CN106518678A - Method for refining diisobutyl sebacate - Google Patents
Method for refining diisobutyl sebacate Download PDFInfo
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- CN106518678A CN106518678A CN201510580135.4A CN201510580135A CN106518678A CN 106518678 A CN106518678 A CN 106518678A CN 201510580135 A CN201510580135 A CN 201510580135A CN 106518678 A CN106518678 A CN 106518678A
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- refining
- water
- stirring
- refining agent
- weight ratio
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for refining diisobutyl sebacate, and the method comprises the following steps: (1) an esterification step, to be more specific, pouring sebacic acid, isobutyl alcohol and concentrated sulfuric acid into a reaction kettle, stirring, and heating to boil for reaction, and keeping a boiling reflux state for separation of water in the reaction kettle; (2) a water washing process; (3) a refining step, to be more specific, adding a refining agent into a mixture after the water washing step, and stirring for refining for an hour; and (4) a filtering step, to be more specific, filtering a mixed solution filter after the refining step to obtain a diisobutyl sebacate product. The refining agent used in the method for preparation of the diisobutyl sebacate is a mixture of calcium hydroxide, magnesium hydroxide, activated carbon and magnesium sulfate, and has the advantages of low cost and easy purchase.
Description
Technical field
The invention belongs to field of organic compound preparation, especially a kind of SA diisobutyl ester is easy, effectively
Process for purification.
Background technology
In industrial production, plastics industry and war production, SA diisobutyl ester organises as one kind is important
Compound and cold resistant plasticizer, with being increasingly widely applied.The usual production method of SA diisobutyl ester is
Direct esterification is reacted, and the color for obtaining product is yellow, is difficult to sell as product, it is necessary to carry out further essence
System, that is, carry out the refinement treatment step that reduces pressure, the problem that such preparation method is present：1, due to the refinement treatment that reduces pressure
Need to realize using expensive high-vacuum pump in step, therefore, the method exist production equipment it is many,
Costly problem, thus it is difficult to reduces cost.2, as the refinement treatment step that reduces pressure is that production SA two is different
Essential and very time-consuming production stage during butyl ester, therefore, there is production time length, life in the method
The low problem of efficiency is produced, is unfavorable for the raising of Business Economic Benefit.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, using the refined SA diisobutyl ester of refining agent,
Equipment investment, reduces cost can be saved, is shortened the production time and is capable of improve production efficiency there is provided a kind of
SA diisobutyl ester preparation method.
It is to employ the following technical solutions realization that the present invention solves its technical problem：
A kind of process for purification of SA diisobutyl ester, the method are comprised the following steps：
(1) step of esterification
By SA, isobutanol, the concentrated sulfuric acid, in input reactor, stirring is heated to boiling reaction, keeps
Boiling reflux state separates moisture therein.
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification removes water layer therein.
(3) purification step
Refining agent will be added in mixture after washing, and stirring is refined one hour.
(4), filtration step
Mixed liquor after will be refined is filtered, and obtains SA diisobutyl ester product.
Described refining agent is potassium carbonate, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio, by 0.3：1：2：
1.8 mix.
The weight ratio of described refining agent and SA is 0.005 0.01：1
Described SA, isobutanol, the weight ratio of the concentrated sulfuric acid is 1：1.15：0.002—0.005
Described water is 0.5 with the weight ratio of SA：1.
Advantages of the present invention and good effect are：
1st, the preparation method of this SA diisobutyl ester is in purification step, using refining agent (calcium hydroxide, hydrogen
Magnesia, activated carbon, sulfuric acid magnesium compound), the product colour for obtaining shoals, it is not necessary to high vacuum refinement treatment
Product sale is can be used as, prepared product quality complies fully with technical requirement.This preparation method is being given birth to
High vacuum purification step is eliminated during product, it is to avoid the input of high-vacuum pump equipment, therefore, save equipment throwing
Money, reduces production cost, improves the competitiveness of product in market.
2nd, the refining agent that the preparation method of this SA diisobutyl ester is used is calcium hydroxide, magnesium hydroxide, activity
Charcoal, sulfuric acid magnesium compound, with cheap, it is easy to the characteristics of purchasing.
3rd, the preparation method of this SA diisobutyl ester have it is easy to operate, it is simple to facilitate implementation industrial metaplasia
Produce, improve production efficiency.
4th, the present invention in process of production, using refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, sulfuric acid
Magnesium compound), it is ensured that product quality and long term storage stability, while the present invention has realizes simple, operation side
Just the characteristics of, the investment of production equipment has been saved, production efficiency has been improve.
