CN110423189A - A kind of novel acetylacetone,2,4-pentanedione synthesis method - Google Patents
A kind of novel acetylacetone,2,4-pentanedione synthesis method Download PDFInfo
- Publication number
- CN110423189A CN110423189A CN201910660834.8A CN201910660834A CN110423189A CN 110423189 A CN110423189 A CN 110423189A CN 201910660834 A CN201910660834 A CN 201910660834A CN 110423189 A CN110423189 A CN 110423189A
- Authority
- CN
- China
- Prior art keywords
- acetylacetone
- pentanedione
- reaction kettle
- rouge
- dilute
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/54—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition of compounds containing doubly bound oxygen atoms, e.g. esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/87—Preparation of ketenes or dimeric ketenes
- C07C45/89—Preparation of ketenes or dimeric ketenes from carboxylic acids, their anhydrides, esters or halides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/46—Preparation of carboxylic acid esters from ketenes or polyketenes
Landscapes
- 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 novel acetylacetone,2,4-pentanediones to synthesize method, includes the following steps: that weighing acetic acid puts into catalytic pyrolysis generation ketenes and vapor in pyrolysis furnace；Obtained ketenes is imported in the first steam generator, acetone is weighed to put into the second steam generator, two steam generators are connect with reaction kettle simultaneously by pipeline, the temperature of reaction kettle is controlled at 337 DEG C or so, catalyst sulfuric acid is slowly added into reaction kettle, ketenes and acetone generate the dilute rouge of isopropyl acetate under the catalysis of sulfuric acid, the dilute rouge of the isopropyl acetate of liquid is passed through in holding furnace by the gas that reaction generates after the separation of multi-stage condensing pipe, holding furnace keeps in-furnace temperature at 300 ~ 600 DEG C, vapor is passed through into holding furnace, make the dilute rouge of isopropyl acetate that isomerization reaction occur and generates acetylacetone,2,4-pentanedione, purification of products is generated to pure acetylacetone,2,4-pentanedione.This invention simplifies production procedures, are reacted using gaseous ketenes with acetone and improve reaction speed, and then improve the production efficiency of ethylene acetone.
Description
Technical field
The present invention relates to organic synthesis fields more particularly to a kind of novel acetylacetone,2,4-pentanedione to synthesize method.
Background technique
The runny transparency liquid of colourless or micro- Huang has the smell of ester, congeals into glossiness crystal when cooling.By light action
When, it is converted to brown liquid, and generate resin.- 23 DEG C of fusing point, 140.5 DEG C of boiling point, 139 DEG C (94.5kPa), relative density
0.9753, refractive index 1.4494, is dissolved in water, ethyl alcohol, ether, chloroform, acetone, benzene, glacial acetic acid by 40.56 DEG C of flash-point.Industrial goods tool
There is unhappy stink, is easily water dispersible as acetic acid and acetone.It is widely used in the fields such as medicine, veterinary drug, feed addictive, such as
The production efficiency of what raising acetylacetone,2,4-pentanedione is the critical issue of acetylacetone,2,4-pentanedione research.
Summary of the invention
It is an object of the invention to overcome problem above of the existing technology, a kind of novel acetylacetone,2,4-pentanedione synthesis side is provided
Method simplifies acetylacetone,2,4-pentanedione production procedure, improves acetylacetone,2,4-pentanedione production efficiency.
To realize above-mentioned technical purpose and the technique effect, the invention is realized by the following technical scheme:
A kind of novel acetylacetone,2,4-pentanedione synthesis method, includes the following steps:
(1) it weighs acetic acid and puts into catalytic pyrolysis generation ketenes and vapor in pyrolysis furnace；
(2) ketenes for obtaining step (1) imports in the first steam generator, weighs acetone and puts into the second steam generator
In, two steam generators are connect with reaction kettle simultaneously by pipeline, by the temperature control of reaction kettle at 337 DEG C or so, to
It is slowly added to catalyst sulfuric acid, ketenes and acetone in reaction kettle and generates the dilute rouge of isopropyl acetate under the catalysis of sulfuric acid, will react
The dilute rouge of the isopropyl acetate of liquid is passed through in holding furnace by the gas of generation after the separation of multi-stage condensing pipe, and holding furnace keeps temperature in furnace
Degree is at 300 ~ 600 DEG C；
(3) it is passed through the vapor of step (1) generation into the holding furnace of step (2), makes the dilute rouge of isopropyl acetate that isomerization reaction occur
Acetylacetone,2,4-pentanedione is generated, purification of products is generated to pure acetylacetone,2,4-pentanedione.
