CN105037123B - A kind of method that continuity method produces DAA - Google Patents
A kind of method that continuity method produces DAA Download PDFInfo
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- CN105037123B CN105037123B CN201510452592.5A CN201510452592A CN105037123B CN 105037123 B CN105037123 B CN 105037123B CN 201510452592 A CN201510452592 A CN 201510452592A CN 105037123 B CN105037123 B CN 105037123B
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- tower
- daa
- acetone
- product
- temperature
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- 238000000034 method Methods 0.000 title claims abstract description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 150000002576 ketones Chemical class 0.000 claims description 2
- XLSMFKSTNGKWQX-UHFFFAOYSA-N hydroxyacetone Chemical compound CC(=O)CO XLSMFKSTNGKWQX-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000007592 spray painting technique Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
- C07C45/73—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups combined with hydrogenation
-
- 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
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method of continuous production DAA, it is comprised the following steps：Acetone is continuously squeezed into by flow reactor by pump, continuous conveying enters destilling tower to reacted feed liquid again, continuous still in a distillation column removes most of unreacted acetone, continuous conveying enters after-fractionating tower again, the remaining acetone of distillation removal, DAA first product is obtained, the acetone that destilling tower and after-fractionating tower are steamed is delivered continuously to flow reactor again to be continued to react.The DAA first product that distillation is obtained is delivered continuously to product rectifying column, and DAA finished product is continuously separated out from rectifying column.The method that the continuity method that the present invention is provided produces DAA, with equipment investment is few, production capacity big, production process energy consumption is low, without " three wastes " discharge, product DAA steady quality, content 99.5%~99.9%, the features such as quality is high.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, and in particular to a kind of yield is high, and steady quality, energy consumption is low,
The DAA continuous producing method of catalyst need not be added.
Technical background
DAA also known as methylpentanolone, diacetone alcohol, are a kind of colourless liquid.With pleasant fragrance, energy
With water, ethanol, ether and other immiscible organic solvents.As high boiling solvent, spray painting diluent, woodstain and anti-corrosion
The raw material of agent, rust remover and dyestuff etc., it is also possible to make the raw material of dyestuff and the solution of resin etc..
Chinese patent CN1787986A, CN102757327A, CN103724172A each provide DAA reaction and use
The method such as catalyst, reaction condition, preparation flow, often have that the reaction time is long, catalyst preparation process is complicated, use the longevity
Life is short, and equipment investment is big, and production capacity is low, high energy consumption and be all batch production process, and process is whard to control, product content is low (general
98.2% or so) deficiency such as, quality is unstable, it is difficult to realize the continuous prodution of DAA.
The content of the invention
Goal of the invention：Deficiency the invention aims to solve prior art presence, there is provided a kind of technological design is closed
Reason, yield is high, steady quality, the low DAA continuous producing method of energy consumption.
Technical scheme：In order to realize the above object the technical scheme that the present invention takes is：
A kind of method that continuity method produces DAA, it is comprised the following steps：
Acetone is continuously squeezed into flow reactor with pump, between -20 DEG C of controlling reaction temperature~35 DEG C, flow reactor goes out
Mouth sampling, conversion per pass reaches 10%~25%, and continuous conveying enters destilling tower to reacted feed liquid again, controls destilling tower tower
54 DEG C~100 DEG C of the temperature in top, 60 DEG C~120 DEG C of destilling tower bottom temperature, distillation removal is most of unreacted in a distillation column
Acetone, then continuous conveying enters after-fractionating tower, 54 DEG C~100 DEG C of control second distillation column overhead temperatures, after-fractionating tower tower
65 DEG C~120 DEG C of kettle temperature degree, the remaining acetone of distillation removal, obtains DAA first product (percentage composition 75%~98%).Will
The acetone that destilling tower and after-fractionating tower are steamed is delivered continuously to flow reactor again to be continued to react, the DAA that distillation is obtained
First product is delivered continuously to product rectifying column, 54 DEG C~100 DEG C of control rectifying column tower top temperature, and tower bottom of rectifying tower temperature 60 C~
120 DEG C of rectifying, DAA finished product is continuously separated out from rectifying column.
Preferably, the method that above-described continuity method produces DAA, the DAA for preparing into
The percentage composition of product is 99.5%~99.9%.
