CN101712812A - Method and device for extracting fat-soluble natural pigment - Google Patents
Method and device for extracting fat-soluble natural pigment Download PDFInfo
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- CN101712812A CN101712812A CN200910095058A CN200910095058A CN101712812A CN 101712812 A CN101712812 A CN 101712812A CN 200910095058 A CN200910095058 A CN 200910095058A CN 200910095058 A CN200910095058 A CN 200910095058A CN 101712812 A CN101712812 A CN 101712812A
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Abstract
The invention provides a method and a device for extracting a fat-soluble natural pigment. The method comprises the following steps of: (1) performing pretreatment on a material, and then performing pressure reduction treatment on the treated material in an extraction container; (2) introducing a solvent into the extraction container to mix the solvent and the material, and extracting the mixture to obtain extract liquor; (3) putting the extract liquor into a vaporization separation device to separate out a crude extract of the fat-soluble natural pigment, and simultaneously separating the solvent, compressing and cooling the solvent, and then reclaiming the solvent for cyclic utilization; and (4) putting the crude extract of the fat-soluble natural pigment into a refining system to perform refining treatment to prepare a refined extract. The extraction device comprises an extraction separation system, the refining system, a solvent purification system, a vacuum system and a heat exchange system. The method and the device can improve the oxidation resistance and the stability of a product, and ensure the biological and chemical activities of the extracts; the product has pure and stable colors; the extraction rate is high; the solvent residue is low; the product has no peculiar smells; and the solvent is easy to reclaim for cyclic utilization.
Description
Technical field
The invention belongs to the fine chemical technology field, be specifically related to a kind of method and apparatus that extracts fat-soluble natural pigment.
Background technology
At present, Chang Yong natural food colour preparation method has solvent-extraction process, enzyme reaction method, supercritical extraction and microwave extraction method.Enzyme reaction method mild condition, low temperature, neutrality, but research is not deep enough.The supercritical extraction energy consumption is low, product purity is high, but is subjected to solvent polarity restriction, facility investment big.Microwave extraction method extracts weak point consuming time, solvent load is few, cost is low, but range of application is limited relatively.Traditional solvent-extraction process equipment is simple, application is general, but has the problem that energy consumption is big, quality product is relatively poor.
Application number is that 90108660.6 Chinese patent discloses a kind of grease and leaches production technique.It adopts liquefied petroleum gas (LPG) as leaching solvent, leaches the grease in the oil plant at normal temperatures.This method is brought peculiar smell into easily owing to use liquefied petroleum gas (LPG) to make solvent, influences product quality.
Application number is that 200780024591.4 Chinese patent application discloses a kind of method that obtains to contain the lipid of high unsaturated fatty acid with liquid dimethyl ether from plant or animal material, this method comprises makes described material contact liquid dimethyl ether to obtain containing dme solution and the plant or the animal material residue of lipid, solution is separated with plant or animal material residue, and use near critical carbonic acid gas and from extraction solution, reclaim lipid, from solution, reclaim lipid.And bigger near critical carbonic acid gas to the dissolving power difference of different substances, with polarity, boiling point and the relative molecular mass of material close pass is arranged.At present, the equipment scale of China's supercritical extraction is less relatively, production cost is higher, generally is used for the added value high product.For the bigger colored class of volume, leaf class medicinal material, adopt the jar of small volume to extract economical inadequately.
Application number is that the Chinese patent application of 200610048835.X discloses the greasy method of a kind of extraction, and this method may further comprise the steps: 1) material is crushed to 10～40 orders; 2) adopting liquid dimethyl ether is extraction solvent, press material: in the weight ratio feeding material of solvent=1: 2～1: 24, be 5～30 kilograms at pressure, extraction temperature is under 30～90 ℃ the condition, to extract 30～120 minutes; 3) be 1～5 kilogram at pressure, temperature is under 20～60 ℃ the condition, to isolate grease.This method only is confined to the oil cake after squeezing, and to equipment requirement of withstand voltage height.
In sum, traditional extraction fat-soluble natural pigment method mainly has the following disadvantages: 1) extraction conditions is harsh relatively, and there are notable difference in the quality of goods, stability and natural material; 2) product extraction yield, extraction selectivity differ greatly, and solvent-oil ratio is big; 3) solvent remains in the extract easily, if solvent is impure then can to bring peculiar smell, influences product quality; 4) equipment requirement of withstand voltage height or investment, energy consumption are higher.
