CN113430053A - Fresh pepper oleoresin separation and purification process - Google Patents
Fresh pepper oleoresin separation and purification process Download PDFInfo
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- 238000000926 separation method Methods 0.000 title claims abstract description 156
- 238000000746 purification Methods 0.000 title claims abstract description 24
- 239000008601 oleoresin Substances 0.000 title claims description 65
- 235000002566 Capsicum Nutrition 0.000 title abstract description 84
- 239000006002 Pepper Substances 0.000 title abstract description 83
- 235000016761 Piper aduncum Nutrition 0.000 title abstract description 83
- 235000017804 Piper guineense Nutrition 0.000 title abstract description 83
- 235000008184 Piper nigrum Nutrition 0.000 title abstract description 83
- 244000203593 Piper nigrum Species 0.000 title 1
- 239000000341 volatile oil Substances 0.000 claims abstract description 149
- 238000000605 extraction Methods 0.000 claims abstract description 130
- 239000011347 resin Substances 0.000 claims abstract description 121
- 229920005989 resin Polymers 0.000 claims abstract description 121
- 241000949456 Zanthoxylum Species 0.000 claims abstract description 98
- 239000003921 oil Substances 0.000 claims abstract description 76
- 239000000126 substance Substances 0.000 claims abstract description 38
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- 239000012530 fluid Substances 0.000 claims abstract description 26
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- 244000291564 Allium cepa Species 0.000 description 1
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Classifications
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- 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
-
- 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/002—Counter-current extraction
-
- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a separation and purification process of fresh zanthoxylum oil resin, which comprises the steps of collecting fresh zanthoxylum, squeezing the fresh zanthoxylum oil resin in two hours, and subjecting the fresh zanthoxylum oil resin to supercritical CO2And (3) performing countercurrent extraction and separation on a liquid substance extraction and separation unit of the fluid dynamic countercurrent extraction and separation system, obtaining fresh pepper resin from the extraction unit after the countercurrent extraction and separation is completed, and obtaining fresh pepper essential oil from the separation unit. The extraction and separation process comprises the following steps: feed rate 40kg/h, CO2The flow rate is 600L/h, the extraction temperature is 45 ℃, the extraction pressure is 20MPa, the separation I temperature is 40 ℃, the separation I pressure is 7.5MPa, the separation temperature is 55 ℃, and the separation II pressure is 4-6 MPa; the total yield of the fresh zanthoxylum oil resin product reaches 98.74-99.19 percent, and the separation efficiency reaches 94.00-99.24 percent; the obtained fresh fructus Zanthoxyli extractThe content of the oil volatile oil can reach 101.94-128.93ml/100g, and the tingling degree is lower than 5 mg/g; the obtained fresh pricklyash peel resin has volatile oil content less than 5ml/100g, tingling degree up to 141.12-182.56mg/g, and tingling degree up to 42.59% -53.17%. The fresh pepper essential oil with high volatile oil content and the fresh pepper resin with high tingling degree can be obtained by the process, and the purification effects of the two products are obvious.
Description
Technical Field
The invention belongs to the technical field of biochemical products, discloses a fresh zanthoxylum oil resin separation and purification process, and particularly discloses a process for separating and purifying fresh zanthoxylum oil resin by using supercritical CO2A process for separating liquid substances by fluid dynamic countercurrent extraction, and fresh pepper essential oil and fresh pepper resin prepared by the process.
Background
The pepper is a unique seasoning with rich resources in China. At present, the research on the flavor characteristics and flavor substance extraction of the pepper in China is reported more, but the extraction is limited to a steam distillation method, an organic solvent (ethanol, acetone and the like) extraction method and the like. The steam distillation method can only extract the volatile oil part with low boiling point in the pepper, and the organic solvent extraction method has the defects of high impurity content, large loss of flavor components, solvent residue and the like. At present, supercritical carbon dioxide fluid has been recognized as a suitable spice oleoresin extraction solvent and is used in the extraction of ginger oleoresin, onion oleoresin, pepper oleoresin, capsicum oleoresin, and the like. At present stage, domestic supercritical CO2The extraction rate of the dry red pepper oleoresin extracted by the fluid can reach 17-18% (calculated by the percentage of the oleoresin obtained by extraction in the total material), the content of the obtained oleoresin volatile oil is about 38-42ml/100g, and the tingling degree is about 110-170mg/100 g; the extraction rate of the extracted dry green zanthoxylum oleoresin can reach 19-20% (calculated by the percentage of the oleoresin obtained by extraction in the total material), the content of the volatile oil of the obtained oleoresin is about 49-53ml/100g, and the tingling degree is about 90-140mg/100 g. However, the extraction process is limited to the extraction of the dry zanthoxylum oleoresin, and the separation and purification of the essential oil and the resin cannot be further carried out on the liquid oleoresin.
