CN101774989B - Method for extracting refined yellow pigment from red flowers - Google Patents
Method for extracting refined yellow pigment from red flowers Download PDFInfo
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- CN101774989B CN101774989B CN2009101132238A CN200910113223A CN101774989B CN 101774989 B CN101774989 B CN 101774989B CN 2009101132238 A CN2009101132238 A CN 2009101132238A CN 200910113223 A CN200910113223 A CN 200910113223A CN 101774989 B CN101774989 B CN 101774989B
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Abstract
The invention provides a preferable method for extracting refined yellow pigment from red flowers, which adopts the technology integration of extracting and refining, resin adsorption, nano filtration separation, outer circulating vacuum reduced pressure concentration and spray drying. The method is as follows: performing particles removing, ashing and sterilization on primary filtrate by a filter; adsorbing resin with large aperture by alcohol, wherein the upper prop adsorbing flow is 1-4BV/h, the adsorbing time is 1.5-2.0 hours, the eluting flow is 2-6BV/h, and the eluting time is 2.5-3.0 hours; collecting eluent, wherein the PH values of upper prop liquid medicine and cleanout fluid are 2-5; depredating macromolecules by a microfiltration membrane, wherein the control pressure is 0.1-0.2MPa, the temperature is 5DEG C higher than the room temperature or 5 DEG C lower than the room temperature; thickening and dewatering by a nanofiltration membrane, wherein the control pressure is 1-4MPa, the temperature is 20-50 DEG C, and the concentration multiplying power is 5-10 times; recycling the alcohol; and drying a material the solid content of which is 40%-60% to obtain the product, wherein the feed temperature is 60-80 DEG C, the entering air temperature is 160-190 DEG C. By implementing the preferable method, the extraction ratio of the yellow pigment reaches more than 80%, and the color value also reaches more than 150.
Description
Technical field
The present invention relates to the extraction of natural plant pigment, the especially extraction of pigment in the safflower, suitable a kind of especially optimum seeking method of from safflower, extracting refined yellow pigment.
Background technology
In recent years, the production development of China's natural pigment is very fast, and the regulation of forbidding using in " A level " green food various chemosynthesis pigments had just been made by government in 2002, has therefore greatly promoted the development in China natural pigment market.According to statistics, only the area of pigment capsicum, safflower, the Flower of Aztec Marigold of ground plantations such as northeast, Shandong, Shanxi and Xinjiang is up to surplus 80 ten thousand mu for China in 2005, and the annual production of natural pigment is only second to India also near 4000 tons.But because the factor of consumer cost, domestic deep processing and precision work to natural pigment is still deficient, and the present invention probes into this field.
The present bibliographical information that extracts of the carthamin yellow of roger: 1. people's " comprehensive extraction of carthamin yellow " method such as lift a sail of the college of traditional Chinese medicine of Xinjiang Medicine University is more suitable for carthamin yellow and extracts on a large scale; 2. land state power waits the people at Shanghai Agricultural College's journal 2000.18 (2)-85-90, and the thing of carrying of 100 " safflower edible flavochrome optimum extraction condition and the physico-chemical property researchs " delivered is a water colo(u)r; 3. the Xue Weiming of Northwest University etc. adopts cellulase to extract yellow pigment, and is better than traditional technology; The report of the separation and purification of the yellow pigment that the while document also relates to: 4. the bright Master's thesis of delivering of HeFei University of Technology's red legend " carthamin yellow extracts, makes with extra care and stability study " is clear and definite once more under acidic conditions, the stability techniques index of AB-8 type resin absorption; 5. the patent No. is that the resin chromatography that adopts of " a kind of extracting method of carthamin yellow " of CN2006100131234 and the technology of reverse osmosis concentration all have reasonableness, but by experimental comparison and detection repeatedly, thinks that still product has flaw.Problems such as long flow path, the energy consumption that exists in the present invention is directed to present carthamin yellow process study and developing is big, yield is low, the fractionation by adsorption of design is purified and is combined with concentrated the effective of technology of membrane sepn, through outer circulation vacuum concentration technology, spray-dired technology, the reasonableness that has proved technological line once more is with effective, and for the technological transformation of industry has increased scientific and technological content, this method is workable, cost is low, and DEVELOPMENT PROSPECT is wide.
