CN1583734A - Apparatus and process for purifying peach aldehyde by decompressing batch rectifying - Google Patents
Apparatus and process for purifying peach aldehyde by decompressing batch rectifying Download PDFInfo
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- CN1583734A CN1583734A CN 200410019539 CN200410019539A CN1583734A CN 1583734 A CN1583734 A CN 1583734A CN 200410019539 CN200410019539 CN 200410019539 CN 200410019539 A CN200410019539 A CN 200410019539A CN 1583734 A CN1583734 A CN 1583734A
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- peach aldehyde
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Abstract
The present invention discloses the device and process for purifying peach aldehyde by vacuum batch distallation, which belongs to extracting and purifying technology. This device includes rectifying tower, condensator, reflux accumulator, surge drum, vacuum pump and reservoir. The rectifying towr is filled with highly efficient stuffs, which is characterized by a lining pipe calorifer with h:d ratio of 0.6-0.3. Said process comprises operating at a pressure between 133.3 Pa and 1333 Pa with a temperature range from 150 deg.C to 180 deg.C to change the relux ratio, and obtained the light components represented by octyl alcohol and peach aldehyde with eligibility purity from the top of said tower. The advantage lies in that the thickness of liguid film formed in the tower is small, therefore provides a high vaporization efficiency, a high heat transfer coefficient and short staying period of materials. Moreover, the tower is easy to handle, yet the product can reach a purity above 99 wt%.
Description
Technical field
The present invention relates to a kind of device and process of intermittent rectification under vacuum purification peach aldehyde, belong to the purification technique of synthetic peach aldehyde.
Background technology
Peach aldehyde is a kind of aroma substance, has slight peach fragrance, and it both can be widely used in also can being applied in the daily cosmetics in the flavor formulation of all kinds of milks and fruity by a kind of flavor of raw material; Patent US6737396 has introduced the application of peach aldehyde in the fragrance setting agent; Patent US5814325, CN1465244 have also reported the application of peach aldehyde in sterilant, rodenticide are produced.The chemical name of peach aldehyde is α-heptyl-gamma-butyrolactone, is to obtain with the synthetic method mostly, and patent US5665696 has reported that peach aldehyde can be made through addition reaction by tetrahydrofuran (THF).The method of separating the purification peach aldehyde at present is to adopt conventional batch fractionating method, and this method is simple, less investment; But the peach aldehyde atmospheric boiling point is 297.0 ℃, and boiling point is higher and have certain thermo-sensitivity, adopts the conventional rectification method to make it suffer to a certain degree destruction easily.Because peach aldehyde is the intermediate component in the synthetic crude product, need it is light, heavy seeds from crude product, to remove respectively, its purity of method of present rectification and purification peach aldehyde can only reach 97wt%.
Summary of the invention
The object of the present invention is to provide a kind of device and process of intermittent rectification under vacuum purification peach aldehyde, adopt this its purity of device purification peach aldehyde to reach more than the 99wt%.
The present invention is realized by following technical proposals: the device of intermittent rectification under vacuum purification peach aldehyde, comprise rectifying tower, condenser, return tank, buffer tank, vacuum tank and vacuum pump composition, dress high efficiency packing in the tower, it is characterized in that the tower still of rectifying tower is that aspect ratio is 0.6～0.3 chuck tube still heater.
The aspect ratio of above-mentioned tower still is 0.5～0.4.
Adopt the reduce pressure process of periodical operation rectification and purification peach aldehyde of said apparatus, it is characterized in that operating with following condition:
1, with the tower top pressure be 133.3Pa～1333Pa, tower still temperature is 150～180 ℃ and carries out the varying reflux ratio operation;
2, when tower still temperature is 145～155 ℃, be the light constituent of representative from cat head extraction octanol with reflux ratio 5～10;
3, when tower still temperature is 155～165 ℃, with reflux ratio 2～8 from the qualified peach aldehyde of cat head extraction purity.
Above-mentioned extraction octanol is that the operating reflux ratio of the light constituent of representative is 8; The optimum operation reflux ratio of the peach aldehyde that extraction purity is qualified is 4.
The invention has the advantages that it is little that the tower still has a thickness of liquid film, vaporization efficiency height, big, the short characteristics of residence time of material of heat transfer coefficient, the operating procedure of tower is simple, product purity can reach more than the 99wt%, does not produce any other organic substance in the process, environmentally safe.
Description of drawings
Fig. 1 is apparatus of the present invention synoptic diagram.