In the deoiling (namely the separation and purification of the oleoresin) processing production of the zanthoxylum oleoresin, secondary molecular distillation equipment with relatively high separation efficiency is mostly adopted, and the processing capacity is about 70-80 kg/h. The deoiling processing production of the zanthoxylum oil resin by adopting supercritical equipment has great technical difficulty, and has not been reported at present. However, the molecular distillation equipment needs continuous production, has small equipment compatibility, can only be used for liquid-liquid separation, and cannot realize other processing operations (such as extraction and separation of solid substances).
Based on the analysis of the processing current situation of the zanthoxylum oil resin, the invention aims to break through the supercritical CO2The fluid extraction and separation technology is a bottleneck in the application of liquid substance extraction and separation, and the fresh pepper oleoresin is used as a raw material, aiming at obtaining the high-efficiency extraction and separation technology of differentiated pepper flavor components. Compared with the traditional supercritical extraction separation technology of the dry pepper oleoresin (only the oleoresin is extracted and separated from the solid pepper powder as a whole), the method realizes the extraction separation of liquid substances, obtains the high-purity pepper essential oil and pepper resin, is the fresh pepper essential oil and the fresh pepper resin with typical fresh pepper flavor, and can also obtain two essential oils I and II with different aroma characteristics from the fresh pepper essential oil. The content of the volatile oil of the fresh pepper essential oil is more than 100ml/100g, and the fresh pepper essential oil is fresh, fragrant and slightly numb and has unique fragrance; the fresh pepper resin has rich numb taste, and the numb value can reach more than 140mg/100g (the numb degree of the dried pepper resin prepared by the process can reach more than 200mg/100 g). The invention also develops the new application of the supercritical equipment, realizes the compatibility of more processing units of the supercritical equipment, provides more possibilities for extracting and applying the flavor of the fresh pepper, and promotes the fine and deep processing and comprehensive utilization of the fresh pepper.
Disclosure of Invention
In view of the defects, the invention provides a method for preparing the fresh zanthoxylum oil resin by using supercritical CO as a raw material2The process for obtaining the fresh zanthoxylum essential oil and the fresh zanthoxylum resin by the fluid dynamic countercurrent extraction separation of the fresh zanthoxylum oleoresin has the total product yield of more than 98 percent and the separation efficiency of more than 94 percent; the content of volatile oil of fresh pricklyash peel essential oil can reach 101.94-128.93ml/100g, and the tingling degree is lower than 5 mg/g; the obtained fresh fructus Zanthoxyli resin contains volatile oil less than 5ml/100g, and has a tingling degree of 141.12-182.56mg/g, and a tingling degree increase of more than 42%.
The invention is realized by the following means:
a separation and purification process of fresh zanthoxylum oil resin comprises the following steps:
subjecting fresh fructus Zanthoxyli oleoresin to supercritical CO2Fluid dynamic countercurrent extraction separation systemPerforming dynamic countercurrent extraction;
wherein:
supercritical CO2A countercurrent extraction separation system comprising:
CO2a gas source unit (100),
a solid matter extraction unit (400) connected with the CO through a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to a solid matter extraction unit (400);
a liquid substance extraction unit (700) connected with the CO via a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to the liquid matter extraction unit (700); and
a separation unit respectively connected to the solid substance extraction unit (400) and the liquid substance extraction unit (700) for separating the extracted substances from supercritical CO2Separating, and separating the separated CO2Through a pipeline via CO2The filter (102) and the cooler (103) are circulated back to the storage tank (104);
the separation and purification process comprises the following steps: feeding rate of 40-60kg/h, CO2The flow rate is 400-; the temperature of the separation I is 35-45 ℃, the pressure of the separation I is 6-11MPa, the separation temperature is 50-60 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is unadjustable and is automatically controlled by a system).
Furthermore, the separation unit comprises a plurality of separation kettles which can be used independently or in series or in parallel, and at least comprises a separation kettle I and a separation kettle II.
Further, the dynamic countercurrent extraction separation of the fresh zanthoxylum oil resin comprises the following steps:
and (3) feeding the fresh zanthoxylum bungeanum oleoresin into a liquid substance extraction unit, obtaining fresh zanthoxylum bungeanum essential oil I and fresh zanthoxylum bungeanum essential oil II through a separation kettle I and a separation kettle II after extraction is finished, and obtaining the fresh zanthoxylum bungeanum oleoresin through a temporary storage tank of the extraction unit.
