CN1911891A - Preparation method of natural benzaldehyde - Google Patents
Preparation method of natural benzaldehyde Download PDFInfo
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- CN1911891A CN1911891A CN 200610030173 CN200610030173A CN1911891A CN 1911891 A CN1911891 A CN 1911891A CN 200610030173 CN200610030173 CN 200610030173 CN 200610030173 A CN200610030173 A CN 200610030173A CN 1911891 A CN1911891 A CN 1911891A
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- alkaline matter
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- natural benzaldehyde
- acetaldehyde
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Abstract
The natural benzaldehyde preparing process includes the following steps: the heated reaction between natural cinnamic aldehyde and water solution of alkaline matter in a reactor to produce natural benzaldehyde and acetaldehyde; rectification in a rectifier in the upper part of the reactor to produce gaseous natural benzaldehyde and acetaldehyde in the top of the rectifier; condensing the gaseous natural benzaldehyde and acetaldehyde; and conveying partial product to post section. The process has continuous elimination of the produced natural benzaldehyde and acetaldehyde, high material concentration, high reaction efficiency, low production cost and high product quality.
Description
Technical field
The present invention relates to a kind of preparation method of natural benzaldehyde.
Background technology
Natural benzaldehyde is a kind of important spices, has very to use widely in food, daily chemical industry.
At present, natural benzaldehyde is that raw material is prepared with cinnamic aldehyde and basic solution, adopts rhythmic reaction.Because it is a kind of reversible reaction that cinnamic aldehyde and alkaline matter generate the reaction of natural benzaldehyde, therefore, carrying out along with reaction, in the reaction product, the content of natural benzaldehyde improves constantly, and speed of response constantly reduces, and the natural benzaldehyde content in the reaction product is owing to the reason of molecular balance, can't further improve, influence reaction yield and reaction efficiency.Owing to be used to prepare the spices of food, detergents and cosmetic certain requirement is arranged, natural cinnamic aldehyde derives from the essential oil of natural plant usually, as oil of bay, therefore price is very expensive, simultaneously, natural benzaldehyde also can condensation, therefore, present production method has caused the production cost of product natural benzaldehyde to reduce, and quality product is not high.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of natural benzaldehyde, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
The aqueous solution of natural cinnamic aldehyde and alkaline matter is added top be provided with reacting by heating in the reactor of rectifier unit, generate natural benzaldehyde and acetaldehyde, and pass through rectifier unit, adopt the method for rectifying, constantly removing natural benzaldehyde and the acetaldehyde that generates the reaction process from the top of rectifier unit, refluxes in the natural benzaldehyde condensation of gas rear section of discharge, and part is as product, be sent to follow-up workshop section, it is standby that the aldehydes gas of discharge is collected the back;
Temperature of reaction is the boiling temperature of the aqueous solution of alkaline matter, is generally 95～105 ℃, and the reaction times is 5～15 hours, and the reflux ratio of rectifying is 1.5～5;
Said alkaline matter is selected from alkali-metal oxyhydroxide or alkali-metal carbonate, preferred sodium hydroxide, potassium hydroxide, yellow soda ash or ammonium hydroxide;
The weight concentration of the aqueous solution of alkaline matter is 1～5%;
The mol ratio of cinnamic aldehyde and alkaline matter is:
Cinnamic aldehyde: alkaline matter=1: 0.1～0.3;
Reaction expression is as follows:
According to preferable methods of the present invention,, can feed rare gas element at reactor bottom, as nitrogen in order effectively to get rid of natural benzaldehyde and the acetaldehyde that generates in the reaction process;
According to preferable methods of the present invention, the aqueous solution with alkaline matter adds reactor earlier, is heated to temperature of reaction then, then natural cinnamic aldehyde is added reactor and reacts.
Advantage of the present invention is very significant, in the reaction process, constantly gets rid of the product that reaction generates: natural benzaldehyde and acetaldehyde, therefore in the reactive system, the concentration of raw material is higher, helps the carrying out that reacts, reaction efficiency is higher, and production cost has descended 15% than prior art.Simultaneously, natural benzaldehyde also is not easy polycondensation, has guaranteed the quality of product.
Embodiment
Embodiment 1
With 500 kilogram weights of concentration is that 2% aqueous sodium hydroxide solution adds top and is provided with in the reactor of rectifier unit, be heated to boiling, then 200 kilograms of cinnamic aldehydes being added reactor reacts, generate natural benzaldehyde and acetaldehyde, and pass through rectifier unit, adopt the method for rectifying, constantly remove natural benzaldehyde and the acetaldehyde that generates the reaction process from the rectifier unit top, reflux in the natural benzaldehyde condensation of gas rear section of discharging, part is as product, be sent to follow-up workshop section, it is standby that the aldehydes gas of discharge is collected the back, and the reflux ratio of rectifying is 2.5;
React after 10 hours, obtain weight concentration and be 140 kilograms of 95% natural benzaldehydes, the reaction yield is 83%.
