CN105037123A - Method for producing diacetone alcohol through continuous method - Google Patents
Method for producing diacetone alcohol through continuous method Download PDFInfo
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- CN105037123A CN105037123A CN201510452592.5A CN201510452592A CN105037123A CN 105037123 A CN105037123 A CN 105037123A CN 201510452592 A CN201510452592 A CN 201510452592A CN 105037123 A CN105037123 A CN 105037123A
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- Prior art keywords
- tower
- diacetone alcohol
- temperature
- distillation
- acetone
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- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 238000011437 continuous method Methods 0.000 title abstract 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000004821 distillation Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 3
- 239000012043 crude product Substances 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 2
- 238000010992 reflux Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009466 transformation Effects 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
- 239000000975 dye Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013461 design Methods 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
- 239000003973 paint 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
- 239000007921 spray Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 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 method for producing diacetone alcohol through a continuous method. The method comprises the following steps: continuously feeding acetone into a continuous reactor through a pump, continuously conveying material liquid after reaction to a distillation tower, continuously distilling in the distillation tower for removing most unreacted acetone, continuously conveying material liquid to a secondary distillation tower, distilling for removing residual acetone so as to obtain a diacetone alcohol crude product, continuously conveying acetone distilled out from the distillation tower and the secondary distillation tower to the continuous reactor for continuous reaction, continuously conveying the diacetone alcohol crude product obtained through distillation to a product distillation tower and continuously separating a diacetone alcohol finished product from the distillation tower. The method for producing diacetone alcohol through the continuous method, provided by the invention, has the characteristics that equipment investment is less, high productivity, low energy consumption in the production process, and no three waste emission are realized, and the product diacetone alcohol is stable in quality, 99.5-99.9% in the content and high in quality.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, it is high to be specifically related to a kind of productive rate, steady quality, and energy consumption is low, does not need the diacetone alcohol continuous production method of adding catalyzer.
Technical background
Diacetone alcohol has another name called methylpentanolone, Pyranton, is a kind of colourless liquid.There is pleasant fragrance, can with water, ethanol, ether and other immiscible organic solvent.As the raw material of high boiling solvent, the thinner that sprays paint, woodstain and sanitas, rust remover and dyestuff etc., also can be used as the raw material of dyestuff and the solution etc. of resin.
Chinese patent CN1787986A, CN102757327A, CN103724172A each provide the method such as catalyzer, reaction conditions, preparation flow of diacetone alcohol reaction, often there is long reaction time, catalyst preparation process is complicated, work-ing life is short, facility investment is large, production capacity is low, energy consumption is high and be all batch production process, the deficiencies such as process is wayward, product content is low (general about 98.2%), quality is unstable, are difficult to the continuous prodution realizing diacetone alcohol.
Summary of the invention
Goal of the invention: the object of the invention is the deficiency existed to solve prior art, provide a kind of technological design reasonable, productive rate is high, steady quality, the diacetone alcohol continuous production method that energy consumption is low.
Technical scheme: in order to realize above object, the technical scheme that the present invention takes is:
Continuous processing produces a method for diacetone alcohol, and it comprises the following steps:
With pump, acetone is squeezed into flow reactor continuously, control between temperature of reaction-20 DEG C ~ 35 DEG C, flow reactor outlet sampling, per pass conversion reaches 10% ~ 25%, reacted feed liquid again continus convergence enters distillation tower, control overhead temperature 54 DEG C ~ 100 DEG C, distillation tower bottom temperature 60 DEG C ~ 120 DEG C, most of unreacted acetone is removed in distillation in a distillation column, continus convergence enters after-fractionating tower again, control second distillation column overhead temperatures 54 DEG C ~ 100 DEG C, after-fractionating tower bottom temperature 65 DEG C ~ 120 DEG C, remaining acetone is removed in distillation, obtain diacetone alcohol first product (percentage composition 75% ~ 98%).Acetone distillation tower and after-fractionating tower steamed is delivered continuously to flow reactor again and continues reaction, distill the diacetone alcohol first product obtained and be delivered continuously to product rectifying tower, control rectifying tower tower top temperature 54 DEG C ~ 100 DEG C, DEG C rectifying of tower bottom of rectifying tower temperature 60 C ~ 120, is continuously separated out diacetone alcohol finished product from rectifying tower.
Preferably, above-described continuous processing produces the method for diacetone alcohol, and the percentage composition of the diacetone alcohol finished product prepared is 99.5% ~ 99.9%.
Preferably, above-described continuous processing produces the method for diacetone alcohol, controls overhead temperature 55 DEG C ~ 65 DEG C, distillation tower bottom temperature 90 DEG C ~ 110 DEG C.