Further, the fresh zanthoxylum oil resin is selected from fresh zanthoxylum oil resin or fresh zanthoxylum oil resin.
Further, the separation and purification process of the fresh zanthoxylum oil resinThe process comprises the following steps: feed rate 40kg/h, CO2The flow rate is 600L/h, the extraction temperature is 45 ℃, and the extraction pressure is 20MPa; the temperature of the separation I is 40 ℃, the pressure of the separation I is 7.5MPa, the separation temperature is 55 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is not adjustable and is automatically controlled by a system).
Furthermore, the separation efficiency of the fresh green zanthoxylum oil resin is 98.59-99.24%, and the total yield is 99.08-99.17%.
Furthermore, the separation efficiency of the fresh red pepper oleoresin is 94.00-94.27%, and the total yield is 98.74-98.99%.
Further, the content of essential oil I volatile oil obtained by extracting and separating the fresh green zanthoxylum oil resin is 105.63-108.11ml/100g, and the tingling degree is 4.11-4.41mg/100 g; the content of essential oil II volatile oil is 111.11-123.97ml/100g, and the tingling degree is 3.72-4.90mg/100 g; the content of resin volatile oil is 0ml/100g, the tingling degree is 141.12-143.24mg/100g, and the tingling degree amplification is 42.59% -48.53%.
Further, the content of essential oil I volatile oil obtained by extracting and separating the fresh red pepper oleoresin is 101.94-109.57ml/100g, and the tingling degree is 2.82-3.53mg/100 g; the essential oil II has volatile oil content of 108.91-128.93ml/100g, and tingling degree of 2.13-3.18mg/100 g; the content of resin volatile oil is 3.84-4.67ml/100g (less than 5ml/100 g), the tingling degree is 179.48-182.56mg/100g, and the tingling degree amplification is 52.49% -53.17%.
The invention also discloses fresh zanthoxylum essential oil and fresh zanthoxylum oleoresin prepared by any one of the fresh zanthoxylum oleoresin separation and purification processes, wherein the fresh zanthoxylum essential oil comprises fresh zanthoxylum essential oil I and fresh zanthoxylum essential oil II with different characteristic aromas, and the fresh zanthoxylum essential oil can be independently applied or combined to be applied.
The invention has the beneficial effects that:
(1) the invention has reasonable design and adopts supercritical CO2The fluid dynamic countercurrent extraction can realize the independent or joint extraction and separation of solid substances and liquid substances, and carbon dioxide can be recycled; the solid substance extraction unit comprises a plurality of extraction kettles, can be used alternately, and can be used for performing unidirectional dynamic extraction on solid substances; the liquid substance extraction unit carries out bidirectional dynamic extraction on the liquid substance and reasonably designs the residual substanceThe tank is stored, so that continuous dynamic extraction of the liquid substance is not influenced when the residual substance is discharged; the invention has high extraction and separation efficiency, increases the types of extracted substances, and has good extraction and separation effect and strong system adaptability; compared with the traditional technology, the system has higher adaptability, and the extracted substance can be in a liquid state or a solid state. Rationally design the extraction cauldron, realize the extraction to solid-state material, this extraction cauldron passes through water bath heating, and the temperature of extraction intracavity portion when conveniently controlling the extraction, the section of thick bamboo is extracted in independent design simultaneously, and this extraction section of thick bamboo is through sealed lid fixed mounting in the cauldron body to this extraction section of thick bamboo can be dismantled in order to make things convenient for the loading and unloading of material, and CO is advanced for the bottom to this extraction cauldron simultaneously2After completion of the extraction, CO2Discharging from the upper end, lengthening the CO in this way2The contact time with solid substances improves the extraction efficiency and the yield. The liquid substance extraction unit is reasonably designed, the liquid substance extraction unit can realize the extraction of the liquid substance, the liquid is conveyed downwards in a spraying mode, and the CO is2Is transported from bottom to top by CO2The liquid is extracted in a counter-current mode, so that the extraction efficiency and the yield are improved.
(2) By using supercritical CO2The fluid extraction separation technology can realize the extraction separation of the zanthoxylum oil resin, is particularly suitable for the extraction separation of the fresh zanthoxylum oil resin, and has the separation efficiency of more than 94 percent. The suitable process conditions for preparing the fresh pepper resin and the fresh pepper essential oil are as follows: feed rate 40kg/h, CO2The flow rate is 600L/h, the extraction temperature is 45 ℃, and the extraction pressure is 20MPa; the temperature of the separation I is 40 ℃, the pressure of the separation I is 7.5MPa, the separation temperature is 55 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is not adjustable and is automatically controlled by a system). Supercritical CO treatment under the process conditions2The fresh zanthoxylum oil resin is extracted and separated by fluid countercurrent, the total yield of the fresh zanthoxylum oil resin product is more than 99.08 percent, and the separation efficiency is more than 98.59 percent; the total yield of the fresh red pepper oleoresin product is more than 98.74 percent, and the separation efficiency is more than 94.00 percent.