Summary of the invention
The objective of the invention is to overcome the deficiency of traditional method, provide a kind of extraction conditions gentle relatively, can improve goods oxidation-resistance, stability, guarantee the biological and chemical activity of extract, combinations color and lustre is just stablized, the extraction yield height, dissolvent residual is low, the goods free from extraneous odour, and solvent is easy to the method for the extraction fat-soluble natural pigment of recycle and reuse, and the present invention also provides the equipment that extracts fat-soluble natural pigment.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of extracting fat-soluble natural pigment may further comprise the steps:
1) material is carried out pre-treatment, in extraction container, the material after handling is carried out reduced pressure treatment then;
2) solvent being fed in the extraction container and mixing of materials, is 20 ℃～60 ℃ in temperature, extracts under the processing condition of pressure 0.4MPa～1.3MPa, obtains extraction liquid;
3) extraction liquid being sent into the vaporization tripping device, is that 20 ℃～60 ℃, pressure are to isolate the fat-soluble natural pigment primary extract under the condition of 0.1MPa～0.2MPa in temperature, and simultaneously with separated from solvent, recycling is reclaimed in compressed, cooling back;
4) the fat-soluble natural pigment primary extract being sent into refining system, is 20 ℃～70 ℃ in temperature, and pressure is to be lower than refinement treatment under the condition of 0.06MPa, makes extract.
The described pre-treatment of step 1) of the present invention is sieving and grading, fermentation, drying, one or more the combination of treatment process in small, broken bits; When material being carried out when in small, broken bits, the raw meal particle size after then in small, broken bits is no more than 15.00mm; Material pressure of living in is not higher than 0.076MPa during described reduced pressure treatment.Step 2) material that is mixed into of described material and solvent: solvent mixes by weight 1: 2～20, extracts 1～16h then.Adopt forced refluence or stirring or microwave auxiliary extraction method in the extraction process.The described solvent of step 3) is a dme.The described solvent of step 3) also can be the mixture of dme and extraction auxiliary agent, and wherein, the shared weight percent of extraction auxiliary agent is no more than 20%.Described extraction auxiliary agent is a kind of in 0.5%～2% citric acid, phenylformic acid, oxysuccinic acid, the aqueous hydrochloric acid; Perhaps be 85%～95% ethanol; Or a kind of and 85%～95% alcoholic acid mixture in 0.5%～2% citric acid, phenylformic acid, oxysuccinic acid, aqueous hydrochloric acid; Wherein 0.5%～2% citric acid or phenylformic acid or oxysuccinic acid or the aqueous hydrochloric acid weight percent in solvent is no more than 5%; The weight percent of 85%～95% ethanol in solvent mixture is no more than 20%.Raw material of the present invention is meant plant or plant fermentation thing or the single-cell algae quasi-microorganism that contains fat-soluble natural pigment; Wherein, plant comprise root, stem, leaf, flower, really, in the seed one or more contain the position of fat-soluble natural pigment.The described solvent recovery cycle utilization of step 3) of the present invention can recycle more than 8 times at the solvent with a kind of materials abstraction; When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.The present invention is material and solvent, extract and isolate the natural pigment primary extract 2～3 times through circulating after, the primary extract that obtains for 2～3 times can be carried out refinement treatment in the lump.
The present invention also provides a kind of equipment that extracts fat-soluble natural pigment, and this equipment comprises extracting and separating system, refining system, solvent purification system, vacuum system and heat-exchange system; The extracting and separating system comprises by the extraction kettle of pipeline connection and vaporization tripping device; The solvent purification system comprises by the dme washing device of pipeline connection and dme adsorption and purification device, the dme washing device is communicated with the vaporization tripping device by pipeline, and dme adsorption and purification device is communicated with vaporization tripping device and gaseous state solvent surge tank respectively by pipeline; Refining system is communicated with vaporization tripping device and dme adsorption and purification device respectively by pipeline; Vacuum system is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises dme storage tank, first interchanger and second interchanger, first interchanger, one end is communicated with the dme storage tank, the other end is communicated with dme adsorption and purification device, and second interchanger, one end is communicated with extraction kettle, and the other end is communicated with the dme storage tank.
