CN106085585A - A kind of okra seed oil and the co-production of caffeine - Google Patents

A kind of okra seed oil and the co-production of caffeine Download PDF

Info

Publication number
CN106085585A
CN106085585A CN201610431547.6A CN201610431547A CN106085585A CN 106085585 A CN106085585 A CN 106085585A CN 201610431547 A CN201610431547 A CN 201610431547A CN 106085585 A CN106085585 A CN 106085585A
Authority
CN
China
Prior art keywords
extraction
caffeine
seed oil
supercritical
rectifying column
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
CN201610431547.6A
Other languages
Chinese (zh)
Inventor
邓爱华
彭友林
王云
谢鹏
李婷
杨洁
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.)
Hunan University of Arts and Science
Original Assignee
Hunan University of Arts and Science
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 Hunan University of Arts and Science filed Critical Hunan University of Arts and Science
Priority to CN201610431547.6A priority Critical patent/CN106085585A/en
Publication of CN106085585A publication Critical patent/CN106085585A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D473/00—Heterocyclic compounds containing purine ring systems
    • C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
    • C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
    • C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
    • C07D473/12—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1, 3, and 7, e.g. caffeine
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/12—Refining fats or fatty oils by distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Microbiology (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Pyridine Compounds (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present invention provides a kind of okra seed oil and the co-production of caffeine, including step: (1), by dry Abelmoschus esculentus seed grinding and sieving, loads in ultrasonic wave added supercritical extraction reactor；(2) in extraction kettle, supercritical CO it is passed through2, open Vltrasonic device, extract enters in separating still, collects extraction seed oil；(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open Vltrasonic device, control Rectification column pressure and temperature, supercritical CO2Extract with cosolvent 75% ~ 95% ethanol mixing circulation；(4) supercritical solution after extraction enters rectifying column separation, collects caffeine from rectifying column the superiors region, and caffeine is vacuum dried, and the yield of seed oil reaches more than 19%, and the yield of caffeine reaches more than 0.5%.The present invention uses ultrasonic wave added enhanced supercritical extraction process, improves extraction efficiency, it is achieved that okra seed oil and the efficient coproduction of caffeine.