(3) The obtained fresh pepper essential oil and fresh pepper resin have excellent characteristic indexes, wherein the content of volatile oil in the fresh pepper essential oil I and the fresh pepper essential oil II exceeds 100ml/100g, and the volatile oil is highly concentrated in the essential oil I and accounts for more than 95 percent; the residual tingling degree of the essential oil I and the essential oil II is lower than 5mg/100 g. In the separated resin components, volatile oil content of fresh green pepper resin is not detected, the volatile oil content of fresh red pepper resin is lower than 5ml/100g, the tingling degree reaches more than 140mg/100g, and the tingling degree is improved by more than 42%. Therefore, the system and the process can better realize the separation and purification of the fresh zanthoxylum oil resin, and the extraction and separation effect of the fresh zanthoxylum oil resin is better than that of the fresh zanthoxylum oil resin.
Drawings
FIG. 1 shows supercritical CO2A process flow chart of countercurrent extraction and separation of fresh zanthoxylum oil resin;
FIG. 2 is a schematic diagram of the system architecture of the present invention;
FIG. 3 is a schematic diagram of the structure of an extraction vessel according to the present invention;
FIG. 4 is a schematic diagram of the structure of a liquid substance extraction unit according to the present invention;
in the figure: 100. CO 22An air source unit; 101. a gas source tank; 102. CO 22A filter; 103. a cooling machine; 104. a storage tank; 200. a purifier; 300. a mixer; 400. a solid matter extraction unit; 500. an extraction kettle; 501. a kettle body; 502. an extraction cylinder; 503. filtering blocks; 504. sealing the cover body; 600. a separation kettle; 700. a liquid substance extraction unit; 701. an extraction column; 702. a liquid extraction chamber; 703. a sealed chamber cover; 704. a shower head; 705. and (7) temporarily storing the tank.
Detailed Description
The invention will be better understood from the following examples. However, it is easily understood by those skilled in the art that the contents of the embodiments described are only for illustrating the present invention and should not be construed as limiting the present invention described in detail in the claims.
Examples
A process for separating and purifying fresh oleum Zanthoxyli Bungeani by supercritical CO2The fluid dynamic countercurrent extraction separation system carries out dynamic countercurrent extraction separation.
Wherein, supercritical CO2A fluid dynamic counter-current extraction separation system comprising:
CO2a gas source unit (100),
a solid matter extraction unit (400) connected with the CO through a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to a solid matter extraction unit (400);
a liquid substance extraction unit (700) connected with the CO via a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to the liquid matter extraction unit (700); and
a separation unit respectively connected to the solid substance extraction unit (400) and the liquid substance extraction unit (700) for separating the extracted substances from supercritical CO2Separating, and separating the separated CO2Through a pipeline via CO2The filter (102) and the cooler (103) are circulated back to the storage tank (104);
wherein, the fresh zanthoxylum oil resin is subjected to dynamic countercurrent extraction separation by the system, which comprises the following steps:
(1) the picked fresh pepper is cold-pressed within 2 hours to prepare the fresh pepper oleoresin.
(2) Opening supercritical CO2The main power switch of the fluid extraction and separation device, and the setting of extraction and separation technological parameters in a computer control system, in turn comprise CO2The flow rate is 400-; the temperature of the separation I is 35-45 ℃, the pressure of the separation I is 6-11MPa, the separation temperature is 50-60 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is unadjustable and is automatically controlled by a system);
(3) opening a water circulating pump and a heating system switch, and automatically controlling temperature rise and fall through a temperature sensor and a computer until the temperature of each unit reaches a set value and is stable;
(4) then sequentially opening an air source unit switch, an extraction unit switch, a separation unit switch and CO2The injection pump is opened and the air inlet valve of each unit is adjusted, and pressure control is realized through a backpressure valve and a computer until the pressure of each unit reaches a set value and is stable;
(5) and (3) opening a feed pump, spraying fresh pepper oleoresin from the upper end of the extraction column through a spray head at a feeding rate of 40-60kg/h, collecting the fresh pepper oleoresin and the fresh pepper essential oil from the extraction unit (temporary storage tank) and the separation unit (separation kettle I and separation kettle II) every two hours, and shutting down and relieving pressure when feeding is finished, no product is increased, and extraction and separation are finished.