Preferably, the method that above-described continuity method produces DAA, control overhead temperature 55
DEG C~65 DEG C, 90 DEG C~110 DEG C of destilling tower bottom temperature.
Preferably, the method that above-described continuity method produces DAA, controls second distillation column overhead temperature
55 DEG C~64 DEG C of degree, 92 DEG C~100 DEG C of after-fractionating tower bottom temperature.
Preferably, the method that above-described continuity method produces DAA, control rectifying column tower top temperature 62
DEG C~64 DEG C, 98 DEG C~100 DEG C rectifying of tower bottom of rectifying tower temperature.
The continuity method that the present invention is provided produces the special equipment of DAA, and it includes：Flow reactor, with successive reaction
The connected destilling tower of device, the after-fractionating tower being connected with destilling tower, the rectifying column being connected with after-fractionating tower.
Compared to the prior art, the present invention has the following advantages：
The present invention screens the method that the continuity method for obtaining produces DAA by many experiments, especially destilling tower, two
The tower reactor and tower top temperature of secondary destilling tower and rectifying column, whole technique have that reaction time is short, equipment investment is small, production capacity
It is high, energy consumption is low, continuous production processes process is easy to control, product content (general 99.5%~99.9%), steady quality, production high
The features such as process is discharged without " three wastes ", with important application value.
Brief description of the drawings
The structural representation of the special equipment of the continuity method production DAA that Fig. 1 is provided for the present invention.
Specific implementation method
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
The modification of form falls within the application appended claims limited range.
Embodiment 1
A kind of method that continuity method produces DAA, it is comprised the following steps：
As shown in figure 1, acetone first is entered into flow reactor (1) with the flow of 2000L/h, 5 DEG C of the temperature of reaction is controlled
~15 DEG C, conversion ratio 18%~22%, the feed liquid of outflow enters back into destilling tower (2), 92~100 DEG C of bottom temperature, tower top temperature
55~64 DEG C, tower top acetone flow 1500L/h, tower reactor feed liquid delivers into after-fractionating tower (3), tower reactor temperature with 500L/h flows
Degree 92~100 DEG C, 55~64 DEG C of tower top temperature, second distillation tower top acetone reflux amount 85L/h, tower reactor DAA first product with
415L/h flows enter rectifying column (4), 98~100 DEG C of bottom temperature, 62~64 DEG C of tower top temperature, rectifying column DAA product
Flow 400l/h, tower top acetone reflux amount 15l/h.The acetone that destilling tower (1), after-fractionating tower (2) and rectifying column (4) are steamed
Continuation is reacted in being transported to flow reactor (1) again.The device continuously runs 168 hours, and being continuously available percentage composition is
99.75%~99.85% DAA.
Embodiment 2
A kind of method that continuity method produces DAA, it is comprised the following steps：
Acetone is entered into flow reactor (1), 0 DEG C of the temperature that control is reacted~10 DEG C, conversion ratio with the flow of 5000L/h
18%~25%, the feed liquid of outflow enters back into destilling tower (2), 90~95 DEG C of bottom temperature, 58~65 DEG C of tower top temperature, tower top third
Ketone flow 4000L/h, tower reactor feed liquid delivers into after-fractionating tower (3), 92~100 DEG C of bottom temperature, tower with 1000L/h flows
55~64 DEG C of the temperature in top, second distillation tower top acetone reflux amount 185L/h, tower reactor DAA first product is entered with 815L/h flows
Rectifying column (4), 98~100 DEG C of bottom temperature, 62~64 DEG C of tower top temperature, rectifying column DAA product flow 800l/h, tower
Push up acetone reflux amount 15l/h.The acetone that destilling tower (1), after-fractionating tower (2) and rectifying column (4) are steamed is transported to continuously again
Continue to react in reactor (1).The device continuously runs 168 hours, and it is 99.55%~99.75% to be continuously available percentage composition
DAA.
