CN102952640A - Geraniol spice and preparation method thereof - Google Patents
Geraniol spice and preparation method thereof Download PDFInfo
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- CN102952640A CN102952640A CN2012104598782A CN201210459878A CN102952640A CN 102952640 A CN102952640 A CN 102952640A CN 2012104598782 A CN2012104598782 A CN 2012104598782A CN 201210459878 A CN201210459878 A CN 201210459878A CN 102952640 A CN102952640 A CN 102952640A
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Abstract
The invention discloses a geraniol spice and a preparation method thereof. The geraniol spice comprises the following components in percentage by weight: 60-70 percent of geraniol and 30-40 percent of nerol. The preparation method of the geraniol spice comprises the following steps of: adding linalool into a reactor; adding a catalyst to perform isomerization reaction, wherein the temperature of the isomerization reaction is 140-170 DEG C, and the pressure of the isomerization reaction is one standard atmospheric pressure; keeping the temperature at 160 DEG C for reaction; starting to sample after 12 hours; stopping reaction until the linalool content is about 60 percent, wherein the reaction time is 14-28 hours; and filtering a product obtained by the isomerization reaction and then performing high-vacuum reduced pressure distillation to obtain the geraniol spice, wherein the catalyst is solid acid, the mass ratio of the catalyst to the linalool is 0.3-0.5:100, the pressure of the distillation is 0.3 Kpa, and the temperature is 74-78 DEG C. Compared with the prior art, the problem of high production cost existing in the conventional geraniol spice and the preparation method thereof can be solved.
Description
Technical field
The present invention relates to chemical industry rosin deep process technology field, especially a kind of Geraniol flavour content be about 65% and vernol content be about Geraniol of 35% and preparation method thereof.
Background technology
Geraniol, also name Geraniol, fragrant Flos Pelargonii alcohol, molecular formula C10H18O, acyclic monoterpene compounds.Colourless to yellow oily liquid, be volatile component, 229～230 ℃ of boiling points (100.925kPa), 114～115 ℃ (1.60kPa), density 0.8894g/cm3, specific refractory power 1.4766 has gentleness, sweet Rose breath, the essence that is widely used in modulating various skincare products, perfume, essential oil as spices also can be used as the seasonings of soft drink, ice-creams, candy, jelly and pudding.
Geraniol spices can extract from plant, also can industrially synthesize.Industrial production Geraniol, generally one-level muriate and the sodium acetate with myrcene is total to the heat generation.This method complex procedures, and production cost is high the time, and the quality of product is not high.
Summary of the invention
The invention provides a kind of Geraniol spices and preparation method thereof, to solve the high problem of existing Geraniol production of flavor cost.
In order to address the above problem, technical scheme of the present invention is: it is 60%～70% Geraniol and 30%～40% vernol that composition of the present invention includes weight percent.
In order to address the above problem, technical scheme of the present invention is: present method may further comprise the steps: phantol is thrown in the reactor, add catalyzer and carry out isomerization reaction, the temperature of described isomerization reaction is 140 ° of C～170 ° C, the pressure of described isomerization reaction is a standard atmospheric pressure, maintaining the temperature at 160 ° of C reacts, began sampling in 12 hours, until phantol content stopped reaction when being about 60%, reaction times is 14～28 hours, the product of described isomerization reaction is carried out the high vacuum underpressure distillation after filtering and get final product; Described catalyzer is solid acid, with the weight ratio of phantol is: 0.3～0.5:100; The pressure of described distillation is 0.3Kpa, and temperature is 74 ° of C～78 ° C.
In the technique scheme, more specifically scheme can be: the temperature of described isomerization reaction is 160 ° of C, and the weight ratio of described catalyzer and phantol is: 0.4:100.