The numbers 1 to 10 shown in table 1 correspond to example 1, example 2, example 3, example 4, example 5, and example 6, and comparative example 1, comparative example 2, comparative example 3, and comparative example 4, respectively, and the extraction and separation process parameters are shown in table 2.
Wherein:
the dry green pepper oleoresin in comparative example 1 was prepared from dry green pepper particles by a pressing process;
the dry zanthoxylum bungeanum oil resin in the comparative example 2 is prepared by pressing dry zanthoxylum bungeanum particles;
in the comparative example 3, the dry green pepper oleoresin is prepared by pre-crushing dry green pepper particles to 20-40 meshes and then performing supercritical CO2Fluid extraction separation device is in' load capacity 200kg, CO2Flow rate of 300L/h, extraction temperature of 45 ℃, extraction pressure of 25MPa, separation
At a temperature of 40 ℃, separating
Pressure 8MPa, separation
At a temperature of 50 ℃, separating
Extracting and separating under the process condition of pressure of 4-6MPa (pressure balance with a gas storage tank);
in comparative example 4, the dry zanthoxylum bungeanum oleoresin is prepared by pre-crushing dry zanthoxylum bungeanum particles to 20-40 meshes and then performing supercritical CO2Fluid extraction separation device is in' load capacity 200kg, CO2Flow rate of 300L/h, temperature of 48 ℃, pressure of 30MPa, separation
At a temperature of 43 ℃ and separation
Pressure 12MPa, separation
At a temperature of 55 ℃, separating
And (4) extracting and separating under the process condition of pressure of 4-6MPa (pressure balance with a gas storage tank).
The volatile oil tester used at this time is a steam distillation device SEHB-1000, Shandong Yiyuan environmental protection science and technology Co. UV spectrophotometry was T6 model, general-purpose instruments of Beijing Puproud. The purity of the carbon dioxide is 99.95 percent, and the carbon dioxide is in food grade. Others are analytically or chemically pure reagents.
TABLE 1 raw oil resin years and associated characteristic indices
TABLE 2 supercritical CO2Corresponding technological parameters of fluid extraction separation pepper oleoresin
Test example 1
And (3) taking the raw oil resin or the product essential oil or the product resin in the embodiments 1-6 and the comparative examples 1-4, obtaining the volatile oil in the sample by a water distillation method, and calculating the content of the volatile oil in the sample to be detected by the following formula.
Content of volatile oil (ml/100 g) = volume of volatile oil (ml)/mass of sample (g) × 100
Test example 2
And (3) carrying out the hemp degree detection on the raw oil resin or the product essential oil or the product resin in the examples 1-6 and the comparative examples 1-4.
Accurately weighing 0.50g of a sample to be detected in a 50.00ml volumetric flask, adding a proper amount of absolute ethyl alcohol, fully shaking up, metering the volume to the scale mark by using the absolute ethyl alcohol, and shaking up again. Taking a diluted sample, measuring the absorbance value A of the diluted sample at the position of 268nm of wavelength by using an ultraviolet spectrophotometer, and obtaining the tingling degree of the sample to be measured by using a tingling degree calculation formulaλ。
λ=A*5.89*m/50
Note: a is the absorbance value of the diluted sample, and m is the dilution multiple;λthe unit is the tingling degree of a sample to be detected and is mg/g.
Test example 3
Comparing the essential oil yield and the resin yield of the examples 1 to 6 and the comparative examples 1 to 4, the calculation formula is as follows:
essential oil yield (%) = essential oil mass (g)/total amount of oleoresin (g) × 100%
Resin yield (%) = mass of resin (g)/total amount of oleoresin (g) × 100%
Test example 4
Comparing the total product yield and the volatile oil separation efficiency in examples 1-6 and comparative examples 1-4, the calculation is given as follows:
total yield (%) = (mass of essential oil + mass of resin)/total mass of oleoresin 100%
Volatile oil separation efficiency (%) = (essential oil volatile oil content · essential oil mass)/(oleoresin volatile oil content · total oleoresin) × 100%
The component yields, the total product yield and the volatile oil separation efficiency of examples 1 to 6 and comparative examples 1 to 4 are shown in tables 3 and 4.
TABLE 3 supercritical CO2Yield and total yield of each component of zanthoxylum oil resin by fluid extraction and separation
As can be seen from table 3:
(1) the total yield of products in each group of examples and comparative examples reaches more than 98 percent; in addition, as can be seen from examples 1 to 6, the total yield of the fresh green zanthoxylum oil resin product is higher than that of the fresh red zanthoxylum oil resinThe total yield of the product is slightly higher; the comparison of the comparative example 5 with the comparative example 6, and the comparison of the comparative example 7 with the comparative example 8 shows that the total yield of the dry zanthoxylum oil resin product is slightly higher than that of the dry zanthoxylum oil resin product; comparing comparative example 5 with comparative example 7, and comparative example 6 with comparative example 8, it can be seen that supercritical CO is present2The total yield of the product prepared by fluid extraction and separation is slightly higher than that of the product prepared by the same type of oleoresin prepared by a squeezing process.