Summary of the invention
The objective of the invention is to: a kind of optimum seeking method of from safflower, extracting refined yellow pigment that provides, the resin absorption that adopts is separated purification, membrane sepn concentrates, outer circulation vacuum concentration (recovered alcohol), spray-dired technology is integrated, has realized mutual supplement with each other's advantages, the extraction yield that makes carthamin yellow is more than 80%, the look valency of pigment is reached more than 150, reached energy-conservation, saved time, product fine purpose.
The object of the present invention is achieved like this: a kind of optimum seeking method of extracting refined yellow pigment from safflower, comprise that filigree is selected, filter is just mentioned in water logging, the refining employing resin absorption of its vat liquor, nanofiltration separation, outer circulation vacuum decompression concentrate, spray-dired step:
Filter is just mentioned in water logging: the filigree of lixiviate and the solid-to-liquid ratio of deionized water are 1: 8-12 times, soak time is 1.5-2.5 hour, and extraction temperature 25--50 ℃, extraction time 2-4 hour, the lixiviate number of times was 2-3 time; Filter just adopts tripodia strainer, plate filter to remove particulate, ash content and sterilization;
Resin absorption: macroporous resin need adopt alcohol-pickled 45-50 hour of 80-95%, clean clean alcohol with treating water then after, inject filtrate absorption just; The upper prop absorption flow is 1-4BV/h, and adsorption time is 1.5-2.0 hour; With the alcohol wash-out of 50-80%, the wash-out flow is 2-6BV/h, and elution time is 2.5-3.0 hour, collects the elutriant that is rich in carthamin yellow;
Nanofiltration separation: remove macromole with microfiltration membrane, controlling pressure is 0.1-0.2MPa, temperature be room temperature ± 5 ℃; Use the nanofiltration membrane thickening: controlling pressure is 1-4MPa, and temperature is 20-50 ℃, and concentration rate 5-10 doubly;
The outer circulation vacuum decompression concentrates: nanofiltration liquid concentrates through the outer circulation vacuum decompression, and temperature is 50-80 ℃, and vacuum tightness is 2-6Pa, recovered alcohol;
Spraying drying: solid content is implemented drying for the 40%-60% material, and feeding temperature is 60-80 ℃, and inlet temperature is 160-190 ℃, and air outlet temperature is 80-90 ℃.
Above-mentioned optimum seeking method, the higher primary school that selects resin column for use is in 150cm, blade diameter length ratio 1: 4-1: 6cm.
Above-mentioned optimum seeking method, the pH value of modulation upper prop soup and scavenging solution is 2-5.
Above-mentioned optimum seeking method, the tripodia strainer of employing are 100-120 order stainless steel filtering net.
Described optimum seeking method, removing molecular weight with membrane filtration is material more than 6000.
Described optimum seeking method adopts this method to extract yellow pigment, more than the extraction rate reached to 80%, the look valency of pigment is reached more than 150.
The technique effect of extraction refined yellow pigment optimum seeking method of the present invention:
Selection is an extraction solvent with water, has verified the best effect of lixiviate number of times and cost;
Select the macroporous adsorbent resin of HB, AB-8 type for use, verified that product impurity is few, the high and good best effect of analysis feature of extraction yield;
The selective membrane isolation technique replaces evaporation concentration, adopts ultra-filtration membrane to remove macromolecular substance, uses the nanofiltration thickening again, has verified that the pollution of film reduces, and guarantees the effect of the best of effective constituent and quality;
Select concentrated solution to adopt the outer circulation vacuum decompression to concentrate, verified and reduced spissated temperature, guarantee that effective constituent is never degenerated in the safflower, reduce the best effect of energy consumption;
The selection rate of drying is fast, and production process is polluted few spraying drying mode, has verified that product has not superheated best effect of good dispersiveness, solvability and product.
