CN106433210A - Ultrasonic wave-microwave assisted orange peel pigment extraction method - Google Patents
Ultrasonic wave-microwave assisted orange peel pigment extraction method Download PDFInfo
- Publication number
- CN106433210A CN106433210A CN201610857885.6A CN201610857885A CN106433210A CN 106433210 A CN106433210 A CN 106433210A CN 201610857885 A CN201610857885 A CN 201610857885A CN 106433210 A CN106433210 A CN 106433210A
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- China
- Prior art keywords
- pigment
- microwave
- pericarpium citri
- citri tangerinae
- ultrasonic
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Abstract
The invention discloses an ultrasonic wave-microwave assisted orange peel pigment extraction method. The method comprises the steps of mixing a dried orange peel residue as a raw material with an extracting agent, sequentially carrying out ultrasonic wave assisted extraction and microwave assisted extraction so as to prepare extraction solutions, and concentrating and drying the extraction solutions, so as to obtain orange peel pigments. The pigments in the orange peels are extracted by virtue of the ultrasonic wave-microwave assisted method, so that the safety is high, and the operation is simple and feasible; and meanwhile, the method has the advantages of high extraction efficiency, strong treating capacity, short operation cycle and the like, and the waste orange peels are adequately and comprehensive utilized.
Description
Technical field
The invention belongs to deep processing of farm products and reclamation of solid wastes reclaim field and in particular to a kind of ultrasound wave-micro-
Ripple works in coordination with the method extracting Pericarpium Citri tangerinae pigment.
Background technology
With the raising of quality of life, synthetic dyestuff more and more attracts much attention to the harm of health.And sky
So pigment not only safety non-toxic evil, and there is certain nutrition and health care effect, therefore application natural pigment substitutes combination color
Element is the development trend of the industries such as current food, beverage, cosmetics.Pericarpium Citri tangerinae pigment is the widely used natural pigment of a class, main
In the peel of the plants such as Fructus Citri tangerinae to be present in, Citrus chachiensis Hort., Fructus Citri grandiss, Fructus Citri sinensiss, Citrus aurantium Linn., Fructus Fortunellae Margaritae, Fructus Gardeniae, the processing using food beverage industry is given up
Material, to extract Pericarpium Citri tangerinae pigment, not only increases economic benefit, can also solve environmental problem, and therefore research and utilization extracts orange peel
The great realistic meaning of plain technique.
The extracting method that orange peel is usually shown in is organic solvent extraction, alkali extraction method, microwave loss mechanisms, supercritical fluid
Extraction and supercritical ultrasonics technology etc..Wherein organic solvent extraction applies relatively wide, the pass of its raising extraction ratio in actual production
Key is to select suitable organic solvent to make extractant, but common organic solvents consumption is big, compares other extracting method high costs,
There is the trend gradually eliminated；Alkali extraction method can be used for extracting the water colo(u)r in Pericarpium Citri tangerinae pigment, relatively inexpensive, practical, yield
Also higher, but because the alkali extraction method course of processing need to consume substantial amounts of alkali liquor and the more difficult recovery of waste liquid, therefore, with people's environmental protection
The enhancing of consciousness, the use of alkali extraction method is restricted.Microwave loss mechanisms have that firing rate is fast, easy to control, system of being heated
The advantages of temperature is uniform, thus extract for Pericarpium Citri tangerinae pigment and there is larger advantage, the extraction ratio of Pericarpium Citri tangerinae pigment can be improved, but micro-
There is problem of temperature rise in ripple extraction method, if misoperation, can cause the destruction of Pericarpium Citri tangerinae pigment, directly affects the extraction ratio of product,
So microwave loss mechanisms require strictly to the operation particularly control to temperature；Supercritical fluid extraction no solvent residue, no
Pollution, can avoid pigment degeneration at high temperature, the activity of protection pigment, but apparatus expensive, trivial operations, to the moisture of raw material,
Degree of grinding etc. has certain technological requirement, limits it and extensively applies.Ultrasonic extraction Pericarpium Citri tangerinae pigment, ultrasound wave can directly be made
For molecule, the warm-up movement of molecule is made to aggravate, rapid damage cell wall, cell component is easy to dissolution, and extraction process need not add
Heat, and the ultrasonic procedure time is shorter, within the limited time, produced heat effect is also not to make system temperature significantly raised,
Safe and operation is simple, have the advantages that extraction efficiency is high, disposal ability is big, the operation cycle is short simultaneously.
