CN113304504B - Industrial method for preparing green coffee bean extract - Google Patents
Industrial method for preparing green coffee bean extract Download PDFInfo
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- CN113304504B CN113304504B CN202110637726.6A CN202110637726A CN113304504B CN 113304504 B CN113304504 B CN 113304504B CN 202110637726 A CN202110637726 A CN 202110637726A CN 113304504 B CN113304504 B CN 113304504B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- A23F5/00—Coffee; Coffee substitutes; Preparations thereof
- A23F5/24—Extraction of coffee; Coffee extracts; Making instant coffee
- A23F5/26—Extraction of water-soluble constituents
- A23F5/267—Extraction of water-soluble constituents using additives, specific extraction media or specific coffee blends
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses an industrial method for preparing green coffee bean extract, which comprises the steps of raw material flaking, supercritical pre-extraction, organic solvent separation and refining, macroporous adsorption resin purification, spray drying and the like. The method has the advantages of high degree of integration innovation, easy realization of industrial production, good product purification effect, high green coffee bean extract yield and the like, the indexes of the product such as water solubility, moisture absorption resistance, caffeine content and the like are obviously superior to those of the same product, the pesticide residue meets the international most stringent standard requirement, and the industrial production is realized.
Description
Technical Field
The invention relates to an industrial method for producing a high-quality green coffee bean extract with specific specifications, in particular to an industrial method for preparing the green coffee bean extract.
Background
The green coffee bean is seed of coffee tree of Rubiaceae, contains abundant active substances, wherein chlorogenic acid and its homologue (also called green coffee bean extract) are main polyphenol active ingredients of green coffee bean, and has multiple biological activities of resisting oxidation, resisting virus, resisting cancer, inhibiting bacteria, etc. Recent research of American scientists considers that the green coffee bean extract has good functions of losing weight and reducing blood pressure, so the green coffee bean extract is popular with consumers.
China is a main production country of green coffee beans, production places are concentrated in Yunnan and Hainan provinces, Yunnan mainly takes the arabian coffee beans and mainly distributes in Puer, Baoshan and other places, and Hainan province plants are mainly concentrated in Wanning, Mian and other places. Every year, tens of thousands of tons of green coffee beans cannot meet the requirement of direct eating and are discarded, thereby causing resource waste and environmental pollution.
The chlorogenic acid isomers in the green coffee beans are more in variety and different in polarity, so that difficulty is brought to extraction and purification of the green coffee bean extract, the extraction yield is low by adopting a conventional extraction solvent and an extraction mode, the ratio of effective components is unstable, and subsequent development and utilization are influenced. In addition, the existence of caffeine, small molecular sugar and lipid substances contained in the green coffee beans leads the green coffee bean extract to have high caffeine content, poor powder flowability and serious moisture absorption and agglomeration, thus greatly influencing the application of the green coffee bean extract in terminal products; meanwhile, in recent years, the limitation on the pesticide residue of the plant extract is continuously tightened, the preparation process of the green coffee bean extract is a component enrichment process, the pesticide residue in the product is also enriched, and the international trade barrier is difficult to break through; therefore, there is a need to develop an industrial technology for producing high-quality green coffee bean extract to improve the product quality and market competitiveness.
Disclosure of Invention
The invention aims to provide an industrial method for preparing green coffee bean extract, which has good product purification effect, high product yield and good quality.
The technical scheme adopted by the method is as follows:
an industrial process for preparing a green coffee bean extract comprising the steps of: directly rolling green coffee beans to obtain green coffee bean embryo pieces; pre-extracting green coffee bean embryo pieces by using supercritical carbon dioxide fluid, recovering carbon dioxide to obtain a separated substance and pre-extracted embryo pieces, and removing the separated substance for harmless treatment; extracting the pre-extracted embryonic slices by using an organic solvent A to obtain an extract, and concentrating the extract until the solvent content is 40 +/-5 wt% to obtain a concentrated solution; sequentially adding an organic solvent B and an organic solvent C into the concentrated solution, respectively carrying out liquid-liquid extraction, adjusting the pH value to 4.8 +/-0.2 in the extraction process, standing and separating after the extraction is finished, sequentially obtaining a lower layer solution of the organic solvent B and an upper layer solution of the organic solvent C, respectively concentrating to respectively obtain byproducts containing caffeine and green coffee bean oil, and simultaneously recycling the solvent B and the solvent C, wherein the recycled solvent C needs to be periodically rectified to reduce the component proportion of the solvent B; combining the lower layer solutions of the organic solvent C, vacuum concentrating until the content of the organic solvent is lower than 1%, and diluting the obtained concentrated solution with pure water until the concentration of total chlorogenic acid is 12 + -2 mg/mL and the temperature is 35 + -2 ℃; purifying the obtained diluent by using macroporous adsorption resin, adjusting the temperature of an organic solvent D to be 35 +/-2 ℃ and the pH value to be 4.3 +/-0.2, analyzing, and collecting an analysis solution; vacuum concentrating the desorption solution, removing solvent residue, and preparing green coffee bean extract powder by using spray drying equipment; adding or not adding adjuvants, and mixing to obtain green coffee bean extract products with different specifications.