Among the figure, 1 is the tower still, and 2 is body of the tower, and 3 is condenser, and 4 is return tank, and 5 is buffer tank, and 6 is vacuum pump, and 7 is storage tank.
Embodiment
(1) at aspect ratio is 0.45 batch fractionating tower (1 meter of tower height, in adorn efficient Stainless Steel Cloth filler) add 150ml peach aldehyde crude product in the still, the content of effective constituent peach aldehyde is 66.77wt% in the crude product, wherein light than peach aldehyde foreign matter content is 17.90wt%, and the foreign matter content heavier than peach aldehyde is 15.33wt%.
(2) regulate pressure regulation electrically heated cover and heat up, at the uniform velocity be elevated to 95 ℃, when drop appears in cat head, carried out total reflux operation about 40 minutes, make light constituent in the cat head enrichment, tower top temperature, column bottom temperature constantly raise at this moment.
(3) regulating reflux ratio then is 12, and light impurity from the cat head extraction, was operated about 50 minutes, and still temperature, top temperature slowly raise at this moment, i.e. the impurity removal stage.
(4) along with the excision of light constituent, when overhead product purity reaches 99.0wt%, regulating constant reflux ratio is 8, product is collected, operated about 180 minutes, i.e. product collection phase, cat head and tower still temperature are stabilized in respectively about 96 ℃ and 155 ℃, purity is stabilized in more than 99.1%, i.e. the product collection phase.
(5) begin to rise when tower still temperature, the heavy constituent impurity in the raw material begins in the cat head enrichment, and product purity descends to some extent; Improve reflux ratio this moment once more is 10, and the purity that always keeps peach aldehyde is in 99% scope; When product purity is lower than 99.0wt%, stop extraction; The part that remains in the tower still is an impurity.
Separating the result who purifies proves that the content of peach aldehyde has reached more than the 99.0wt% in the product, and yield is 72.4wt%, and octanol content can not influence quality product less than 5ppm.The finished product of above embodiment are composed as follows:
Octanol 0.00004wt%
Peach aldehyde 99.35wt%
Other compositions 0.64996wt%
Claims (4)
1, a kind of device of intermittent rectification under vacuum purification peach aldehyde, comprise rectifying tower, condenser, return tank, buffer tank, vacuum pump and storage tank composition, dress high efficiency packing in the tower, it is characterized in that: the tower still of rectifying tower is that aspect ratio is 0.6～0.3 chuck tube still heater.
2, by the device of the described intermittent rectification under vacuum purification of claim 1 peach aldehyde, it is characterized in that: the aspect ratio of tower still is 0.5～0.4.
3 one kinds of employings are carried out the process of intermittent rectification under vacuum purification peach aldehyde by the described device of claim 1, it is characterized in that operating with following condition:
1), be 133.3Pa～1333Pa with the tower top pressure, tower still temperature is 150～180 ℃ and carries out the varying reflux ratio operation;
2), when tower still temperature is 145～155 ℃, be the light constituent of representative with reflux ratio 5～10 from cat head extraction octanol;
3), when tower still temperature is 155～165 ℃, with reflux ratio 2～8 from the qualified peach aldehyde of cat head extraction purity.