Content of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of extraction ratio height, low cost, food
The good ultrasonic-microwave of product safety works in coordination with the method extracting Pericarpium Citri tangerinae pigment.
To achieve these goals, the technical solution used in the present invention is as follows：
A kind of ultrasonic-microwave work in coordination with extract Pericarpium Citri tangerinae pigment method, the method with citrus peel residue as raw material, first by its with extract
Agent mixes, then extracts to produce lixiviating solution with ultrasound wave and microwave-assisted successively, finally concentrates lixiviating solution, dries and obtain Pericarpium Citri tangerinae
Pigment.
Specifically include following steps：
1）Pretreatment：First citrus peel residue is dried at 60 DEG C and is less than 15% to moisture content, then pulverize and cross 20-50 mesh sieve,
Extracting screen underflow, obtains peel of Citrus reticulata Blanco powder.
2）Ultrasonic extraction：To step 1）Add extractant mix homogeneously in the peel of Citrus reticulata Blanco powder obtaining, mixed
Liquid；Again by this mixed liquor at 60 DEG C, use Ultrasonic Wave-Assisted Extraction 20-25min.
3）Microwave-assisted extracts：Will be through step 2）The mixed liquor processing is placed in 3- in the microwave that power is 150-250w
5min, carries out microwave-assisted extraction, obtains lixiviating solution.
4）Lixiviating solution concentrates：By step 3）The lixiviating solution obtaining carries out vacuum filtration, then the filtrate that sucking filtration is obtained is 60
Carry out concentrating under reduced pressure at DEG C, the effective ingredient of the extractant in lixiviating solution is distilled, in case reclaim using.
When filtrate volume concentration to original volume 10 ~ 15% when, stop concentrating, and be cooled to room temperature, obtain concentrated solution；
5）Concentrated solution is dried：By step 4）The concentrated solution obtaining is dried 0.5-1h in 55-60 DEG C of vacuum drying oven, to remove
Ethanol and moisture, obtaining reddish black powder is Pericarpium Citri tangerinae pigment.
Wherein：Step 1）In drying time be 3 ~ 4h, the moisture content of peel of Citrus reticulata Blanco powder is less than 13%.
Step 2）In the selected extractant stated be the ethanol water that volumetric concentration is 55 ~ 70%.
Step 2）Described in the mass volume ratio of Pericarpium Citri tangerinae powder and extractant be 1:9~11g/mL.
Step 2）Described in ultrasound wave frequency be 40 ~ 47.6kHz, power be 200-300w.
When the present invention is to solid-liquid ratio, concentration of alcohol, ultrasonic frequency and power, sonication times, microwave power, microwave
Between, Extracting temperature these impact Pericarpium Citri tangerinae pigments extract factor be optimized, thus improving the extraction ratio of Pericarpium Citri tangerinae pigment, promote
Food safety, improves natural pigment resource utilization rate.Extract the pigment in peel of Citrus reticulata Blanco, peace using ultrasonic-microwave Synergistic method
Quan Xinggao and operation is simple, has the advantages that extraction efficiency is high, disposal ability is strong, the operation cycle is short simultaneously, makes discarded Fructus Citri tangerinae
Skin is more fully comprehensively utilized.
