Method for preparing ethylene glycol monobutyl ether

A technology of ethylene glycol butyl ether and n-butanol, which is applied in ether preparation, organic chemistry, etc., can solve the problems of long process route, high energy consumption and material consumption, and large equipment investment, and overcome the long process flow and product selectivity High, high utilization effect

Inactive Publication Date: 2008-02-13
胡先念
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Problems solved by technology

Therefore, the process route using this method is longer, the equipment invest

Method used

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  • Method for preparing ethylene glycol monobutyl ether

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preparation example Construction

[0016] The preparation method of the modified titanium-silicon molecular sieve in the example is: add 10 g of titanium-silicon molecular sieve synthesized according to the method disclosed in CN1301599A into 100 g of distilled water, stir and heat up to 65 ° C, add 1.1 g of Tween 80 and stir for 10 minutes, add 1.45 g aluminum isopropoxide and 1.3 g Siben 80, raise the temperature to 90°C and stir for 4 hours, pressurize to 5Kg / cm2, raise the temperature to 120°C, react at constant temperature and pressure for 24 hours, take out, wash and filter, and bake at 110°C Dry for 5 hours, and bake at 600°C for 6 hours to obtain the modified titanium-silicon molecular sieve.

[0017] In an embodiment, the hydrogen peroxide is 30% H 2 o 2 , analytically pure; ethylene, analytically pure; n-butanol, analytically pure. All three are commercially available.

[0018] In the embodiment, the reactor is a COF2 / 10 stainless steel reactor produced by Beijing Research Institute of Chemical Ind...

Embodiment 1

[0025] 100g titanium silicon molecular sieve, 887g n-butanol, 113g concentration of 30% H 2 o 2 Add in the reaction kettle that volume is 2L successively, and the molar ratio of n-butanol and hydrogen peroxide is 12 at this moment. After airtight, start stirring while raising the temperature, and stop heating when the temperature reaches 100°C.

[0026] Continuously feed ethylene into the reactor, control the pressure of the reactor to 2.5MPa, and control the temperature to 100°C by adjusting the amount of water fed into the heating coil of the reactor. After reacting for 0.5 h, the selectivity of ethylene glycol butyl ether was 100%, the conversion rate of n-butanol was 7.2%, and the utilization rate of hydrogen peroxide was 86.4%.

Embodiment 2

[0028] 5g titanium silicon molecular sieve, 907.4g n-butanol, 92.6g concentration of 30% H 2 o 2 Add in the reaction kettle that volume is 2L successively, and the molar ratio of n-butanol and hydrogen peroxide is 15 at this moment. After airtight, start stirring while raising the temperature, and stop heating when the temperature reaches 40°C.

[0029] Continuously feed ethylene into the reactor, control the pressure of the reactor to 3.0 MPa, and control the temperature to 40° C. by adjusting the amount of water fed into the heating coil of the reactor. After 10 hours of reaction, the selectivity of ethylene glycol butyl ether was 100%, the conversion rate of n-butanol was 4.8%, and the utilization rate of hydrogen peroxide was 72%.

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Abstract

The present invention discloses a method for preparing glycol butyl ether with one step reaction taking ethylene, hydrogen peroxide and n-Butyl alcohol as the raw material; the method makes ethylene, hydrogen peroxide and n-Butyl alcohol mix under titanium silicon molecule screen or alkaline titanium silicon molecule screen; the molar ratio between n-Butyl alcohol and hydrogen peroxide is 1-20; the temperature and the pressure are respectively 5-280 Celsius system and 0.1-5.0 Mpa; the contact time is 0.2-10 hours; the dose of the titanium silicon molecule screen or alkaline titanium silicon molecule screen should be the degree to make with 0.001-0.5 molecule screen in each gram of the reaction liquid. The method not only overcomes the problem in the traditional technical that: the flow is much longer; the device investment is much larger and the resource consumption is much higher and so on, but also the selectivity for the purposed product is much higher; the utilization ratio for hydrogen peroxide is much higher; the activity and the stability of the catalyzer is much higher; the product can be reused and recycled; hydrogen peroxide is oxidated to change water, which does not pollute the environment.

Description

technical field [0001] The present invention relates to the preparation method of ethylene glycol butyl ether, specifically relates to the use of titanium-silicon molecular sieve or modified titanium-silicon molecular sieve as a catalyst, and ethylene, hydrogen peroxide, and n-butanol as raw materials to prepare ethylene glycol butyl ether by one-step reaction method. Background technique [0002] Ethylene glycol monobutyl ether, chemical name ethylene glycol monobutyl ether (or ethylene glycol butyl ether), alias butyl cellosolve, is a colorless and flammable liquid with a moderate ether odor and low Toxic, boiling point 171°C, relative density (d 4 20 ) 0.9015, refractive index (nD20) 1.4198, vapor pressure (20°C) 0.101kPa, flash point 61.1°C, spontaneous ignition point 472°C. Ethylene glycol butyl ether is soluble in most organic solvents and mineral oil. It is miscible with benzene, acetone, carbon tetrachloride, ether and n-heptane, and has the characteristics of lo...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/01
Inventor 胡先念李华林榕伟
Owner 胡先念
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