CN107814713A - A kind of preparation method of butyl caprylate - Google Patents

A kind of preparation method of butyl caprylate Download PDF

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Publication number
CN107814713A
CN107814713A CN201610823222.2A CN201610823222A CN107814713A CN 107814713 A CN107814713 A CN 107814713A CN 201610823222 A CN201610823222 A CN 201610823222A CN 107814713 A CN107814713 A CN 107814713A
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China
Prior art keywords
preparation
butyl caprylate
water
stirring
dealcoholysis
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CN201610823222.2A
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Chinese (zh)
Inventor
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 CN201610823222.2A priority Critical patent/CN107814713A/en
Publication of CN107814713A publication Critical patent/CN107814713A/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)
  • Fats And Perfumes (AREA)

Abstract

The present invention relates to a kind of preparation method of butyl caprylate, method comprises the following steps：(1) step of esterification, octanoic acid, the concentrated sulfuric acid, is put into reactor butanol, 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 this butyl caprylate 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 butyl caprylate
Technical field
The invention belongs to field of organic compound preparation, especially a kind of butyl caprylate is easy, effective preparation method.
Background technology
In industrial production, in plastics industry and war production, butyl caprylate is as a kind of important organic compounds and resists cold Plasticizer has more and more extensive application.The usual production method of butyl caprylate is direct esterification reaction, obtains the face of product Color is yellow, is difficult to sell as product, it is necessary to is further refined, that is, carries out depressurizing refinement treatment step, such preparation The problem of method is present：1, due to needing to use expensive high-vacuum pump to realize in decompression refinement treatment step, because This, there is the problem of production equipment is more, costly in this method, thus be difficult to reduce cost.2, due to depressurizing refinement treatment step It is to produce production stage that is essential and taking very much during butyl caprylate, therefore, it is long, raw that this method has the production time The problem of efficiency is low 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, and butyl caprylate is refined using refining agent, there is provided a kind of Equipment investment can be saved, cost is reduced, shorten the production time and the butyl caprylate preparation method of production efficiency can be improved.
The present invention, which solves its technical problem, to be realized using following technical scheme：
A kind of preparation method of butyl caprylate, it is characterised in that this method comprises the following steps：
(1) step of esterification
By octanoic acid, butanol, the concentrated sulfuric acid, put into reactor, stirring, micro-vacuum, be heated to boiling reaction, holding is seethed with excitement back Stream mode separates 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, butyl caprylate 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 butyl caprylate product.
Moreover, described refining agent is calcium oxide, magnesia, activated carbon, silica weight ratio, by 1：1：2：1 mixing Form.
Moreover, the weight ratio of described refining agent and octanoic acid is 0.005-0.01：1
Moreover, described octanoic acid, butanol, the weight ratio of the concentrated sulfuric acid is 1：1.6：0.002—0.005
Moreover, described water is 0.5 with pungent weight ratio：1.
The advantages and positive effects of the present invention are：
1st, the preparation method of this butyl caprylate uses refining agent (calcium oxide, magnesia, activated carbon, two in purification step Aktivton), obtained product colour shoals, it is not necessary to which high vacuum refinement treatment can be used as product sale, prepared Product quality comply fully with technical requirement.This preparation method eliminates high vacuum purification step in production, avoids The input of high-vacuum pump equipment, therefore, equipment investment is saved, reduced production cost, improve the competitiveness of product in market.
2nd, the refining agent that the preparation method of this butyl caprylate uses is calcium oxide, magnesia, activated carbon, silica mixing Thing, there is the characteristics of cheap, to be easy to buying.
3rd, the preparation method of this butyl caprylate has easy to operate, simple and easy to be easy to implement industrialized production, improves life Produce 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 butyl caprylate 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 sad double centner in kettle successively, 160 kilograms of butanol, 0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, heat simultaneously To boiling reaction, boiling reflux state is kept, is constantly separated water into away from oil water separator, until being generated without moisture Afterwards, heating is stopped, 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, butyl caprylate 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 butyl caprylate finished product, the butyl caprylate content 99.5%, face Color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2
The preparation method of this butyl caprylate comprises the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Sad double centner is put into 300 liters of reactors of device successively, 160 kilograms of butanol, 0.3 kilogram of the concentrated sulfuric acid, is being stirred Under, micro-vacuum, while boiling reaction is heated to, boiling reflux state is kept, is constantly separated water into away from oil water separator, 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, butyl caprylate 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 butyl caprylate finished product, the butyl caprylate content 99.5%, face Color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3
The preparation method of this butyl caprylate comprises the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Sad double centner is put into 300 liters of reactors of device successively, 160 kilograms of butanol, 0.3 kilogram of the concentrated sulfuric acid, is being stirred Under, micro-vacuum, while boiling reaction is heated to, boiling reflux state is kept, is constantly separated water into away from oil water separator, 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, butyl caprylate 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 butyl caprylate finished product, the butyl caprylate content 99.5%, face Color is 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 butyl caprylate, it is characterised in that：Method comprises the following steps：
    (1) step of esterification
    By octanoic acid, butanol, the concentrated sulfuric acid, put into reactor, stirring, micro-vacuum, be heated to boiling reaction, keep boiling reflux shape State separates 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, butyl caprylate 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 butyl caprylate product.
  2. 2. the preparation method of butyl caprylate according to claim 1, it is characterised in that：Described refining agent be calcium oxide, Magnesia, activated carbon, silica weight ratio, by 1：1：2：1 mixes.
  3. 3. the preparation method of butyl caprylate according to claim 1, it is characterised in that：Described refining agent and the weight of octanoic acid Amount is than being 0.005-0.01：1.
  4. 4. the preparation method of butyl caprylate according to claim 1, it is characterised in that：Described octanoic acid, butanol, the concentrated sulfuric acid Weight ratio be 1：1.6：0.002—0.005.
  5. 5. the preparation method of butyl caprylate according to claim 1, it is characterised in that：Described water is with pungent weight ratio 0.5：1.
CN201610823222.2A 2016-09-14 2016-09-14 A kind of preparation method of butyl caprylate Pending CN107814713A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610823222.2A CN107814713A (en) 2016-09-14 2016-09-14 A kind of preparation method of butyl caprylate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610823222.2A CN107814713A (en) 2016-09-14 2016-09-14 A kind of preparation method of butyl caprylate

Publications (1)

Publication Number Publication Date
CN107814713A true CN107814713A (en) 2018-03-20

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610823222.2A Pending CN107814713A (en) 2016-09-14 2016-09-14 A kind of preparation method of butyl caprylate

Country Status (1)

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CN (1) CN107814713A (en)

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