CN106518667A - Method for refining di-n-butyl adipate - Google Patents
Method for refining di-n-butyl adipate Download PDFInfo
- Publication number
- CN106518667A CN106518667A CN201510579873.7A CN201510579873A CN106518667A CN 106518667 A CN106518667 A CN 106518667A CN 201510579873 A CN201510579873 A CN 201510579873A CN 106518667 A CN106518667 A CN 106518667A
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- China
- Prior art keywords
- refining
- butyl adipate
- purification
- product
- stirring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- 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
Abstract
The invention relates to a method for refining di-n-butyl adipate. The method includes the esterification reaction step, the water washing step, the dealcoholization, the refining step and the filtering step. In the refining step, a refining agent is added into a crude product obtained after dealcoholization, and stirring and refining are conducted for one hour, wherein the refining agent is formed by mixing sodium carbonate, magnesium carbonate, activated carbon and magnesium sulfate according to the weight ratio of 1:1:2:1.5. In the filtering step, the prepared mixed solution is filtered to obtain a di-n-butyl adipate product. According to the method for refining di-n-butyl adipate, in the refining step, the product obtained through the refining agent is light in color and can be sold without being subjected to high-vacuum refining, and the quality of the prepared product completely meets requirements of technical indexes. The preparation method omits the high-vacuum refining step during production, and investment of high-vacuum pump equipment is avoided, so that equipment investment is saved, production cost is reduced, and market competitiveness of the product is improved.
Description
Technical field
The invention belongs to field of organic compound preparation, especially a kind of easy, effective Di-n-butyl Adipate process for purification.
Background technology
In industrial production, plastics industry and war production, Di-n-butyl Adipate is used as a kind of important organic compounds and cold-resistant increasing
Modeling agent, with being increasingly widely applied.The usual production method of Di-n-butyl Adipate is direct esterification reaction, obtains product
Color is yellow, is difficult to sell as product, it is necessary to further refined, that is, carry out the refinement treatment step that reduces pressure, such preparation
The problem that method is present：1. due to needing to realize using expensive high-vacuum pump in the refinement treatment step that reduces pressure, therefore,
The method has that production equipment is more, costly, thus is difficult to reduces cost；2. as the refinement treatment step that reduces pressure is production
Essential and very time-consuming production stage during Di-n-butyl Adipate, therefore, there is production time length, production in the method
The low problem of efficiency, 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, there is provided a kind of using the refined Di-n-butyl Adipate of refining agent, energy
Equipment investment, reduces cost is enough saved, is shortened the production time and is capable of the Di-n-butyl Adipate preparation method of improve production efficiency.
It is to employ the following technical solutions realization that the present invention solves its technical problem：
A kind of process for purification of Di-n-butyl Adipate, comprises the following steps：
(1) step of esterification
By in adipic acid, n-butanol, concentrated sulfuric acid input reactor, stirring is heated to boiling reaction, keeps boiling reflux state point
From moisture therein；
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification removes water layer therein；
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, Di-n-butyl Adipate crude product is obtained；
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined 1 hour；
The refining agent is sodium carbonate, magnesium carbonate, activated carbon, magnesium sulfate weight compare 1：1：2：1.5 mix；
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains Di-n-butyl Adipate product.
And, the weight ratio of described refining agent and adipic acid is 0.005 0.01：1.
And, described adipic acid, n-butanol, the weight ratio of the concentrated sulfuric acid is 1：3：0.002—0.005.
And, described water is 0.5 with the weight ratio of adipic acid：1.
The advantages of the present invention are：
1. in purification step, the product colour obtained using refining agent is shoaled the process for purification of this Di-n-butyl Adipate, it is not necessary to
High vacuum refinement treatment can be used as product sale, and prepared product quality complies fully with technical requirement.
2. this preparation method eliminates high vacuum purification step in production, it is to avoid the input of high-vacuum pump equipment, therefore, save
Equipment investment, reduces production cost, improves the competitiveness of product in market.
3. the refining agent that the process for purification of this Di-n-butyl Adipate is used be sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid magnesium compound,
With cheap, it is easy to the characteristics of purchasing.
4. the process for purification of this Di-n-butyl Adipate have it is easy to operate, it is simple to facilitate implementation industrialized production, improve production
Efficiency.
5. the present invention ensures product quality and long term storage stability using refining agent in process of production, while the present invention has realizing
Simply, easy to operate the characteristics of, the investment of production equipment has been saved, production efficiency has been improve.
Specific embodiment
With reference to embodiment, following embodiments are illustrative, are not determinate, it is impossible to limit this with following embodiments
Bright protection domain.