Solvent purification of the present invention system also comprises gaseous solvent surge tank and the compressor by pipeline connection, the gaseous solvent surge tank is communicated with dme adsorption and purification device, compressor is the oil free compressor that has filtering and purifying, and is communicated with first interchanger.
The invention has the beneficial effects as follows: 1. extraction conditions is gentle relatively, improves goods oxidation-resistance, stability, guarantees biology, the chemically reactive of extract, keep the product of goods have color and luster just, characteristic such as stable, pure natural.2. product extraction yield height; Extraction selectivity is good.3. compare extract free from extraneous odour and residual with conventional solvent sherwood oil, butane, propane, 6# solvent, ethyl acetate, acetone etc.4. the dme production cost is low, and is easy to be recycled, environmental friendliness, and production cost is low, is easy to industrialization, and solvent loss is little, and facility investment, energy consumption reduce.
Further set forth content of the present invention below in conjunction with Figure of description.
Description of drawings
Fig. 1 is the synoptic diagram that the present invention extracts equipment.
Among the figure, 1-dme storage tank, 2-first valve, the 3-volume pump, 4-second interchanger, 5-second valve, the 6-vacuum system, 7-the 3rd valve, 8-the 4th valve, the 9-extraction kettle, 10-solvent cycle hydrocarbon pump, 11-the 5th valve, 12-the 6th valve, 13-reducing valve, 14-the 7th valve, 15-the 8th valve, the 16-tripping device of vaporizing, 17-dme washing device, 18-dme adsorption and purification device, 19-the 9th valve, 20-first interchanger, 21-compressor, 22-gaseous solvent surge tank, the 23-refining system, 24-the tenth valve.
Embodiment
As shown in the figure, extraction equipment of the present invention mainly comprises extracting and separating system, refining system 23, solvent purification system, vacuum system 6 and heat-exchange system; The extracting and separating system comprises by the extraction kettle 9 of pipeline connection and vaporization tripping device 16; The solvent purification system comprises by the dme washing device 17 of pipeline connection and dme adsorption and purification device 18, dme washing device 17 is communicated with vaporization tripping device 16 by pipeline, and dme adsorption and purification device 18 is communicated with vaporization tripping device 16 and gaseous state solvent surge tank 22 respectively by pipeline; Refining system 23 is communicated with vaporization tripping device 16 and dme adsorption and purification device 18 respectively by pipeline; Vacuum system 6 is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises that dme storage tank 1, first interchanger 20 and second interchanger, 4, the first interchanger, 20 1 ends are communicated with dme storage tank 1, and the other end is communicated with gaseous solvent surge tank 22 by compressor 21; Second interchanger, 4 one ends are communicated with extraction kettle 9, and the other end is communicated with dme storage tank 1 by volume pump 3.The extracting and separating system can adopt pot group type, extraction kettle 2～16 (cover), vaporization tripping device 1～4 (cover), dme washing device 2～4 (cover), 2～6 in dme adsorption and purification devices (cover) are set as required, compressor should adopt oil free compressor or the compressor unit that has filtration unit, configuration 1～4 on compressor (group).Extraction solvent used in the present invention belongs to inflammable, explosive material, can move the vacuum system that needs setting can be simultaneously vacuumizes total system or individual equipment according to equipment.
The extraction process flow process is as follows:
1) will be in the raw material of pre-treatment be packed extraction kettle 9 into, close first valve 2, the 9th valve 19, starting 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline vacuumizes, in extraction container the material after handling is carried out reduced pressure treatment then, material pressure of living in is not higher than 0.076MPa during reduced pressure treatment.
2) close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent is fed extraction kettle 9 by required raw material and weight of solvent ratio, closing second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, is 20 ℃～60 ℃ in temperature, carry out extracting operation under the processing condition of pressure 0.4MPa～1.3MPa, obtain extraction liquid.
3) be extracted to required time after, open the 6th valve 12, the 9th valve 19 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting the vaporization separation temperature and be 20 ℃～60 ℃, pressure is 0.1MPa～0.2MPa, and liquid is isolated the fat-soluble natural pigment primary extract through vaporization tripping device 16.One batch raw material is repeated 2～3 extractions successively and separates, and gradation obtains the fat-soluble natural pigment primary extract.Simultaneously, the solvent gas feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back in the dme storage tank 1 and is reclaimed solvent, and recirculation is used; But after solvent cycle is used 6 times, need close the 8th valve 15, open the 7th valve 14, will feed dme washing device 17 and dme adsorption and purification device 18 washing and purifying successively through the isolating gas of dimethyl ether of vaporizing, enter gaseous solvent surge tank 22 then, finish the recovery solvent.At solvent, only need to replenish a small amount of fresh solvent and extract auxiliary agent promptly to can be recycled more than 8 times with a kind of materials abstraction.When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.