Specific embodiment
Below by specific embodiment, the present invention is further described：
Embodiment 1
The preparation method of this SA diisobutyl ester is comprised the following steps：
1. step of esterification
To carry heater, electricity stirring, thermometer water circulation condenser and oil water separator 300 liters
Put into SA double centner in reactor successively, 115 kilograms of isobutanol, 0.3 kilogram of the concentrated sulfuric acid, under agitation,
Micro-vacuum, while being heated to boiling reaction, keeps boiling reflux state, constantly by moisture from oil water separator
Separate out, until after no moisture is generated, stopping heating, esterification terminates.
2. water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification is removed
Water layer therein.
3. purification step
(calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate are mixed to add refining agent in the mixed liquor after washing
Compound) 0.5 kilogram, stirring mixing 1 hour.
4. filtration step
Refined mixed liquor is filtered, the liquid for obtaining is SA diisobutyl ester finished product, and the SA two is different
Butyl ester content 99.5%, color are less than No. 30 (platinum cobalt colorimetric).
Embodiment 2
The preparation method of this SA diisobutyl ester is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Put into SA double centner in 300 liters of reactors of device successively, 115 kilograms of isobutanol, 0.3 kilogram of the concentrated sulfuric acid,
Under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling reflux state, constantly from water-oil separating
Separate water into away in device, until after no moisture is generated, stopping heating, esterification terminates.
2. water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification is removed
Water layer therein.
3. purification step
(calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate are mixed to add refining agent in the mixed liquor after washing
Compound) 0.6 kilogram, stirring mixing 1 hour.
4. filtration step
Refined mixed liquor is filtered, the liquid for obtaining is SA diisobutyl ester finished product, and the SA two is different
Butyl ester content 99.5%, color are less than No. 30 (platinum cobalt colorimetric).
Embodiment 3
The preparation method of this SA diisobutyl ester is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
SA double centner, `115 kilogram of isobutanol, the concentrated sulfuric acid 0.3 thousand is put into successively in 300 liters of reactors of device
Gram, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling reflux state, constantly from profit
Separate water into away in separator, until after no moisture is generated, stopping heating, esterification terminates.
2. water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification is removed
Water layer therein.
3. purification step
(calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate are mixed to add refining agent in the mixed liquor after washing
Compound) 0.7 kilogram, stirring mixing 1 hour.
4. filtration step
Refined mixed liquor is filtered, the liquid for obtaining is SA diisobutyl ester finished product, and the SA two is different
Butyl ester content 99.5%, color are less than No. 30 (platinum cobalt colorimetric).
It is emphasized that example of the present invention is illustrative, rather than it is determinate, therefore this
The bright embodiment being not limited to described in specific embodiment, it is every of the invention by those skilled in the art
The other embodiment that technical scheme draws, also belongs to the scope of protection of the invention.
Claims (1)
1. a kind of process for purification of SA diisobutyl ester, it is characterised in that：The method is comprised the following steps：
(1) step of esterification
By SA, isobutanol, the concentrated sulfuric acid, in input reactor, stirring is heated to boiling reaction, keeps
Boiling reflux state separates moisture therein；
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification removes water layer therein；
(3) purification step
Refining agent will be added in mixture after washing, and stirring is refined one hour；
(4) filtration step
Mixed liquor after will be refined is filtered, and obtains SA diisobutyl ester product；
Described refining agent is potassium carbonate, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio, by 0.3: 1: 2:
1.8 mix；
The weight ratio of described refining agent and SA is 0.005-0.01: 1；
Described SA：Isobutanol：The weight ratio of the concentrated sulfuric acid is 1: 1.15: 0.002-0.005；
Described water is 0.5: 1 with the weight ratio of SA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510580135.4A CN106518678A (en) | 2015-09-11 | 2015-09-11 | Method for refining diisobutyl sebacate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510580135.4A CN106518678A (en) | 2015-09-11 | 2015-09-11 | Method for refining diisobutyl sebacate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518678A true CN106518678A (en) | 2017-03-22 |
Family
ID=58348074
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510580135.4A Pending CN106518678A (en) | 2015-09-11 | 2015-09-11 | Method for refining diisobutyl sebacate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518678A (en) |
-
2015
- 2015-09-11 CN CN201510580135.4A patent/CN106518678A/en active Pending
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Application publication date: 20170322 |