CN102399632A - Crude mint oil freeze crystallization method - Google Patents
Crude mint oil freeze crystallization method Download PDFInfo
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- CN102399632A CN102399632A CN2010102803567A CN201010280356A CN102399632A CN 102399632 A CN102399632 A CN 102399632A CN 2010102803567 A CN2010102803567 A CN 2010102803567A CN 201010280356 A CN201010280356 A CN 201010280356A CN 102399632 A CN102399632 A CN 102399632A
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Abstract
The present invention discloses a crude mint oil freeze crystallization method. According to the present invention, the crude mint oil is subjected to two freeze crystallization to carry out separation to obtain primary crystallization oil, secondary crystallization oil and non-crystallized oil. Compared to the prior art, the crude mint oil freeze crystallization method of the present invention has the following significant advantages that: the product produced by the method of the present invention has high yield and good quality.
Description
Technical field
The present invention relates to a kind of separation method of crude peppermint oil bu, be specifically related to a kind ofly crude peppermint oil bu is separated into first cerebrol, two method of cerebrols and hair vegetable oil just through freezing precipitation and crystallization.
Background technology
Crude peppermint oil bu is by the fresh cauline leaf of peppermint, gets through steam distillation, and proterties is colourless to flaxen clear liquid, and no moisture and any mechanical impurity have inferior state peppermint characteristic perfume, do not have other unpleasant odor.The separation of crude peppermint oil bu is the indispensable operation of preparation TK-10 and peppermint wet goods product, and the control of this process conditions directly influences the output and the quality of corresponding product.
Summary of the invention
Goal of the invention: the objective of the invention is in order to solve the deficiency of prior art, a kind of effective, method that crude peppermint oil bu that output is high freezes precipitation and crystallization is provided.
Technical scheme: crude peppermint oil bu of the present invention freezes the method for precipitation and crystallization, and its objective is such realization: a kind of crude peppermint oil bu freezes the method for precipitation and crystallization, may further comprise the steps:
1) with oil pump crude peppermint oil bu in the crude oil basin is sent into and frozen in the parser, with brinepump the chilled brine in the refrigerator is sent into to freeze in the parser cooling coil then and circulate, once freeze and analyse to specified quantity, during beginning, first frozen cooling, needing the time is 5～6 hours;
2) crude oil begins crystallization, needs insulation 4～6 hours, and brine temp is controlled at-6 ± 1 ℃;
3) insulation end brine temp reduces until-21 ± 2 ℃ gradually, and temperature fall time was controlled at 8～10 hours, and oily temperature is finally reduced to-2 ± 2 ℃;
4) at this moment, isolate crystalline and be " first brain ", uncrystallized is secondary oil;
5) once freeze analyse end after; Open and freeze parser oil strain valve, secondary oil is put into the oil strain groove, oil filtration time is general more than 18 hours; Using the hot salt brine pump then is that 75～80 ℃ hot salt brine is sent into to freeze in the parser comb and circulated with temperature in the hot salt brine basin; Make first brain dissolve cerebrol just, the back is sent it into the dehydration pot with oil pump and is carried out vacuum hydro-extraction, or it is subsequent use to send into the cerebrol basin;
6) with oil pump secondary oil is thrown into and frozen parser, the beginning secondary freezes analyses, and this class of operation is similar to once to freeze and analyses, and brine temp is controlled at-22 ± 2 ℃;
7) secondary freezes and analyses end, and this moment, crystalline was two first cerebrols, and is uncrystallized for hair vegetable oil.
As preferably: brine temp is-6 ℃ step 2).
As preferably: brine temp is reduced to-21 ℃ in the step 3), makes oily temperature finally reduce to-2 ℃.
As preferably: brine temp is controlled at-22 ℃ in the step 6).
Beneficial effect: the method that crude peppermint oil bu of the present invention freezes precipitation and crystallization compared with prior art, its remarkable advantage is: the product production of producing through present method is high, and quality is good.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1
A kind of crude peppermint oil bu freezes the method for precipitation and crystallization, may further comprise the steps:
1) with oil pump crude peppermint oil bu in the crude oil basin is sent into and frozen in the parser, with brinepump the chilled brine in the refrigerator is sent into to freeze in the parser cooling coil then and circulate, once freeze and analyse to specified quantity, during beginning, first frozen cooling, needing the time is 5 hours;
2) crude oil begins crystallization, needs insulation 4 hours, and brine temp is controlled at-7 ℃;
3) insulation end brine temp reduces until-23 ℃ gradually, and temperature fall time was controlled at 8 hours, and oily temperature is finally reduced to-4 ℃;
4) at this moment, isolate crystalline and be " first brain ", uncrystallized is secondary oil;
5) once freeze analyse end after; Open and freeze parser oil strain valve, secondary oil is put into the oil strain groove, oil filtration time is general more than 18 hours; Using the hot salt brine pump then is that 75 ℃ hot salt brine is sent into to freeze in the parser comb and circulated with temperature in the hot salt brine basin; Make first brain dissolve cerebrol just, the back is sent it into the dehydration pot with oil pump and is carried out vacuum hydro-extraction, or it is subsequent use to send into the cerebrol basin;
6) with oil pump secondary oil is thrown into and frozen parser, the beginning secondary freezes analyses, and this class of operation is similar to once to freeze and analyses, and brine temp is controlled at-24 ℃;
7) secondary freezes and analyses end, and this moment, crystalline was two first cerebrols, and uncrystallized be a mao vegetable oil.