(2) From the resin yield, the yield of the fresh red pepper resin is higher than that of the fresh green pepper resin; supercritical CO produced by pressing process2The resin yield of the same kind of oleoresin prepared by fluid extraction and separation is high.
(3) From essential oils
And essential oils
The yield of the fresh pepper is mainly concentrated in the separation kettle, and the essential oil is
Accounts for more than 95 percent of the total amount of the essential oil; while the essential oil of the dry pepper is not intensively distributed, wherein the essential oil prepared by the squeezing process
The yield of (A) is about essential oil
The yield is more than 1.8 times; supercritical CO2Extracting and separating the obtained oil from the oil resin of dry fructus Zanthoxyli by fluid extraction
The yield reaches essential oil
The yield is more than 2.8 times.
(4) The difference is mainly in the oleoresin prepared by different raw materials and different preparation processesThe material components are different and the viscosity is inconsistent; but the difference is only shown in the resin and the essential oil
The essential oil yield and the total yield of each group are only slightly different, namely the system can be suitable for the extraction and separation of different zanthoxylum oleoresin, and is particularly suitable for the extraction and separation of fresh zanthoxylum oleoresin.
TABLE 4 supercritical CO2The volatile oil content and separation efficiency of each component of the zanthoxylum oil resin by fluid extraction
As can be seen from table 4:
(1) the separation efficiency of the fresh zanthoxylum oleoresin is more than 94%, and particularly the separation efficiency of the fresh zanthoxylum oleoresin is the highest and reaches more than 98%; the separation efficiency of the dry pepper oleoresin is relatively low by about 4-10%, and the reason may be related to that the viscosity of the dry pepper oleoresin is generally higher than that of the fresh pepper oleoresin, the viscosity is increased, the carbon dioxide penetrating power is reduced, and the separation efficiency among substances is reduced; wherein, supercritical CO2The separation efficiency of the dry zanthoxylum oil resin prepared by the fluid extraction separation process is about 2 percent higher than that of the dry zanthoxylum oil resin prepared by the squeezing process, and the separation efficiency of the dry zanthoxylum oil resin prepared by the same preparation process is slightly higher than that of the dry zanthoxylum oil resin.
(2) In addition, except that the fresh zanthoxylum essential oil shown in Table 3 is mainly concentrated in essential oil I, and the dried zanthoxylum essential oil is mainly concentrated in essential oil
From Table 4, it can also be seen that the essential oils
Bifangji oil
The content of the volatile oil is generally higher by 15-30 ml/100g, and the fresh pepper essential oil,
The volatile oil content is above 100ml/100g, and the essential oil obtained by separating the dry pepper oil resin is only essential oil
The content of the volatile oil reaches more than 100ml/100g, namely the content of the volatile oil of the fresh pepper essential oil is obviously higher than that of the volatile oil of the dry pepper essential oil, which further proves that the components of the fresh pepper essential oil and the dry pepper essential oil are different, and further verifies that the separation difference is caused by different raw material oil resin substance components.
(3) The content of the resin volatile oil in the comparative examples 1-6 and the comparative examples 1-4 is visible, the content of the volatile oil remained in the fresh zanthoxylum resin is lower than 5ml/100g, and particularly, the volatile oil is not detected in the fresh zanthoxylum resin; the dried pricklyash peel resin has volatile oil residue of about 10ml/100 g. On one hand, the method is related to the difference of components of the fresh pepper essential oil and the dry pepper essential oil, and is also related to the difference of components of the fresh pepper resin and the dry pepper resin, so that the dry pepper resin and the dry pepper essential oil can be combined more tightly (shown in appearance, namely the viscosity of the dry pepper essential oil resin is higher than that of the fresh pepper essential oil resin), and the separation difficulty is higher than that of the fresh pepper resin and the fresh pepper essential oil.
The zanthoxylum oil resin of each group of examples and comparative examples is subjected to supercritical CO2The change of the tingling degree of each component after fluid extraction separation is shown in table 5.