Description

A kind of okra seed oil and the co-production of caffeine
Technical field
The invention belongs to technical field of bioseparation, be specifically related to a kind of okra seed oil and the co-production of caffeine.
Background technology
Abelmoschus esculentus seed profile approximation Semen phaseoli radiati, rich in the unsaturated fatty acid of multiple needed by human body, its oil content is up to 20% Above, can be as a kind of novel oil resource exploitation.At present, in Abelmoschus esculentus seed, the extracting method of oils and fats is mainly solvent Extraction, as extracted with petroleum ether-normal hexane, ethyl acetate, acetone etc., the method exists that extraction efficiency is low, organic solvent residual And the problem such as oils and fats is impure.In order to solve the problem of organic solvent residual, Chinese patent technology CN104498179A(mono-kind extraction The method taking okra seed oil) and the method for a CN101703539A(extracting okra by using supercritical carbon dioxide) disclose and adopt By the method for supercritical fluid technology extracting okra seed oil, the problem this method solving organic solvent residual, if but wanted Obtaining higher extraction yield, the temperature of its extracting system, pressure must be high, and the amount ratio of entrainer is relatively big, and extraction time compares Long.
In Abelmoschus esculentus seed, caffeine content is about 1%, can develop as a kind of novel caffeine resource.Yellow In Flos abelmoschi manihot seed, the extraction process of caffeine mainly has microwave, ultrasonic assistant ethanol water to extract, due to the existence of oils and fats Hinder the dissolution of caffeine, cause this technique to there is yield low (less than 0.15%), the high deficiency of impurity content.
Summary of the invention
For solving the problems referred to above, present invention aim at providing a kind of okra seed oil and the co-production of caffeine.
The purpose of the present invention is achieved through the following technical solutions:
A kind of okra seed oil and the co-production of caffeine, comprise the steps:
(1) by Abelmoschus esculentus seed 55-75 DEG C of forced air drying, dried Abelmoschus esculentus seed crosses 50 ~ 60 mesh sieves after pulverizing, and loads In ultrasonic wave added-supercritical extraction reactor；
(2) in ultrasonic wave added-supercritical extraction reactor, it is passed through supercritical CO2, open Vltrasonic device, in extraction kettle, extraction temperature is 25-65 DEG C, pressure is 10-30MPa, CO2Flow is 10 ~ 50L/h, and ultrasonic power is 200-800W, and extraction time is 0.5- 3.0h；Then, during extract enters separating still, controlling separating still pressure is 5-10MPa, and temperature is 30-45 DEG C, collects Abelmoschus esculentus Seed oil, the yield of okra seed oil is not less than 19%；
(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open Vltrasonic device, super Acoustic device power is 200 ~ 800W, and control Rectification column pressure is 8 ~ 15Mpa, and in rectifying column, the temperature in four regions is divided from top to bottom It is not 40 DEG C, 55 DEG C, 70 DEG C, 80 DEG C, supercritical CO2With 75% ~ 95% ethanol mixing circulation extraction, extraction time is 0.5 ~ 3h；
(4) after rectification terminates, the fraction in the superiors region in collection rectifying column, through vacuum drying, obtains caffeine；Caffeine Yield is not less than 0.5%.
Compared with prior art, the invention has the beneficial effects as follows: a kind of okra seed oil of the present invention and the connection of caffeine Product technology, at supercritical CO2Use ultrasonic wave added strengthening on the basis of extraction, and be combined with distillation technology.Add super facing Boundary CO2The fluid extracting power to oils and fats, substantially increases extraction efficiency.Supercritical CO2Extraction is combined with rectification, in extraction Product is divided into some different products by its character and boiling range simultaneously, can effectively ensure that and improve caffeine extraction efficiency and Content.Simultaneously in whole preparation process, contamination-free is got rid of, without chemical residual, pure natural, nonhazardous, safety, green, ring Protect.
Detailed description of the invention
The following examples can illustrate in greater detail the present invention, but limits the present invention the most in any form.
Embodiment 1:
(1) by Abelmoschus esculentus seed 200g 55 DEG C of forced air dryings, dried Abelmoschus esculentus seed crosses 50 mesh sieves after pulverizing, and loads super In sound auxiliary-supercritical extraction reactor；
(2) in ultrasonic wave added-supercritical extraction reactor, it is passed through supercritical CO2, open Vltrasonic device, in extraction kettle, extraction temperature is 25 DEG C, pressure is 30MPa, CO2Flow is 10L/h, and Vltrasonic device power is 200W, and extraction time is 0.5h；Then extract Entering in separating still, controlling separating still pressure is 5MPa, and temperature is 30 DEG C, collects okra seed oil, the yield of okra seed oil It is 19.2%；
(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open ultrasonic dress simultaneously Putting, Vltrasonic device power is 200W, and control Rectification column pressure is 8Mpa, and in rectifying column, the temperature in four regions is distinguished from top to bottom It is 40 DEG C, 55 DEG C, 70 DEG C, 80 DEG C, supercritical CO2With 75% ethanol mixing circulation extraction, extraction time is 0.5h；
(4) after rectification terminates, the fraction in the superiors region in collection rectifying column, through vacuum drying, obtains caffeine；Caffeine Yield is 0.5%.
Embodiment 2:
(1) by Abelmoschus esculentus seed 200g 75 DEG C of forced air dryings, dried Abelmoschus esculentus seed crosses 60 mesh sieves after pulverizing, and loads super In sound auxiliary-supercritical extraction reactor；
(2) in ultrasonic wave added-supercritical extraction reactor, it is passed through supercritical CO2, open Vltrasonic device, in extraction kettle, extraction temperature is 65 DEG C, pressure is 10MPa, CO2Flow is 50L/h, and ultrasonic power is 800W, and extraction time is 3.0h；Then extract enters In separating still, controlling separating still pressure is 10MPa, and temperature is 45 DEG C, collects okra seed oil, and the yield of okra seed oil is 19.3%；
(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open Vltrasonic device, super Acoustic device power is 800W, and control Rectification column pressure is 15Mpa, and in rectifying column, the temperature in four regions is respectively 40 from top to bottom DEG C, 55 DEG C, 70 DEG C, 80 DEG C, supercritical CO2With 95% ethanol mixing circulation extraction, extraction time is 3h；
(4) after rectification terminates, the fraction in the superiors region in collection rectifying column, through vacuum drying, obtains caffeine；Caffeine Yield is 0.55%.
Embodiment 3:
(1) by Abelmoschus esculentus seed 200g 65 DEG C of forced air dryings, dried Abelmoschus esculentus seed crosses 55 mesh sieves after pulverizing, and loads super In sound auxiliary-supercritical extraction reactor；
(2) in ultrasonic wave added-supercritical extraction reactor, it is passed through supercritical CO2, open Vltrasonic device, in extraction kettle, extraction temperature is 40 DEG C, pressure is 20MPa, CO2Flow is 30L/h, and ultrasonic power is 500W, and extraction time is 2.0h；Then extract enters In separating still, controlling separating still pressure is 8MPa, and temperature is 40 DEG C, collects okra seed oil, and the yield of okra seed oil is 19.5%；
(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open Vltrasonic device, super Acoustic device power is 500W, and control Rectification column pressure is 10Mpa, and in rectifying column, the temperature in four regions is respectively 40 from top to bottom DEG C, 55 DEG C, 70 DEG C, 80 DEG C, supercritical CO2With 85% ethanol mixing circulation extraction, extraction time is 2h；；
(4) after rectification terminates, the fraction in the superiors region in collection rectifying column, through vacuum drying, obtains caffeine；Caffeine Yield is 0.6%.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, Any those familiar with the art in the technical scope of present disclosure, according to technical scheme and Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.