4) opening the tenth valve 24, the fat-soluble natural pigment primary extract that is enriched in vaporization tripping device 16 is fed refining systems 23 through the tenth valve 24, is 20 ℃～70 ℃ in temperature, and pressure is to be lower than refinement treatment under the condition of 0.06MPa, makes extract.From extraction kettle 9, take out extract remainder then.
The heat transferring medium that uses in the heat-exchange system is generally 0 ℃～90 ℃ deionized waters, if extraction kettle 9 service temperatures, should dispose refrigerator and the suitable refrigeration agent of configuration less than 0 ℃, second interchanger 4 and extraction kettle 9 is forced cooling.
Separation system, refining system 23, solvent purification system, vacuum system 6 and heat-exchange system etc. are adopted in the present device stand-alone device and parts all can adopt prior art, only need these stand-alone device and parts are assembled by the present invention to get final product.
Embodiment 1: Capsorubin extracts
Capsicum is dried under 120 ℃ of temperature, make water content below 10%, pulverize and sieving and grading, grinding particle size control size is 0.2mm～5mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.07MPa; Close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, solvent (all being dme) is pressed material fed extraction kettle 9 than 1: 10 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 55 ℃～60 ℃ of 1.2MPa～1.3MPa and extraction temperature, forced refluence extraction 4h opens the 6th valve 12, reducing valve 13, and extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 55 ℃～60 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment crude extract under the condition of 0.2MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 5 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 65 ℃～70 ℃, pressure are the refining extract that obtains under the condition of 0.05MPa in temperature.Primary extract be material heavy 10.5%, the extract of making accounts for 97% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 2: natural alkannin extracts
With Asian puccoon drying, chopping, in small, broken bits and screening, control size is at 0.83mm～1.5mm, in the extraction kettle 9 of packing into then, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.06MPa; Close the 3rd valve 7, the 4th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, (wherein dme is 80 parts with solvent, 20 parts of 85% ethanol) press material and fed extraction kettle 9 than 1: 20 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 20 ℃～25 ℃ of 0.4MPa～0.5MPa and extraction temperature, forced refluence extraction 16h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 20 ℃～25 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.15MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 4 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 20 ℃～25 ℃, pressure are the refining extract that obtains under the condition of 0.04MPa in temperature.Primary extract be material heavy 6.0%, the extract of making accounts for 96% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 3: the peel of Citrus reticulata Blanco yellow pigment extracts
With fresh peel of Citrus reticulata Blanco, the peel of Citrus reticulata Blanco of carrying essential oil or dried peel of Citrus reticulata Blanco, it is rotten to require nothing to go mouldy, clean with the clear water Rapid Cleaning, is cut into 3～15mm fine grained chippings.Pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.076MPa; Close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, (wherein dme is 85 parts, 3 parts of 0.5～2% citric acids with solvent; 12 parts of 90% ethanol) press material and fed extraction kettle 9 than 1: 10 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 40 ℃～45 ℃ of 0.8MPa～0.9MPa and extraction temperature, forced refluence extraction 8h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 40 ℃～45 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.10MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 3 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 40 ℃～45 ℃, pressure are the refining extract that obtains under the condition of 0.02MPa in temperature.Primary extract be material heavy 3.5%, the extract of making accounts for 97% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 4: Lyeopene extracts in the tomato skin
Tomato seed, centrifuge dehydration are gone in the eccysis of tomato skin raw water, in the extraction kettle 9 of packing into then, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.05MPa; Close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, (wherein dme is 96 parts with solvent, 4 parts of 2% oxysuccinic acid) press material and fed extraction kettle 9 than 1: 6 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 35 ℃～40 ℃ of 0.75MPa～0.gMPa and extraction temperature, behind the forced refluence extraction 1.5h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 35 ℃～40 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.20MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 8 times.Should emphasize especially after solvent cycle is used 6 times, gas of dimethyl ether is fed after dme washing device 17 washs, feed dme adsorption and purification device 18 purifying again, carry out solvent recuperation after entering gaseous solvent surge tank 22 then.After finishing above-mentioned extracting operation 3 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 35 ℃～40 ℃, pressure are the refining extract that obtains under the condition of 0.03MPa in temperature.Primary extract be material heavy 6.5%, the extract of making accounts for 95% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 5: wolfberry pigment extracts