The invention uses the anti-collision hydraulic blank rolling machine to directly roll the green coffee beans into sheets, the thickness of the green coffee beans is controlled to be 0.3 +/-0.05 mm, and the pressing roller continuously cools to ensure that the temperature is controlled to be below 60 ℃.
The pressure of the supercritical extraction kettle is 18 +/-1 MPa, the temperature is 50 +/-2 ℃, the pre-extraction time is 5 +/-0.5 hours, and the flow value of carbon dioxide is 8-16 times of the weight of the embryo piece; two separation kettles are used for two-stage separation and analysis, wherein the first-stage analysis pressure is 8 +/-1 MPa, and the second-stage analysis pressure is 5 +/-0.5 MPa.
The organic solvent A is high ethanol, the concentration of the high ethanol is 80 +/-2 wt%, the extraction temperature is 40 +/-2 ℃, the ratio of materials to liquids is 1: 3-8, and the times are 4-6.
The concentrated solution is sequentially added with an organic solvent B and an organic solvent C, and liquid-liquid extraction is respectively carried out, and the method comprises the following specific steps:
(1) firstly, adding an organic solvent B, wherein the solvent is one of dichloromethane, dichloroethane and diethyl ether, the volume ratio of concentrated solution to the solvent B is 1: 3-6, the extraction temperature is 30 +/-2 ℃, stirring and circulating are carried out in the liquid-liquid extraction process, the extraction time is 1-4 hours, the extraction times are 2-5 times, standing and separating are carried out after each extraction is finished to discharge lower layer liquid, and the lower layer liquid is combined and concentrated to obtain a caffeine-containing byproduct for harmless treatment; combining the upper layer liquid for each time to obtain the feed liquid without caffeine;
(2) and adding an organic solvent C into the decaffeinated feed liquid, wherein the solvent is one of normal hexane, a vegetable oil extraction solvent and cyclohexane, the volume ratio of the decaffeinated feed liquid to the solvent C is 1: 3-6, the extraction temperature is 45 +/-2 ℃, the continuous stirring is carried out in the liquid-liquid extraction process, the extraction time is 1-4 hours, the extraction times are 2-5 times, the lower layer liquid is discharged by standing and separating after the extraction is finished each time, the lower layer liquid is combined and concentrated, and the residual upper layer liquid is combined and concentrated to obtain the green coffee bean oil-containing by-product.
In the process of adding the organic solvent B for liquid-liquid extraction, the stirring speed is not lower than 130rpm, and a pump and an equipment bypass pipeline are used for circulating at the same time, wherein the circulating amount is 2-6 times of the volume of the equipment per hour; during the liquid-liquid extraction process by adding the organic solvent C, the stirring speed is controlled at 130 +/-2 rpm.
When the proportion of the solvent B mixed and brought in the recycled solvent C exceeds 10 percent, the solvent C is rectified to reduce the proportion to be within 2 percent.
The gas phase temperature in the vacuum concentration process is 55 +/-3 ℃, and the vacuum degree is 0.08 +/-0.005 MPa.
The flow rate of the diluent on the column is 1.0 +/-0.2 BV/h, the organic solvent D is ethanol, the preparation concentration is 70 +/-5 wt%, and the flow rate is 1.2 +/-0.3 BV/h; the resin model is DM 700.
The invention uses a pressure type spray drying device, the solid content of the liquid to be sprayed before spraying is controlled to be 35 +/-5%, the spraying pressure is controlled to be 6-12 MPa, and the air outlet temperature is controlled to be 85 +/-5 ℃.
