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Olefin oxidation method

A technology for olefins and oxidants, applied in chemical instruments and methods, organic chemistry, molecular sieve catalysts, etc., can solve problems such as unfavorable safe production, difficult activity, reduced selectivity of target products, etc., to improve device operation safety and device operation safety. The effect of good performance and cost saving of separation

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

AI Technical Summary

Problems solved by technology

The problem with this kind of regeneration is that when re-running after regeneration, especially when re-running after in-device regeneration, the activity and selectivity of the catalyst fluctuate greatly, and it takes a long time to stabilize. The smooth operation of the reaction, but this will further accelerate the deactivation of the catalyst and reduce the selectivity of the target product, which will affect the refining and separation of subsequent products, and is not conducive to safe production
However, this method is not conducive to the repeated regeneration of the catalyst, that is, it affects the total life of the catalyst, because the rate of catalyst deactivation is accelerated after the reaction temperature is increased, and the catalyst deactivated after the elevated temperature is not easy to be regenerated in the device. , and the activity is not easy to recover completely after regeneration

Method used

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Examples

Experimental program
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Effect test

preparation Embodiment 1

[0082] Refer to the method described in Zeolites, 1992, Vol.12 pages 943-950 to prepare titanium-silicon molecular sieve TS-1, the specific method is as follows.

[0083] 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 with water, dried at 110° C. for 60 minutes, ...

preparation Embodiment 2

[0086] Prepare spherical catalyst Q2 according to the method for preparing Example 1, the difference is that the titanium-silicon molecular sieve used is prepared as follows:

[0087] 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 experienc...

preparation Embodiment 3

[0089] Prepare spherical catalyst Q3 according to the method for Preparation Example 1, the difference is that the titanium-silicon molecular sieve used is prepared as follows:

[0090] 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 100:2:10:600, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of alkali source template agent in N. The above-mentioned dispersion liquid was sealed in a beaker with a parafilm and then left to stand at 40° C. for 10 h, followed by magnetic stirring at 25° C. for 0.5 h to re-disperse it. Transfer the re-dispersed dispersion to a sealed reactor, and undergo the first stage of crystallization at 130°C for 8 hours, then cool the mixture down to 50°C and experience the ...

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Abstract

The present invention relates to the field of olefin oxidation, and specifically provides an olefin oxidation method, which is performed in a distillation reactor, wherein the kettle bottoms of the reaction zone and the distillation zone of the distillation reactor are respectively provided with a first catalyst and a second catalyst, and the first catalyst and the second catalyst respectively contain a titanium-silicon molecular sieve. The method comprises that an olefin, an oxidizing agent and an optional solvent contact in the reaction zone under an oxidative reaction condition. According to the present invention, the second catalyst is filled on the kettle bottom of the distillation zone, such that the small amount of the un-reacted oxidizing agent entering the distillation zone can be further completely converted, and the heating of the distillation zone is stable so as to improve the operation safety of the apparatus; and with the method of the present invention, the service life of the catalyst can be prolonged, the oxidizing reaction of the olefin can be continuously performed for a long time, the high olefin conversion rate, the high oxidative selectivity of the olefin, and the effective utilization rate of the oxidizing agent can be obtained, and the operation safety of the apparatus is good.

Description

technical field [0001] The present invention relates to a method for oxidizing olefins. Background technique [0002] Alkylene oxide is an important class of oxygen-containing organic compounds, such as propylene oxide, also known as propylene oxide (PO for short), is an important basic organic chemical raw material, and its output in propylene derivatives is second only to poly propylene. The biggest use of PO is to produce polyether polyols for further processing to make polyurethane, and it can also be used to produce propylene glycol which is widely used. In addition, propylene oxide can also be used in the production of surfactants, oilfield demulsifiers, etc. [0003] With the wide application of polyurethane materials, etc., the demand for propylene oxide is increasing year by year. At present, there are disadvantages in the process of producing propylene oxide in industry, especially it does not meet the requirements of green chemical industry. Therefore, there i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/04B01J29/89
CPCB01J29/89B01J2229/12B01J2229/37C07D301/12C07D303/04
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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