Embodiment 2
With 200 kilogram weights of concentration is that 5% aqueous sodium carbonate adds top and is provided with in the reactor of rectifier unit, be heated to boiling, then 80 kilograms of natural cinnamic aldehydes being added reactor reacts, generate natural benzaldehyde and acetaldehyde, and pass through rectifier unit, adopt the method for rectifying, constantly remove natural benzaldehyde and the acetaldehyde that generates the reaction process from the rectifier unit top, reflux in the natural benzaldehyde condensation of gas rear section of discharging, part is as product, be sent to follow-up workshop section, it is standby that the aldehydes gas of discharge is collected the back, and the reflux ratio of rectifying is 3;
React after 12 hours, obtain weight concentration and be 54 kilograms of 94% natural benzaldehydes, the reaction yield is 79%.
Claims (9)
1. the preparation method of a natural benzaldehyde, it is characterized in that, comprise the steps: that the aqueous solution of natural cinnamic aldehyde and alkaline matter is added top is provided with reacting by heating in the reactor of rectifier unit, generate natural benzaldehyde and acetaldehyde, and, adopt the method for rectifying by rectifier unit, constantly remove natural benzaldehyde and the acetaldehyde that generates the reaction process from the top of rectifier unit, reflux in the natural benzaldehyde condensation of gas rear section of discharging, part is sent to follow-up workshop section as product.
2. method according to claim 1 is characterized in that, temperature of reaction is the boiling temperature of the aqueous solution of alkaline matter.
3. method according to claim 1 is characterized in that, the reaction times is 5～15 hours.
4. method according to claim 1 is characterized in that, the reflux ratio of rectifying is 1.5～5.
5. according to each described method of claim 1～4, it is characterized in that said alkaline matter is selected from alkali-metal oxyhydroxide or alkali-metal carbonate or ammonium hydroxide.
6. method according to claim 5 is characterized in that alkaline matter is selected from sodium hydroxide, potassium hydroxide or yellow soda ash.
7. method according to claim 5 is characterized in that, the weight concentration of the aqueous solution of alkaline matter is 1～5%, and the mol ratio of cinnamic aldehyde and alkaline matter is:
Cinnamic aldehyde: alkaline matter=1: 0.1～0.3.
8. method according to claim 1 is characterized in that, feeds rare gas element at reactor bottom.
9. method according to claim 1 is characterized in that, the aqueous solution with alkaline matter adds reactor earlier, is heated to temperature of reaction then, more natural cinnamic aldehyde is added reactor and reacts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610030173 CN1911891A (en) | 2006-08-17 | 2006-08-17 | Preparation method of natural benzaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610030173 CN1911891A (en) | 2006-08-17 | 2006-08-17 | Preparation method of natural benzaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1911891A true CN1911891A (en) | 2007-02-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610030173 Pending CN1911891A (en) | 2006-08-17 | 2006-08-17 | Preparation method of natural benzaldehyde |
Country Status (1)
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| CN (1) | CN1911891A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985414A (en) * | 2010-09-27 | 2011-03-16 | 高要市华新香料有限公司 | Production method for natural benzaldehyde |
| 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 |
| CN105016994A (en) * | 2015-07-28 | 2015-11-04 | 广西壮族自治区林业科学研究院 | Device for preparing benzaldehyde from cinnamaldehyde |
| 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 |
| CN114057555A (en) * | 2021-11-02 | 2022-02-18 | 盐城市春竹香料有限公司 | Benzaldehyde preparation process and device with disodium hydrogen phosphate as alkaline catalyst |
-
2006
- 2006-08-17 CN CN 200610030173 patent/CN1911891A/en active Pending
Cited By (8)
| 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 |
| CN101985414A (en) * | 2010-09-27 | 2011-03-16 | 高要市华新香料有限公司 | Production method for natural benzaldehyde |
| CN101985414B (en) * | 2010-09-27 | 2013-08-07 | 高要市华新香料有限公司 | Production method for natural benzaldehyde |
| CN105016994A (en) * | 2015-07-28 | 2015-11-04 | 广西壮族自治区林业科学研究院 | Device for preparing benzaldehyde from cinnamaldehyde |
| CN105016994B (en) * | 2015-07-28 | 2017-05-10 | 广西壮族自治区林业科学研究院 | Device for preparing benzaldehyde from cinnamaldehyde |
| 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 |
| CN114057555A (en) * | 2021-11-02 | 2022-02-18 | 盐城市春竹香料有限公司 | Benzaldehyde preparation process and device with disodium hydrogen phosphate as alkaline catalyst |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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