All in Geraniol, add the vernol with the rose main note in the prescription modulation of a lot of essence, because in the fragrance of these two kinds of spices all with rose fragrance, this is their excessive fragrance just, make their fragrance be easy to just be fused together, the characteristics that can not project oneself very much make this mixture that own unique fragrance, the delicate fragrance of existing flower be arranged, the fragrance that rose and flores aurantii are arranged again is well suited for doing essence and uses.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
The monomer Geraniol content 60%～70% of this Geraniol spices, the content 96%～100% of Geraniol and vernol sum.This Geraniol spices contains vernol, and the fragrance of pleasant rose and flores aurantii is arranged, and fragrance is more gentle, little fruital with the lemon sample, vernol are the isomer of Geraniol, and its fragrance is than the soft grace of Geraniol, relatively partially clear, and with fresh delicate fragrance and oranges and tangerines aromatic.Because vernol is the isomers of Geraniol, when producing Geraniol, can be accompanied by the production of vernol, both physical property are similar, separate to be difficult to.The Geraniol that obtains 98% above content need to consume a large amount of energy, and output, yield are very low.If as long as Geraniol content is more than 65%, the words of two pure content more than 96% just can reduce energy consumption greatly, and output also can significantly improve.The indexs such as fragrance change little.
Embodiment
Embodiment one:
The phantol of 4 ton of 90.8% content is added all in the reactor, drop into 0.016 ton of solid acid and make catalyzer, depress at a standard atmosphere and to carry out stirring heating, maintain the temperature at 160 ° of C and carry out isomerization reaction, began sampling in 12 hours, until phantol content stopped reaction when being about 60%, the end reaction time is 20 hours.The final content of the product through isomerization reaction--reaction solution is phantol 60.3%, Geraniol 19.3%, vernol 9.1%.Reaction solution is carried out press filtration filters out solid acid catalyst, filtrate after the filtration enters into distillation tower and carries out the high vacuum underpressure distillation, at first unreacted phantol being distilled the raw material of doing the next batch reaction continues to use, then the distillation pressure be under the 0.3Kpa, temperature be the lower vernol of 74 ° of C～78 ° C condition and Geraniol mixture distillation out.Obtain at last 2.60 tons of content and be 90.3% phantol and 1.05 tons of content and be 65.8% Geraniol and content and be the mixture of 30.5% vernol.This mixture has own unique fragrance, and the delicate fragrance of existing flower has again the fragrance of rose and flores aurantii, is well suited for doing essence and uses.
Embodiment two:
The phantol of 4 ton of 90.8% content is added all in the reactor, drop into 0.012 ton of solid acid and make catalyzer, depress at a standard atmosphere and to carry out stirring heating, maintain the temperature at 150 ° of C and carry out isomerization reaction, began sampling in 12 hours, until phantol content stopped reaction when being about 60%, the end reaction time is 26 hours.The final content of the product through isomerization reaction--reaction solution is phantol 61.2 %, Geraniol 18.5%, vernol 10.1%.Reaction solution is carried out press filtration filters out solid acid catalyst, filtrate after the filtration enters into distillation tower and carries out the high vacuum underpressure distillation, at first unreacted phantol being distilled the raw material of doing the next batch reaction continues to use, then the distillation pressure be under the 0.3Kpa, temperature be the lower vernol of 73 ° of C～78 ° C condition and Geraniol mixture distillation out.Obtain at last 2.56 tons of content and be 90.6% phantol and 1.08 tons of content and be 60.2% Geraniol and content and be the mixture of 36.6% vernol.This mixture has own unique fragrance, and the delicate fragrance of existing flower has again the fragrance of rose and flores aurantii, is well suited for doing essence and uses.
