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Method for removing water from ethyl acetate and butanone mixed solvent

A technology of ethyl acetate and mixed solvent, applied in the field of precise water removal, can solve the problems of easy agglomeration of sodium sulfate, poor economic effect, unsuitable for water removal, etc., and achieves simple post-treatment process, good treatment effect, and easy operation. Effect

Active Publication Date: 2013-03-20
JINAN SHENGQUAN GROUP SHARE HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pervaporation membrane can realize the water removal effect through the difference in the dissolution and diffusion rate of each component in the membrane, but firstly, it needs to introduce equipment. For the recovery of solvents, large-scale production is not required, and the cost of introducing equipment is too high; for hydrogenation The post-treatment of calcium and sodium hydride may cause an explosion when it meets water, which is quite dangerous; although sodium sulfate can also remove water, it is used in a large amount, and sodium sulfate is easy to agglomerate when it meets water, which is time-consuming and labor-intensive when cleaning equipment ; Anhydrous copper sulfate must be used in a large amount to remove water, and the economic effect is not good; molecular sieves are generally used for removing water from gases, not suitable for removing water in solvents

Method used

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  • Method for removing water from ethyl acetate and butanone mixed solvent
  • Method for removing water from ethyl acetate and butanone mixed solvent
  • Method for removing water from ethyl acetate and butanone mixed solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Take the mixture of ethyl acetate and methyl ethyl ketone, the water content in the mixture is between 2.5-3.2%, then add the mixture and calcium oxide into the distillation kettle at the same time, the amount of calcium oxide is respectively 10%, 12%, and 19%, 22%, 25%. After the addition, heat the still to 75-80°C, and heat to reflux at this temperature for 2-4 hours. After the reflux, continue to distill the mixed solution in the still, and recover ethyl acetate with a water content that meets the requirements through the condenser. The mixed solvent of ester and butanone, the water content in the mixed solvent is shown in Table 1 below.

[0020]

[0021] It can be seen from the above table that when the water content is below 4%, the dosage of calcium oxide in the range of 12-19% is more appropriate, and the removal effect of water in the mixed solvent is the best, which can not only meet the water content requirements, but also affect the later stage. There is ...

Embodiment 2

[0023] Take the mixture of ethyl acetate and methyl ethyl ketone, and detect that the moisture content in the mixture is 4-4.5%, then add the mixture and calcium oxide to the distillation kettle at the same time, and the consumption of calcium oxide is 15%, 19%, and 25%, 27%, 30%. After the addition, heat the still to 75-80°C, and heat to reflux at this temperature for 2-4 hours. After the reflux, continue to distill the mixed solution in the still, and recover ethyl acetate with a water content that meets the requirements through the condenser. The mixed solvent of ester and butanone, the water content in the mixed solvent is shown in Table 2 below.

[0024]

Embodiment 3

[0026] It is detected that the moisture content in the mixture obtained by distillation is 3.2%, and then the mixture and calcium oxide are added to the distillation kettle simultaneously, and the consumption of calcium oxide is 15.6% of the mixture quality. After the addition, heat the still to 75-80°C, and heat to reflux at this temperature for 2-3 hours. After the reflux, the moisture content in the still is detected to be 0.021%. After the reflux, pour out the mixed solution in the still. The generated calcium hydroxide is removed by centrifugation to obtain a mixed solvent of ethyl acetate and butanone with a water content meeting the requirements. The distillation pot from which the mixed solution is poured out can be cleaned with deionized water.

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Abstract

The invention discloses a method for removing water from an ethyl acetate and butanone mixed solvent. The method comprises a step of adding a drying agent into a water-containing mixture of ethyl acetate and butanone to remove water, wherein the drying agent is solid calcium oxide in an amount which is 12 to 25 percent of the weight of the water-containing mixture of the ethyl acetate and the butanone. A small amount of water is removed from the water-containing mixture of the ethyl acetate and the butanone by a drying method; the method is easy to operate, time-saving and labor-saving; the drying agent is the calcium oxide and has low price; the processing process is mild without danger; and the posttreatment process is simple, namely a kettle can be directly washed with deionized water and can also be properly washed with diluted hydrochloric acid. By the method, production cost is greatly reduced; the treatment effect is good; the water content of the treated mixed solvent can be reduced to below 0.05 percent; the effect is remarkable; and the actual application requirement is met.

Description

technical field [0001] The invention relates to a method for accurately removing water from a solvent, in particular to a method for accurately removing water from a mixture of ethyl acetate and butanone containing a small amount of water. Background technique [0002] The mixed solvent of ethyl acetate and methyl ethyl ketone generally acts as a reaction medium in organic synthesis, so the dosage is generally large. The price of ethyl acetate per ton is above 7,000 RMB, and the price of butanone per ton is about 12,000 RMB. After the organic synthesis reaction, more than 80% of each ton of ethyl acetate can be recovered, and more than 50% of each ton of butanone can be recovered. Quite a waste of raw material if not recycled. [0003] In some organic synthesis, a mixed solvent of ethyl acetate and methyl ethyl ketone with anhydrous or very little water content is often required. Treatment, so that the moisture contained in the solvent containing traces of water increases....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/56C07C49/10C07C45/79
Inventor 刘顶高绍丰柴小永郗遵波
Owner JINAN SHENGQUAN GROUP SHARE HLDG
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