TABLE 5 supercritical CO2Method for extracting and separating various components of zanthoxylum oil resin by using fluid
As can be seen from the data in table 5:
(1) examples 1-6 show that the degree of tingling of the fresh red pepper oleoresin is higher than that of the fresh green pepper oleoresin, and comparative examples 1-4 show that the degree of tingling of the dry red pepper oleoresin is higher than that of the dry green pepper oleoresin;
(2) after the zanthoxylum oil resin is extracted and separated, the numb value of the obtained resin is obviously increased, the increase is more than 42 percent and is different from 42.59 percent to 64.83 percent, the numb degree increase of the zanthoxylum resin is higher than that of each zanthoxylum resin, and the presumption is related to the characteristics of variety components;
(3) after the zanthoxylum oil resin is extracted and separated, the tingling degree of the obtained fresh zanthoxylum essential oil I and fresh zanthoxylum essential oil II is lower than 5mg/100g, and compared with the corresponding oleoresin, the tingling degree is reduced by more than 95 percent; the tingling degree of the dry pepper essential oil I is more than 40mg/100g, and although the tingling degree of the dry pepper essential oil II is obviously lower than that of the dry pepper essential oil I, the tingling degree of the dry pepper essential oil II is slightly higher than that of the fresh pepper essential oil II. The partial data further has component difference between the dry pepper essential oil and the fresh pepper essential oil, so that the separation effect of the fresh pepper oleoresin is obviously better than that of the dry pepper oleoresin.
In conclusion, the system and the process can be used for extracting and separating the dry pepper oleoresin from the dry peppers and preparing the pepper resin and the pepper essential oil from the pepper oleoresin, and are particularly suitable for extracting and separating the fresh pepper oleoresin. Wherein, when the fresh pepper oleoresin is extracted and separated to prepare the fresh pepper resin and the fresh pepper essential oil:
(1) the optimal process parameters are as follows: feed rate 40kg/h, CO2The flow rate is 600L/h, the extraction temperature is 45 ℃, and the extraction pressure is 20MPa; the temperature of the separation I is 40 ℃, the pressure of the separation I is 7.5MPa, the separation temperature is 55 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is not adjustable and is automatically controlled by a system).
(2) The total yield of the product is 98.74-99.17%, wherein the total yield of the fresh zanthoxylum oil resin (99.08-99.17%) is slightly higher than the total yield of the zanthoxylum oil resin (98.74-98.99%).
(3) The separation efficiency of volatile oil is more than 94%, wherein the separation efficiency (98.59% -99.24%) of the fresh green zanthoxylum oil resin is obviously higher than that (94.00% -94.27%) of the fresh red zanthoxylum oil resin.
(4) Can obtain two kinds of fresh pepper essential oil with the volatile oil content of more than 100ml/100g, the tingling degree of less than 5mg/100g and different aroma characteristics, but the essential oil is used
Mainly accounts for more than 95 percent. Wherein the content of volatile oil of fresh green pricklyash peel essential oil I is 105.63-108.11ml/100g, the tingling degree is 4.11-4.41mg/100g (less than 5mg/100 g), the content of volatile oil of essential oil II is 111.11-123.97ml/100g, and the tingling degree is 3.72-4.90mg/100 g; the content of volatile oil of fresh fructus Zanthoxyli volatile oil I is 101.94-109.57ml/100g, the oil content is 2.82-3.53mg/100g (less than 5mg/100 g), the content of volatile oil of essential oil II is 108.91-128.93ml/100g, and the oil content is 2.13-3.18mg/100 g.
(5) Can obtain fresh pepper resin with the tingling degree of more than 140mg/100g and the residual content of volatile oil of less than 5ml/100 g. Wherein, the content of the volatile oil of the fresh green pricklyash peel resin is 0ml/100g, the tingling degree is 141.12-143.24mg/100g, and the tingling degree is increased by 42.59% -48.53%; the content of fresh red pepper resin volatile oil is 3.84-4.67ml/100g (less than 5ml/100 g), the tingling degree is 179.48-182.56mg/100g, and the tingling degree amplification is 52.49% -53.17%.
