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Aromatic hydrocarbon oxidation method

An aromatic hydrocarbon and oxidant technology, applied in chemical instruments and methods, organic chemistry, molecular sieve catalysts, etc., can solve the problems of reactor shutdown, increase the operating cost of the device, and reduce the catalytic activity, so as to reduce the regeneration frequency, prolong the single-pass service life, The effect of extending the total service life

Active Publication Date: 2017-07-21
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, with the prolongation of the reaction time, the catalytic activity of titanium-silicon molecular sieves will show a downward trend, resulting in a significant decrease in the selectivity of the target oxidation product.
When the reaction is carried out in a fixed-bed reactor, due to the reduction of the catalytic activity of the titanium-silicon molecular sieve, the titanium-silicon molecular sieve needs to be regenerated inside or outside the reactor, resulting in shutdown of the reactor, thereby affecting production efficiency and increasing the operating cost of the device

Method used

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Examples

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Embodiment approach

[0067] According to the method of the present invention, the amounts (mass) of the titanium-silicon molecular sieves loaded in the first to nth catalyst beds may be the same or different. According to one implementation, when m is any integer in the interval [2, n], W m-1 / W m 0.1-20, W m-1 / W m Preferably it is 0.5 or more, More preferably, it is 1 or more, More preferably, it is 2 or more. Here, W m-1 is the quality of the catalyst packed in the upstream catalyst bed in any pair of adjacent catalyst beds from the first catalyst bed to the last nth catalyst bed, W m is the mass of the catalyst loaded in the downstream catalyst bed in any pair of adjacent catalyst beds from the first catalyst bed to the nth catalyst bed. W m-1 / W m Preferably it is 15 or less, and more preferably 10 or less. More preferably, W m-1 / W m for 2-8. W m-1 and W m It is determined by the content of the titanium-silicon molecular sieve in the shaped titanium-silicon molecular sieve. In ...

Embodiment 1

[0097] The catalyst used in this example is titanium-silicon molecular sieve TS-1, prepared according to the method described in Zeolites, 1992, Vol.12, pages 943-950, and the specific method is as follows.

[0098] At room temperature (20°C), mix 22.5g tetraethyl orthosilicate with 7.0g tetrapropylammonium hydroxide as a template, add 59.8g distilled water, stir and mix, then hydrolyze at normal pressure and 60°C for 1.0h , to obtain a hydrolysis solution of tetraethyl orthosilicate. Under vigorous stirring, a solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of anhydrous isopropanol was slowly added to the hydrolysis solution, and the resulting mixture was stirred at 75° C. for 3 h to obtain a clear transparent colloid. The colloid was placed in a sealed stainless steel reaction kettle, and kept at a constant temperature of 170° C. for 36 hours to obtain a mixture of crystallized products. The obtained mixture was filtered, the collected solid matter was washed ...

Embodiment 2

[0104] Benzene was oxidized by the same method as in Example 1, except that the titanium-silicon molecular sieve TS-1 used was prepared by the following method.

[0105] Dissolve tetrabutyl titanate in the alkali source template agent tetrapropyl ammonium hydroxide aqueous solution first, then add silica gel (purchased from Qingdao Silica Gel Factory) to obtain a dispersion. In the dispersion, silicon source: titanium source: alkali source Template agent: water molar ratio is 100:4:12:400, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of alkali source template agent in N. Seal the above dispersion in the beaker with a parafilm and let it stand at room temperature (25°C, the same below) for 24h, then stir at 35°C for 2h with magnetic stirring to redisperse it. Transfer the re-dispersed dispersion liquid to a sealed reaction kettle, undergo the first stage of crystallization at 140°C for 6h, then cool the mixture down to 30°C and experience the second s...

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Abstract

The present invention discloses an aromatic hydrocarbon oxidation method, which comprises that a reaction material containing at least an aromatic hydrocarbon, an oxidizing agent and a solvent sequentially flows through catalyst bed layers from 1 to n under an oxidation reaction condition, wherein n is an integer of more than 2, and the catalyst bed layer is filled with at least a titanium-silicon molecular sieve; and when the reaction material passes through the catalyst bed layers from 1 to n, at least a flow carrier is introduced into the position between at least a pair of the adjacent catalyst bed layers among the catalyst bed layers from 1 to n, such that the apparent velocity of the reaction stream positioned in the downstream catalyst bed layer is higher than the apparent velocity of the reaction stream positioned in the upstream catalyst bed layer in the pair of the adjacent catalyst bed layers by adopting the flowing direction of the reaction material as the reference. With the method of the present invention, the one-way service life of the titanium-silicon molecular sieve can be effectively prolonged, the effective utilization rate of the oxidizing agent can be improved, and the target product selectivity can be improved.

Description

technical field [0001] The invention relates to an aromatic hydrocarbon oxidation method. Background technique [0002] Phenolic compounds are substances that widely exist in nature and have important uses in industry. In nature, the well-known anthocyanins, vanillin and catechol are polyphenols. In the industrial field, phenolic substances are important intermediates in the synthesis of many organic compounds. In addition, phenolic substances also act as living dyes, dyes and drugs. The important role and wide application of phenolic substances determine the importance of their synthesis. At present, the commonly used methods for preparing phenolic compounds mainly include the oxidation of aromatic hydrocarbons, the displacement hydrolysis of aryl thallium salts, the hydrolysis of halogenated benzene, and the diazonium salt method. The hydrolysis of halogenated benzene usually requires high temperature and high pressure and the presence of a catalyst; while the preparati...

Claims

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Application Information

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IPC IPC(8): C07C37/60C07C39/04B01J29/89
CPCB01J29/89C07C37/60C07C39/04Y02P20/52
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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