The present invention has both two methods of ultrasound wave and the advantage of microwave-assisted, carries out Ultrasonic Wave-Assisted Extraction first, utilizes
It is thin that the special effects such as judder of ultrasound wave generation, very high acceleration, strong cavitation effect, stirring, destroys Pericarpium Citri tangerinae
Born of the same parents, break cell wall, so that cellular content is directly contacted with plant under ultrasonication, accelerate solvent and plant is effective
The interpenetrating and dissolve of composition.Meanwhile, the effect of vibration of ultrasound wave enhances the release of intracellular matter, diffusion and molten
Solution.And make intracellular chemical composition quickly proceed to solvent, make intraor extracellular that concentration difference to occur, promote chemical composition by highly concentrated
Spread in the solution of low concentration in the cell of degree, greatly accelerate the process of extraction.And ultrasonic can be obviously reduced liquid
The surface tension of body and frictional force, destroy liquid-solid interface boundary-layer, thus accelerate the release of intracellular matter, diffusion and
Dissolving.Carry out microwave-assisted extraction after carrying out Ultrasonic Wave-Assisted Extraction, because above-mentioned ultrasonic Treatment is thin to Pericarpium Citri tangerinae
Born of the same parents carry out a certain degree of destruction, have broken cell wall, weaken surface tension and the frictional force of liquid, destroy liquid-solid interface
Boundary-layer, adds in microwave field due to the difference of material absorbing microwave ability, makes some regions in extraction system or some groups
Divide and heated by selectivity, and the electromagnetic field that microwave produces accelerates the diffusion velocity to solvent interface for the pigment, makes extraction time
Greatly shorten.Simultaneously because the synergism of ultrasound wave and microwave, process time greatly shortens additionally it is possible to reduce the temperature extracted
Degree, thus ensure that the quality that is stable, improve extraction of pigment.If after note finally that conversion process order is first microwave treatment
Carry out Ultrasonic Wave-Assisted Extraction and then can not give full play to the two advantage, substantially reduce extraction efficiency and energy utilization rate.
Compared with prior art, the present invention has the advantages that：
1st, the present invention utilizes ultrasonic-microwave Synergistic method to extract the pigment in peel of Citrus reticulata Blanco, the one kind extracted as pigment first
New technique, ultrasonic-microwave is worked in coordination with extraction and is had broad prospects.
2nd, the ultrasonic-microwave Synergistic method that the present invention adopts has that extraction efficiency is high, disposal ability is strong, the operation cycle
Short, solvent load is few, is conducive to the advantages of recovery, mitigation environmental pollution.
3rd, the ultrasonic-microwave Synergistic method that the present invention adopts is safe and operation is simple, is suitable for pushing away on a large scale
Wide application, makes discarded Pericarpium Citri tangerinae more fully be comprehensively utilized.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment one：
Pericarpium Citri tangerinae pigment is extracted using the method that following ultrasonic-microwave is worked in coordination with, comprises the following steps that：
1）Pretreatment：Citrus are provided, clean remove impurity, bark fetching, 60 DEG C of drying 3h（Moisture content is made to be less than 15%）, pulverized 30 mesh sieves,
Extracting screen underflow, obtains peel of Citrus reticulata Blanco powder；
2）Ultrasonic Wave-Assisted Extraction：Take the ethanol water that Pericarpium Citri tangerinae powder and volumetric concentration are 55% according to 1g Pericarpium Citri tangerinae powder/9ml second
The ratio mixing of alcohol-water solution, ultrasonic extraction 21min at a temperature of 60 DEG C, ultrasonic frequency is 40kHz, power is
200w；
3）Microwave-assisted extracts：Set microwave power 200w, microwave digestion 4min, obtain lixiviating solution.
4）Lixiviating solution concentrates：By step 3）The lixiviating solution obtaining carries out vacuum filtration, then the filtrate that sucking filtration is obtained is 60
At DEG C（In case pigment is by high temperature）Carry out concentrating under reduced pressure, by the ethanol distillation in lixiviating solution out, in case reclaim using；
When lixiviating solution volume concentration to original volume 10 ~ 15% when, stop concentrating, and be cooled to room temperature, obtain concentrated solution.
5）Concentrated solution is dried：Wine-colored concentrated solution is moved in vacuum drying oven, carries out vacuum under temperature 60 C and do
Dry 1h removes residual ethanol and moisture, and the reddish black powder obtaining is Pericarpium Citri tangerinae pigment.
20g dry Pericarpium Citri tangerinae powder can be obtained pigment 4.862g with this understanding, and that is, yield is 24.3%.
Embodiment two：
Pericarpium Citri tangerinae pigment is extracted using the method that following ultrasonic-microwave is worked in coordination with, comprises the following steps that：
1）Pretreatment：Citrus are provided, clean remove impurity, bark fetching, 60 DEG C of drying 3.5h（Moisture content is made to be less than 15%）, pulverized 40 mesh
Sieve, extracting screen underflow, obtain peel of Citrus reticulata Blanco powder；
2）Ultrasonic Wave-Assisted Extraction：Take the Pericarpium Citri tangerinae powder of pulverizing and ethanol water that volumetric concentration is 60% according to 1g Pericarpium Citri tangerinae powder/
The liquid ratio mixing of 10ml ethanol water, ultrasonic extraction 23min at a temperature of 60 DEG C, ultrasonic frequency is 45kHz, work(
Rate is 250w；
3）Microwave-assisted extracts：Set microwave power 200w, microwave digestion 5min, obtain lixiviating solution.