Embodiment 2
A kind of crude peppermint oil bu freezes the method for precipitation and crystallization, may further comprise the steps:
1) with oil pump crude peppermint oil bu in the crude oil basin is sent into and frozen in the parser, with brinepump the chilled brine in the refrigerator is sent into to freeze in the parser cooling coil then and circulate, once freeze and analyse to specified quantity, during beginning, first frozen cooling, needing the time is 5.5 hours;
2) crude oil begins crystallization, needs insulation 5 hours, and brine temp is controlled at-6 ℃;
3) insulation end brine temp reduces until-21 ℃ gradually, and temperature fall time was controlled at 9 hours, and oily temperature is finally reduced to-2 ℃;
4) at this moment, isolate crystalline and be " first brain ", uncrystallized is secondary oil;
5) once freeze analyse end after; Open and freeze parser oil strain valve, secondary oil is put into the oil strain groove, oil filtration time is general more than 18 hours; Using the hot salt brine pump then is that 77 ℃ hot salt brine is sent into to freeze in the parser comb and circulated with temperature in the hot salt brine basin; Make first brain dissolve cerebrol just, the back is sent it into the dehydration pot with oil pump and is carried out vacuum hydro-extraction, or it is subsequent use to send into the cerebrol basin;
6) with oil pump secondary oil is thrown into and frozen parser, the beginning secondary freezes analyses, and this class of operation is similar to once to freeze and analyses, and brine temp is controlled at-22 ℃;
7) secondary freezes and analyses end, and this moment, crystalline was two first cerebrols, and is uncrystallized for hair vegetable oil.
Embodiment 3
A kind of crude peppermint oil bu freezes the method for precipitation and crystallization, may further comprise the steps:
1) with oil pump crude peppermint oil bu in the crude oil basin is sent into and frozen in the parser, with brinepump the chilled brine in the refrigerator is sent into to freeze in the parser cooling coil then and circulate, once freeze and analyse to specified quantity, during beginning, first frozen cooling, needing the time is 6 hours;
2) crude oil begins crystallization, needs insulation 6 hours, and brine temp is controlled at-5 ℃;
3) insulation end brine temp reduces until-19 ℃ gradually, and temperature fall time was controlled at 10 hours, and oily temperature is finally reduced to 0 ℃;
4) at this moment, isolate crystalline and be " first brain ", uncrystallized is secondary oil;
5) once freeze analyse end after; Open and freeze parser oil strain valve, secondary oil is put into the oil strain groove, oil filtration time is general more than 18 hours; Using the hot salt brine pump then is that 80 ℃ hot salt brine is sent into to freeze in the parser comb and circulated with temperature in the hot salt brine basin; Make first brain dissolve cerebrol just, the back is sent it into the dehydration pot with oil pump and is carried out vacuum hydro-extraction, or it is subsequent use to send into the cerebrol basin;
6) with oil pump secondary oil is thrown into and frozen parser, the beginning secondary freezes analyses, and this class of operation is similar to once to freeze and analyses, and brine temp is controlled at 20 ℃;
7) secondary freezes and analyses end, and this moment, crystalline was two first cerebrols, and uncrystallized be a mao vegetable oil.
Claims (4)
1. method that crude peppermint oil bu freezes precipitation and crystallization is characterized in that: may further comprise the steps:
1) with oil pump crude peppermint oil bu in the crude oil basin is sent into and frozen in the parser, with brinepump the chilled brine in the refrigerator is sent into to freeze in the parser cooling coil then and circulate, once freeze and analyse to specified quantity, during beginning, first frozen cooling, needing the time is 5～6 hours;
2) crude oil begins crystallization, needs insulation 4～6 hours, and brine temp is controlled at-6 ± 1 ℃;
3) insulation end brine temp reduces until-21 ± 2 ℃ gradually, and temperature fall time was controlled at 8～10 hours, and oily temperature is finally reduced to-2 ± 2 ℃;
4) at this moment, isolate crystalline and be " first brain ", uncrystallized is secondary oil;
5) once freeze analyse end after; Open and freeze parser oil strain valve, secondary oil is put into the oil strain groove, oil filtration time is general more than 18 hours; Using the hot salt brine pump then is that 75～80 ℃ hot salt brine is sent into to freeze in the parser comb and circulated with temperature in the hot salt brine basin; Make first brain dissolve cerebrol just, the back is sent it into the dehydration pot with oil pump and is carried out vacuum hydro-extraction, or it is subsequent use to send into the cerebrol basin;
6) with oil pump secondary oil is thrown into and frozen parser, the beginning secondary freezes analyses, and this class of operation is similar to once to freeze and analyses, and brine temp is controlled at-22 ± 2 ℃;
7) secondary freezes and analyses end, and this moment, crystalline was two first cerebrols, and uncrystallized be a mao vegetable oil.
2. a kind of crude peppermint oil bu according to claim 1 freezes the method for precipitation and crystallization, it is characterized in that: brine temp is-6 ℃ said step 2).
3. a kind of crude peppermint oil bu according to claim 1 freezes the method for precipitation and crystallization, it is characterized in that: brine temp is reduced to-21 ℃ in the said step 3), makes oily temperature finally reduce to-2 ℃.
4. a kind of crude peppermint oil bu according to claim 1 freezes the method for precipitation and crystallization, it is characterized in that: brine temp is controlled at-22 ℃ in the said step 6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102803567A CN102399632A (en) | 2010-09-14 | 2010-09-14 | Crude mint oil freeze crystallization method |
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| CN2010102803567A CN102399632A (en) | 2010-09-14 | 2010-09-14 | Crude mint oil freeze crystallization method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660377A (en) * | 2012-05-28 | 2012-09-12 | 杨玉赞 | Method for extracting animal offal oil |
| CN106619807A (en) * | 2016-12-23 | 2017-05-10 | 黄山天目薄荷药业有限公司 | Production process of peppermint oil |
| CN106631700A (en) * | 2016-12-23 | 2017-05-10 | 黄山天目薄荷药业有限公司 | Production process of menthol |
| CN110643426A (en) * | 2019-10-18 | 2020-01-03 | 安徽爱迪香料股份有限公司 | Peppermint oil production process |
| CN112047814A (en) * | 2020-08-14 | 2020-12-08 | 黄山天目薄荷药业有限公司 | Preparation method of high-purity menthol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09217085A (en) * | 1996-02-09 | 1997-08-19 | Ogawa Koryo Kk | Modified mint oils and the production of the same |
| CN101265162A (en) * | 2007-03-16 | 2008-09-17 | 高砂香料工业株式会社 | Process for purifying menthol |
-
2010
- 2010-09-14 CN CN2010102803567A patent/CN102399632A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09217085A (en) * | 1996-02-09 | 1997-08-19 | Ogawa Koryo Kk | Modified mint oils and the production of the same |
| CN101265162A (en) * | 2007-03-16 | 2008-09-17 | 高砂香料工业株式会社 | Process for purifying menthol |
Non-Patent Citations (3)
| Title |
|---|
| 刘红杰等: "《薄荷油研究进展》", 《山东中医药大学学报》, vol. 30, no. 6, 31 December 2006 (2006-12-31), pages 502 - 505 * |
| 庞承新: "《精馏-冷冻结晶技术分离天然薄荷脑的研究条件》", 《广西师范学院学报（自然科学版）》, vol. 20, no. 4, 31 December 2003 (2003-12-31), pages 61 - 63 * |
| 陶贤平等: "《化工实习及毕业论文（设计）指导》", 30 August 2010, article "《薄荷脑的生产》", pages: 73-75 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660377A (en) * | 2012-05-28 | 2012-09-12 | 杨玉赞 | Method for extracting animal offal oil |
| CN106619807A (en) * | 2016-12-23 | 2017-05-10 | 黄山天目薄荷药业有限公司 | Production process of peppermint oil |
| CN106631700A (en) * | 2016-12-23 | 2017-05-10 | 黄山天目薄荷药业有限公司 | Production process of menthol |
| CN110643426A (en) * | 2019-10-18 | 2020-01-03 | 安徽爱迪香料股份有限公司 | Peppermint oil production process |
| CN112047814A (en) * | 2020-08-14 | 2020-12-08 | 黄山天目薄荷药业有限公司 | Preparation method of high-purity menthol |
| CN112047814B (en) * | 2020-08-14 | 2023-01-17 | 黄山天目薄荷药业有限公司 | Preparation method of high-purity menthol |
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Application publication date: 20120404 |