CN102531871A - Method for purifying 2,4-dichloroacetophenone - Google Patents
Method for purifying 2,4-dichloroacetophenone Download PDFInfo
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- CN102531871A CN102531871A CN2011104318096A CN201110431809A CN102531871A CN 102531871 A CN102531871 A CN 102531871A CN 2011104318096 A CN2011104318096 A CN 2011104318096A CN 201110431809 A CN201110431809 A CN 201110431809A CN 102531871 A CN102531871 A CN 102531871A
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- ethyl ketone
- dichloro benzene
- benzene ethyl
- slicing machine
- rotary drum
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Abstract
The invention relates to a method for purifying 2,4-dichloroacetophenone, comprising the following steps: feeding 92-98% by weight of crude 2,4-dichloroacetophenone into an industrial roller slicer filled with a flowing medium, crystallizing and slicing; directly moving slices to a centrifugal machine, and rising with a solvent while centrifuging; or moving the slices into a drying chamber to make the surfaces of the slices sweat, and centrifuging to obtain the 2,4-dichloroacetophenone with the purity of more than 99%. The centrifugal mother solution can be recycled. The method for purifying the 2,4-dichloroacetophenone is easy to operate and has the advantages of low production cost, high yield, high product purity and stable performance, thereby being suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method of the 2,4 dichloro benzene ethyl ketone of purifying.
Background technology
The 2,4 dichloro benzene ethyl ketone is important fine-chemical intermediate, is mainly used in synthetic nitrogen azole broad spectrum antibiotic KETOKONAZOL.At present, industrial production 2, the method for 4-dichloroacetophenone mainly is to be raw material with m-dichlorobenzene and chloroacetic chloride, reacts acquisition with alchlor as catalyst.Impurity such as isomers 2 in the thick product that is synthesized, the content of 6-dichloroacetophenone is generally between 1.6%～2.0%.
Propose through underpressure distillation among the Chinese patent 101898947A, crystallisation by cooling obtains purity at the 2,4 dichloro benzene ethyl ketone product more than 99% then.Because 2,4 dichloro benzene ethyl ketone and 2, the volatility of 6-dichloroacetophenone is more or less the same, so pass through to need point-device operation when rectificating method separates, be not easy control, and energy consumption is higher, and is uneconomical.
At present, domestic manufacturer generally adopts first distillation, advances the freezer freezing and crystallizing then, breaks into pieces then, and the method for centrifugal (using an amount of solvent rinsing simultaneously) is purified.Also there is the people to join solvent in the distillage earlier, advances the freezer freezing and crystallizing again, then the method for spinning.No matter which kind of method all must be broken into pieces through the freezer freezing and crystallizing then, and this not only need cost the construction freezer, and needs labor intensive to break crystallisate into pieces, and cost is higher.
Rotary drum condensation-crystallization slicing machine is the device that the heating liquids raw material is converted to solid slice; Rotary drum through internal cooling rotates adhesive tape liquid material condensation-crystallization to slicing knife device it is cut into slices in hopper, thereby accomplishes the conversion of liquid to the solid sheet stock, also can cut into slices through the raw material that cooling becomes xln to liquid; This section can directly move to whizzer; The limit is centrifugal with solvent rinsing limit, is widely used in chemical industry, industries such as pharmacy.Through the raw material of slicing machine moulding,, more improve the class of product than the raw material of other crush type processing.And stabilization of equipment performance is good, and is easy to operate, and the output of section material can be according to Material Characteristics, rotor speed, and input speed decides.Slicer is simple in structure, operation easily, and also cheap, be applicable to Chemical Manufacture, yet there are no this type of application in the like product at present.
Summary of the invention
The objective of the invention is deficiency, and proposed a kind of method of new purification 2,4 dichloro benzene ethyl ketone to existing 2,4 dichloro benzene ethyl ketone method of purification.This method is simple to operate, and cost is low, and product purity is high, is applicable to industrial production.
Technical scheme of the present invention is: a kind of purification 2; The method of 4-dichloroacetophenone, its concrete steps are following: 2,4 dichloro benzene ethyl ketone bullion is discharged to the rotary drum condensation-crystallization slicing machine crystallization section of inner through-flow moving medium; To cut into slices and directly move to whizzer, centrifugal with rinsing limit, solvent limit; Maybe section is moved on in the drying room, let its surperficial sweating, it is centrifugal to move to whizzer then; 2,4 dichloro benzene ethyl ketone after obtaining purifying.
Preferred described slicing machine is that the rotary drum model size of rotary drum condensation-crystallization slicing machine is: Φ 400mm*500mm-Φ 3000mm*4000mm; Slicing machine rotary drum rotating speed is 2r/min-12r/min.Preferred institute uses the rotating speed of whizzer to be 500r/min-3500r/min; Its volume is: 0.1m
3-3.0m
3
Preferred slicing machine internal flow medium is salt solution or thermal oil; Slicing machine internal flow medium temperature is-20 ℃ to 0 ℃, to guarantee 2,4 dichloro benzene ethyl ketone rapid crystallization.
