially suitable for the regeneration of the titanium-silicon molecular sieve used in the phenol hydroxylation reaction in a reactor. Background technique [0002] Titanium silicate molecular sieve, namely TS-1, has an MFI structure and is a commercial catalyst widely used in the fields of olefin epoxidation, phenol hydroxylation and amidoximation. In recent years, it has received more and more attention due to its unique catalytic oxidation performance more attention. [0003] Under the action of TS-1, phenol and hydrogen peroxide undergo a hydroxylation reaction to form o / hydroquinone, which is a green process for the synthesis of diphenols. At present, in industrial plants, except for Solvay, other manufacturers use the TS-1 method To synthesize o / hydroquinone. During the phenol hydroxylation reaction, a large amount of tar will be generat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/90B01J38/52B01J38/54B01J38/48
CPCB01J29/90B01J38/52B01J38/54B01J38/48
Inventor 丁大康刘释水冯民昌刘振峰范立耸曹鹤李俊平
Owner WANHUA CHEM GRP CO LTD
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