4）Lixiviating solution concentrates：By step 3）The lixiviating solution obtaining carries out vacuum filtration, then the filtrate that sucking filtration is obtained is 60
At DEG C（In case pigment is by high temperature）Carry out concentrating under reduced pressure, by the ethanol distillation in lixiviating solution out, in case reclaim using；
When lixiviating solution volume concentration to original volume 10 ~ 15% when, stop concentrating, and be cooled to room temperature, obtain concentrated solution.
5）Concentrated solution is dried：Wine-colored concentrated solution is moved in vacuum drying oven, carries out vacuum at 58 DEG C of temperature and do
Dry 1h removes residual ethanol and moisture, and the reddish black powder obtaining is Pericarpium Citri tangerinae pigment.
20g dry Pericarpium Citri tangerinae powder can be obtained pigment 5.1g with this understanding, and that is, yield is 25.5%.
Embodiment three
Pericarpium Citri tangerinae pigment is extracted using the method that following ultrasonic-microwave is worked in coordination with, comprises the following steps that：
1）Pretreatment：Citrus are provided, clean remove impurity, bark fetching, 60 DEG C of drying 4h（Moisture content is made to be less than 13%）, pulverized 50 mesh sieves,
Extracting screen underflow, obtains peel of Citrus reticulata Blanco powder；
2）Ultrasonic Wave-Assisted Extraction：Take the Pericarpium Citri tangerinae powder of pulverizing and ethanol water that volumetric concentration is 65% according to 1g Pericarpium Citri tangerinae powder/
11ml ethanol water liquid ratio mixing, ultrasonic extraction 25min at a temperature of 60 DEG C, ultrasonic frequency be 47.6kHz,
Power is 300w；
3）Microwave-assisted extracts：Set microwave power 250w, microwave digestion 5min, obtain lixiviating solution.
4）Lixiviating solution concentrates：By step 3）The lixiviating solution obtaining carries out vacuum filtration, then the filtrate that sucking filtration is obtained is 60
At DEG C（In case pigment is by high temperature）Carry out concentrating under reduced pressure, by the ethanol distillation in lixiviating solution out, in case reclaim using；
When lixiviating solution volume concentration to original volume 10 ~ 15% when, stop concentrating, and be cooled to room temperature, obtain concentrated solution.
5）Concentrated solution is dried：Wine-colored concentrated solution is moved in vacuum drying oven, carries out vacuum under temperature 60 C and do
Dry 1h removes residual ethanol and moisture, and the reddish black powder obtaining is Pericarpium Citri tangerinae pigment.
With this understanding, 20g dry Pericarpium Citri tangerinae powder can be obtained pigment 5.317g, and that is, yield is 26.6%.
The above embodiment of the present invention only example to illustrate the invention, and it is not the enforcement to the present invention
The restriction of mode.For those of ordinary skill in the field, can also be made other not on the basis of the above description
Change and variation with form.Here all of embodiment cannot be exhaustive.Every belong to technical scheme
The obvious change amplified out or change the row still in protection scope of the present invention.
Claims (6)
1. a kind of ultrasonic-microwave works in coordination with the method extracting Pericarpium Citri tangerinae pigment it is characterised in that with citrus peel residue as raw material, first will
It is mixed with extractant, then is extracted to produce lixiviating solution with ultrasound wave and microwave-assisted successively, finally concentrates lixiviating solution, dries
Obtain Pericarpium Citri tangerinae pigment.