The present invention uses centrifugal, the rinsing purification of will cut into slices of the organic solvent that can dissolve each other with the 2,4 dichloro benzene ethyl ketone or organic mixed solvent.Solvent for use is at least the sherwood oil of 40 ℃-80 ℃ of methyl alcohol, ethanol, boiling point during preferred rinsing, or methylene dichloride.
The speed that preferred 2,4 dichloro benzene ethyl ketone bullion blowing gets into slicing machine is 0.1m
3/ h-3m
3/ h.
Preferably make the drying room internal temperature of slice surface sweating be controlled at 30～60 ℃.
The quality percentage composition 92-98% of 2,4 dichloro benzene ethyl ketone in the 2,4 dichloro benzene ethyl ketone bullion of the present invention; The quality percentage composition of 2,4 dichloro benzene ethyl ketone is 99.0%-99.8% in the 2,4 dichloro benzene ethyl ketone of purification back.
Beneficial effect:
The method of purification of 2,4 dichloro benzene ethyl ketone of the present invention compared with prior art has the following advantages: one, the present invention need not build freezer, uses the required labor force of slicing machine few, practices thrift manufacturing cost.Two, the product purity that obtains of this method of purification is high, can reach more than 99.0%, and stable performance, product yield is high, is fit to scale operation.
Embodiment
The method of purification of 2,4 dichloro benzene ethyl ketone of the present invention can be passed through following instance explanation.
[embodiment 1] is that 92.5% bullion is with 0.2m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is 500r/min, volume 0.1m that section is moved to rotating speed in the rotary drum condensation-crystallization slicing machine that it is 2r/min that the speed of/h is discharged to inner logical 0 ℃ of thermal oil, rotary drum Φ 600mm*600mm, rotating speed
3Whizzer, make the 2,4 dichloro benzene ethyl ketone that rinsing limit, solvent limit obtains purity 99.0% after centrifugal with methyl alcohol.The used rotary drum condensation-crystallization of this instance slicing machine is that Wuxi China precious medicine equipment ltd manufactures and designs.
[embodiment 2] are that 95% bullion is with 0.5m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is 1000r/min, volume 0.5m that section is moved to volume in the rotary drum condensation-crystallization slicing machine that it is 5r/min that the speed of/h is discharged to inner logical-5 ℃ of thermal oils, rotary drum Φ 1000mm*1500mm, rotating speeds
3Whizzer, make the 2,4 dichloro benzene ethyl ketone that rinsing limit, solvent limit obtains purity 99.2% after centrifugal with methyl alcohol.
[embodiment 3] are that 95.0% bullion is with 2m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is that 3000r/min, volume are 3m that section is moved to volume in the rotary drum condensation-crystallization slicing machine that it is 8r/min that the speed of/h is discharged to inner logical-15 ℃ of thermal oils, rotary drum Φ 2000mm*2500mm, rotating speeds
3Whizzer, make the 2,4 dichloro benzene ethyl ketone that rinsing limit, solvent limit obtains purity 99.4% after centrifugal with methylene dichloride.
[embodiment 4] are that 92.5% bullion is with 2m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is that 3500r/min, volume are 3m that section is moved to volume in the rotary drum condensation-crystallization slicing machine that it is 2r/min that the speed of/h is discharged to inner logical-18 ℃ of thermal oils, rotary drum Φ 3000mm*3500mm, rotating speeds
3Whizzer, make the 2,4 dichloro benzene ethyl ketone that rinsing limit, solvent limit obtains purity 99.8% after centrifugal with the sherwood oil of 40 ℃-80 ℃ of boiling points.
[embodiment 4] are that 94.8% bullion is with 1.0m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is that 1500r/min, volume are 1m that section is moved to volume in the rotary drum condensation-crystallization slicing machine that it is 12r/min that the speed of/h is discharged to inner logical-10 ℃ of chilled brines, rotary drum Φ 1000mm*1500mm, rotating speeds
3Whizzer, make the 2,4 dichloro benzene ethyl ketone that rinsing limit, solvent limit obtains purity 99.6% after centrifugal with the sherwood oil of 40 ℃-80 ℃ of boiling points.
[embodiment 5] are that 94.8% bullion blowing is with 1.0m with 2,4 dichloro benzene ethyl ketone content
3After the crystallization section, it is to treat in 40 ℃ of drying rooms to use volume to be 1m as 2500r/min, volume after the surperficial sweating that section is moved to temperature in the rotary drum condensation-crystallization slicing machine that it is 6r/min that the speed of/h is discharged to inner logical-10 ℃ of chilled brines, rotary drum Φ 1000mm*1500mm, rotating speeds
3The centrifugal purification of whizzer obtain the 2,4 dichloro benzene ethyl ketone of purity 99.5%.