Embodiment three:
The phantol of 4 ton of 90.8% content is added all in the reactor, drop into 0.020 ton of solid acid and make catalyzer, depress at a standard atmosphere and to carry out stirring heating, maintain the temperature at 170 ° of C and carry out isomerization reaction, began sampling in 12 hours, until phantol content stopped reaction when being about 60%, the end reaction time is 16 hours.The final content of the product through isomerization reaction--reaction solution is phantol 59.6%, Geraniol 20.9%, vernol 9.0%.Reaction solution is carried out press filtration filters out solid acid catalyst, filtrate after the filtration enters into distillation tower and carries out the high vacuum underpressure distillation, at first unreacted phantol being distilled the raw material of doing the next batch reaction continues to use, then the distillation pressure be under the 0.3Kpa, temperature be the lower vernol of 74 ° of C～79 ° C condition and Geraniol mixture distillation out.Obtain at last 2.52 tons of content and be 90.7% phantol and 1.05 tons of content and be 70.5% Geraniol and content and be the mixture of 26.2% vernol.This mixture has own unique fragrance, and the delicate fragrance of existing flower has again the fragrance of rose and flores aurantii, is well suited for doing essence and uses.
Claims (3)
1. Geraniol spices is characterized in that: it is 60%～70% Geraniol and 30%～40% vernol that its composition includes weight percent.
2. the preparation method of a Geraniol spices, may further comprise the steps: phantol is thrown in the reactor, add catalyzer and carry out isomerization reaction, it is characterized in that: the temperature of described isomerization reaction is 140 ° of C～170 ° C, the pressure of described isomerization reaction is a standard atmospheric pressure, maintaining the temperature at 160 ° of C reacts, began sampling in 12 hours, until phantol content stopped reaction when being about 60%, reaction times is 14～28 hours, the product of described isomerization reaction is carried out the high vacuum underpressure distillation after filtering and get final product;
Described catalyzer is solid acid, with the weight ratio of phantol is: 0.3～0.5:100;
The pressure of described distillation is 0.3Kpa, and temperature is 74 ° of C～78 ° C.
3. Geraniol spices according to claim 1 and 2 and preparation method thereof, it is characterized in that: the temperature of described isomerization reaction is 160 ° of C, and the weight ratio of described catalyzer and phantol is: 0.4:100.
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| CN2012104598782A CN102952640A (en) | 2012-11-15 | 2012-11-15 | Geraniol spice and preparation method thereof |
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| CN2012104598782A CN102952640A (en) | 2012-11-15 | 2012-11-15 | Geraniol spice and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1200028A (en) * | 1995-08-31 | 1998-11-25 | 普罗格特-甘布尔公司 | Use of allylic alcohol perfumes as a malodour reduction agent |
| CN1599706A (en) * | 2001-12-07 | 2005-03-23 | 巴斯福股份公司 | Method for isomerizing allyl alcohols |
| CN1194950C (en) * | 2003-02-21 | 2005-03-30 | 中国科学院广州化学研究所 | Process for synthesizing geraniol/nerol from linalool |
-
2012
- 2012-11-15 CN CN2012104598782A patent/CN102952640A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1200028A (en) * | 1995-08-31 | 1998-11-25 | 普罗格特-甘布尔公司 | Use of allylic alcohol perfumes as a malodour reduction agent |
| CN1599706A (en) * | 2001-12-07 | 2005-03-23 | 巴斯福股份公司 | Method for isomerizing allyl alcohols |
| CN1194950C (en) * | 2003-02-21 | 2005-03-30 | 中国科学院广州化学研究所 | Process for synthesizing geraniol/nerol from linalool |
Non-Patent Citations (3)
| Title |
|---|
| 孙立宏；孙立明: "香叶醇的研究进展", 《西北药学杂志》, vol. 24, no. 5, 15 October 2009 (2009-10-15), pages 428 - 430 * |
| 韩金玉 等: "真空间歇精馏分离橙花醇和香叶醇的研究", 《化学工业与工程》, vol. 20, no. 6, 30 December 2003 (2003-12-30), pages 430 - 434 * |
| 黄宇平 等: "钒化合物催化芳樟醇酯化异构制取香叶醇、橙花醇", 《林产化工通讯》, vol. 39, no. 2, 30 April 2005 (2005-04-30) * |
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Application publication date: 20130306 |