The technical advantages of the invention are as follows: the green coffee bean powder has the advantages of high degree of technical and equipment integration innovation, easiness in realization of industrial production, good product purification effect, high green coffee bean extract yield and the like, the indexes of the product such as water solubility, moisture absorption resistance, caffeine content and the like are obviously superior to those of the same-row product (the collection of other same-row products shows that the same-row product with the same content specification is dissolved in water at 20 ℃ and then stands for 12 hours to generate precipitation or suspension, the powder product is placed in an open room for 3 hours to generate moisture absorption and agglomeration, the caffeine content is about 0.5-5 percent), the pesticide residue meets the international most stringent standard requirement (less than 0.01 ppm), and the industrial production is realized.
The supercritical technology is used for removing pesticide residues in green coffee bean embryo pieces, and pesticide residues with high international concern such as ethion, triazophos, dimethoate and the like are fully removed, so that even if subsequent processing and enrichment are carried out, the residual quantity can be ensured to be less than 0.01ppm, the product quality is greatly improved, the product quality safety is ensured, and the international market competitiveness is improved; the high-efficiency solvent residue removal technology can realize that the total solvent residue is less than 50ppm while the content loss is minimized; the innovative technology for removing the caffeine by the solvent method ensures that the content of the caffeine in the extract is less than 0.3 percent, and meets the most severe customer requirements; the solvent C, the solvent B and the macroporous adsorption resin are sequentially combined, so that various impurities in the product are fully removed, and the unit content and the moisture absorption resistance of the product are ensured to be high; and the solvent B is replaced by the solvent C, so that the residue of the solvent B with strict requirements is below the detection limit, and the solvent B is successfully sold to the European and American markets; by controlling the parameters of the rolled sheets of the raw materials, optimizing the extraction conditions, optimizing the purification conditions and strictly controlling the temperature to be not higher than 60 ℃ in the whole process, the loss of the effective components of the chlorogenic acid is minimum, the conversion is minimum, the high yield (more than 98 percent) is ensured, the product quality is greatly improved, the product quality safety is ensured, and the international market competitiveness is improved.
The specific implementation mode is as follows:
example 1
Weighing 100.0kg of green coffee bean raw material, detecting that the content of chlorogenic acid is 7.05% and the content of caffeine is 1.58%, rolling into pieces with a collision-proof hydraulic blank rolling machine, wherein the thickness is 0.31mm, and continuously cooling by a compression roller to below 58 ℃.
Pre-extracting green coffee bean embryo pieces with supercritical carbon dioxide fluid at a carbon dioxide flow of 800L/h at 50 deg.C under 18MPa for 5 hr, and performing two-stage separation and analysis with two separation kettles at a first-stage analysis pressure of 8MPa and a second-stage analysis pressure of 5 MPa. And recovering carbon dioxide to obtain two-stage separated substances and pre-extracted embryonic slices, and discarding the two-stage separated substances for harmless treatment.
Pre-extracting at 40 deg.C, maintaining pH at 4.7, extracting with 80wt% ethanol solution (material-to-liquid ratio of 1: 3) for 4 times to obtain extractive solution, and concentrating the extractive solution to solvent content of 40.3% to obtain concentrated solution. At 30 ℃, adding a dichloromethane solvent into the concentrated solution according to the proportion of 1:3 (volume ratio), stirring and beating for 3 times in a circulating way while stirring for 1 hour each time, wherein the stirring speed is 135rpm, and the circulating amount is 2 times of the volume of the equipment per hour; standing for separation to give subnatant, mixing subnatants, and concentrating to obtain caffeine-containing by-product for harmless treatment. Adding n-hexane solvent into the upper layer liquid for extraction (material-liquid ratio is 1: 4), extracting for 3 times at 45 ℃ and a stirring speed of 130rpm, each time for 1 hour, standing for separation, combining and concentrating the upper layer liquid for each time to obtain a green coffee bean oil-containing by-product, vacuum concentrating the lower layer liquid at a vacuum degree of 0.08MPa and a temperature of 55 ℃ to a solvent residual amount of 0.8%, diluting with pure water to obtain a diluent with a total chlorogenic acid concentration of 12mg/mL, keeping the temperature at 35 ℃, purifying with macroporous adsorption resin, wherein the upper column flow rate of the diluent is 1.0BV/h, resolving with 65% ethanol with a preset pH value of 4.3, and the resolving flow rate is 1.5BV/h, and realizing the cyclic operation of serial adsorption of two resin columns and single resolution to obtain the resolving liquid. Vacuum concentrating the collected desorption solution, removing solvent residues, keeping the gas phase temperature at 57 ℃, keeping the vacuum degree at 0.08MPa, obtaining concentrated liquid to be sprayed, controlling the solid content at 35.8%, using pressure type spray drying equipment, controlling the pressure at 6MPa, controlling the air outlet temperature at 85 +/-2 ℃, spraying to obtain green coffee bean extract powder, adding no auxiliary material, mixing through high-low content matching to obtain 14.3kg of green coffee bean extract product with the purity of 48.38%, wherein the content yield reaches 98.1%, detecting, the pesticide residue content in the product is below 0.01ppm detection limit, the caffeine content is 0.13%, standing for 24h after water dissolving at 20 ℃ without precipitation or suspension, and standing for 24h in a powder product chamber without moisture absorption and agglomeration.
