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Production method for sulfone

A production method and technology of titanium-silicon molecular sieves, which are applied in chemical instruments and methods, preparation of organic compounds, molecular sieve catalysts, etc., can solve the problems that the application research of dimethyl sulfone has not been carried out well, and achieve easy implementation and prolong service life , the effect of delaying the inactivation speed

Active Publication Date: 2018-11-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, dimethyl sulfone is widely used as a nutritional product that is as important as vitamins. The research on the application of dimethyl sulfone in my country has not yet been carried out well. At present, the products are mainly used for export.

Method used

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  • Production method for sulfone
  • Production method for sulfone
  • Production method for sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0098] The titanium-silicon molecular sieve TS-1 used in this example was prepared according to the method described in Zeolites, 1992, Vol.12, pages 943-950, and the specific method is as follows.

[0099] 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 wate...

Embodiment 2

[0109] Adopt the same method as Example 1 to prepare dimethyl sulfone, the difference is that the prepared titanium-silicon molecular sieve TS-1 is modified by the following method before molding (that is, the same method as in Example 1 will be used to prepare Titanium-silicon molecular sieve TS-1 was used as a raw material for modification treatment), and the obtained modified titanium-silicon molecular sieve TS-1 was molded by the same method as in Example 1 to obtain the catalyst used in this example.

[0110] Titanium silicate molecular sieve TS-1 with HNO 3 (HNO 3 The mass concentration of hydrogen peroxide is 10%) and the aqueous solution of hydrogen peroxide (the mass concentration of hydrogen peroxide is 7.5%) is mixed, and the obtained mixture is stirred and reacted at 70 ℃ for 5h in a closed container, and the temperature of the obtained reaction mixture is down to room temperature After filtering, the obtained solid-phase substance was dried at 120° C. to a consta...

Embodiment 3

[0113] Dimethyl sulfone was prepared by the same method as in Example 2, except that the titanium-silicon molecular sieve TS-1 was prepared by the following method.

[0114] 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 seco...

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Abstract

The invention discloses a production method for sulfone. The production method for the sulfone comprises the steps of enabling a reaction mixture which contains thioether, at least one oxidizing agentand at least one selectable solvent to be in contact reaction with a titanium silicalite molecular sieve in a reactor; transferring out reaction heat by using a heat exchange medium in a contact reaction process, wherein the molar ratio of the oxidizing agent to the thioether is greater than 2; when sulfone selectivity is reduced, adjusting the condition of heat exchange to reduce the amount of the transferred reaction heat until the sulfone selectivity returns to an expected value; and maintaining the amount of the transferred reaction heat. By the method, the deactivation speed of the titanium silicalite molecular sieve as a catalyst can be reduced effectively, the single-strip service life of the titanium silicalite molecular sieve is prolonged, the regeneration frequency of the titanium silicalite molecular sieve is reduced, on the one hand, thioether conversion rate and the sulfone selectivity are maintained at high level for a long time, and on the other hand, the total servicelife of the titanium silicalite molecular sieve is prolonged, the production cost is reduced, and meanwhile, the running efficiency of the device can further be prolonged.

Description

technical field [0001] The invention relates to a production method of sulfone. Background technique [0002] Sulfones are important sulfur-containing compounds. For example, dimethyl sulfone is a white crystalline powder, easily soluble in water, ethanol, benzene, methanol and acetone, and slightly soluble in ether. Potassium permanganate cannot be discolored at room temperature, and strong oxidizing agents can oxidize dimethyl sulfone to methanesulfonic acid. Aqueous solution of dimethyl sulfone is neutral. At 25°C, there is a small amount of sublimation, and the sublimation speed is accelerated at 60°C, so the dimethyl sulfone product should be dried at low temperature and vacuum. [0003] Dimethyl sulfone is used in industry as a high-temperature solvent and raw material for organic synthesis, as a stationary liquid for gas chromatography, as a analytical reagent, as a food additive, and as a drug. As an organic sulfide, dimethyl sulfone can enhance the ability of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/02C07C317/04B01J29/89B01J37/12
CPCB01J29/89B01J37/12C07C315/02C07C317/04
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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