A kind of method for preparing sec-butyl acetate

A technology of sec-butyl acetate and n-butene, applied in the field of preparation of sec-butyl acetate, can solve the problems such as difficult control of reaction hot spot temperature, poor selectivity of sec-butyl acetate, different reaction heat, etc., and prolong the service life. , The effect of strong controllability of response and precise control

Active Publication Date: 2016-02-10
HUIZHOU YUSSEN CHEM CO LTD
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Problems solved by technology

[0009] But, in the existing method for preparing sec-butyl acetate by n-butene and acetic acid addition method, there are following deficiencies in reaction control: (1) because n-butene has three isomers (1-butane ene, cis-2-butene and trans-2-butene), the reactivity of the three is different, and the heat of reaction is also different. Therefore, when the n-butene raw material used is not a pure single compound, the existing reaction control method It cannot meet the different requirements of different olefin components on the reaction temperature, resulting in low conversion of butene and poor selectivity of sec-butyl acetate; (2) When the composition of feed butene changes, the heat of reaction will decrease Changes accordingly, resulting in difficult control of reaction hot spot temperature and easy coking and deactivation of the catalyst

Method used

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  • A kind of method for preparing sec-butyl acetate

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Effect test

Embodiment 1

[0027] 300ml of good strong acidic cation exchange resin catalysts with catalytic activity are respectively housed in four series-connected tubular fixed-bed reactors R1, R2, R3, R4. At the same time, the speed is continuously passed into R1, and flows through R2, R3 and R4 in sequence. The mass composition of the C4 mixture is: isobutane 11%, n-butane 16.9%, 1-butene 38.96%, cis-2-butene 13.58%, trans-2-butene 18.76%, and the total content of n-butene is 71.3%. The reactor feed temperature is sequentially: 50°C, 53°C, 60°C, 65°C. The jacket water temperature of the four reactors is controlled by adjusting the jacket water volume and the circulating water volume of the jacket water cooler: 50°C, 53°C, 60°C, and 65°C. The pressure of the reaction system is maintained at 1.20 MPa by controlling the back pressure valve.

[0028] The results of sampling and analysis at the outlet of R4 are as follows: the conversion rate of butene is 92%, and the mass content of sec-butyl aceta...

Embodiment 2

[0030] 300ml of strong acidic cation exchange resin catalysts with good catalytic activity are respectively housed in four series-connected tubular fixed-bed reactors R1, R2, R3, and R4, and acetic acid is continuously passed through from R1 at a speed of 4.5 kg / hour. into and flow through R2, R3 and R4 in sequence, and the C4 mixture is divided into four streams and enters R1, R2, R3, R4 respectively at a feed rate of 0.75 kg / h, 0.75 kg / h, 0.50 kg / h, and 0.50 kg / h. middle. The mass composition of the C4 mixture is: isobutane 6.21%, n-butane 11.95%, 1-butene 45.64%, cis-2-butene 14.74%, trans-2-butene 20.77%, and the total content of n-butene is 81.15%. The reactor feed temperature is sequentially: 52°C, 55°C, 58°C, 63°C. The jacket water temperature of the four reactors is controlled by adjusting the jacket water volume and the circulating water volume of the jacket water cooler: 52°C, 55°C, 58°C, and 63°C. The pressure of the reaction system is controlled by the back pres...

Embodiment 3

[0033] 300ml of strong acidic cation exchange resin catalyst with good catalytic activity is installed in each of R1 and R2 two tubular fixed-bed reactors, and 300ml of catalytic activity catalyst is installed in each of R3 and R4 two tubular fixed-bed reactors. Same catalyst in the mid-term. Acetic acid is simultaneously and continuously fed into R1 at a rate of 4.5 kg / h and C4 mixture at a rate of 2.5 kg / h, and flows through R2, R3 and R4 in sequence. The mass composition of the C4 mixture is: isobutane 11.37%, n-butane 16.22%, 1-butene 33.19%, cis-2-butene 17.01%, trans-2-butene 20.99%, and the total content of n-butene is 71.19%. The reactor feed temperature is: 55°C, 60°C, 90°C, 90°C in sequence. The jacket water temperature of the four reactors is controlled by adjusting the jacket water volume and the circulating water volume of the jacket water cooler: 55°C, 60°C, 90°C, and 90°C. The pressure of the reaction system is controlled by the back pressure valve to be 1.20...

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Abstract

The invention discloses a method for preparing sec-butyl acetate, relates to the technical field of sec-butyl acetate, and aims at solving the technical problems in the existing method for preparing sec-butyl acetate through addition reaction between n-butene and acetic acid that the butene conversion rate is low and the selectivity of sec-butyl acetate product is poor. The method comprises the process of addition reaction between n-butene and acetic acid in the presence of a catalyst under the addition reaction condition and is characterized in that the n-butene raw material contains three isomers: 1-butene, cis-2-butene and trans-2-butenen, the catalyst is a strong acid cation exchange resin, the reaction pressure is 1.2MPa, the reaction temperature is controlled to gradually rise in the process of the addition reaction so that the three isomers gradually react, and the corresponding reaction temperature is approximately adjusted according to the life stage of the catalyst. Through the adoption of the method, the butene conversion rate and the selectivity of the sec-butyl acetate product can be effectively improved, so that the sec-butyl acetate is capable of being adapted to butene raw materials containing different ingredients and catalysts in different life stages.

Description

technical field [0001] The present invention relates to the technical field of sec-butyl acetate, in particular to the preparation method of sec-butyl acetate. Background technique [0002] S-butyl acetate (SBAC) is an important chemical raw material. It is a kind of colorless, flammable and fruity liquid. It can dissolve various resins and organic substances. It is the four isomers of butyl acetate. one. Similar to the performance of other isomers, it has a wide range of uses, and can be widely used in fine chemical industries such as fruit fragrances, medicines, coatings, inks and adhesives, replacing solvents such as toluene, xylene and ketones. It is a green environmental protection solvent. It can be used as a reaction medium component, an extractant component and a metal cleaning agent component, etc., and can also be used as an entrainer in the production of PTA, acrylic acid production and purification of crude acetic acid. [0003] In the 1950s and 1960s, my coun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04
CPCC07C67/04C07C69/14
Inventor 胡先念罗庆金余良军甘军华魏力晶
Owner HUIZHOU YUSSEN CHEM CO LTD
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