Embodiment 3
A kind of method that continuity method produces DAA, it is comprised the following steps：
Acetone is entered into flow reactor (1), 2 DEG C of the temperature that control is reacted~17 DEG C, conversion ratio with the flow of 8000L/h
20%~25%, the feed liquid of outflow enters back into destilling tower (2), 92~100 DEG C of bottom temperature, 55~64 DEG C of tower top temperature, tower top
Acetone flow 5800L/h, tower reactor feed liquid delivers into after-fractionating tower (3) with 2200L/h flows, 92~100 DEG C of bottom temperature,
55~64 DEG C of tower top temperature, second distillation tower top acetone reflux amount 320L/h, tower reactor DAA first product is entered with 1900L/h flows
Enter rectifying column (4), 98~100 DEG C of bottom temperature, 62~64 DEG C of tower top temperature, rectifying column DAA product flow 1800l/h,
Tower top acetone reflux amount 100L/h.The acetone that destilling tower (1), after-fractionating tower (2) and rectifying column (4) the are steamed company of being transported to again
Continue to react in continuous reactor (1).Continuous operation 168 hours of the device, be continuously available percentage composition for 99.60%~
99.85% DAA.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of method that continuity method produces DAA, it is characterised in that comprise the following steps：
Acetone is entered into flow reactor (1) with the flow of 5000L/h, 0 DEG C~10 DEG C of the temperature of reaction, conversion ratio 18% is controlled
~25%, the feed liquid of outflow enters back into destilling tower (2), 90~95 DEG C of bottom temperature, 58~65 DEG C of tower top temperature, tower top acetone stream
Amount 4000L/h, tower reactor feed liquid delivers into after-fractionating tower (3), 92~100 DEG C of bottom temperature, tower top temperature with 1000L/h flows
55~64 DEG C of degree, second distillation tower top acetone reflux amount 185L/h, tower reactor DAA first product enters rectifying with 815L/h flows
Tower (4), 98~100 DEG C of bottom temperature, 62~64 DEG C of tower top temperature, rectifying column DAA product flow 800L/h, tower top third
Ketone capacity of returns 15L/h；The acetone that destilling tower (2), after-fractionating tower (3) and rectifying column (4) are steamed is transported to successive reaction again
Continue in device (1) to react, continuous operation 168 hours of the device, be continuously available that percentage composition is 99.55%~99.75% two
Pyruvic alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510452592.5A CN105037123B (en) | 2015-07-28 | 2015-07-28 | A kind of method that continuity method produces DAA |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510452592.5A CN105037123B (en) | 2015-07-28 | 2015-07-28 | A kind of method that continuity method produces DAA |
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| Publication Number | Publication Date |
|---|---|
| CN105037123A CN105037123A (en) | 2015-11-11 |
| CN105037123B true CN105037123B (en) | 2017-06-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510452592.5A Expired - Fee Related CN105037123B (en) | 2015-07-28 | 2015-07-28 | A kind of method that continuity method produces DAA |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496414B (en) * | 2019-09-19 | 2021-04-27 | 福州大学 | Continuous reaction rectification equipment for synthesizing diacetone alcohol and process thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004101485A1 (en) * | 2003-05-15 | 2004-11-25 | Mitsubishi Chemical Corporation | Process for producing diacetone alcohol |
| CN103724172B (en) * | 2014-01-17 | 2016-01-20 | 天津市道福化工新技术开发有限公司 | The synthesis technique of diacetone alcohol |
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| CN105037123A (en) | 2015-11-11 |
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