CN102911050A - Preparation method of diisobutyl adipate - Google Patents
Preparation method of diisobutyl adipate Download PDFInfo
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- CN102911050A CN102911050A CN 201210460509 CN201210460509A CN102911050A CN 102911050 A CN102911050 A CN 102911050A CN 201210460509 CN201210460509 CN 201210460509 CN 201210460509 A CN201210460509 A CN 201210460509A CN 102911050 A CN102911050 A CN 102911050A
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- diisobutyl adipate
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Abstract
The invention relates to a preparation method of diisobutyl adipate. The preparation method comprises the following steps of: (1) esterificatiion reaction; (2) water washing; (3) dealcoholization; (4) refining: adding a refining agent in a crude product after dealcoholization, stirring and refining for 1 hour, wherein the refining agent is formed by mixing calcium hydroxide, magnesium hydroxide and magnesium sulfate in a weight ratio of 1:1:2:1.5; and (5) filtering: filtering the refined mixed liquid to obtain the diisobutyl adipate product. According to the preparation method of diisobutyl adipate, in the refining step, the color of the product obtained by using the refining agent is light, the product can be sold without high-vacuumizing treatment, and the quality of the prepared product completely meets the technical index requirements. According to the preparation method, the high-vacuumizing refining step is omitted during production, and the investment of a high-vacuumizing pump is avoided, thus equipment investment is saved, production cost is reduced, and the market competitiveness of the product is improved.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of easy, effective diisobutyl adipate preparation method.
Background technology
In industrial production, in plastics industry and the war production, diisobutyl adipate has more and more widely and uses as a kind of important organic compounds and cold resistant plasticizer.The common production method of diisobutyl adipate is the direct esterification reaction, obtain the color of product for yellow, be difficult to sell as product, must further make with extra care, the refinement treatment that namely reduces pressure step, the problem that this type of preparation method exists: 1. owing to needing to use expensive high-vacuum pump to realize in the decompression refinement treatment step, therefore, there is the problem that production unit is many, expense is high in the method, thereby is difficult to reduce cost; 2. because decompression refinement treatment step is to produce essential and very consuming time production stage in the diisobutyl adipate process, therefore, there is the problem that the production time is long, production efficiency is low in the method, is unfavorable for the raising of Business Economic Benefit.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of use finishing agent to make with extra care diisobutyl adipate, the diisobutyl adipate preparation method who can save facility investment, reduces cost, shortens the production time and can enhance productivity.
It is to realize by the following technical solutions that the present invention solves its technical problem:
A kind of preparation method of diisobutyl adipate may further comprise the steps:
⑴ step of esterification
Hexanodioic acid, isopropylcarbinol, the vitriol oil are dropped in the reactor, stir, be heated to boiling reaction, keep boiling reflux state separation moisture wherein;
⑵ water-washing step
To add entry in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains the diisobutyl adipate crude product;
⑷ purification step
To add finishing agent in the crude product after the dealcoholysis, stirred refining 1 hour;
Described finishing agent is that calcium hydroxide, magnesium hydroxide, gac, sal epsom weight ratio 1:1:2:1.5 mix;
⑸ filtration step
Mixed solution after refining is filtered, obtain the diisobutyl adipate product.
And the weight ratio of described finishing agent and hexanodioic acid is 0.005-0.01:1.
And, described hexanodioic acid, isopropylcarbinol, the weight ratio of the vitriol oil is 1:3:0.002-0.005.
And the weight ratio of described water and hexanodioic acid is 0.5:1.
Advantage of the present invention and beneficial effect are:
1. the preparation method of this diisobutyl adipate is in purification step, and the product colour that uses finishing agent to obtain shoals, and does not need the high vacuum refinement treatment namely to can be used as product and sells, and prepared quality product meets the technical requirements fully.
2. this preparation method has saved the high vacuum purification step when producing, and has avoided the input of high-vacuum pump equipment, therefore, has saved facility investment, reduces production costs, and has improved the competitiveness of product in market.
3. the finishing agent that uses of the preparation method of this diisobutyl adipate is calcium hydroxide, magnesium hydroxide, gac, sal epsom mixture, have cheap, the characteristics that are easy to purchase.
4. the preparation method of this diisobutyl adipate has easy to operately, simplely is convenient to realize suitability for industrialized production, enhances productivity.
5. the present invention uses finishing agent to guarantee quality product and prolonged storage stability in process of production, and it is simple that simultaneously the present invention has realization, easy to operate characteristics, and the investment of having saved production unit has improved production efficiency.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of preparation method of diisobutyl adipate, step is as follows:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 300 kilograms of isopropylcarbinols, 0.3 kilogram of the vitriol oil, under agitation, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, diisobutyl adipate.
⑷ purification step
Add 0.5 kilogram of finishing agent (calcium hydroxide, magnesium hydroxide, gac, sal epsom mixture mix by weight 1:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is the diisobutyl adipate finished product, this diisobutyl adipate content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2
A kind of preparation method of diisobutyl adipate, step is as follows:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 300 kilograms of isobutyl ester alcohol, 0.3 kilogram of the vitriol oil, under agitation, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, diisobutyl adipate.
⑷ purification step
Add 0.6 kilogram of finishing agent (calcium hydroxide, magnesium hydroxide, gac, sal epsom mixture mix by weight 1:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is the diisobutyl adipate finished product, this diisobutyl adipate content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3
A kind of preparation method of diisobutyl adipate, step is as follows:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, isobutyl ester alcohol `300 kilogram, 0.3 kilogram of the vitriol oil, under agitation, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, diisobutyl adipate.
⑷ purification step
Add 0.7 kilogram of finishing agent (calcium hydroxide, magnesium hydroxide, gac, sal epsom mixture mix by weight 1:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is diisobutyl adipate ester finished product, this diisobutyl adipate ester content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Claims (4)
1. the preparation method of a diisobutyl adipate is characterized in that: may further comprise the steps:
⑴ step of esterification
Hexanodioic acid, isopropylcarbinol, the vitriol oil are dropped in the reactor, stir, be heated to boiling reaction, keep boiling reflux state separation moisture wherein;
⑵ water-washing step
To add entry in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains the diisobutyl adipate crude product;
⑷ purification step
To add finishing agent in the crude product after the dealcoholysis, stirred refining 1 hour;
Described finishing agent is that calcium hydroxide, magnesium hydroxide, gac, sal epsom weight ratio 1:1:2:1.5 mix;
⑸ filtration step
Mixed solution after refining is filtered, obtain the diisobutyl adipate product.
2. the preparation method of diisobutyl adipate according to claim 1, it is characterized in that: the weight ratio of described finishing agent and hexanodioic acid is 0.005-0.01:1.
3. the preparation method of diisobutyl adipate according to claim 1 is characterized in that: described hexanodioic acid, and isopropylcarbinol, the weight ratio of the vitriol oil is 1:3:0.002-0.005.
4. the preparation method of diisobutyl adipate according to claim 1, it is characterized in that: the weight ratio of described water and hexanodioic acid is 0.5:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210460509 CN102911050A (en) | 2012-11-14 | 2012-11-14 | Preparation method of diisobutyl adipate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210460509 CN102911050A (en) | 2012-11-14 | 2012-11-14 | Preparation method of diisobutyl adipate |
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| CN102911050A true CN102911050A (en) | 2013-02-06 |
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| CN 201210460509 Pending CN102911050A (en) | 2012-11-14 | 2012-11-14 | Preparation method of diisobutyl adipate |
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Application publication date: 20130206 |