Example 2
Weighing 500.0kg of green coffee bean raw material, detecting that the content of chlorogenic acid is 7.33%, the content of caffeine is 2.24%, rolling the green coffee bean raw material into slices with the thickness of 0.35mm by using an anti-collision hydraulic blank rolling machine, and continuously cooling a compression roller to below 56 ℃.
Pre-extracting green coffee bean embryo pieces with supercritical carbon dioxide fluid at flow rate of 4000L/h at 52 deg.C under pressure of 19MPa for 5.5 hr, and performing two-stage separation and analysis with two separation kettles at first-stage analysis pressure of 9MPa and second-stage analysis pressure of 5.5 MPa. And recovering carbon dioxide to obtain two-stage separated substances and pre-extracted embryonic slices, and discarding the two-stage separated substances for harmless treatment.
Pre-extracting at 42 deg.C, maintaining pH at 4.6, extracting with 82wt% ethanol solution (material-to-liquid ratio of 1: 8) for 6 times to obtain extractive solution, and concentrating the extractive solution to solvent content of 45% to obtain concentrated solution. At 32 ℃, adding dichloroethane solvent into the concentrated solution according to the proportion of 1:6 (volume ratio), stirring and beating for 3 times circularly while extracting for 1 hour each time, wherein the stirring speed is 140rpm, and the circulating amount is 6 times of the volume of the equipment per hour; standing for separation to give subnatant, mixing subnatants, and concentrating to obtain caffeine-containing by-product for harmless treatment. Adding vegetable oil extraction solvent into the supernatant for extraction (material-liquid ratio is 1: 6), extracting for 5 times at 47 ℃ and stirring speed of 132rpm, each time for 2 hours, standing for separation, combining and concentrating the supernatant for each time to obtain a green coffee bean oil-containing by-product, vacuum concentrating the supernatant at vacuum degree of 0.085MPa and temperature of 58 ℃ until the residual solvent amount is 0.8%, diluting with pure water to obtain a diluent with total chlorogenic acid concentration of 14mg/mL, keeping the temperature at 37 ℃, purifying with macroporous adsorption resin, wherein the flow rate of the diluent on the column is 1.2BV/h, resolving with 75% ethanol with preset pH value of 4.5, the resolving flow rate is 1.5BV/h, and realizing the cycle operation of serial adsorption of two resin columns and single resolution to obtain the resolving solution. Vacuum concentrating the collected desorption solution, removing solvent residues, keeping the gas phase temperature at 56 ℃, keeping the vacuum degree at 0.085MPa, obtaining concentrated liquid to be sprayed, controlling the solid content at 40%, using a pressure type spray drying device, controlling the pressure at 12MPa, controlling the air outlet temperature at 85 +/-5 ℃, spraying to obtain green coffee bean extract powder, adding no auxiliary material, mixing through high-low content matching to obtain 71.03kg of a green coffee bean extract product with the purity of 50.71%, wherein the content yield reaches 98.3%, detecting, the pesticide residue content in the product is below the detection limit of 0.01ppm, the caffeine content is 0.11%, standing for 24 hours after water dissolving at 20 ℃ without precipitation or suspension, and standing for 24 hours in a powder product chamber without moisture absorption and agglomeration.
Embodiment 3
Weighing 200.0kg of green coffee bean raw material, detecting that the content of chlorogenic acid is 7.86% and the content of caffeine is 1.15%, rolling the green coffee bean raw material into slices with the thickness of 0.25mm by using an anti-collision hydraulic blank rolling machine, and continuously cooling a compression roller to below 55 ℃.
