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Preparation method for dibutyl adipate

A technology of dibutyl adipate and adipic acid, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low esterification rate and long synthesis reaction time, and achieve reagent Safety, increase the reaction esterification rate, reduce the effect of reaction time

Inactive Publication Date: 2014-09-24
QINGDAO DONGFANG RECYCLING ENERGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem of long synthesis reaction time and low esterification rate of dibutyl oxalate in the prior art, the invention provides a kind of preparation method of dibutyl adipate

Method used

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  • Preparation method for dibutyl adipate
  • Preparation method for dibutyl adipate
  • Preparation method for dibutyl adipate

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preparation example Construction

[0012] The invention discloses a preparation method of dibutyl adipate, and those skilled in the art can refer to the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar substitutions and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The method and application of the present invention have been described through preferred embodiments, and the relevant personnel can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention to realize and Apply the technology of the present invention.

[0013] The invention provides a method for preparing dibutyl adipate, a compound whose structure is shown in formula I. FeCl 3 ·6H 2 O is a catalyst, and adipic acid and n-butanol are synthesized un...

Embodiment 1

[0020] The influence of embodiment 1 microwave on reaction

[0021] with FeCl 3 ·6H 2 O is a catalyst, with adipic acid and n-butanol as raw materials, esterification reaction occurs under the conditions of conventional heating and microwave radiation heating respectively, and the reaction time and reaction esterification rate are analyzed. The results are shown in Table 1:

[0022] Table 1 Effect of conventional heating and microwave radiation heating on the reaction

[0023]

[0024] Wherein, the calculation of esterification rate is calculated according to the following formula:

[0025]

[0026] The data in Table 1 shows that by using FeCl 3 ·6H 2 O was used as a catalyst, adipic acid and n-butanol were used as raw materials, and the synthesis reaction occurred under the condition of microwave radiation heating. The reaction time was shortened to 30 minutes, and the esterification rate was increased to 89.1%. In the synthesis reaction of dibutyl adipate, microwa...

Embodiment 2

[0027] The preparation of embodiment 2 dibutyl adipate

[0028] With 1.46g (0.01mol) adipic acid, 29.6g (0.4mol) n-butanol, 2.0g (0.007mol) FeCl 3 ·6H 2 O Equipped with a water separator, a thermometer and a reflux condenser in a three-necked quartz flask, dissolve the tape and shake it evenly, take a sample to measure its acid value, place it in a modified microwave reactor, and react with a microwave radiation power of 130w for 30min, then take a sample to measure its acid value after cooling down slightly Acid value, neutralize the reaction solution to weak acidity, then wash with water, dilute sodium carbonate and water respectively, dry and distill, distill n-butanol at normal pressure, distill under reduced pressure to obtain 2.29g of dimethyl adipate, The esterification rate is 88.8%, and the refractive index is 1.432 (25°C).

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Abstract

The invention relates to the field of chemical synthesis, and discloses a preparation method for dibutyl adipate. The preparation method is as follows: by taking FeCl3.6H2O as a catalyst and taking adipic acid and n-butyl alcohol as raw materials, generating synthesis reaction under microwave condition to prepare dibutyl adipate. The preparation method provided by the invention can effectively reduce reaction time, can improve a reaction esterification rate; and moreover, the preparation method is simple, adopts a safe reagent, and is beneficial to industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of dibutyl adipate. Background technique [0002] Dibutyl adipate (dibutyl adipate) is an organic acid ester compound, mainly used in flavors and flavor control agents, as well as plasticizers for vinyl and cellulose resins, as well as solvents and organic synthesis . Because this product has good compatibility with polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, polyvinyl butyral, nitrocellulose, butyl acetate fiber, etc., it is often used as a synthetic rubber for vinyl fiber resin plasticizer. In addition, it has low viscosity, good cold resistance but poor durability, and can also be used in nitrocellulose coatings. [0003] Usually dibutyl adipate (structure as shown in formula I) is obtained by the esterification reaction of adipic acid and n-butanol under the catalysis of sulfuric acid. This method has the advantages of high sulfuric ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08
CPCC07C67/08C07C69/44
Inventor 建方方马连湘石营蒋林年
Owner QINGDAO DONGFANG RECYCLING ENERGY
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