Preferably, above-described continuous processing produces the method for diacetone alcohol, controls second distillation column overhead temperatures 55 DEG C ~ 64 DEG C, after-fractionating tower bottom temperature 92 DEG C ~ 100 DEG C.
Preferably, above-described continuous processing produces the method for diacetone alcohol, controls rectifying tower tower top temperature 62 DEG C ~ 64 DEG C, 98 DEG C ~ 100 DEG C rectifying of tower bottom of rectifying tower temperature.
Continuous processing provided by the invention produces the specific equipment of diacetone alcohol, and it comprises: flow reactor, the distillation tower be connected with flow reactor, the after-fractionating tower be connected with distillation tower, the rectifying tower be connected with after-fractionating tower.
Compared to the prior art, the present invention has the following advantages:
The present invention screens by great many of experiments the method that the continuous processing obtained produces diacetone alcohol, especially distillation tower, the tower reactor of after-fractionating tower and rectifying tower and tower top temperature, whole technique has that reaction time is short, facility investment is little, production capacity is high, energy consumption is low, continuous production processes process is easy to control, product content is high (general 99.5% ~ 99.9%), steady quality, production process without features such as " three wastes " discharges, there is important using value.
Accompanying drawing explanation
Fig. 1 is the structural representation that continuous processing provided by the invention produces the specific equipment of diacetone alcohol.
Specific implementation method
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Embodiment 1
Continuous processing produces a method for diacetone alcohol, and it comprises the following steps:
As shown in Figure 1, first acetone is entered flow reactor (1) with the flow of 2000L/h, control the temperature 5 DEG C ~ 15 DEG C of reaction, transformation efficiency 18% ~ 22%, the feed liquid flowed out enters distillation tower (2) again, bottom temperature 92 ~ 100 DEG C, tower top temperature 55 ~ 64 DEG C, tower top acetone flow 1500L/h, tower reactor feed liquid delivers into after-fractionating tower (3) with 500L/h flow, bottom temperature 92 ~ 100 DEG C, tower top temperature 55 ~ 64 DEG C, second distillation tower top acetone reflux amount 85L/h, tower reactor diacetone alcohol first product enters rectifying tower (4) with 415L/h flow, bottom temperature 98 ~ 100 DEG C, tower top temperature 62 ~ 64 DEG C, rectifying tower diacetone alcohol product flow 400l/h, tower top acetone reflux amount 15l/h.The acetone that distillation tower (1), after-fractionating tower (2) and rectifying tower (4) steam is transported in flow reactor (1) again and continues reaction.This device runs 168 hours continuously, obtains the diacetone alcohol that percentage composition is 99.75% ~ 99.85% continuously.
Embodiment 2
Continuous processing produces a method for diacetone alcohol, and it comprises the following steps:
Acetone is entered flow reactor (1) with the flow of 5000L/h, control the temperature 0 DEG C ~ 10 DEG C of reaction, transformation efficiency 18% ~ 25%, the feed liquid flowed out enters distillation tower (2) again, bottom temperature 90 ~ 95 DEG C, tower top temperature 58 ~ 65 DEG C, tower top acetone flow 4000L/h, tower reactor feed liquid delivers into after-fractionating tower (3) with 1000L/h flow, bottom temperature 92 ~ 100 DEG C, tower top temperature 55 ~ 64 DEG C, second distillation tower top acetone reflux amount 185L/h, tower reactor diacetone alcohol first product enters rectifying tower (4) with 815L/h flow, bottom temperature 98 ~ 100 DEG C, tower top temperature 62 ~ 64 DEG C, rectifying tower diacetone alcohol product flow 800l/h, tower top acetone reflux amount 15l/h.The acetone that distillation tower (1), after-fractionating tower (2) and rectifying tower (4) steam is transported in flow reactor (1) again and continues reaction.This device runs 168 hours continuously, obtains the diacetone alcohol that percentage composition is 99.55% ~ 99.75% continuously.
