CN1308278C - Process for directly producing natural benzaldehyde using cassia twig leaf and cassia bark as raw material - Google Patents
Process for directly producing natural benzaldehyde using cassia twig leaf and cassia bark as raw material Download PDFInfo
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- CN1308278C CN1308278C CNB2005100196056A CN200510019605A CN1308278C CN 1308278 C CN1308278 C CN 1308278C CN B2005100196056 A CNB2005100196056 A CN B2005100196056A CN 200510019605 A CN200510019605 A CN 200510019605A CN 1308278 C CN1308278 C CN 1308278C
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Abstract
The present invention relates to a method for directly producing natural benzaldehyde with cassia twig leaves and cassia as raw materials. Cassia twig leaves or cassia are chopped and arranged in a distillating still for distillation, and an outlet of the distillating still is connected with an inlet of a hydrolysis reactor. Cassia oil is carried by steam passing through the cassia twig leaves or the cassia, formed mixed steam contacts with an alkali catalyst, hydrolysis reaction is carried out under the condition of gas phase, generated benzaldehyde and the steam are output from the outlet of the hydrolysis reactor, and the crude products of the benzaldehyde are obtained after condensed. When the method of the present invention is used for producing natural benzaldehyde, original equipment for producing the cassia oil only needs to add the hydrolysis reactor, and compared with the existing cassia oil benzaldehyde making technology, the present invention has the advantages of less investment, short technological lines, power consumption saving and low production cost. The yield of the crude benzaldehyde is 0.5 % according to the cassia twig leaves.
Description
Technical field
The invention belongs to cassia twig leaf, cassia bark is the method for raw material direct production natural benzaldehyde.
Background technology
The food grade natural benzaldehyde can carry out deep processing with natural oil of bay and make, and this method main production of present domestic use has hydrolysis (anti-aldol reaction) method under ozonization method [seeing " natural benzaldehyde is produced in the ozonize of natural meat oil of bay " " fine chemistry industry " 1996.6.P32-34], the alkaline condition [to see " research that the Bay leaves oil hydrolysis prepares natural benzaldehyde " " Guangxi chemical industry " 1997.3.P1～3; " research for preparing natural benzaldehyde under the phase transfer catalysis condition from Bay leaves oil " " chemistry world " 2002.6.P315～317].Applied for the having of Chinese invention patent " novel method that a kind of Bay leaves oil hydrolysis prepares natural benzaldehyde " (CN03115229.5), " process for preparing natural benzaldehyde " (200410092062.6) etc.Above production technique is raw materials used all to be the commodity oil of bay.
The commodity oil of bay adopts water vapor distillation extraction from cassia twig leaf or cassia bark usually, promptly feeds water vapor in cassia twig leaf or cassia bark, and the mixed steam condensation that contains oil of bay is after oily water separation obtains product.If again with the commodity oil of bay as the feedstock production natural benzaldehyde, obviously increased production process, energy consumption and the cost of product.
Summary of the invention
It is the method for raw material direct production natural benzaldehyde with cassia twig leaf, cassia bark that the technical problem to be solved in the present invention provides a kind of, in the hope of reaching the production technique of farthest simplifying natural benzaldehyde, reduce energy consumption, reducing production costs.
The present invention solves the problems of the technologies described above with following technical scheme: distill putting into still kettle after cassia twig leaf or the cassia bark chopping, water vapor has been carried oil of bay during by the cassia twig leaf secretly, it is characterized in that still kettle exports the inlet that direct water receiving is separated reactor, the hot mixed steam that enters hydrolysis reactor contacts with basic catalyst, reaction is hydrolyzed under the situation of gas phase, the phenyl aldehyde that generates from hydrolysis reactor outlet output, obtains the crude benzol formaldehyde products with steam after the condensation.
The present invention is the method for raw material production natural benzaldehyde with cassia twig leaf, cassia bark, only need to add a hydrolysis reactor and just can carry out, compare less investment with existing oil of bay producing benzaldehyde technology in former oil of bay production unit back, operational path is short, energy efficient, and production cost is low.Calculating crude benzol formaldehyde yield by the cassia twig leaf is 0.5%.
Embodiment
The present invention adopts following route to carry out: cassia twig leaf or cassia bark are chopped into about 3-9cm, put into the charging frame, frame is put into still kettle, add basic catalyst (sodium hydroxide, potassium hydroxide, calcium hydroxide, yellow soda ash, salt of wormwood, the perhaps mixture between them), cover lid, the inlet of hydrolysis reactor is received in the outlet of still kettle, still kettle is fed water vapor, water vapor has been carried oil of bay during by the cassia twig leaf secretly, the mixed steam that has oil of bay contacts with catalyzer, reaction is hydrolyzed under the situation of gas phase, the phenyl aldehyde that obtains is exported hydrolysis reactor together with steam, distillation time is 2-4h, obtain the crude benzol formaldehyde products after condensation and the oily water separation, its phenyl aldehyde content is 65-82.5% (vapor-phase chromatography), can directly use as foodstuff additive or purify by rectifying separation under reduced pressure at last, obtains the food-class high-purity phenyl aldehyde.