2. ultrasonic-microwave according to claim 1 work in coordination with extract Pericarpium Citri tangerinae pigment method it is characterised in that include with
Lower step：
1）Pretreatment：First citrus peel residue is dried at 60 DEG C and is less than 15% to moisture content, then pulverize and cross 20-50 mesh sieve,
Extracting screen underflow, obtains peel of Citrus reticulata Blanco powder；
2）Ultrasonic extraction：To step 1）Add extractant mix homogeneously in the peel of Citrus reticulata Blanco powder obtaining, obtain mixed liquor；Again
By this mixed liquor at 60 DEG C, use Ultrasonic Wave-Assisted Extraction 20-25min；
3）Microwave-assisted extracts：Will be through step 2）The mixed liquor processing is placed in 3-5min in the microwave that power is 150-250w,
Carry out microwave-assisted extraction, obtain lixiviating solution；
4）Lixiviating solution concentrates：By step 3）The lixiviating solution obtaining carries out vacuum filtration, then the filtrate that sucking filtration is obtained is at 60 DEG C
Carry out concentrating under reduced pressure, the effective ingredient of the extractant in lixiviating solution is distilled, in case reclaim using；
When filtrate volume concentration to original volume 10 ~ 15% when, stop concentrating, and be cooled to room temperature, obtain concentrated solution；
5）Concentrated solution is dried：By step 4）The concentrated solution obtaining is dried 0.5-1h in 55-60 DEG C of vacuum drying oven, to remove
Ethanol and moisture, obtaining reddish black powder is Pericarpium Citri tangerinae pigment.
3. ultrasonic-microwave according to claim 2 works in coordination with the method extracting Pericarpium Citri tangerinae pigment it is characterised in that step 1）
In drying time be 3 ~ 4h, the moisture content of peel of Citrus reticulata Blanco powder is less than 13%.
4. ultrasonic-microwave according to claim 2 works in coordination with the method extracting Pericarpium Citri tangerinae pigment it is characterised in that step 2）
In the selected extractant stated be the ethanol water that volumetric concentration is 55 ~ 70%.
5. ultrasonic-microwave according to claim 2 works in coordination with the method extracting Pericarpium Citri tangerinae pigment it is characterised in that step 2）
Described in the mass volume ratio of Pericarpium Citri tangerinae powder and extractant be 1:9~11g/mL.
6. ultrasonic-microwave according to claim 2 works in coordination with the method extracting Pericarpium Citri tangerinae pigment it is characterised in that step 2）
Described in ultrasound wave frequency be 40 ~ 47.6kHz, power be 200-300w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610857885.6A CN106433210A (en) | 2016-09-28 | 2016-09-28 | Ultrasonic wave-microwave assisted orange peel pigment extraction method |
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| CN201610857885.6A CN106433210A (en) | 2016-09-28 | 2016-09-28 | Ultrasonic wave-microwave assisted orange peel pigment extraction method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299846A (en) * | 2018-01-08 | 2018-07-20 | 罗莱生活科技股份有限公司 | A kind of orange peel dyestuff and its preparation method and application |
| CN112845568A (en) * | 2020-12-31 | 2021-05-28 | 福建龙净环保股份有限公司 | Remediation method for heavy metal contaminated soil |
| CN113321752A (en) * | 2021-07-21 | 2021-08-31 | 佛山职业技术学院 | Extraction method of shaddock ped polysaccharide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194387A (en) * | 2014-08-07 | 2014-12-10 | 信阳师范学院 | Method for extracting citrus peel pigments |
-
2016
- 2016-09-28 CN CN201610857885.6A patent/CN106433210A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194387A (en) * | 2014-08-07 | 2014-12-10 | 信阳师范学院 | Method for extracting citrus peel pigments |
Non-Patent Citations (1)
| Title |
|---|
| 刘兆芳等: "超声波-微波协同辅助提取橘皮色素的研究", 《食品研究与开发》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299846A (en) * | 2018-01-08 | 2018-07-20 | 罗莱生活科技股份有限公司 | A kind of orange peel dyestuff and its preparation method and application |
| CN112845568A (en) * | 2020-12-31 | 2021-05-28 | 福建龙净环保股份有限公司 | Remediation method for heavy metal contaminated soil |
| CN112845568B (en) * | 2020-12-31 | 2023-09-08 | 福建龙净环保股份有限公司 | Restoration method for heavy metal contaminated soil |
| CN113321752A (en) * | 2021-07-21 | 2021-08-31 | 佛山职业技术学院 | Extraction method of shaddock ped polysaccharide |
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Application publication date: 20170222 |