Claims (1)

1. an okra seed oil and the co-production of caffeine, it is characterised in that comprise the steps:
(1) by Abelmoschus esculentus seed 55-75 DEG C of forced air drying, dried Abelmoschus esculentus seed crosses 50 ~ 60 mesh sieves after pulverizing, and loads In ultrasonic wave added-supercritical extraction reactor；
(2) in ultrasonic wave added-supercritical extraction reactor, it is passed through supercritical CO2, open Vltrasonic device, in extraction kettle, extraction temperature is 25-65 DEG C, pressure is 10-30MPa, CO2Flow is 10 ~ 50L/h, and ultrasonic power is 200-800W, and extraction time is 0.5- 3.0h；Then, during extract enters separating still, controlling separating still pressure is 5-10MPa, and temperature is 30-45 DEG C, collects Abelmoschus esculentus Seed oil, the yield of okra seed oil is not less than 19%；
(3) after seed oil has extracted, close separating still valve, open extraction kettle and rectifying column valve, open Vltrasonic device, super Acoustic device power is 200 ~ 800W, and control Rectification column pressure is 8 ~ 15Mpa, and in rectifying column, the temperature in four regions is divided from top to bottom It is not 40 DEG C, 55 DEG C, 70 DEG C, 80 DEG C, supercritical CO2With 75% ~ 95% ethanol mixing circulation extraction, extraction time is 0.5 ~ 3h；
(4) after rectification terminates, the fraction in the superiors region in collection rectifying column, through vacuum drying, obtains caffeine；Caffeine Yield is not less than 0.5%.
CN201610431547.6A 2016-06-17 2016-06-17 A kind of okra seed oil and the co-production of caffeine Pending CN106085585A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610431547.6A CN106085585A (en) 2016-06-17 2016-06-17 A kind of okra seed oil and the co-production of caffeine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610431547.6A CN106085585A (en) 2016-06-17 2016-06-17 A kind of okra seed oil and the co-production of caffeine

Publications (1)

Publication Number Publication Date
CN106085585A true CN106085585A (en) 2016-11-09

Family

ID=57235662

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610431547.6A Pending CN106085585A (en) 2016-06-17 2016-06-17 A kind of okra seed oil and the co-production of caffeine

Country Status (1)

Country Link
CN (1) CN106085585A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112473174A (en) * 2020-12-09 2021-03-12 海南一哟食品有限公司 Method for accelerating coffee extraction by adopting ultrasonic waves

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102358740A (en) * 2011-09-28 2012-02-22 张海 Process for extracting caffeine from tea
CN104498179A (en) * 2014-12-18 2015-04-08 贵州航天乌江机电设备有限责任公司 Method for extracting okra seed oil

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102358740A (en) * 2011-09-28 2012-02-22 张海 Process for extracting caffeine from tea
CN104498179A (en) * 2014-12-18 2015-04-08 贵州航天乌江机电设备有限责任公司 Method for extracting okra seed oil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
唐萍等: "超声波辅助提取黄秋葵籽油及其脂肪酸组成分析", 《油脂加工》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112473174A (en) * 2020-12-09 2021-03-12 海南一哟食品有限公司 Method for accelerating coffee extraction by adopting ultrasonic waves

Similar Documents

Publication Publication Date Title
CN104987956B (en) A kind of method and its extraction element of ultrasonic wave extraction cinnamon oil
CN101781606B (en) Extraction method of rosa rugosa essential oil
CN101732359B (en) Integrated method for poly-generation of Chinese medicinal extracts
CN100453629C (en) Method of extracting safflower oil using super-critical carbon dioxide
CN104694248B (en) A kind of extracting method of litsea citrate oil
CN105505558A (en) Method for synchronously extracting soybean oil, soybean milk powder and soybean dietary fiber by aqueous enzymatic method
CN102061220B (en) Method for preparing onion functional components by using double-stage extraction based on subcritical water and solvent method
CN105130941A (en) Preparation method of grape seed extract
CN103627528A (en) Method for extracting lavender essential oil
CN103923743A (en) Extraction method for effective compositions of antrodia camphorata
CN105349241A (en) Aqueous enzymatic extraction of soybean oil and application of by-products of extraction
CN102533433A (en) Method for supercritical extraction of sea buckthorn oil
CN107858207A (en) A kind of supercritical CO of golden flower tea essential oils2Extracting process
CN105505556A (en) Method for simultaneously extracting soybean oil and soybean milk powder by aqueous enzymatic method
CN105062686A (en) Method for extracting lavender essential oil
CN105038992A (en) Multifunctional volatile oil distilling and extracting tank
CN105038947A (en) Supercritical extraction method of walnut oil
CN104388178A (en) Method for extracting DHA algae oil from algae cells
CN105878323A (en) Method using ultrasonically-assisted supercritical extraction rectification to purify cynarin in globe artichoke
CN106085585A (en) A kind of okra seed oil and the co-production of caffeine
CN105777929A (en) Extracting method for pleurotus eryngii polysaccharide
CN102258639A (en) Supercritical carbon dioxide extraction method for tetrastlgma hemsleyanum total flavonoid
CN102219669B (en) Method for extracting purslane linolenic acid with supercritical CO2 fluid
CN104031018A (en) Method for extracting cyanidin from purple common yam rhizome
Quitain et al. Coupling microwave-assisted drying and supercritical carbon dioxide extraction for coconut oil processing

Legal Events

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

Application publication date: 20161109

RJ01 Rejection of invention patent application after publication