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Method for preparing titanium-based catalyst and synthesizing epoxypropane and dicumyl peroxide

A technology of dicumyl peroxide and cumene hydroperoxide, which is applied in chemical instruments and methods, molecular sieve catalysts, and preparation of peroxygen compounds, and can solve the problems of environmental pollution caused by many by-products and inorganic salt wastewater. , achieve the effects of high atomic economy, overcoming equipment corrosion, and good industrial application prospects

Inactive Publication Date: 2013-07-24
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Purpose of the invention: for the above-mentioned existing problems and defects, the invention provides a method for the preparation of propylene oxide and dicumyl peroxide with a titanium-based catalyst and atom-economical efficiency, in which cumene hydroperoxide recycles The preparation of dicumyl peroxide DCP overcomes the equipment corrosion caused by the chlorohydrin method and the indirect oxidation method, and the by-products pollute the environment; it also overcomes the reduction of cumene hydroperoxide by water-soluble sulfur compounds to prepare dicumyl peroxide Benzene easily produces inorganic salt wastewater to pollute the environment

Method used

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  • Method for preparing titanium-based catalyst and synthesizing epoxypropane and dicumyl peroxide

Examples

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Effect test

Embodiment 1

[0030] Propylene epoxidation reaction: Weigh 1.0 g of 20-40 mesh catalyst, and fill it in a stainless steel fixed-bed tubular reactor with an inner diameter of 6 mm. After the reaction temperature stabilizes at 90 ℃, the feeding reaction starts. The system pressure is 4 MPa, the propylene is fed in the liquid phase, the feed rate is 6 ml / h, the CHP (mass fraction is about 30%, the other components are cumene, 3% n-butylamine), the feed rate is 10 L / h, propylene The molar ratio to cumene hydrogen peroxide is about 5, and the total mass space velocity (WHSV) is 12.4 h -1 . The reaction product was collected in a cold trap, and samples were taken every 1 hour to analyze the product composition. After 10 hours of reaction, calculate the average value, the conversion rate of cumene hydroperoxide X CHP 62.3%, the utilization rate of cumene hydrogen peroxide U CHP 63.5%, selectivity S for propylene oxide PO PO It was 94.3%.

[0031] After the reaction in the previous step is over, tak...

Embodiment 2

[0034] Propylene epoxidation reaction: reaction temperature is 100 ℃, other conditions are the same as in Example 1, react for 10 hours, calculate the average value, conversion rate of cumene hydroperoxide X CHP Is 77.9%, the utilization rate of cumene hydrogen peroxide U CHP 60.4%, selectivity S of propylene oxide PO PO It was 92.6%.

[0035] After the reaction in the previous step is over, take 150 ml of the product and distill out the propylene oxide, 1,2-propylene glycol, n-butylamine and other low-boiling substances in the product. The product contains about 8.7 g of cumene hydroperoxide CHP. Containing about 18.5 g of α,α-dimethylbenzyl alcohol, add 7.3 g of 70% CHP to a three-necked flask to make the molar ratio of α,α-dimethylbenzyl alcohol to cumene hydrogen peroxide approximately 1.5. The remaining steps are the same as in Example 1, and then the synthesis of dicumyl peroxide DCP is carried out, and 19.3 g of DCP product can be obtained, and the yield is about 78.9%.

Embodiment 3

[0037] Propylene epoxidation reaction: the reaction temperature is 100°C, the amount of catalyst is 2.0 g, other conditions are the same as in Example 1, and the reaction is 10 hours, and the average value is calculated. The conversion rate of cumene hydroperoxide is X CHP Is 84.9%, the utilization rate of cumene hydrogen peroxide U CHP 61.6%, selectivity S of propylene oxide PO PO It was 93.1%.

[0038] After the reaction in the previous step is over, take 150 ml of the product and distill out the propylene oxide, 1,2-propylene glycol, n-butylamine and other low-boiling substances in the product. The product contains about 5.9 g of cumene hydroperoxide CHP. Containing about 20.6 g of α,α-dimethylbenzyl alcohol DMPC, add 13.4 g of 70% CHP to a three-necked flask to make the molar ratio of α,α-dimethylbenzyl alcohol to cumene hydrogen peroxide approximately The other steps are the same as in Example 1, and then the synthesis of dicumyl peroxide DCP is carried out, and 21.7 g of DC...

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Abstract

The invention discloses a method for preparing a titanium-based catalyst and synthesizing epoxypropane and dicumyl peroxide. According to the method, when the epoxypropane is synthesized on the basis of the titanium-based molecular sieve based catalyst, a byproduct, namely dimethyl-benzyl carbinol is continuously recycled to synthesize and prepare dicumyl peroxide; the problems of equipment corrosion, large quantity of byproducts and environmental pollution caused by the traditional chlorohydrins method and an indirect oxidation method are solved; the problem of environmental pollution caused by inorganic-salt-containing wastewater produced in a process of preparing the dicumyl peroxide by reducing cumyl hydroperoxide by using inorganic matters, such as water-soluble sulfur compounds is solved; and therefore the method is a synthesis process with high atom economy and has a favorable industrial application prospect.

Description

Technical field [0001] The invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing a titanium-based catalyst and synthesizing propylene oxide and dicumyl peroxide. Background technique [0002] Propylene oxide (PO) is the third largest organic chemical product in the production of propylene derivatives after polypropylene and acrylonitrile. PO has a wide range of uses. At present, in addition to the production of polyether polyols, nonionic surfactants and propylene glycol, it can also be used to produce oilfield demulsifiers, glycerol, and pesticide emulsifiers. [0003] The main methods for producing propylene oxide and epichlorohydrin at home and abroad are the chlorohydrin method and the indirect oxidation (Halcon) method. The chlorohydrin process is a traditional industrial production route of propylene oxide, which began in the 1930s. This method has short process flow, mature technology, large operating load flexibi...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D303/04C07D301/19C07C409/16C07C407/00
CPCY02P20/52
Inventor 刘靖倪晓磊王巧谭涓王安杰胡永康
Owner DALIAN UNIV OF TECH
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