CN102399632A - Crude mint oil freeze crystallization method - Google Patents

Crude mint oil freeze crystallization method Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
oil
freeze
crude
brine
freezes
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2010102803567A
Other languages
Chinese (zh)
Inventor
王建兵
张贤梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NANTONG MENTHOL FACTORY CO Ltd
Original Assignee
NANTONG MENTHOL FACTORY CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NANTONG MENTHOL FACTORY CO Ltd filed Critical NANTONG MENTHOL FACTORY CO Ltd
Priority to CN2010102803567A priority Critical patent/CN102399632A/en
Publication of CN102399632A publication Critical patent/CN102399632A/en
Pending legal-status Critical Current

Links

Landscapes

  • Fats And Perfumes (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

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

A kind of crude peppermint oil bu freezes the method for precipitation and crystallization
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).
CN2010102803567A 2010-09-14 2010-09-14 Crude mint oil freeze crystallization method Pending CN102399632A (en)

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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102803567A CN102399632A (en) 2010-09-14 2010-09-14 Crude mint oil freeze crystallization method

Publications (1)

Publication Number Publication Date
CN102399632A true CN102399632A (en) 2012-04-04

Family

ID=45882292

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010102803567A Pending CN102399632A (en) 2010-09-14 2010-09-14 Crude mint oil freeze crystallization method

Country Status (1)

Country Link
CN (1) CN102399632A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN102399632A (en) Crude mint oil freeze crystallization method
CN104944447B (en) Method for preparing battery grade lithium hydroxide monohydrate
CN102775277A (en) Production technique of menthol and dementholized peppermint oil
CN107778142B (en) Purification process of menthol and dementholized peppermint oil
CN103274901A (en) Refining technology for menthol
CN104560371A (en) Oil tea seed cold pressing technique
CN106629787A (en) Preparation method of cell-grade lithium hydroxide
CN103734580A (en) Production technology of sweet potato vermicelli
NZ601169A (en) Frozen fresh cream to be whipped, method for producing the frozen fresh cream, whipped cream, and method for producing the whipped cream
CN102976379A (en) Method for crystal seed precipitation of sodium aluminate solution
CN113862083A (en) Method for improving oil yield and quality of rosa damascena essential oil
CN102178007A (en) Method for producing eucommia male flower tea
CN101991157A (en) Fruit jelly freeze concentration method
RU2008122264A (en) METHOD FOR PRODUCING PLUM DISTILLATE
CN103525546A (en) Rice oil dewaxing process
CN102578654A (en) Method for preparing roselle juice by freezing and juicing
CN102676287B (en) Processing process of quick-freezing aroma-coagulating type peanut oil
CN102766536A (en) Flavor onion oil and preparation method thereof
CN109180723B (en) Concentrated phospholipid and preparation method thereof
KR20180011742A (en) Manufacturing method for perilla seed oil and perilla seed oil using the same
CN101935589A (en) Preparation method of crude menthol crystal used for producing peppermint oil
WO2011131771A3 (en) Method and device for producing slurry ice
CN101353612B (en) Method for enriching polyunsaturated fatty acid from pine caterpillar
CN107674764A (en) The carbon dioxide method for extracting of galic essential oil
CN106922864A (en) A kind of processing technology of green tea

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20120404