CN106518680A - Preparation method of dihexyl sebacate - Google Patents
Preparation method of dihexyl sebacate Download PDFInfo
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- CN106518680A CN106518680A CN201510579641.1A CN201510579641A CN106518680A CN 106518680 A CN106518680 A CN 106518680A CN 201510579641 A CN201510579641 A CN 201510579641A CN 106518680 A CN106518680 A CN 106518680A
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- water
- sebacic acid
- ester
- mixture
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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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- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation 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 under micro-vacuum, 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 water layer from the mixture; (3) dealcoholization: dealcoholizing the washed mixture to obtain a crude product of dihexyl sebacate; (4) refining; (5) filtering. The preparation method of the dihexyl sebacate is convenient to operate, simple, easy and favorable for implementation of industrial production, and the production efficiency is improved.
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
Preparation method.
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 have and are increasingly widely applied.The usual production method of the own ester of sebacic acid di-n is straight
Esterification is connect, the color for obtaining product is yellow, is difficult to sell as product, it is necessary to further refined,
The refinement treatment step that reduces pressure, the problem that such preparation method is present are carried out：1, due to the refinement treatment step that reduces pressure
In need to realize using expensive high-vacuum pump, therefore, the method has that production equipment is more, expense
High problem, thus it is difficult to reduces cost.2, as the refinement treatment step that reduces pressure is the own ester of production sebacic acid di-n
During essential and very time-consuming production stage, therefore, there is production time length, production effect in the method
The low problem of rate, 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 preparation method 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 preparation method 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, micro-vacuum are heated to boiling anti-
Should, keep boiling reflux state to separate 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 oxide, magnesia, activated carbon, silica weight ratio, by 1：1：2：1
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 preparation method of the own ester of this sebacic acid di-n is in purification step, using refining agent (calcium oxide, oxidation
Magnesium, activated carbon, silica mixture), the product colour for obtaining shoals, it is not necessary to which high vacuum refinement treatment is
Can sell as product, prepared product quality complies fully with technical requirement.This preparation method is in production
When eliminate high vacuum purification step, it is to avoid the input of high-vacuum pump equipment, therefore, saved equipment investment,
Production cost is reduced, the competitiveness of product in market is improve.
2nd, the refining agent that the preparation method of the own ester of this sebacic acid di-n is used be calcium oxide, magnesia, activated carbon,
Silica mixture, with cheap, it is easy to the characteristics of purchasing.
3rd, the preparation method 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 oxide, magnesia, activated carbon, silica
Mixture), it is ensured that product quality and long term storage stability, while the present invention has realize simply, it is easy to operate
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 the own ester of this sebacic acid di-n is comprised the following steps：
1. step of esterification
The 300 of heater, electricity stirring, thermometer water circulation condenser and vacuum oil-in-water separator is carried to one
Put into SA double centner in rising reactor successively, 160 kilograms 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 oxide, magnesia, activated carbon, silica mixture) is added in the crude product after dealcoholysis
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 preparation method of the own ester of this sebacic acid di-n 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, 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 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. 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 oxide, magnesia, activated carbon, silica mixture) is added in the crude product after dealcoholysis
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 preparation method of the own ester of this sebacic acid di-n 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, 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 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. 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 oxide, magnesia, activated carbon, silica mixture) is added in the crude product after dealcoholysis
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 preparation method 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, micro-vacuum are heated to boiling anti-
Should, keep boiling reflux state to separate 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 oxide, magnesia, activated carbon, silica weight ratio, by 1: 1: 2: 1
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: 1 with the weight ratio of SA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579641.1A CN106518680A (en) | 2015-09-11 | 2015-09-11 | Preparation method of dihexyl sebacate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579641.1A CN106518680A (en) | 2015-09-11 | 2015-09-11 | Preparation method of dihexyl sebacate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518680A true CN106518680A (en) | 2017-03-22 |
Family
ID=58348055
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510579641.1A Pending CN106518680A (en) | 2015-09-11 | 2015-09-11 | Preparation method of dihexyl sebacate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518680A (en) |
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2015
- 2015-09-11 CN CN201510579641.1A patent/CN106518680A/en active Pending
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |