CN107814711A - A kind of preparation method of sad 2 ethylhexyl - Google Patents

A kind of preparation method of sad 2 ethylhexyl Download PDF

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Publication number
CN107814711A
CN107814711A CN201610823058.5A CN201610823058A CN107814711A CN 107814711 A CN107814711 A CN 107814711A CN 201610823058 A CN201610823058 A CN 201610823058A CN 107814711 A CN107814711 A CN 107814711A
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China
Prior art keywords
octanoic acid
preparation
ethylhexyls
water
stirring
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CN201610823058.5A
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Chinese (zh)
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张富强
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Tianjin Chemical Reagent Research Institute
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Tianjin Chemical Reagent Research Institute
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Priority to CN201610823058.5A priority Critical patent/CN107814711A/en
Publication of CN107814711A publication Critical patent/CN107814711A/en
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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
    • C07C67/62—Use of additives, e.g. for stabilisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of preparation method of sad 2 ethylhexyl, this method comprises the following steps：(1) step of esterification, SA, the concentrated sulfuric acid, is put into reactor 2 ethyl hexanols, stirring, micro-vacuum, is heated to boiling reaction, keeps boiling reflux state to separate moisture therein；(2) water-washing step, water will be added in the mixture after esterification, after stirring, stratification, remove water layer therein；(3) dealcoholysis step；(4) purification step；(5) filtration step.The refining agent that the preparation method of the ethylhexyl of this octanoic acid 2 uses is calcium oxide, magnesia, activated carbon, silica mixture, has the characteristics of cheap, to be easy to buying.

Description

A kind of preparation method of octanoic acid -2- ethylhexyls
Technical field
The invention belongs to field of organic compound preparation, especially a kind of octanoic acid -2- ethylhexyls are easy, effective to prepare Method.
Background technology
In industrial production, in plastics industry and war production, octanoic acid -2- ethylhexyls are as a kind of important organic compounds And cold resistant plasticizer has more and more extensive application.The usual production method of octanoic acid -2- ethylhexyls is direct esterification reaction, The color for obtaining product is yellow, is difficult to sell as product, it is necessary to is further refined, that is, carries out depressurizing refinement treatment step Suddenly, the problem of such preparation method is present：1, due to needing to use expensive high-vacuum pump in decompression refinement treatment step It could realize, therefore, this method has the problem of production equipment is more, costly, thus is difficult to reduce cost.2, due to decompression essence Processing step processed is to produce production stage that is essential and taking very much during octanoic acid -2- ethylhexyls, therefore, this method The problem of long production time, low production efficiency be present, be 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, and octanoic acid -2- ethylhexyls are refined using refining agent, there is provided It is a kind of to save equipment investment, reduce cost, shorten the production time and the octanoic acid -2- ethyl hexyls of production efficiency can be improved Ester preparation method.
The present invention, which solves its technical problem, to be realized using following technical scheme：
A kind of preparation method of octanoic acid -2- ethylhexyls, it is characterised in that this method comprises the following steps：
(1) step of esterification
By SA, 2-Ethylhexyl Alcohol, the concentrated sulfuric acid, put into reactor, stirring, micro-vacuum, be heated to boiling reaction, protect Hold boiling reflux state and separate moisture therein.
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification, remove water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, octanoic acid -2- ethylhexyls are obtained.
(4) purification step
Refining agent will be added in crude product after dealcoholysis, stirring is refined one hour.
(5) filtration step
Mixed liquor after will be refined filters, and obtains octanoic acid -2- ethylhexyl products.
Moreover, described refining agent is calcium oxide, magnesia, activated carbon, silica weight ratio, by 1：1：2：1 mixing Form.
Moreover, described refining agent and the weight ratio of SA are 0.005-0.01：1.
Moreover, described SA：2-Ethylhexyl Alcohol：The weight ratio of the concentrated sulfuric acid is 1：1.6：0.002—0.005.
Moreover, described water and the weight ratio of SA are 0.5：1.
The advantages and positive effects of the present invention are：
1st, the preparation method of this octanoic acid -2- ethylhexyls uses refining agent (calcium oxide, magnesia, work in purification step Property charcoal, silica mixture), obtained product colour shoals, it is not necessary to high vacuum refinement treatment can be used as product sale, Prepared product quality complies fully with technical requirement.This preparation method eliminates high vacuum purification step in production, The input of high-vacuum pump equipment is avoided, therefore, equipment investment has been saved, has reduced production cost, the market for improving product is competing Strive power.
2nd, the refining agent that the preparation method of this octanoic acid -2- ethylhexyls uses is calcium oxide, magnesia, activated carbon, dioxy SiClx mixture, there is the characteristics of cheap, to be easy to buying.
3rd, the preparation method of this octanoic acid -2- ethylhexyls has easy to operate, simple and easy to be easy to implement industrialized production, Improve production efficiency.
4th, the present invention in process of production, using refining agent (calcium oxide, magnesia, activated carbon, silica mixture), Ensure product quality and long term storage stability, while the present invention has the characteristics of realizing simply, easy to operate, has saved production The investment of equipment, improves production efficiency.
Embodiment
Below by specific embodiment, the present invention is further described：
Embodiment 1
The preparation method of this octanoic acid -2- ethylhexyls comprises the following steps：
(1) step of esterification
Heater is carried to one, and electricity stirring, 300 liters of thermometer water circulation condenser and vacuum oil-in-water separator are anti- Answer and put into SA double centner in kettle successively, 160 kilograms of 2-Ethylhexyl Alcohol, 0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, Boiling reaction is heated to simultaneously, boiling reflux state is kept, is constantly separated water into away from oil water separator, until not having water Mitogenetic to stop heating into rear, esterification terminates.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor after to esterification, after stirring, stratification, remove therein Water layer.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, octanoic acid -2- ethylhexyls are obtained.
(4) purification step
Refining agent (calcium oxide, magnesia, activated carbon, silica mixture) 0.5 thousand is added into the crude product after dealcoholysis Gram, it is stirred 1 hour.
(5) filtration step
Refined mixed liquor is filtered, obtained liquid is octanoic acid -2- ethylhexyl finished products, the octanoic acid -2- ethyl hexyls Ester content 99.5%, color are less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2
The preparation method of this octanoic acid -2- ethylhexyls comprises 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, 160 kilograms of 2-Ethylhexyl Alcohol, the concentrated sulfuric acid 0.3 thousand are put into 300 liters of reactors of device successively Gram, under agitation, micro-vacuum, while boiling reaction is heated to, boiling reflux state is kept, by water constantly from oil water separator Separate, until after without moisture generation, stop heating, esterification terminates.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor after to esterification, after stirring, stratification, remove therein Water layer.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, octanoic acid -2- ethylhexyls are obtained.
(4) purification step
Refining agent (calcium oxide, magnesia, activated carbon, silica mixture) 0.6 thousand is added into the crude product after dealcoholysis Gram, it is stirred 1 hour.
(5) filtration step
Refined mixed liquor is filtered, obtained liquid is octanoic acid -2- ethylhexyl finished products, the octanoic acid -2- ethyl hexyls Ester content 99.5%, color are less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3
The preparation method of this octanoic acid -2- ethylhexyls comprises 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, 160 kilograms of 2-Ethylhexyl Alcohol, the concentrated sulfuric acid 0.3 thousand are put into 300 liters of reactors of device successively Gram, under agitation, micro-vacuum, while boiling reaction is heated to, boiling reflux state is kept, by water constantly from oil water separator Separate, until after without moisture generation, stop heating, esterification terminates.
(2) water-washing step
Obtain adding 50 kilograms of water in mixed liquor after to esterification, after stirring, stratification, remove therein Water layer.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, octanoic acid -2- ethylhexyls are obtained.
(4) purification step
Refining agent (calcium oxide, magnesia, activated carbon, silica mixture) 0.7 thousand is added into the crude product after dealcoholysis Gram, it is stirred 1 hour.
(5) filtration step
Refined mixed liquor is filtered, obtained liquid is octanoic acid -2- ethylhexyl finished products, the octanoic acid -2- ethyl hexyls 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 limited, therefore the present invention is not It is limited to the embodiment described in embodiment, it is every to be drawn by those skilled in the art's technique according to the invention scheme Other embodiment, also belong to the scope of protection of the invention.

Claims (5)

  1. A kind of 1. preparation method of octanoic acid -2- ethylhexyls, it is characterised in that：This method comprises the following steps：
    (1) step of esterification
    By SA, 2-Ethylhexyl Alcohol, the concentrated sulfuric acid, put into reactor, stirring, micro-vacuum, be heated to boiling reaction, keep boiling Rise reflux state and separate moisture therein；
    (2) water-washing step
    Water will be added in mixture after esterification, after stirring, stratification, remove water layer therein；
    (3) dealcoholysis step
    By the mixture after washing, dealcoholysis, crude product, octanoic acid -2- ethylhexyls are obtained；
    (4) purification step
    Refining agent will be added in crude product after dealcoholysis, stirring is refined one hour；
    (5) filtration step
    Mixed liquor after will be refined filters, and obtains octanoic acid -2- ethylhexyl products.
  2. 2. the preparation method of octanoic acid -2- ethylhexyls according to claim 1, it is characterised in that：Described refining agent is Calcium oxide, magnesia, activated carbon, silica weight ratio, by 1：1：2：1 mixes.
  3. 3. the preparation method of octanoic acid -2- ethylhexyls according to claim 1, it is characterised in that：Described refining agent and The weight ratio of SA is 0.005-0.01：1.
  4. 4. the preparation method of octanoic acid -2- ethylhexyls according to claim 1, it is characterised in that：Described SA：2- Ethyl hexanol：The weight ratio of the concentrated sulfuric acid is 1：1.6：0.002—0.005.
  5. 5. the preparation method of octanoic acid -2- ethylhexyls according to claim 1, it is characterised in that：Described water and certain herbaceous plants with big flowers two The weight ratio of acid is 0.5：1.
CN201610823058.5A 2016-09-14 2016-09-14 A kind of preparation method of sad 2 ethylhexyl Pending CN107814711A (en)

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Application Number Priority Date Filing Date Title
CN201610823058.5A CN107814711A (en) 2016-09-14 2016-09-14 A kind of preparation method of sad 2 ethylhexyl

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610823058.5A CN107814711A (en) 2016-09-14 2016-09-14 A kind of preparation method of sad 2 ethylhexyl

Publications (1)

Publication Number Publication Date
CN107814711A true CN107814711A (en) 2018-03-20

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

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Application publication date: 20180320