The dried fruit of lycium barbarum drying and crushing to 0.25mm～0.40mm, in the extraction kettle 9 of packing into then, is closed first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.07MPa; Close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, (wherein dme is 90 parts, 3 parts in 0.5% phenylformic acid with solvent; 7 parts of 95% ethanol) press material and fed extraction kettle 9 than 1: 12 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 45 ℃～50 ℃ of 0.90MPa～1.00MPa and extraction temperature, behind the forced refluence extraction 1h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 45 ℃～50 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.20MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 5 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 50 ℃～55 ℃, pressure are the refining extract that obtains under the condition of 0.05MPa in temperature.Primary extract be material heavy 8.5%, the extract of making accounts for 96% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 6: the sea-buckthorn fat-soluble pigment extracts
Smash the sea-buckthorn tissue to pieces 5min, in the extraction kettle 9 of packing into then, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.05MPa; Close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, (wherein dme is 95 parts with solvent, 5 parts of 2% hydrochloric acid) press material and fed extraction kettle 9 than 1: 10 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 25 ℃～25 ℃ of 0.4MPa～0.5MPa and extraction temperature, behind the forced refluence extraction 2h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 25 ℃～25 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.15MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 5 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 25 ℃～25 ℃, pressure are the refining extract that obtains under the condition of 0.03MPa in temperature.Primary extract be material heavy 6.0%, the extract of making accounts for 97% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 7: salt algae carotene extracts
Salt algae (Dunaliella) belongs to volvocales (Volvocales) in classification a kind ofly lacks the unicellular of polysaccharide cell walls, and two flagellum green algas are collected frond with algae liquid through centrifugation.Pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.07MPa; Close the 3rd valve the 7, the 6 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, dme is pressed material: the dme weight ratio feeds extraction kettle 9 at 1: 2, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 40 ℃～45 ℃ of 0.8MPa～0.9MPa and extraction temperature, behind the forced refluence extraction 8h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 40 ℃～45 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.2MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 5 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 40 ℃～45 ℃, pressure are the refining extract that obtains under the condition of 0.02MPa in temperature.Primary extract be material heavy 3.4%, the extract of making accounts for 97% of crude extract weight.From extraction kettle 9, take out extract remainder.
Embodiment 8: extract xenthophylls from marigold flower
Will be through Flower of Aztec Marigold drying, pulverizing and the sieving and grading of fermentation, the control size is at 0.42mm～1mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline and be evacuated to 0.06MPa; Close the 3rd valve the 7, the 6 12, reducing valve 13, open first valve 2, material is carried out reduced pressure treatment.Start volume pump 3, dme is pressed material: the dme weight ratio feeds extraction kettle 9 at 1: 10, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 35 ℃～40 ℃ of 0.75MPa～0.8MPa and extraction temperature, behind the forced refluence extraction 2h, open the 6th valve 12, reducing valve 13, extraction liquid enters into vaporization tripping device 16; Closing the 7th valve 14, open the 8th valve 15, adjust vaporization separation temperature and pressure, is that 35 ℃～40 ℃, pressure are to isolate gas of dimethyl ether and fat-soluble natural pigment primary extract under the condition of 0.1MPa in temperature; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 4 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the fat-soluble natural pigment primary extract of vaporization tripping device 16 bottoms, feeding refining systems through the tenth valve 24 is that 35 ℃～40 ℃, pressure are not more than the refining extract that obtains under the condition of 0.06MPa in temperature.Primary extract be material heavy 8%, the extract of making accounts for 95% of crude extract weight.From extraction kettle 9, take out extract remainder.