Pre-extracting green coffee bean embryo pieces with supercritical carbon dioxide fluid at a flow rate of 2000L/h at 48 deg.C under 17MPa for 4.5 hr, and performing two-stage separation and analysis with two separation kettles at a first-stage analysis pressure of 9MPa and a second-stage analysis pressure of 5.4 MPa. And recovering carbon dioxide to obtain two-stage separated substances and pre-extracted embryonic slices, and discarding the two-stage separated substances for harmless treatment.
Pre-extracting at 40 deg.C and pH of 4.6, extracting with 78wt% ethanol solution (material-to-liquid ratio of 1: 5) for 5 times to obtain extractive solution, and concentrating the extractive solution to solvent content of 35% to obtain concentrated solution. At 28 ℃, adding an ether solvent into the concentrated solution according to the proportion of 1:4 (volume ratio), stirring and beating for 4 times in a circulating way while stirring for 2 hours each time, wherein the stirring speed is 138rpm, and the circulating amount is 4 times of the volume of equipment per hour; standing for separation to give subnatant, mixing subnatants, and concentrating to obtain caffeine-containing by-product for harmless treatment. Adding cyclohexane solvent into the upper layer liquid for extraction (material-liquid ratio is 1: 4), extracting for 3 times at 45 ℃ and the stirring speed of 130rpm, each time for 1 hour, standing and separating, combining and concentrating the upper layer liquid for each time to obtain a green coffee bean oil-containing by-product, vacuum concentrating the lower layer liquid at the vacuum degree of 0.08MPa and the temperature of 55 ℃ until the solvent residue is 0.8%, diluting with pure water to obtain a diluent with the total chlorogenic acid concentration of 13mg/mL, keeping the temperature at 35 ℃, purifying by using macroporous adsorption resin, wherein the upper column flow rate of the diluent is 1.0BV/h, resolving by using pre-adjusted 65% ethanol with the temperature of 35 ℃ and the pH value of 4.3, and the resolving flow rate is 1.5BV/h, and realizing the cyclic operation of serial adsorption of two resin columns and single resolution to obtain the resolving liquid. Vacuum concentrating the collected desorption solution, removing solvent residues, keeping the gas phase temperature at 52 ℃, keeping the vacuum degree at 0.078MPa, obtaining concentrated liquid to be sprayed, controlling the solid content at 35.8%, using pressure type spray drying equipment, controlling the pressure at 10MPa, controlling the air outlet temperature at 85 +/-2 ℃, spraying to obtain green coffee bean extract powder, adding no auxiliary material, mixing through high-low content matching to obtain 32.35kg of green coffee bean extract product with the purity of 48.11%, wherein the content yield reaches 99.0%, detecting, the pesticide residue content in the product is below 0.01ppm detection limit, the caffeine content is 0.15%, standing for 24h after water dissolving at 20 ℃ without precipitation or suspension, and standing the powder product indoors for 24h without moisture absorption and caking.
The proportion of the ether solvent brought by mixing in the cyclohexane solvent recycled by the extraction and detection is 11.6 percent, and the ether proportion is reduced to 0.94 percent by rectifying the cyclohexane solvent.
Example 4
Weighing 400.0kg of green coffee bean raw material, detecting that the content of chlorogenic acid is 6.60% and the content of caffeine is 2.22%, rolling the green coffee bean raw material into slices with the thickness of 0.33mm by using an anti-collision hydraulic blank rolling machine, and continuously cooling a compression roller to below 54 ℃.
Pre-extracting green coffee bean embryo pieces with supercritical carbon dioxide fluid at flow rate of 4000L/h at 50 deg.C under pressure of 18MPa for 5.2 hr, and performing two-stage separation and analysis with two separation kettles at first-stage analysis pressure of 8.4MPa and second-stage analysis pressure of 5.2 MPa. And recovering carbon dioxide to obtain two-stage separated substances and pre-extracted embryonic slices, and discarding the two-stage separated substances for harmless treatment.
