CN106518681A - Refining method of dihexyl sebacate - Google Patents
Refining method of dihexyl sebacate Download PDFInfo
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- CN106518681A CN106518681A CN201510579874.1A CN201510579874A CN106518681A CN 106518681 A CN106518681 A CN 106518681A CN 201510579874 A CN201510579874 A CN 201510579874A CN 106518681 A CN106518681 A CN 106518681A
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- Prior art keywords
- mixture
- ester
- sebacic acid
- water
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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
-
- 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 refining method of dihexyl sebacate. The method comprises the following steps: (1) esterification reaction: adding sebacic acid, hexyl alcohol and concentrated sulfuric acid into a reaction kettle, stirring, heating to realize boiling reaction, and keeping in a boiling reflux state to separate water from a mixture; (2) washing: adding water into the mixture prepared by the esterification reaction, stirring uniformly, standing and layering to remove a water layer from the mixture; (3) dealcoholization: dealcoholizing the washed mixture to obtain a crude product of dihexyl sebacate; (4) refining and filtering, thus obtaining a dihexyl sebacate product. A refining agent used in the refining method of the dihexyl sebacate is a mixture of calcium hydroxide, magnesium hydroxide, activated carbon and magnesium sulfate, and has the characteristics of low cost and easiness for purchasing.
Description
Technical field
The invention belongs to the own ester of field of organic compound preparation, especially a kind of sebacic acid di-n is easy, effectively
Process for purification.
Background technology
In industrial production, plastics industry and war production, the own ester of sebacic acid di-n organises as one kind is important
Compound and cold resistant plasticizer, with being increasingly widely applied.The usual production method of the own ester of sebacic acid di-n 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 process for purification 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 production sebacic acid di-n
Essential and very time-consuming production stage during own 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 refining agent own ester of refined sebacic acid di-n,
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
The own ester process for purification of sebacic acid di-n.
It is to employ the following technical solutions realization that the present invention solves its technical problem：
A kind of process for purification of the own ester of sebacic acid di-n, the method are comprised the following steps：
(1) step of esterification
By SA, n-hexyl alcohol, 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) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, the own ester of sebacic acid di-n is obtained.
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour.
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains the own ester product of sebacic acid di-n.
Described refining agent is calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio, by 1：1：2：
1.5 mix.
The weight ratio of described refining agent and SA is 0.005 0.01：1
Described SA, n-hexyl alcohol, the weight ratio of the concentrated sulfuric acid is 1：1.6：0.002—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 process for purification of the own ester of this sebacic acid di-n 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 process for purification 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 process for purification of the own ester of this sebacic acid di-n 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 process for purification of the own ester of this sebacic acid di-n 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 process for purification of the own ester of this sebacic acid di-n 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, 160 kilograms of n-hexyl alcohol, 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. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, the own ester of sebacic acid di-n is obtained.
4. purification step
Refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixing is added in the crude product after dealcoholysis
Thing) 0.5 kilogram, stirring mixing 1 hour.
5. filtration step
By refined mixed liquor filter, the liquid for obtaining be the own ester finished product of sebacic acid di-n, the sebacic acid di-n
Own ester content 99.5%, color are less than No. 30 (platinum cobalt colorimetric).
Embodiment 2
The process for purification of the own ester of this sebacic acid di-n 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, 160 kilograms of n-hexyl alcohol, 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. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, the own ester of sebacic acid di-n is obtained.
4. purification step
Refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixing is added in the crude product after dealcoholysis
Thing) 0.6 kilogram, stirring mixing 1 hour.
5. filtration step
By refined mixed liquor filter, the liquid for obtaining be the own ester finished product of sebacic acid di-n, the sebacic acid di-n
Own ester content 99.5%, color are less than No. 30 (platinum cobalt colorimetric).
Embodiment 3
The process for purification of the own ester of this sebacic acid di-n 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, `160 kilogram of n-hexyl alcohol, 0.3 kilogram of the concentrated sulfuric acid are being stirred
Under, micro-vacuum, while being heated to boiling reaction, keeps boiling reflux state, constantly will from oil water separator
Water is separated, 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. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, the own ester of sebacic acid di-n is obtained.
4. purification step
Refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixing is added in the crude product after dealcoholysis
Thing) 0.7 kilogram, stirring mixing 1 hour.
5. filtration step
By refined mixed liquor filter, the liquid for obtaining be the own ester finished product of sebacic acid di-n, the sebacic acid di-n
Own 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. the process for purification of the own ester of a kind of sebacic acid di-n, it is characterised in that：The method is comprised the following steps：
(1) step of esterification
By SA, n-hexyl alcohol, 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) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, the own ester of sebacic acid di-n is obtained；
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour；
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains the own ester product of sebacic acid di-n；
Described refining agent is calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio, by 1：1：2：
1.5 mix；
The weight ratio of described refining agent and SA is 0.005 0.01：1；
Described SA：N-hexyl alcohol：The weight ratio of the concentrated sulfuric acid is 1：1.6：0.002—0.005；
Described water is 0.5 with the weight ratio of SA：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579874.1A CN106518681A (en) | 2015-09-11 | 2015-09-11 | Refining method of dihexyl sebacate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579874.1A CN106518681A (en) | 2015-09-11 | 2015-09-11 | Refining method of dihexyl sebacate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518681A true CN106518681A (en) | 2017-03-22 |
Family
ID=58348109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510579874.1A Pending CN106518681A (en) | 2015-09-11 | 2015-09-11 | Refining method of dihexyl sebacate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518681A (en) |
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2015
- 2015-09-11 CN CN201510579874.1A patent/CN106518681A/en active Pending
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| Date | Code | Title | Description |
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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 |