Therefore, the system and the process can achieve higher separation efficiency by extracting and separating the fresh zanthoxylum oil resin, and the separation effect of the fresh zanthoxylum oil resin is superior to that of the zanthoxylum oil resin. This not only realizes the supercritical CO of the liquid oleoresin2The extraction separation is a zero breakthrough in the industry, more possibilities are provided for the purification and the application of the pepper resin and the pepper essential oil, and the diversified deep processing development of the pepper industry is promoted.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A separation and purification process of fresh zanthoxylum oil resin comprises the following steps:
subjecting fresh fructus Zanthoxyli oleoresin to supercritical CO2The fluid dynamic countercurrent extraction separation system carries out dynamic countercurrent extraction;
wherein:
supercritical CO2A fluid dynamic counter-current extraction separation system comprising:
CO2a gas source unit (100),
a solid matter extraction unit (400) connected with the CO through a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to a solid matter extraction unit (400);
a liquid substance extraction unit (700) connected with the CO via a pipeline2Gas source units (100) are connected and used for introducing supercritical CO through pipelines2Counter-currently to the liquid matter extraction unit (700); and
a separation unit respectively connected to the solid substance extraction unit (400) and the liquid substance extraction unit (700) for separating the extracted substances from supercritical CO2Separating, and separating the separated CO2Through a pipeline via CO2The filter (102) and the cooler (103) are circulated back to the storage tank (104);
the separation and purification process comprises the following steps:
feeding rate of 40-60kg/h, CO2The flow rate is 400-; the temperature of the separation I is 35-45 ℃, the pressure of the separation I is 6-11MPa, the separation temperature is 50-60 ℃, and the pressure of the separation II is 4-6MPa (a dynamic value which is determined by an air source and is unadjustable and is automatically controlled by a system).
2. The fresh zanthoxylum oil resin separation and purification process according to claim 1, wherein:
the separation unit comprises a plurality of separation kettles which can be used independently or in series or in parallel, and at least comprises a separation kettle I and a separation kettle II.
3. The fresh zanthoxylum oil resin separation and purification process according to claim 1, wherein:
the dynamic countercurrent extraction separation of the fresh zanthoxylum oil resin comprises the following steps:
the fresh zanthoxylum oil resin enters a liquid substance extraction unit, after extraction is finished, the fresh zanthoxylum essential oil I and the fresh zanthoxylum essential oil II are obtained through a separation kettle I and a separation kettle II of the separation unit, and the fresh zanthoxylum resin is obtained through a temporary storage tank of the extraction unit.
4. The fresh zanthoxylum oil resin separation and purification process according to claim 1, wherein:
the fresh zanthoxylum oil resin is selected from fresh zanthoxylum oil resin or fresh red zanthoxylum oil resin.
5. The fresh zanthoxylum oil resin separation and purification process according to claims 1-4, wherein:
the extraction and separation process of the fresh zanthoxylum oil resin comprises the steps of feeding rate of 40kg/h and CO2The flow rate is 600L/h, the extraction temperature is 45 ℃, the extraction pressure is 20MPa, the separation I temperature is 40 ℃, the separation I pressure is 7.5MPa, the separation temperature is 55 ℃, and the separation II pressure is 4-6MPa (the dynamic value is determined by an air source and is unadjustable and is automatically controlled by a system).
6. The fresh zanthoxylum oil resin separation and purification process according to claim 5, wherein:
the separation efficiency of the fresh green zanthoxylum oil resin is 98.59-99.24%, and the total yield is 99.08-99.17%.
7. The fresh zanthoxylum oil resin separation and purification process according to claim 5, wherein:
the separation efficiency of the fresh red pepper oleoresin is 94.00-94.27%, and the total yield is 98.74-98.99%.
8. The fresh zanthoxylum oil resin separation and purification process according to claim 5, wherein:
the content of essential oil I volatile oil obtained by extracting and separating the fresh green zanthoxylum oleoresin is 105.63-108.11ml/100g, and the tingling degree is 4.11-4.41mg/100 g; the content of essential oil II volatile oil is 111.11-123.97ml/100g, and the tingling degree is 3.72-4.90mg/100 g; the content of resin volatile oil is 0ml/100g, the tingling degree is 141.12-143.24mg/100g, and the tingling degree amplification is 42.59% -48.53%.
9. The fresh zanthoxylum oil resin separation and purification process according to claim 5, wherein:
the content of essential oil I volatile oil obtained by extracting and separating the fresh red pepper oleoresin is 101.94-109.57ml/100g, and the tingling degree is 2.82-3.53mg/100 g; the essential oil II has volatile oil content of 108.91-128.93ml/100g, and tingling degree of 2.13-3.18mg/100 g; the content of resin volatile oil is 3.84-4.67ml/100g (less than 5ml/100 g), the tingling degree is 179.48-182.56mg/100g, and the tingling degree amplification is 52.49% -53.17%.
10. The fresh zanthoxylum bungeanum essential oil and the fresh zanthoxylum bungeanum resin prepared by the fresh zanthoxylum bungeanum oil resin separation and purification process according to any one of claims 1 to 9, wherein the fresh zanthoxylum bungeanum essential oil comprises fresh zanthoxylum bungeanum essential oil I and fresh zanthoxylum bungeanum essential oil II with different characteristic aromas, and can be independently applied or applied together.
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| CN103611331B (en) * | 2013-12-09 | 2016-08-17 | 大连工业大学 | A kind of supercritical extraction/reaction integrated apparatus |
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