CN105541586A - Natural-grade benzaldehyde preparation method - Google Patents
Natural-grade benzaldehyde preparation method Download PDFInfo
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- CN105541586A CN105541586A CN201410600270.6A CN201410600270A CN105541586A CN 105541586 A CN105541586 A CN 105541586A CN 201410600270 A CN201410600270 A CN 201410600270A CN 105541586 A CN105541586 A CN 105541586A
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Abstract
The present invention relates to a natural-grade benzaldehyde preparation method, and belongs to the field of food additives and preparation methods thereof. The preparation method comprises that a raw material cinnamomum cassia presl oil and an alkali catalyst are poured into a reaction kettle, complete stirring is performed, N2 is introduced to protect, heating is started after 10 min, a reaction is performed at a reflux temperature under continuous stirring, the reaction product is separated through rectification and then is distilled through the top portion of a rectification column, water returns to a reaction bottle, and the distillate is dried on the top portion of the rectification column so as to obtain the natural-grade benzaldehyde. According to the present invention, the synthesis method has characteristics of simple process, strong operability, easy industrial production, high product quality, and the like; and the determination results show that the yield of the natural-grade benzaldehyde is 81%, and the cinnamaldehyde conversion rate is 82%.
Description
Technical field
The present invention relates to a kind of preparation method of Natural Benzaldehyde, belong to foodstuff additive and preparation method thereof field.
Background technology
Natural benzaldehyde has Semen Armeniacae Amarum aromatic odour, is a kind of important spices.For in various fruit flavour type food flavor(ing).Natural benzaldehyde be mainly derived from Semen Armeniacae Amarum, walnut and other contain in the nut oil of Vitamin B17, resource-constrained, world wide production is about 20 tons/year.But, comparatively large to edible phenyl aldehyde demand on world market, only about 3000 tons of the every annual consumption of food service industry, and the market requirement just increases progressively with the rate of rise in year 6%.Pure natural phenyl aldehyde obviously can not meet market demand.The eighties middle and later periods, there is report abroad with natural oil of bay for Natural Benzaldehyde prepared by raw material, be namely oxidized by Oleum Cinnamomi or make cinnamic aldehyde in Oleum Cinnamomi under alkali lye effect, obtain phenyl aldehyde through inverse aldol condensation.China's Oleum Cinnamomi aboundresources, and Oleum Cinnamomi consumption is limited, there is unsalable situation, needs development of meat oil of bay deep process technology.Be raw material production phenyl aldehyde by Oleum Cinnamomi be economically and technically all feasible.
Summary of the invention
It is simple, workable that the present invention aims to provide a kind of technique, is applicable to the preparation method of suitability for industrialized production and the high Natural Benzaldehyde of quality product.
The preparation method of described Natural Benzaldehyde, comprises the following steps:
Raw meat oil of bay and alkaline catalysts are put in reactor and also fully stir, pass into N2 protection, start after 10 minutes and heat, reflux temperature also reacts under Keep agitation, and reaction product is distillated by rectifying column top after rectifying separation, and water comes back in reaction flask.Natural Benzaldehyde is drying to obtain at rectifying column overhead.
Preferably, raw meat oil of bay of the present invention requires phenylacrolein mass content more than 91%.
Preferred, alkaline catalysts of the present invention is sodium carbonate, and consumption is the 3%-4% of raw meat oil of bay weight.
Preferred further, reflux temperature of the present invention is 100 DEG C, and stirring velocity is 150rpm, and the reaction times is 9-10h.
Preparation method of the present invention, under alkaline catalysts effect, the inverse aldol reaction of phenylacrolein adopts reactive distillation working method, namely the phenyl aldehyde produced in reaction process and acetaldehyde rectification method separate in time, to reduce by product and the further condensation of phenylacrolein, increase the generation that the reaction times is conducive to transforming completely of phenylacrolein and phenyl aldehyde.This reaction is liquid-liquid-liquid heterogeneous reaction, and the degree of uniformity that agitation as appropriate increases two-phase mixtures is conducive to improving speed of reaction.
