Process method for synthesizing sec-butyl acetate from C4 fractions

A technology of sec-butyl acetate and C4 fraction, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. The effect of low ene molar ratio, prolonging service life and improving product quality

Inactive Publication Date: 2011-11-09
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the production of sec-butyl acetate, Chinese patent CN10112656A has proposed the method that modified resin catalyst synthesizes sec-butyl acetate under the condition of acid-ene ratio 1: 1.15-1.80, because olefin esterification reaction takes place under acidic catalyst catalysis , the polymerization reaction also occurs to produce by-products such as C8, C12 and C16. The selectivity of sec-butyl acetate is up to 98%, which not only reduces the yield of sec-butyl acetate, but also affects product quality
And Chinese patent CN101143819A has reported the method that adopts catalytic distillation process to synthesize sec-butyl acetate with C4 raw material, although sec-butyl acetate selectivity can reach 99%, but does not contain 1,3-butadiene in the C4 raw material that it adopts, However, the 1,3-butadiene content in the C4 fraction of oil refineries is relatively high. If the process requirements are met, the selective hydrogenation process of precious metal catalysts must be adopted, which not only has a complicated process flow, but also has high operating costs.
[0003] At present, the main...

Method used

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  • Process method for synthesizing sec-butyl acetate from C4 fractions
  • Process method for synthesizing sec-butyl acetate from C4 fractions

Examples

Experimental program
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Embodiment 1

[0022] according to figure 1 As shown in the flow chart of the process and equipment, the macroporous strongly acidic cation exchange resin, model A-35, 90 g on a dry basis, is evenly divided into 3 equal parts, each 30 grams, and loaded into 3 boxes with an inner diameter of 10 mm and a length of 80 mm. Tube-and-tube reactors 7, 8, and 9 of stainless steel tubes, hot water is passed through the shell side, and then acetic acid is loaded into storage tank 1, and the C4 fraction is loaded into storage tank 2. The molar ratio of the two olefins is 3, and the acetic acid Add olefin polymerization inhibitor RP-1412, the content is 100μg / g, acetic acid is continuously fed through each stage with pump 3 from the top of the first stage, and the feed rate of acetic acid per hour is 120 grams, and then the molar ratio of ester acid to C4 fraction olefin The amount greater than 9 passes through the metering pumps 11, 12, 13 of each section and the acetic acid pipes 4, 5, 6 to mix and th...

Embodiment 2

[0024] With the equipment of embodiment 1, add a reactor (accompanying drawing not shown), macroporous strongly acidic cation exchange resin, model K-300, dry basis 120g is evenly divided into 4 equal parts, every part of 30 grams, respectively packs into 4 The inner diameter is 10 millimeters, long 80 millimeters of stainless steel tube tube type thousand 4 reactor shell pass hot water, then put acetic acid into storage tank 1, C4 distillate into storage tank 2, the olefin molar ratio of the two is 2, And add olefin polymerization inhibitor RP-1412 in acetic acid, the content is 200μg / g, acetic acid is fed through each section continuously with the pump from the top of the first section, and the acetic acid feeding amount per hour is 192 grams, and then the ester acid and the C4 fraction The amount of olefins with a molar ratio greater than 9 is connected to each section through the metering pumps of each section and the acetic acid pipe, and then mixed, and then passed into e...

Embodiment 3

[0026] With embodiment 1 equipment, increase two reactors (accompanying drawing is not shown), with macroporous strongly acidic cation exchange resin, model D-06, dry basis 150g is evenly divided into 5 equal parts, every part of 30 grams, packs 5 respectively A tube-and-tube reactor with an internal diameter of 10 mm and a length of 80 mm stainless steel tube is passed through hot water in the shell side, then the acetic acid is loaded into the storage tank 1, and the C4 fraction is loaded into the storage tank 2, and the olefin molar ratio of the two is 2. , and add olefin polymerization inhibitor RP-1412 in acetic acid, the content is 20μg / g, acetic acid is fed through each section continuously with the pump from the top of the first section, and the acetic acid feeding amount per hour is 150 grams, and then ester acid and C4 The amount of distillate olefin molar ratio greater than 9 is connected to each section through the metering pump of each section and the acetic acid p...

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Abstract

The invention relates to a process method for synthesizing sec-butyl acetate from C4 fractions. The process method is characterized in that acetic acid and C4 fractions are used as raw materials, macroporous strongly-acidic cation exchange resin is used as a catalyst, a 3-5-segment tubular fixed-bed reactor is employed, the acetic acid is fed in only one step, the C4 fractions are fed segment by segment, and the molar ratio of acetic acid to olefin in each segment of the reactor is greater than 9 when the total molar ratio of acetic acid to olefin in the reaction is 2-3; and an olefin polymerization inhibitor is simultaneously added to the reaction system at the adding amount of 20-200 mu g/g, and reaction is carried out at the reaction temperature of 50-120 DEG C and the reaction pressure of 1.0-2.0 MPa to generate sec-butyl acetate. The method has the advantages and effects that the selectivity of sec-butyl acetate is improved, the catalyst can be recycled and has long life, and the product has good quality.

Description

technical field [0001] The invention relates to a process for synthesizing sec-butyl acetate by fractionation of C4, which belongs to the field of organic chemical industry. Background technique [0002] Second-butyl acetate is a good organic solvent, which is widely used in nitrocellulose, paint, artificial leather, medicine, ink and plastic industries. The traditional method of producing sec-butyl acetate both at home and abroad is to adopt the batch-type tank reaction, and use sulfuric acid as a catalyst to catalyze the reaction of acetic acid and butanol. Because water is produced simultaneously in the esterification process of acetic acid and butanol, and water will not only cause the ester hydrolysis reaction of the reverse reaction of the esterification reaction, but also cause separation difficulties due to the azeotropy of water and acetic acid, so the current research mainly focuses on acetic acid and acetic acid. On the direct esterification of butene, as US60180...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04
CPCY02P20/584
Inventor 姚志龙尹振晏高俊斌
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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