Embodiment 1
A kind of process for purification of Di-n-butyl Adipate, step are as follows：
(1) step of esterification
To in 500 liters of reactors for carrying heater, electricity stirring, thermometer water circulation condenser and oil water separator successively
Input adipic acid double centner, 300 kilograms of n-butanol, 0.3 kilogram of the concentrated sulfuric acid, under agitation, while boiling reaction is heated to,
Boiling reflux state is kept, is constantly separated water into away from oil water separator, until after no moisture is generated, stopping heating, ester
Change reaction terminating.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification removes water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, Di-n-butyl Adipate is obtained.
(4) purification step
(sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid magnesium compound, by weight 1 to add refining agent in the crude product after dealcoholysis：1：
2：1.5 mixing) 0.5 kilogram, stirring mixing 1 hour.
(5) filtration step
By refined mixed liquor filter, the liquid for obtaining be Di-n-butyl Adipate finished product, the Di-n-butyl Adipate content
99.5%, color is less than No. 30 (platinum cobalt colorimetric).
Embodiment 2
A kind of process for purification of Di-n-butyl Adipate, step are as follows：
(1) step of esterification
To in 500 liters of reactors for carrying heater, electricity stirring, thermometer water circulation condenser and oil water separator successively
Input adipic acid double centner, 300 kilograms of N-butyl alcohol, 0.3 kilogram of the concentrated sulfuric acid, under agitation, while boiling reaction is heated to,
Boiling reflux state is kept, is constantly separated water into away from oil water separator, until after no moisture is generated, stopping heating, ester
Change reaction terminating.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification removes water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, Di-n-butyl Adipate is obtained.
(4) purification step
(sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid magnesium compound, by weight 1 to add refining agent in the crude product after dealcoholysis：1：
2：1.5 mixing) 0.6 kilogram, stirring mixing 1 hour.
(5) filtration step
By refined mixed liquor filter, the liquid for obtaining be Di-n-butyl Adipate finished product, the Di-n-butyl Adipate content
99.5%, color is less than No. 30 (platinum cobalt colorimetric).
Embodiment 3
A kind of process for purification of Di-n-butyl Adipate, step are as follows：
(1) step of esterification
To in 500 liters of reactors for carrying heater, electricity stirring, thermometer water circulation condenser and oil water separator successively
Input adipic acid double centner, `300 kilogram of N-butyl alcohol, 0.3 kilogram of the concentrated sulfuric acid, under agitation, while boiling reaction is heated to,
Boiling reflux state is kept, is constantly separated water into away from oil water separator, until after no moisture is generated, stopping heating, ester
Change reaction terminating.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor to after esterification, after stirring, stratification removes water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, Di-n-butyl Adipate is obtained.
(4) purification step
(sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid magnesium compound, by weight 1 to add refining agent in the crude product after dealcoholysis：1：
2：1.5 mixing) 0.7 kilogram, stirring mixing 1 hour.
(5) filtration step
By refined mixed liquor filter, the liquid for obtaining be Di-n-butyl Adipate ester finished product, the Di-n-butyl Adipate ester content
99.5%, color is less than No. 30 (platinum cobalt colorimetric).
Claims (4)
1. a kind of process for purification of Di-n-butyl Adipate, it is characterised in that：Comprise the following steps：
(1) step of esterification
By in adipic acid, n-butanol, concentrated sulfuric acid input reactor, stirring is heated to boiling reaction, keeps boiling reflux state point
From moisture therein；
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification removes water layer therein；
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, Di-n-butyl Adipate crude product is obtained；
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined 1 hour；
The refining agent is sodium carbonate, magnesium carbonate, activated carbon, magnesium sulfate weight compare 1：1：2：1.5 mix；
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains Di-n-butyl Adipate product.
2. the process for purification of Di-n-butyl Adipate according to claim 1, it is characterised in that：Described refining agent and oneself two
The weight ratio of acid is 0.005 0.01：1.
3. the process for purification of Di-n-butyl Adipate according to claim 1, it is characterised in that：Described adipic acid, positive fourth
Alcohol, the weight ratio of the concentrated sulfuric acid is 1：3：0.002—0.005.
4. the process for purification of Di-n-butyl Adipate according to claim 1, it is characterised in that：Described water and adipic acid
Weight ratio is 0.5：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579873.7A CN106518667A (en) | 2015-09-11 | 2015-09-11 | Method for refining di-n-butyl adipate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579873.7A CN106518667A (en) | 2015-09-11 | 2015-09-11 | Method for refining di-n-butyl adipate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518667A true CN106518667A (en) | 2017-03-22 |
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ID=58348116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510579873.7A Pending CN106518667A (en) | 2015-09-11 | 2015-09-11 | Method for refining di-n-butyl adipate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518667A (en) |
-
2015
- 2015-09-11 CN CN201510579873.7A patent/CN106518667A/en active Pending
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |
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| WD01 | Invention patent application deemed withdrawn after publication |