Pre-extracting at 40.7 deg.C and pH of 4.6, extracting with 80.5wt% ethanol solution (material-to-liquid ratio of 1: 3) for 4 times to obtain extractive solution, and concentrating the extractive solution to solvent content of 40.8% to obtain concentrated solution. At 30.7 ℃, adding a dichloromethane solvent into the concentrated solution according to the proportion of 1:3.5 (volume ratio), stirring and beating for 3 times in a circulating way, wherein each time lasts for 2 hours, the stirring speed is 137rpm, and the circulating amount is 2.5 times of the volume of equipment per hour; standing for separation to give subnatant, mixing subnatants, and concentrating to obtain caffeine-containing by-product for harmless treatment. Adding n-hexane solvent into the supernatant for extraction (material-liquid ratio is 1: 4.5), extracting for 3 times at 45 ℃ and stirring speed of 133rpm, each time for 1.5 hours, standing for separation, combining and concentrating the supernatant for each time to obtain a by-product containing green coffee bean oil, concentrating the supernatant in vacuum at a vacuum degree of 0.08MPa and a temperature of 55 ℃ until the solvent residue is 0.8%, diluting with pure water to obtain a diluted solution with a total chlorogenic acid concentration of 12.2mg/mL, keeping the temperature at 35.9 ℃, purifying with macroporous adsorption resin, wherein the flow rate of the diluted solution on an upper column is 1.0BV/h, resolving with 70.6% ethanol with a preset pH value of 4.4, and the resolving flow rate is 1.5BV/h, and realizing the cyclic operation of serial adsorption of two resin columns and single resolving to obtain the resolving solution. Vacuum concentrating the collected desorption solution, removing solvent residues, keeping the gas phase temperature at 57 +/-1 ℃, keeping the vacuum degree at 0.08 +/-0.002 MPa to obtain concentrated liquid to be sprayed, controlling the solid content to be 36.8%, using a pressure type spray drying device, controlling the pressure to be 9MPa, controlling the air outlet temperature to be 85 +/-2 ℃, spraying to obtain green coffee bean extract powder, adding no auxiliary materials, mixing by high and low content matching to obtain 51.75kg of green coffee bean extract product with the purity of 50.33%, wherein the content yield reaches 98.6%, detecting, controlling the pesticide residue content in the product to be below 0.01ppm, controlling the caffeine content to be 0.09%, standing for 24 hours after water dissolving at 20 ℃, not causing precipitation or suspension, placing the powder product indoors for 24 hours, and not absorbing moisture and blocking.
Claims (9)
1. An industrial process for preparing a green coffee bean extract comprising the steps of:
(1) directly rolling green coffee beans to obtain green coffee bean embryo pieces;
(2) pre-extracting green coffee bean embryo pieces by using supercritical carbon dioxide fluid, recovering carbon dioxide to obtain a separated substance and pre-extracted embryo pieces, and removing the separated substance for harmless treatment;
(3) extracting the pre-extracted embryonic slices by using an organic solvent A to obtain an extract, and concentrating the extract until the solvent content is 40 +/-5 wt% to obtain a concentrated solution;
(4) sequentially adding an organic solvent B and an organic solvent C into the concentrated solution, respectively carrying out liquid-liquid extraction, adjusting the pH value to 4.8 +/-0.2 in the extraction process, standing and separating after the extraction is finished, sequentially obtaining a lower layer solution of the organic solvent B and an upper layer solution of the organic solvent C, respectively concentrating to respectively obtain byproducts containing caffeine and green coffee bean oil, and simultaneously recycling the solvent B and the solvent C, wherein the recycled solvent C needs to be periodically rectified to reduce the component proportion of the solvent B; the method comprises the following specific steps:
firstly, adding an organic solvent B, wherein the solvent is one of dichloromethane, dichloroethane and diethyl ether, the volume ratio of concentrated solution to the solvent B is 1: 3-6, the extraction temperature is 30 +/-2 ℃, stirring and circulating are carried out in the liquid-liquid extraction process, the extraction time is 1-4 hours, the extraction times are 2-5 times, the lower layer liquid is discharged by standing and separating after the extraction is finished each time, and the lower layer liquid is combined and concentrated to obtain a caffeine-containing byproduct for harmless treatment; combining the upper layer liquid for each time to obtain the feed liquid without caffeine;
secondly, adding an organic solvent C into the decaffeinated feed liquid, wherein the solvent is one of normal hexane, a vegetable oil extraction solvent and cyclohexane, the volume ratio of the decaffeinated feed liquid to the solvent C is 1: 3-6, the extraction temperature is 45 +/-2 ℃, the continuous stirring is carried out in the liquid-liquid extraction process, the extraction time is 1-4 hours, the extraction times are 2-5 times, standing and separating the mixture after each extraction is finished to discharge a lower layer liquid, combining and concentrating the lower layer liquids, and combining and concentrating the remaining upper layer liquids to obtain a byproduct containing the green coffee bean oil;
(5) combining the lower layer solutions of the organic solvent C, vacuum concentrating until the content of the organic solvent is lower than 1%, and diluting the obtained concentrated solution with pure water until the concentration of total chlorogenic acid is 12 + -2 mg/mL and the temperature is 35 + -2 ℃;
(6) purifying the obtained diluent by using macroporous adsorption resin, adjusting the temperature of an organic solvent D to be 35 +/-2 ℃ and the pH value to be 4.3 +/-0.2, analyzing, and collecting an analysis solution;
(7) vacuum concentrating the desorption solution, removing solvent residue to obtain a solution to be sprayed, and preparing green coffee bean extract powder by using spray drying equipment;
(8) adding or not adding adjuvants, and mixing to obtain green coffee bean extract products with different specifications.
2. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: and (3) directly rolling green coffee beans into sheets by using an anti-collision hydraulic blank rolling machine, wherein the thickness of the green coffee beans is controlled to be 0.3 +/-0.05 mm, and a compression roller continuously cools to ensure that the temperature is controlled below 60 ℃.
3. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: the pressure of the supercritical extraction kettle is 18 +/-1 MPa, the temperature is 50 +/-2 ℃, the pre-extraction time is 5 +/-0.5 hours, and the flow value of carbon dioxide is 8-16 times of the weight of the embryo piece; two separation kettles are used for two-stage separation and analysis, wherein the first-stage analysis pressure is 8 +/-1 MPa, and the second-stage analysis pressure is 5 +/-0.5 MPa.
4. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: the organic solvent A is high ethanol with the concentration of 80 +/-2 wt%, the extraction temperature is 40 +/-2 ℃, the ratio of materials to liquids is 1: 3-8, and the times are 4-6.
5. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: in the process of adding the organic solvent B for liquid-liquid extraction, stirring at a rotating speed of not less than 130rpm, and circulating by using a pump and an equipment bypass pipeline, wherein the circulating amount is 2-6 times of the volume of the equipment per hour; during the liquid-liquid extraction with the organic solvent C, the stirring speed was controlled at 130. + -.2 rpm.
6. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: when the proportion of the solvent B mixed and brought in the recycled solvent C exceeds 10 percent, rectifying the solvent C to reduce the proportion to be within 2 percent.
7. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: the gas phase temperature in the vacuum concentration process is 55 +/-3 ℃, and the vacuum degree is 0.08 +/-0.005 MPa.
8. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: the flow rate of the diluent on the column is 1.0 +/-0.2 BV/h, the organic solvent D is ethanol, the preparation concentration is 70 +/-5 wt%, and the flow rate is 1.2 +/-0.3 BV/h; the resin model is DM 700.
9. The industrial process for producing a green coffee bean extract according to claim 1, characterized in that: and (3) using pressure type spray drying equipment, controlling the solid content of the liquid to be sprayed to be 35 +/-5% before spraying, controlling the spraying pressure to be 6-12 MPa, and controlling the air outlet temperature to be 85 +/-5 ℃.
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|---|---|---|---|---|
| US4255461A (en) * | 1979-11-13 | 1981-03-10 | General Foods Corporation | Preparation of a decaffeinated roasted coffee blend |
| AU2007227384A1 (en) * | 2006-03-23 | 2007-09-27 | Herbalscience Singapore Pte. Ltd. | Extracts and methods comprising green tea species |
| CN105899222B (en) * | 2013-10-18 | 2020-04-14 | 晨光生物科技集团股份有限公司 | Green coffee bean extract and production method thereof |
| CN103977595B (en) * | 2014-05-23 | 2015-11-18 | 中国烟草总公司郑州烟草研究院 | A kind of method utilizing subcritical abstraction technology to reduce tobacco extract content of beary metal |
| CN105646428A (en) * | 2015-12-18 | 2016-06-08 | 安徽红星药业股份有限公司 | Tea polyphenol production process |
| US10893685B2 (en) * | 2016-10-26 | 2021-01-19 | Kao Corporation | Chlorogenic acid-containing composition manufacturing method |
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