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Synthesis method of dibutyl maleate

A technique for the synthesis of dibutyl maleate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as large amount of raw materials used, low product yield, and long production time , achieve the effect of shortening the reaction time of esterification, lowering the reaction temperature and saving cost

Inactive Publication Date: 2018-06-29
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is: long production time, high reaction temperature, high by-products, large raw material usage, low product yield, corrosion equipment and other problems in the existing sulfuric acid catalyzed dibutyl maleate synthesis process , the invention provides a kind of synthetic method of dibutyl maleate

Method used

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  • Synthesis method of dibutyl maleate
  • Synthesis method of dibutyl maleate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Such as figure 1 The schematic diagram of the technological process shown is operated, and in reactor, add 98kg maleic anhydride, 111kg n-butanol, 25kg hydrogen type cation exchange resin, heat up, open condenser, after being dissolved, open heat exchanger steam, Open the bottom valve of the reaction tank and the transfer pump, turn on the internal circulation, turn on the condenser to vacuumize, separate the produced water, control the reaction temperature in the tank at 90-125°C, react for 4 hours, distill, neutralize, and wash with water to obtain Product, testing product, the esterification rate is 99.3%.

Embodiment 2

[0019] Such as figure 1 The schematic diagram of the technological process shown is operated, and in reactor, add 98kg maleic anhydride, 148kg n-butanol, 35kg hydrogen type cation exchange resin, heat up, open condenser, after being dissolved, open heat exchanger steam, Open the bottom valve of the reaction tank and the transfer pump, turn on the internal circulation, and at the same time turn on the condenser to vacuumize, separate the produced water, control the reaction temperature in the tank at 80~110°C, react for 3 hours, distill, neutralize, wash with water, Obtain product, detect product, the esterification rate is 99.4%.

Embodiment 3

[0021] Such as figure 1 The schematic diagram of the technological process shown is operated, and in reactor, add 98kg maleic anhydride, 129kg n-butanol, 30kg hydrogen type cation exchange resin, heat up, open condenser, after being dissolved, open heat exchanger steam, Open the bottom valve of the reaction tank and the transfer pump, turn on the internal circulation, and at the same time open the condenser to vacuumize, separate the produced water, control the reaction temperature in the tank at 90~120°C, react for 3.5 hours, distill, neutralize, wash with water, Obtain product, detect product, the esterification rate is 99.4%.

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Abstract

The invention discloses a synthesis method of dibutyl maleate. The synthesis method of the dibutyl maleate comprises the steps of feeding maleic anhydride and n-butyl alcohol according to the proportion of 1:1.5 to 2.5, adding appropriate amount of catalyst, carrying out internal circulation by a circulating pump and a heat exchanger, reducing a system vacuum degree through vacuumizing, reflowingand separating water through a condenser, accelerating to separate water generated through esterification reaction out of a reaction system, reflowing the n-butyl alcohol into the system, continuouslyreacting, and controlling the reaction temperature to be 80 to 130 DEG C and the reaction time to be 3 to 4 hours. The industrial synthesis method of the dibutyl maleate provided by the invention hasthe advantages of short esterification reaction time and less side effect, the esterification rate can reach to notless than 99 percent, and the industrial production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, in particular to a synthetic method of dibutyl maleate. Background technique [0002] When dibutyl maleate is used in polyvinyl chloride products, it can make the products soft, smooth and transparent. Dibutyl maleate has a strong solvent ability and can effectively plasticize resins that are generally not easily plasticized (such as acrylonitrile and methacrylate resins). Dibutyl maleate is used as a raw material for synthetic resins and coatings, as well as impregnants, dispersants, lubricants, etc. in the petroleum industry, fabrics, plastics, and paper industries. The present industrial production of dibutyl maleate mainly uses sulfuric acid as a catalyst to synthesize maleic anhydride and n-butanol through direct esterification. Cause side reactions such as carbonization, oxidation, polymerization, isomerization, addition, etc., affect product quality, low product yield, a...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/60
CPCC07C67/08C07C69/60
Inventor 陈成效李鹏飞王宁宁程终发万振涛林胜涛
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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