Further, the condensation temperature of the multi-stage condensing pipe respectively is 300 DEG C, 150 DEG C, 40 DEG C, makes sulfuric acid 300
The condensation of DEG C region is passed through the dilute rouge of isopropyl acetate in holding furnace in 150 DEG C of regions condensations, makes third along flowing back into reaction kettle
Ketone is in 40 DEG C of region condensing recoveries, residual gas recycling.
Further, the vapor generated in step (1) is stored in step (2) in the collet of reaction kettle.
Further, the reaction kettle, holding furnace, condenser pipe are all made of electrically heated mode and are heated.
The beneficial effects of the present invention are: ketenes, acetone, sulfuric acid first to be generated to gaseous state respectively, then hybrid reaction obtains second
The dilute rouge separation of isopropyl acetate in product gas is passed through in holding furnace through multi-stage condensing pipe and carries out isomerization reaction by the sour dilute rouge of isopropyl
Acetylacetone,2,4-pentanedione crude product is generated, production procedure is simplified, is reacted using gaseous ketenes with acetone and improve reaction speed, in turn
Improve the production efficiency of ethylene acetone.
Specific embodiment
Below in conjunction with embodiment, next the present invention will be described in detail.
A kind of novel acetylacetone,2,4-pentanedione synthesis method, includes the following steps:
(1) it weighs acetic acid and puts into catalytic pyrolysis generation ketenes and vapor in pyrolysis furnace；
(2) ketenes for obtaining step (1) imports in the first steam generator, weighs acetone and puts into the second steam generator
In, two steam generators are connect with reaction kettle simultaneously by pipeline, by the temperature control of reaction kettle at 337 DEG C or so, to
It is slowly added to catalyst sulfuric acid, ketenes and acetone in reaction kettle and generates the dilute rouge of isopropyl acetate under the catalysis of sulfuric acid, will react
The dilute rouge of the isopropyl acetate of liquid is passed through in holding furnace by the gas of generation after the separation of multi-stage condensing pipe, and holding furnace keeps temperature in furnace
Degree is at 300 ~ 600 DEG C；
(3) it is passed through the vapor of step (1) generation into the holding furnace of step (2), makes the dilute rouge of isopropyl acetate that isomerization reaction occur
Acetylacetone,2,4-pentanedione is generated, purification of products is generated to pure acetylacetone,2,4-pentanedione.
The condensation temperature of multi-stage condensing pipe respectively is 300 DEG C, 150 DEG C, 40 DEG C, makes 300 DEG C of regions of sulfuric acid condensation edge
Flow back into reaction kettle, making the dilute rouge of isopropyl acetate in 150 DEG C of regions, condensation is passed through in holding furnace, makes acetone in 40 DEG C of regions
Condensing recovery, residual gas recycling.
The vapor generated in step (1) is stored in step (2) in the collet of reaction kettle.
Reaction kettle, holding furnace, condenser pipe are all made of electrically heated mode and are heated.
Embodiment one: a kind of novel acetylacetone,2,4-pentanedione synthesis method includes the following steps:
(1) it weighs 100Kg acetic acid and puts into catalytic pyrolysis generation ketenes and vapor in pyrolysis furnace；
(2) ketenes for obtaining step (1) imports in the first steam generator, weighs 75Kg acetone and puts into the second steam generation
In devices, two steam generators are connect with reaction kettle simultaneously by pipeline, the temperature of reaction kettle is controlled at 337 DEG C or so,
It is slowly added to 6Kg catalyst sulfuric acid, ketenes and acetone into reaction kettle and generates the dilute rouge of isopropyl acetate under the catalysis of sulfuric acid, it will
It reacts the gas generated the dilute rouge of the isopropyl acetate of liquid is passed through in holding furnace after the separation of multi-stage condensing pipe, holding furnace keeps furnace
Interior temperature is at 300 ~ 600 DEG C；
(3) it is passed through the vapor of step (1) generation into the holding furnace of step (2), makes the dilute rouge of isopropyl acetate that isomerization reaction occur
Acetylacetone,2,4-pentanedione is generated, purification of products is generated to pure acetylacetone,2,4-pentanedione.
The condensation temperature of multi-stage condensing pipe respectively is 300 DEG C, 150 DEG C, 40 DEG C, makes 300 DEG C of regions of sulfuric acid condensation edge
Flow back into reaction kettle, making the dilute rouge of isopropyl acetate in 150 DEG C of regions, condensation is passed through in holding furnace, makes acetone in 40 DEG C of regions
Condensing recovery, residual gas recycling.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.