Embodiment 1:
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, in the 6L hydrolysis reactor, add catalyzer 1% (weight percent, as follows) sodium hydroxide 1L, feed 0.1Mpa steam, reaction 4h stops heating, obtain crude benzol formaldehyde 40.0g, its phenyl aldehyde content is 82.1% (vapor-phase chromatography, down together).
Embodiment 2
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, adds catalyzer 1% potassium hydroxide 1L in the 6L hydrolysis reactor, feeds 0.1Mpa steam, and reaction 4h stops heating, obtains crude benzol formaldehyde 40.1g, and its phenyl aldehyde content is 80.2%.
Embodiment 3
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, adds catalyzer 4% calcium hydroxide 1L in the 6L hydrolysis reactor, feeds 0.1Mpa steam, and reaction 4h stops heating, obtains crude benzol formaldehyde 20g, and its phenyl aldehyde content is 65.1%.
Embodiment 4
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, add each 0.5L of yellow soda ash of catalyzer 0.6% sodium hydroxide+8% in the 6L hydrolysis reactor, feed 0.1Mpa steam, reaction 4h stops heating, obtain crude benzol formaldehyde 36g, its phenyl aldehyde content is 76.6%.
Embodiment 5
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, add each 0.5L of salt of wormwood of catalyzer 0.5% potassium hydroxide+8% in the 6L hydrolysis reactor, feed 0.1Mpa steam, reaction 4h stops heating, obtain crude benzol formaldehyde 37g, its phenyl aldehyde content is 78.5%.
Embodiment 6
The cassia twig leaf 8kg that takes by weighing 3-6cm length puts into still kettle charging frame, adds catalyzer 1% sodium hydroxide in the 6L hydrolysis reactor, feeds 0.5Mpa steam, reaction 2h steams cut oil-containing not substantially, stops heating, oily water separation obtains crude benzol formaldehyde 38g, and its phenyl aldehyde content is 79.4%.
Embodiment 7:
The cassia twig leaf 8kg that takes by weighing 7-9cm length puts into still kettle charging frame, adds 1% sodium hydroxide catalyst 1L in hydrolysis reactor, feeds 0.1Mpa steam, reaction 4h steams cut oil-containing not substantially, stops heating, oily water separation obtains crude benzol formaldehyde 39.6g, and its phenyl aldehyde content is 80.4%.
Embodiment 8:
The broked bark 5kg that takes by weighing the 2-3cm size puts into still kettle charging frame, adds 1% sodium hydroxide catalyst 1L in hydrolysis reactor, feeds 0.1Mpa steam, reaction 4h steams cut oil-containing not substantially, stops heating, oily water separation obtains crude benzol formaldehyde 31.5g, and its phenyl aldehyde content is 80.6%.
Claims (1)
1. one kind is the method for raw material direct production natural benzaldehyde with cassia twig leaf, cassia bark, distill putting into still kettle after cassia twig leaf or the cassia bark chopping, water vapor has been carried oil of bay during by the cassia twig leaf secretly, it is characterized in that still kettle exports the inlet that direct water receiving is separated reactor, the hot mixed steam that enters hydrolysis reactor contacts with basic catalyst, the reaction that is hydrolyzed under the situation of gas phase, the phenyl aldehyde of generation from hydrolysis reactor outlet output, obtains the crude benzol formaldehyde products with steam after the condensation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100196056A CN1308278C (en) | 2005-10-13 | 2005-10-13 | Process for directly producing natural benzaldehyde using cassia twig leaf and cassia bark as raw material |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100196056A CN1308278C (en) | 2005-10-13 | 2005-10-13 | Process for directly producing natural benzaldehyde using cassia twig leaf and cassia bark as raw material |
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| CN1749231A CN1749231A (en) | 2006-03-22 |
| CN1308278C true CN1308278C (en) | 2007-04-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101355476B (en) * | 2008-05-23 | 2011-05-11 | 林云帆 | System and method for storing, distributing and applying data files based on server cluster |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456799B (en) * | 2008-12-30 | 2012-07-04 | 上海华盛香料有限公司 | Method for producing natural benzaldehyde by employing three-way nozzle atomization |
| CN107141211B (en) * | 2017-07-03 | 2020-11-13 | 广西大学 | Preparation method of benzaldehyde |
| CN110257173A (en) * | 2019-06-11 | 2019-09-20 | 广西大学 | The method for being rich in natural benzaldehyde fragrance essential oil from cinnamon leaf preparation |
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2005
- 2005-10-13 CN CNB2005100196056A patent/CN1308278C/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
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| 相转移催化条件下从桂叶油制备天然苯甲醛的研究 崔建国等，化学世界，第6卷 2001 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101355476B (en) * | 2008-05-23 | 2011-05-11 | 林云帆 | System and method for storing, distributing and applying data files based on server cluster |
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| CN1749231A (en) | 2006-03-22 |
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Granted publication date: 20070404 Termination date: 20111013 |