Claims (12)
1. a method of extracting fat-soluble natural pigment is characterized in that, may further comprise the steps:
1), in extraction container, the material after handling is carried out reduced pressure treatment then with the material pre-treatment;
2) solvent being fed in the extraction container and mixing of materials, is 20 ℃～60 ℃ in temperature, extracts under the processing condition of pressure 0.4MPa～1.3MPa, obtains extraction liquid;
3) extraction liquid being sent into the vaporization tripping device, is that 20 ℃～60 ℃, pressure are to isolate the fat-soluble natural pigment primary extract under the condition of 0.1MPa～0.2MPa in temperature, and simultaneously with separated from solvent, recycling is reclaimed in compressed, cooling back;
4) the fat-soluble natural pigment primary extract being sent into refining system, is 20 ℃～70 ℃ in temperature, and pressure is to be lower than refinement treatment under the condition of 0.06MPa, makes extract.
2. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that, the described pre-treatment of step 1) is sieving and grading, fermentation, drying, one or more the combination of treatment process in small, broken bits; When material being carried out when in small, broken bits, the raw meal particle size after then in small, broken bits is no more than 15.00mm; Material pressure of living in is not higher than 0.076MPa during described reduced pressure treatment.
3. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that step 2) material that is mixed into of described material and solvent: solvent mixes by weight 1: 2～20, extracts 1～16h then.
4. as the method for claim 1 or 3 described extraction fat-soluble natural pigments, it is characterized in that, adopt forced refluence or stirring or microwave auxiliary extraction method in the extraction process.
5. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that, the described solvent of step 3) is a dme.
6. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that, the described solvent of step 3) is the mixture of dme and extraction auxiliary agent, and wherein, the shared weight percent of extraction auxiliary agent is no more than 20%.
7. the method for extraction fat-soluble natural pigment as claimed in claim 6 is characterized in that, described extraction auxiliary agent is
0.5%～
20%A kind of in citric acid, phenylformic acid, oxysuccinic acid, the aqueous hydrochloric acid; Perhaps be 85%～95% ethanol; Or a kind of and 85%～95% alcoholic acid mixture in 0.5%～2% citric acid, phenylformic acid, oxysuccinic acid, aqueous hydrochloric acid; Wherein 0.5%～2% citric acid or phenylformic acid or oxysuccinic acid or the aqueous hydrochloric acid weight percent in solvent is no more than 5%; The weight percent of 85%～95% ethanol in solvent mixture is no more than 20%.
8. as the method for claim 1 or 2 or 3 described extraction fat-soluble natural pigments, it is characterized in that described raw material is meant plant or plant fermentation thing or the single-cell algae quasi-microorganism that contains fat-soluble natural pigment; Wherein, plant comprise root, stem, leaf, flower, really, in the seed one or more contain the position of fat-soluble natural pigment.
9. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that, the described solvent recovery cycle utilization of step 3) can recycle more than 8 times at the solvent with a kind of materials abstraction; When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.
10. the method for extraction fat-soluble natural pigment as claimed in claim 1 is characterized in that, with material and solvent, extract and isolate the natural pigment primary extract 2～3 times through circulating after, the primary extract that obtains for 2～3 times is carried out refinement treatment in the lump.
11. an equipment that extracts fat-soluble natural pigment is characterized in that, this equipment comprises extracting and separating system, refining system (23), solvent purification system, vacuum system (6) and heat-exchange system; The extracting and separating system comprises extraction kettle (9) and the vaporization tripping device (16) by pipeline connection; The solvent purification system comprises by the dme washing device (17) of pipeline connection and dme adsorption and purification device (18), dme washing device (17) is communicated with vaporization tripping device (16) by pipeline, and dme adsorption and purification device (18) is communicated with vaporization tripping device (16) and gaseous state solvent surge tank (22) respectively by pipeline; Refining system (23) is communicated with vaporization tripping device (16) and dme adsorption and purification device (18) respectively by pipeline; Vacuum system (6) is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises dme storage tank (1), first interchanger (20) and second interchanger (4), first interchanger (20) one ends are communicated with dme storage tank (1), the other end is communicated with dme adsorption and purification device (18), second interchanger (4) one ends are communicated with extraction kettle (9), and the other end is communicated with dme storage tank (1).
12. a kind of equipment that extracts fat-soluble natural pigment as claimed in claim 11, it is characterized in that, described solvent purification system also comprises gaseous solvent surge tank (22) and the compressor (21) by pipeline connection, gaseous solvent surge tank (22) is communicated with dme adsorption and purification device (18), compressor (21) is the oil free compressor that has filtering and purifying, and is communicated with first interchanger (20).
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| CN200910095058A CN101712812A (en) | 2009-10-15 | 2009-10-15 | Method and device for extracting fat-soluble natural pigment |
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