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Oxidation method for tert-butyl alcohol

A technology of tert-butanol and oxidant, which is applied in chemical instruments and methods, preparation of peroxygen compounds, chemical recovery, etc., can solve the problem of oxidant conversion rate, oxidant effective utilization rate, target oxidation product selectivity reduction, catalyst activity and selectivity fluctuation. It is suitable for large-scale application, stabilizes the oxidant conversion rate, and reduces the difficulty.

Inactive Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] A kind of method of preparing tert-butyl hydroperoxide is disclosed in CN1699339A, this method is simply with titanium silicon molecular sieve as catalyst, with hydrogen peroxide as oxidant, tert-butanol conversion rate still has bigger room for improvement
[0005] When titanium-silicon molecular sieves are used as catalysts to oxidize tert-butanol, the common problem is that with the prolongation of the reaction time, the catalytic activity of titanium-silicon molecular sieves will show a downward trend, resulting in the conversion rate of oxidant, the effective utilization rate of oxidant and the selectivity of target oxidation products. reduce
[0007] However, when the regenerated catalyst is put into operation again, especially after being regenerated in the device, the activity and selectivity of the catalyst fluctuate greatly, and it takes a long time to stabilize; at the same time, it is necessary to combine operations such as increasing the reaction temperature To achieve the smooth operation of the reaction, but this will further accelerate the deactivation of the catalyst and reduce the selectivity of the target oxidation product, which will affect the refining and separation of subsequent products, and is also not conducive to safe production

Method used

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  • Oxidation method for tert-butyl alcohol
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  • Oxidation method for tert-butyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0073] The reaction is carried out in two miniature fixed-bed reactors connected in series, wherein each reactor is filled with a catalyst bed with a circular cross-section and an equal diameter. Based on the flow direction of the liquid material, the first upstream The ratio of the inner diameter of the first catalyst bed in the first reactor to the inner diameter of the second catalyst bed in the downstream second reactor is 2:1, and the first catalyst bed is filled with a hollow titanium-silicon molecular sieve ( A spherical catalyst with a volume average particle size of 500 μm and a catalyst density of 0.70 g / cm 3 ), the second catalyst bed is filled with titanium-silicon molecular sieve TS-1 (a spherical catalyst with a volume average particle diameter of 500 μm and a density of 0.76 g / cm 3 ), the weight ratio of hollow titanium-silicon molecular sieve to titanium-silicon molecular sieve TS-1 is 2:1.

[0074] tert-butanol, hydrogen peroxide (provided in the form of 30% ...

Embodiment 2

[0088] Adopt the method identical with embodiment 1 to oxidize tert-butanol, difference is, the molding titanium-silicon molecular sieve TS-1 in the second catalyst bed uses the same amount of molding titanium-silicon molecular sieve Ti-MCM-41 (volume average particle diameter is 500μm spherical catalyst with a density of 0.61g / cm 3 )replace.

[0089] The results are listed in Table 1 for reaction times of 2 hours, 360 hours and 720 hours.

Embodiment 3

[0091] Adopt the same method oxidation tert-butanol as embodiment 1, difference is, the molding titanium-silicon molecular sieve TS-1 in the second catalyst bed layer in the second reactor uses an equivalent amount of molding titanium-silicon molecular sieve Ti-Beta ( A spherical catalyst with a volume average particle size of 500 μm and a density of 0.77 g / cm 3 )replace.

[0092] The results are listed in Table 1 for reaction times of 2 hours, 360 hours and 720 hours.

[0093] Table 1

[0094]

[0095]

[0096] Comparing the data of Example 1 with Comparative Examples 1-3, it can be seen that when the hollow titanium-silicon molecular sieve is used in combination with the titanium-silicon molecular sieve, and the hollow titanium-silicon molecular sieve is located upstream of the titanium-silicon molecular sieve, the liquid mixture flows through the hollow The superficial velocity of the titanium-silicon molecular sieve is lower than the superficial velocity of the tit...

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Abstract

The invention provides an oxidation method for tert-butyl alcohol. The method comprises the step of subjecting a liquid mixture containing cyclohexane and an oxidant to passing through catalyst beds under the condition of oxidation reaction, wherein the catalyst beds comprise a first catalyst bed and a second catalyst bed; on the basis of the flow direction of the liquid mixture, the first catalyst bed is located at the upper stream of the second catalyst bed; a titanium-silicon molecular sieve filled in the first catalyst bed is a hollow titanium-silicon molecular sieve; and the titanium-silicon molecular sieve filled in the second catalyst bed is the titanium-silicon molecular sieve different from the hollow titanium-silicon molecular sieve. The method provided by the invention can effectively prolong the single-way service life of the titanium-silicon molecular sieve used as a catalyst, reduce regeneration frequency of the catalyst, improve production efficiency, and enhance operation stability and prolong the total service life of the catalyst at the same time.

Description

technical field [0001] The invention relates to a method for oxidizing tert-butanol. Background technique [0002] Tert-butyl hydroperoxide is a colorless transparent or yellow liquid, which is miscible with organic solvents such as ethanol and ether. It is stable below 75°C, loses oxygen at 90-100°C, and explodes at 250°C. Tert-butyl hydroperoxide is mainly used as a catalyst for polymerization reactions, and as an introduction agent for peroxide groups in substituent reactions. It is used for dyeing and printing cotton, viscose, silk, nylon and other fibers and their fabrics. Used for polyester / viscose blended fabric dyeing. [0003] Tert-butyl hydroperoxide can also be used as a drying agent for unsaturated melamine resin coatings, a polymerization initiator, and an intermediate in organic synthesis. The existing preparation methods mainly include: first, after diazotization of p-nitroaniline o-sulfonic acid, coupling with gamma acid, then reducing the nitro group in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/04C07C407/00
CPCY02P20/584
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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