4, by the process of the described intermittent rectification under vacuum purification of claim 3 peach aldehyde, it is characterized in that: the extraction octanol is that the operating reflux ratio of the light constituent of representative is 8; The operating reflux ratio of the peach aldehyde that extraction purity is qualified is 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019539 CN1255395C (en) | 2004-06-09 | 2004-06-09 | Apparatus and process for purifying peach aldehyde by decompressing batch rectifying |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410019539 CN1255395C (en) | 2004-06-09 | 2004-06-09 | Apparatus and process for purifying peach aldehyde by decompressing batch rectifying |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1583734A true CN1583734A (en) | 2005-02-23 |
| CN1255395C CN1255395C (en) | 2006-05-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410019539 Expired - Fee Related CN1255395C (en) | 2004-06-09 | 2004-06-09 | Apparatus and process for purifying peach aldehyde by decompressing batch rectifying |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219288B (en) * | 2007-09-28 | 2010-12-08 | 天津大学 | Multi-point dispersion heating type stripping column device and technique for column body |
| CN101982214A (en) * | 2010-10-29 | 2011-03-02 | 邢台旭阳煤化工有限公司 | Separating and purifying device and process for heavy-component residual liquid of hydrogenation process of coking crude benzene |
| CN102503915A (en) * | 2011-10-25 | 2012-06-20 | 靖江泰达香料化工有限公司 | Peach aldehyde continuous reaction device |
| CN102757411A (en) * | 2012-06-29 | 2012-10-31 | 天津大学 | Device and method for preparing peach aldehyde |
| CN102766117A (en) * | 2012-07-19 | 2012-11-07 | 天津大学 | Method for removing molecule n-caprylic alcohol in peach aldehyde |
| CN103232892A (en) * | 2010-01-26 | 2013-08-07 | 田志勇 | Five-section extraction method for preparing mint essential oil by distillation |
| CN104059780A (en) * | 2014-07-07 | 2014-09-24 | 广西壮族自治区林业科学研究院 | Equipment for thermo-sensitivity aromatic oil fractionation |
| CN104592176A (en) * | 2015-02-15 | 2015-05-06 | 上海化工研究院 | Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material |
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN108997270A (en) * | 2018-08-06 | 2018-12-14 | 安徽华业香料股份有限公司 | A kind of production method of reactive distillation synthesis gamma decalactone synthetic perfume |
| CN109439433A (en) * | 2018-11-11 | 2019-03-08 | 陕西海升果业发展股份有限公司乾县分公司 | A kind of production method improving natural fruit and vegetables essence aldehydes, esters |
-
2004
- 2004-06-09 CN CN 200410019539 patent/CN1255395C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219288B (en) * | 2007-09-28 | 2010-12-08 | 天津大学 | Multi-point dispersion heating type stripping column device and technique for column body |
| CN103232892B (en) * | 2010-01-26 | 2014-04-09 | 田志勇 | Five-section extraction method for preparing mint essential oil by distillation |
| CN103232892A (en) * | 2010-01-26 | 2013-08-07 | 田志勇 | Five-section extraction method for preparing mint essential oil by distillation |
| CN101982214B (en) * | 2010-10-29 | 2012-08-22 | 邢台旭阳煤化工有限公司 | Separating and purifying device and process for heavy-component residual liquid of hydrogenation process of coking crude benzene |
| CN101982214A (en) * | 2010-10-29 | 2011-03-02 | 邢台旭阳煤化工有限公司 | Separating and purifying device and process for heavy-component residual liquid of hydrogenation process of coking crude benzene |
| CN102503915A (en) * | 2011-10-25 | 2012-06-20 | 靖江泰达香料化工有限公司 | Peach aldehyde continuous reaction device |
| CN102503915B (en) * | 2011-10-25 | 2013-11-20 | 靖江泰达香料化工有限公司 | Peach aldehyde continuous reaction device |
| CN102757411A (en) * | 2012-06-29 | 2012-10-31 | 天津大学 | Device and method for preparing peach aldehyde |
| CN102766117A (en) * | 2012-07-19 | 2012-11-07 | 天津大学 | Method for removing molecule n-caprylic alcohol in peach aldehyde |
| CN104059780A (en) * | 2014-07-07 | 2014-09-24 | 广西壮族自治区林业科学研究院 | Equipment for thermo-sensitivity aromatic oil fractionation |
| CN104059780B (en) * | 2014-07-07 | 2016-01-27 | 广西壮族自治区林业科学研究院 | A kind of equipment for the fractionation of thermo-sensitivity perfume oil |
| CN104592176A (en) * | 2015-02-15 | 2015-05-06 | 上海化工研究院 | Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material |
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN108997270A (en) * | 2018-08-06 | 2018-12-14 | 安徽华业香料股份有限公司 | A kind of production method of reactive distillation synthesis gamma decalactone synthetic perfume |
| CN109439433A (en) * | 2018-11-11 | 2019-03-08 | 陕西海升果业发展股份有限公司乾县分公司 | A kind of production method improving natural fruit and vegetables essence aldehydes, esters |
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|---|---|
| CN1255395C (en) | 2006-05-10 |
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Assignee: Anhui Hyea Chemical Co., Ltd. Assignor: Tianjin University Contract fulfillment period: 2006.10.22 to 2011.10.21 contract change Contract record no.: 2009340000103 Denomination of invention: Apparatus and process for purifying peach aldehyde by decompressing batch rectifying Granted publication date: 20060510 License type: Exclusive license Record date: 2009.5.31 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.10.22 TO 2011.10.21; CHANGE OF CONTRACT Name of requester: ANHUI HUAYE CHEMICAL CO., LTD. Effective date: 20090531 |