It is simple, workable that synthetic method of the present invention has technique, is applicable to suitability for industrialized production and quality product high, and after measured, the Natural Benzaldehyde yield that present method obtains is 81%, and phenylacrolein transformation efficiency is 82%.
Embodiment
Embodiment one:
The raw meat oil of bay 1000g of phenylacrolein mass content more than 91% and alkaline catalysts sodium carbonate 30g is put in reactor and adds water and fully stir; pass into N2 protection; heating is started after 10 minutes; react 9 hours reflux temperature 100 DEG C and under being 150rpm Keep agitation with speed; reaction product is distillated by rectifying column top after rectifying separation, and water comes back in reaction flask.Be drying to obtain Natural Benzaldehyde 810g at rectifying column overhead, after measured, the Natural Benzaldehyde yield that present method obtains is 81%, and phenylacrolein transformation efficiency is 82%.
Embodiment two:
The raw meat oil of bay 1000g of phenylacrolein mass content more than 91% and alkaline catalysts sodium carbonate 40g is put in reactor and adds water and fully stir; pass into N2 protection; heating is started after 10 minutes; react 10 hours reflux temperature 100 DEG C and under being 150rpm Keep agitation with speed; reaction product is distillated by rectifying column top after rectifying separation, and water comes back in reaction flask.Be drying to obtain Natural Benzaldehyde 805g at rectifying column overhead, after measured, the Natural Benzaldehyde yield that present method obtains is 80.5%, and phenylacrolein transformation efficiency is 81.8%.
Claims (4)
1. the preparation method of Natural Benzaldehyde, comprises the following steps:
Raw meat oil of bay and alkaline catalysts are put in reactor and also fully stir; pass into N2 protection; heating is started after 10 minutes; reflux temperature also reacts under Keep agitation; reaction product is distillated by rectifying column top after rectifying separation; water comes back in reaction flask, is drying to obtain Natural Benzaldehyde at rectifying column overhead.
2. the preparation method of Natural Benzaldehyde as claimed in claim 1, is characterized in that described raw meat oil of bay requires phenylacrolein mass content more than 91%.
3. the preparation method of Natural Benzaldehyde as claimed in claim 1, it is characterized in that described alkaline catalysts is sodium carbonate, consumption is the 3%-4% of raw meat oil of bay weight.
4. the preparation method of Natural Benzaldehyde as claimed in claim 1, it is characterized in that described reflux temperature is 100 DEG C, stirring velocity is 150rpm, and the reaction times is 9-10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410600270.6A CN105541586A (en) | 2014-10-31 | 2014-10-31 | Natural-grade benzaldehyde preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410600270.6A CN105541586A (en) | 2014-10-31 | 2014-10-31 | Natural-grade benzaldehyde preparation method |
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| CN105541586A true CN105541586A (en) | 2016-05-04 |
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| CN201410600270.6A Pending CN105541586A (en) | 2014-10-31 | 2014-10-31 | Natural-grade benzaldehyde preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534970A (en) * | 2018-11-22 | 2019-03-29 | 湖南湘硕化工有限公司 | A kind of preparation method of high-purity natural benzaldehyde |
| CN110343035A (en) * | 2019-06-18 | 2019-10-18 | 福建森美达生物科技有限公司 | A method of injection continuous hydrolysis prepares natural benzaldehyde |
-
2014
- 2014-10-31 CN CN201410600270.6A patent/CN105541586A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534970A (en) * | 2018-11-22 | 2019-03-29 | 湖南湘硕化工有限公司 | A kind of preparation method of high-purity natural benzaldehyde |
| CN110343035A (en) * | 2019-06-18 | 2019-10-18 | 福建森美达生物科技有限公司 | A method of injection continuous hydrolysis prepares natural benzaldehyde |
| CN110343035B (en) * | 2019-06-18 | 2022-09-30 | 福建森美达生物科技有限公司 | Method for preparing natural benzaldehyde by spraying continuous hydrolysis |
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Application publication date: 20160504 |
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| WD01 | Invention patent application deemed withdrawn after publication |