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Method for preparing epoxy butane

A technology of butylene oxide and butylene oxide, which is applied in the direction of organic chemistry, can solve the problems of high price and low economy, and achieve the effects of high selectivity, high atom economy and simple process

Active Publication Date: 2014-12-03
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses barium sulfate, zirconium dioxide or titanium dioxide as the hydrogenation reaction carried out by the palladium catalyst supported by the carrier or the palladium catalyst containing rhenium carrier. The catalyst is a noble metal catalyst, which is expensive and economical.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 1.0g titanium silicon molecular sieve Ti / MSU-1 raw powder (specific surface area is 1021.3m 2 / g, the average pore diameter is 2.1nm), and add a certain amount of quartz sand for dilution, and then place it in the constant temperature zone of the fixed bed reactor. The system pressure was maintained at 2.0MPa, and the reaction temperature was controlled at 80.0°C. Butene-1 and the cumene solution containing 25wt% cumene hydroperoxide solute were mixed before the reactor, and entered into the fixed-bed reactor in the way of top in and bottom out. The molar ratio of butene-1 to cumene hydroperoxide is 10.0:1, and the weight space velocity of cumene hydroperoxide feed is 1.0h -1 . After the reaction was carried out for 2 hours, the product was analyzed by on-line gas chromatography and chemical iodometric titration.

Embodiment 2

[0020] Weigh 1.0g titanium silicon molecular sieve Ti / MSU-1 raw powder (specific surface area is 1021.3m 2 / g, the average pore diameter is 2.1nm), and add a certain amount of quartz sand for dilution, and then place it in the constant temperature zone of the fixed bed reactor. The system pressure was maintained at 2.0MPa, and the reaction temperature was controlled at 80.0°C. Butene-2 ​​and the cumene solution containing 25wt% cumene hydroperoxide solute are mixed before the reactor, and enter the fixed-bed reactor in the way of top in and bottom out. The mol ratio of butene-2 ​​to cumene hydroperoxide is 10.0:1, and the weight space velocity of cumene hydroperoxide feed is 1.0h -1 . After the reaction was carried out for 2 hours, the product was analyzed by on-line gas chromatography and chemical iodometric titration. The results of the cumene hydroperoxide conversion rate and 2,3-epoxybutane selectivity are shown in Table 1.

Embodiment 3

[0022] Weigh 2.0g bar-shaped titanium-silicon molecular sieve Ti / MSU-2 (the specific surface area is 941.6m 2 / g, the average pore diameter is 2.7nm), and add a certain amount of quartz sand for dilution, and then place it in the constant temperature zone of the fixed bed reactor. The system pressure was maintained at 1.0 MPa, and the reaction temperature was controlled at 60.0°C. Butene-1 and the cumene solution containing 25wt% cumene hydroperoxide solute were mixed before the reactor, and entered into the fixed-bed reactor in the way of top in and bottom out. The mol ratio of butene-1 to cumene hydroperoxide is 5.0:1, and the weight space velocity of cumene hydroperoxide feed is 1.0h -1 . After the reaction was carried out for 2 hours, the product was analyzed by on-line gas chromatography and chemical iodometric titration.

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Abstract

The invention relates to a method for preparing epoxy butane, which comprises the following step: in an isopropyl benzene solution containing 25 wt% of cumene hydroperoxide solute, preparing epoxy butane from butylene oxide by using the cumene hydroperoxide solute as an oxidizer and a titanium-silicon molecular sieve with three-dimensional pore canal structure as a catalyst, wherein the fixed bed reaction conditions are as follows: the mole ratio of butylene to the cumene hydroperoxide solute is (5.0-12.0):1, the weight hourly space velocity of the cumene hydroperoxide is 1.0-5.0 h<-1>, the reaction pressure is 1.0-6.0 MPa, and the temperature is 60.0-120.0 DEG C. The catalyst is the titanium-silicon molecular sieve with three-dimensional pore canal structure; the molecular sieve has hysteresis loop on the low-temperature nitrogen adsorption and desorption isotherm; the average pore size is 2.0-8.0nm, and the specific area is 650.0-1100.0 m<2> / g; and the catalyst has the advantages of favorable activity and high epoxy butane selectivity, and can be widely popularized and applied to industrial production of epoxy butane by butylene epoxidation.

Description

technical field [0001] The invention relates to a method for preparing butylene oxide. Specifically, a titanium-silicon molecular sieve with a three-dimensional pore structure is used as a catalyst to catalyze the oxidation of butene and cumene hydroperoxide to prepare butylene oxide. Background technique [0002] In addition to being used as the base oil of new synthetic lubricants, polyether is also an important raw material for the production of polyurethane, and has multiple functions such as defoaming, demulsification, dispersion, penetration, and emulsification. The monomers for the synthesis of polyethers have been developed to include ethylene oxide, propylene oxide, butylene oxide and tetrahydrofuran. Due to the limitation of butylene oxide production technology, the polyether synthesized with butylene oxide as a monomer accounts for a small market share. Butylene oxide has developed rapidly since it was developed in the 1970s. For example, in the 1980s and 1990s i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/19C07D303/04
CPCC07D301/19C07D303/04
Inventor 吴美玲周灵杰陈玮娜赵耀马颖涛
Owner CHINA PETROLEUM & CHEM CORP
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