[embodiment 6] working method is with instance 5, and just the drying room temperature becomes 55 ℃, and obtaining 2,4 dichloro benzene ethyl ketone purity is 99.8%.
Claims (8)
1. method of 2,4 dichloro benzene ethyl ketone of purifying, its concrete steps are following: 2,4 dichloro benzene ethyl ketone bullion are discharged to the rotary drum condensation-crystallization slicing machine crystallization section of inner through-flow moving medium, will cut into slices and directly move to whizzer, centrifugal with rinsing limit, solvent limit; Maybe section is moved on in the drying room, let its surperficial sweating, it is centrifugal to move to whizzer then; 2,4 dichloro benzene ethyl ketone after obtaining purifying.
2. the method for claim 1 is characterized in that described slicing machine is that the rotary drum model size of rotary drum condensation-crystallization slicing machine is: Φ 400mm*500mm-Φ 3000mm*4000mm; Slicing machine rotary drum rotating speed is 2r/min-12r/min.
3. the method for claim 1 is characterized in that institute uses the rotating speed of whizzer to be 500r/min-3500r/min.
4. the method for claim 1 is characterized in that slicing machine internal flow medium is salt solution or thermal oil; Slicing machine internal flow medium temperature is-20 ℃ to 0 ℃.
5. the method for claim 1, solvent for use is at least a kind of in the sherwood oil of 40 ℃-80 ℃ of methyl alcohol, ethanol, methylene dichloride or boiling points when it is characterized in that rinsing.
6. the method for claim 1 is characterized in that the speed of 2,4 dichloro benzene ethyl ketone bullion blowing entering slicing machine is 0.1m
3/ h-3m
3/ h.
7. the method for claim 1 is characterized in that making the drying room internal temperature of slice surface sweating to be controlled at 30～60 ℃.
8. the method for claim 1, the quality percentage composition that it is characterized in that 2,4 dichloro benzene ethyl ketone in the 2,4 dichloro benzene ethyl ketone bullion is 92-98%; The quality percentage composition of 2,4 dichloro benzene ethyl ketone is 99.0%-99.8% in the 2,4 dichloro benzene ethyl ketone of purification back.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104318096A CN102531871A (en) | 2011-12-21 | 2011-12-21 | Method for purifying 2,4-dichloroacetophenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104318096A CN102531871A (en) | 2011-12-21 | 2011-12-21 | Method for purifying 2,4-dichloroacetophenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102531871A true CN102531871A (en) | 2012-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104318096A Pending CN102531871A (en) | 2011-12-21 | 2011-12-21 | Method for purifying 2,4-dichloroacetophenone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180418A (en) * | 2018-10-09 | 2019-01-11 | 江苏扬农化工集团有限公司 | A kind of propylene oxide co-production object resource utilization synthetic pesticide intermediate 2,4 dichloro benzene ethyl ketone method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3360566A (en) * | 1964-11-25 | 1967-12-26 | Hooker Chemical Corp | Manufacture of 2', 4'-dichloroacetophenones and beta-polychlorinated 2', 4'-dichloroacetophenones from mixed dichlorobenzenes |
| CN201500530U (en) * | 2009-09-14 | 2010-06-09 | 浙江汉邦化工有限公司 | slicing machine |
| CN101898947A (en) * | 2010-08-19 | 2010-12-01 | 江苏隆昌化工有限公司 | Method for producing 2,4-dichloroacetophenone by using solid waste chlorobenzene tar as raw material |
-
2011
- 2011-12-21 CN CN2011104318096A patent/CN102531871A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3360566A (en) * | 1964-11-25 | 1967-12-26 | Hooker Chemical Corp | Manufacture of 2', 4'-dichloroacetophenones and beta-polychlorinated 2', 4'-dichloroacetophenones from mixed dichlorobenzenes |
| CN201500530U (en) * | 2009-09-14 | 2010-06-09 | 浙江汉邦化工有限公司 | slicing machine |
| CN101898947A (en) * | 2010-08-19 | 2010-12-01 | 江苏隆昌化工有限公司 | Method for producing 2,4-dichloroacetophenone by using solid waste chlorobenzene tar as raw material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180418A (en) * | 2018-10-09 | 2019-01-11 | 江苏扬农化工集团有限公司 | A kind of propylene oxide co-production object resource utilization synthetic pesticide intermediate 2,4 dichloro benzene ethyl ketone method |
| CN109180418B (en) * | 2018-10-09 | 2021-03-30 | 江苏扬农化工集团有限公司 | Method for synthesizing pesticide intermediate 2, 4-dichloroacetophenone by recycling propylene oxide co-product materials |
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Application publication date: 20120704 |