Embodiment 3
Continuous processing produces a method for diacetone alcohol, and it comprises the following steps:
Acetone is entered flow reactor (1) with the flow of 8000L/h, control the temperature 2 DEG C ~ 17 DEG C of reaction, transformation efficiency 20% ~ 25%, the feed liquid flowed out enters distillation tower (2) again, bottom temperature 92 ~ 100 DEG C, tower top temperature 55 ~ 64 DEG C, tower top acetone flow 5800L/h, tower reactor feed liquid delivers into after-fractionating tower (3) with 2200L/h flow, bottom temperature 92 ~ 100 DEG C, tower top temperature 55 ~ 64 DEG C, second distillation tower top acetone reflux amount 320L/h, tower reactor diacetone alcohol first product enters rectifying tower (4) with 1900L/h flow, bottom temperature 98 ~ 100 DEG C, tower top temperature 62 ~ 64 DEG C, rectifying tower diacetone alcohol product flow 1800l/h, tower top acetone reflux amount 100L/h.The acetone that distillation tower (1), after-fractionating tower (2) and rectifying tower (4) steam is transported in flow reactor (1) again and continues reaction.This device runs 168 hours continuously, obtains the diacetone alcohol that percentage composition is 99.60% ~ 99.85% continuously.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. continuous processing produces a method for diacetone alcohol, it is characterized in that, comprises the following steps:
With pump, acetone is squeezed into flow reactor continuously, control between temperature of reaction-20 DEG C ~ 35 DEG C, reactor feed liquid out again continus convergence enters distillation tower, control overhead temperature 54 DEG C ~ 100 DEG C, distillation tower bottom temperature 60 DEG C ~ 120 DEG C, most of unreacted acetone is removed in continuous still battery in a distillation column, continus convergence enters after-fractionating tower again, control second distillation column overhead temperatures 54 DEG C ~ 100 DEG C, after-fractionating tower bottom temperature 65 DEG C ~ 120 DEG C, remaining acetone is removed in continuous still battery, obtain diacetone alcohol first product, acetone distillation tower and after-fractionating tower steamed is delivered continuously to flow reactor again and continues reaction, distill the diacetone alcohol first product obtained and be delivered continuously to product rectifying tower, control rectifying tower tower top temperature 54 DEG C ~ 100 DEG C, DEG C rectifying of tower bottom of rectifying tower temperature 60 C ~ 120, diacetone alcohol finished product is continuously separated out from rectifying tower.
2. continuous processing according to claim 1 produces the method for diacetone alcohol, and it is characterized in that, the percentage composition of diacetone alcohol finished product is 99.5% ~ 99.9%.
3. continuous processing according to claim 1 produces the method for diacetone alcohol, it is characterized in that, controls overhead temperature 55 DEG C ~ 65 DEG C, distillation tower bottom temperature 90 DEG C ~ 110 DEG C.
4. continuous processing according to claim 1 produces the method for diacetone alcohol, it is characterized in that, controls second distillation column overhead temperatures 55 DEG C ~ 64 DEG C, after-fractionating tower bottom temperature 92 DEG C ~ 100 DEG C.
5. continuous processing according to claim 1 produces the method for diacetone alcohol, it is characterized in that, controls rectifying tower tower top temperature 62 DEG C ~ 64 DEG C, 98 DEG C ~ 100 DEG C rectifying of tower bottom of rectifying tower temperature.
6. the continuous processing described in any one of Claims 1-4 produces the specific equipment of diacetone alcohol, it is characterized in that, it comprises: flow reactor (1), the distillation tower (2) be connected with flow reactor (1), the after-fractionating tower (3) be connected with distillation tower (2), the rectifying tower (4) be connected with after-fractionating tower (3).
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105037123A true CN105037123A (en) | 2015-11-11 |
| CN105037123B CN105037123B (en) | 2017-06-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496414A (en) * | 2019-09-19 | 2019-11-26 | 福州大学 | Synthesize the continuous reaction rectification equipment and its technique of diacetone alcohol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787986A (en) * | 2003-05-15 | 2006-06-14 | 三菱化学株式会社 | Process for producing diacetone alcohol |
| CN103724172A (en) * | 2014-01-17 | 2014-04-16 | 天津市道福化工新技术开发有限公司 | Synthesis process of diacetone alcohol |
-
2015
- 2015-07-28 CN CN201510452592.5A patent/CN105037123B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787986A (en) * | 2003-05-15 | 2006-06-14 | 三菱化学株式会社 | Process for producing diacetone alcohol |
| CN103724172A (en) * | 2014-01-17 | 2014-04-16 | 天津市道福化工新技术开发有限公司 | Synthesis process of diacetone alcohol |
Non-Patent Citations (1)
| Title |
|---|
| 梁世强等: "连续反应装置合成二丙酮醇研究", 《精细石油化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496414A (en) * | 2019-09-19 | 2019-11-26 | 福州大学 | Synthesize the continuous reaction rectification equipment and its technique of diacetone alcohol |
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| Publication number | Publication date |
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| CN105037123B (en) | 2017-06-23 |
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