Claims (4)
1. a kind of novel acetylacetone,2,4-pentanedione synthesizes method, which comprises the steps of:
(1) it weighs acetic acid and puts into catalytic pyrolysis generation ketenes and vapor in pyrolysis furnace；
(2) ketenes for obtaining step (1) imports in the first steam generator, weighs acetone and puts into the second steam generator
In, two steam generators are connect with reaction kettle simultaneously by pipeline, by the temperature control of reaction kettle at 337 DEG C or so, to
It is slowly added to catalyst sulfuric acid, ketenes and acetone in reaction kettle and generates the dilute rouge of isopropyl acetate under the catalysis of sulfuric acid, will react
The dilute rouge of the isopropyl acetate of liquid is passed through in holding furnace by the gas of generation after the separation of multi-stage condensing pipe, and holding furnace keeps temperature in furnace
Degree is at 300 ~ 600 DEG C；
(3) it is passed through the vapor of step (1) generation into the holding furnace of step (2), makes the dilute rouge of isopropyl acetate that isomerization reaction occur
Acetylacetone,2,4-pentanedione is generated, purification of products is generated to pure acetylacetone,2,4-pentanedione.
2. novel acetylacetone,2,4-pentanedione according to claim 1 synthesizes method, it is characterised in that: the condensation of the multi-stage condensing pipe
Temperature respectively is 300 DEG C, 150 DEG C, 40 DEG C, makes 300 DEG C of region condensations of sulfuric acid along flowing back into reaction kettle, makes acetic acid
The dilute rouge of isopropyl is passed through in holding furnace in 150 DEG C of region condensations, makes acetone in 40 DEG C of region condensing recoveries, residual gas recycling.
3. novel acetylacetone,2,4-pentanedione according to claim 1 synthesizes method, it is characterised in that: the water generated in step (1) steams
Gas is stored in step (2) in the collet of reaction kettle.
4. novel acetylacetone,2,4-pentanedione according to claim 1 synthesizes method, it is characterised in that: the reaction kettle, holding furnace, cold
Solidifying pipe is all made of electrically heated mode and is heated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910660834.8A CN110423189A (en) | 2019-07-22 | 2019-07-22 | A kind of novel acetylacetone,2,4-pentanedione synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910660834.8A CN110423189A (en) | 2019-07-22 | 2019-07-22 | A kind of novel acetylacetone,2,4-pentanedione synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110423189A true CN110423189A (en) | 2019-11-08 |
Family
ID=68411621
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910660834.8A Withdrawn CN110423189A (en) | 2019-07-22 | 2019-07-22 | A kind of novel acetylacetone,2,4-pentanedione synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110423189A (en) |
-
2019
- 2019-07-22 CN CN201910660834.8A patent/CN110423189A/en not_active Withdrawn
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20210139402A1 (en) | Acrylic acid, and methods of producing thereof | |
| CN101143821B (en) | Method for preparing diethyl oxalate by coupling CO | |
| Liu et al. | Experimental investigation of hydrogen production integrated methanol steam reforming with middle-temperature solar thermal energy | |
| CN206701242U (en) | A kind of pipeline reactor for fine chemistry industry production | |
| CN102584775B (en) | Method for preparing epsilon-caprolactone | |
| CN106928021A (en) | A kind of method of preparing ethylene glycol by using dimethyl oxalate plus hydrogen | |
| CN103435483A (en) | Synthesis method for methyl acrylate from methyl acetate and formaldehyde | |
| CN103864615B (en) | A kind of method that continuous on-catalytic method prepares Trifluoroacetic Acid Ethyl Ester | |
| Song et al. | Conceptual design of water separation process in glycerol-based acrylic acid production | |
| CN105073705A (en) | Process for the preparation of succinic acid ester | |
| CN110423189A (en) | A kind of novel acetylacetone,2,4-pentanedione synthesis method | |
| CN110950754A (en) | Novel process for preparing chloro-propionyl chloride | |
| CN101875663A (en) | Preparation method and device of phenyl trichlorosilane | |
| CN102181135A (en) | Polybutylene terephthalate (PBT) material special for optical cables and band cables and manufacturing method of PBT material | |
| CN113387921A (en) | Method for synthesizing glycolide | |
| CN100420668C (en) | Process for synthesizing dimethylacetamide by ethyl acetate and dimethylamine | |
| CN102863316B (en) | Ethylene glycol production device | |
| CN102766029B (en) | Catalytic reaction rectification production method and device for high-purity natural benzaldehyde | |
| SG189954A1 (en) | Method for synthesizing beta-dicarbonyl compounds | |
| CN106977370A (en) | The method for preparing allyl alcohol | |
| CN107056612B (en) | Synthesis method of trifluoropyruvate compound | |
| CN108751180B (en) | Method for preparing carboxylation modified graphene by utilizing solid-phase reaction | |
| CN104829525B (en) | A kind of continuous reaction produces the method for the chloro-nicotinonitrile of 2- | |
| Pearson et al. | Phosphoric acid systems. 2. Catalytic conversion of fermentation ethanol to ethylene | |
| CN108191731A (en) | A kind of novel butyrolactam preparation process based on biomass material aminobutyric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20191108 |