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Method for preparing sec-butyl acetate by utilizing etherified C4 fraction

A technology for sec-butyl acetate and C4 fraction, which is applied in the field of preparing sec-butyl acetate, can solve the problems of easy loss of stability of active components, low selectivity of sec-butyl acetate, low purity of reaction products, etc., and achieves easy separation. , long service life, high selectivity effect

Active Publication Date: 2014-01-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of existing catalysts for producing sec-butyl acetate are that they are not resistant to high temperatures, are not easy to regenerate, and the active components are easy to lose during use, that is, they have poor stability, and the selectivity of generating sec-butyl acetate is not high.
The currently built industrial units use strong acidic cationic resin catalysts, but the raw material carbon tetraolefins used need to be purified, the operation is complicated and cumbersome, and the purity of the reaction products is not high, and the separation is complicated

Method used

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  • Method for preparing sec-butyl acetate by utilizing etherified C4 fraction

Examples

Experimental program
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Effect test

preparation example Construction

[0030] Catalyst preparation

[0031] Mix 200 grams of HY-type zeolite, 100 grams of hydrogen-type mordenite, 70 grams of silicon oxide and 2 g of scallop powder; add an appropriate amount of 5% nitric acid after mixing, extrude into a 2mm cylindrical shape after mixing, and cut into 2- 3mm; dried at 80°C and 120°C for 10 hours respectively, then calcined at 580°C for 6 hours, taken out and cooled to room temperature, and placed in a desiccator for later use. Catalysts prepared in this way are denoted shaped catalysts. Take 100g of shaped catalysts and impregnate them with appropriate amount of 5% phosphoric acid and boric acid solutions respectively, dry them at 80°C and 120°C for 10 hours respectively, calcinate at 580°C for 6 hours, put them in a desiccator for later use. Catalyst A is obtained.

Embodiment 1

[0033] The acetic acid raw material is glacial acetic acid with a purity greater than 99.5%. Reactor 1 is composed of 44.19% isobutane, 13.23% n-butane, 13.76% 1-butene, 16.55% t-2-butene, 0.23% isobutene, c -2-Butene 11.75% ether C4 fraction, reactor 2 uses n-butene with a purity greater than 99.5%.

[0034] 20 grams of the prepared catalyst A were taken out and packaged respectively, and then put into two reactors as a whole.

[0035] Step i: The temperature at the top of the reactor is 50°C, the temperature at the bottom of the reactor is 180°C, the pressure is 1.0MPa, the butene / acetic acid in the C4 fraction after ether is 0.8, and the space velocity of the C4 fraction after ether is 3h -1 . Acetic acid enters from the top of reactor 1 with a metering pump, and the C4 fraction after ether enters from the bottom of reactor 1 through a liquid mass flow meter.

[0036] Step ii: The temperature at the top of the reactor is 30°C, the temperature at the bottom of the reactor ...

Embodiment 2

[0039] The acetic acid raw material is glacial acetic acid with a purity greater than 99.5%. Reactor 1 is composed of 0.25% isobutane, 20.45% n-butane, 5.11% 1-butene, 43.72% t-2-butene, 0.12% isobutene, c- 2-Butene 30.17% ether C4 fraction, reactor 2 uses n-butene with a purity greater than 99.5%.

[0040] 20 grams of the prepared catalyst A were taken out and packaged respectively, and then put into two reactors as a whole.

[0041] Step i: The temperature at the top of the reactor is 50°C, the temperature at the bottom of the reactor is 180°C, the pressure is 1.0MPa, the butene / acetic acid in the C4 fraction after ether is 0.8, and the space velocity of the C4 fraction after ether is 2h -1 . Acetic acid enters from the top of reactor 1 with a metering pump, and the C4 fraction after ether enters from the bottom of reactor 1 through a liquid mass flow meter.

[0042] Step ii: The temperature at the top of the reactor is 30°C, the temperature at the bottom of the reactor is...

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Abstract

The invention discloses a method for synthesizing sec-butyl acetate by utilizing an etherified C4 fraction. The method comprises the following steps: step 1), contacting the etherified C4 fraction containing butene with excess acetic acid in the presence of a zeolite catalyst to obtain a sec-butyl acetate crude product containing the acetic acid; and step 2), contacting excess n-butene with the sec-butyl acetate crude product containing the acetic acid, which is obtained in the step 1) in the presence of the zeolite catalyst to obtain the high-purity sec-butyl acetate. According to the method, the zeolite catalyst is adopted, the catalyst has the advantages of good stability and long service life and is easy to regenerate, and the selectivity of the generated sec-butyl acetate is high. When the etherified C4 fraction is taken as a raw material to prepare the sec-butyl acetate, olefins and alkanes in the etherified C4 fraction can be separated, the separation step is not required, the high-purity sec-butyl acetate can be obtained, and the process flow is simple; the etherified C4 fraction is taken as the raw material, so that the utilization rate of the C4 fraction is improved, and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to the field of petrochemical industry, and furthermore, relates to a method for preparing sec-butyl acetate by utilizing the carbon four fraction after ether. Background technique [0002] Second-butyl acetate, namely second-butyl acetate and dibutyl acetate, is one of the four isomers of butyl acetate. It is a colorless, flammable, fruit-flavored liquid, and its performance is comparable to that of other isomers. Similar in most cases, it can dissolve various resins and organic substances. Its boiling point is lower than that of commonly used n-butyl ester and isobutyl ester, and its evaporation rate is faster. [0003] Secondary butyl acetate has a wide range of uses, and is suitable for medicine, paint, high-grade paint, ink, resin, and acetic acid dehydration and solvents. It can also replace MTBE as an additive for gasoline. It is a fine chemical with a wide range of uses. [0004] The traditional production process of sec...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04
CPCC07C67/04C07C69/14
Inventor 王定博张明森郭敬杭马志元
Owner CHINA PETROLEUM & CHEM CORP
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