The refining experimental result of fractionation by adsorption of the present invention is as follows:
The influence of pH value:
Adopt macroporous resin, wet method dress post transfers PH 3.0 or 4.0 to cross post with the flow velocity of 4BV/h respectively then, the Fractional Collections effluent liquid respectively the pigment solution of 2mg/ml.
| The pH value of feed liquid | Effluent liquid (column volume) BV | Pigment content |
| 3.0 | 10 20 40 | 0.18 0.25 0.6 |
| 4.0 | 10 20 40 | 0.22 0.5 0.9 |
By last table gained, the pH value of solution, reduces with the increase of pH value by remarkably influenced pigment absorption.
The influence of absorption flow velocity:
Get Flos Carthami extract, transferring pH value is 3.0, and respectively with 2,4,6,8, effluent liquid is collected in the absorption of the flow velocity upper prop of 10BV/h, measures content, calculates retention rate.
| Upper prop absorption flow velocity (BV/h) | Pigment retention rate % |
| 2 | 95.5 |
| 4 | 95.1 |
| 6 | 91.2 |
| 8 | 85.5 |
| 10 | 73.8 |
By last table gained, comparatively suitable with the flow velocity of 4BV/h.
The influence of material loading amount:
The carthamin extracting solution is respectively with 250mg/g, 220mg/g, and sample on the 190mg/g resin is resolved with 60% ethanol, collects desorbed solution, calculates the yield of pigment.
| Material loading amount (mg/g) | Pigment yield (%) |
| 250 | 85.9 |
| 220 | 90.1 |
| 190 | 89.2 |
By last table gained, 220mg/g is more suitable for the material loading amount.
The selection of elution requirement:
Resolve with the flow velocity of 2BV/h with 15%, 30%, 60%, 80% ethanolic soln respectively, collect elutriant, measure pigment content, calculated yield.
| Elutriant (ethanol) | Pigment yield % |
| 15％ | 52 |
| 30％ | 86 |
| 60％ | 91.5 |
| 80％ | 83 |
By last table gained, when alcohol concn elutive power greater than 60% time the highest.
The purification with macroreticular resin method:
Resin dress post, blade diameter length ratio is 1: 8, and Flos Carthami extract is transferred PH3.0, material loading amount 220mg/g, material loading flow velocity 4BV/h, 60% ethanol is resolved with 2BV/h, collects desorbed solution, concentrating under reduced pressure or membrane concentration final vacuum drying, product yield and look valency result are as follows:
| Method | Pigment yield % | Solid substance look valency |
| Ethanol precipitation | 84.1 | 71.8 |
| Amberlyst process | 88.6 | 170 |
Technological design of the present invention had not both had waste gas, discharge of wastewater, do not have the generation of waste residue again, reached the environmental protection standard of GB138978-88 " sewage qualified discharge standard ", GB12348-49-90 " plant area circle of industrial enterprise noise strength standard ", TJ 36-79 " Design of Industrial Enterprises hygienic standard ".
Optimum seeking method is made with extra care in extraction of the present invention, has effectively solved solvent precipitation, the column chromatography of the water extraction, organic solvent extraction method and the Mierocrystalline cellulose enzyme process that adopt traditional technology and separation and purification process, the drawback of absorption method; Polymeric adsorbent fractionation by adsorption purification techniques, the concentrated technology of membrane sepn, outer circulation vacuum concentration technology, spray drying technology are applied to carthamin yellow production, make more than the extraction rate reached to 80% of carthamin yellow, the look valency of carthamin yellow is reached more than 150; This optimum seeking method integrated reached mutual supplement with each other's advantages, and large-scale production is energy-conservation, the timesaving goal of the invention, shows technical progress.
Embodiment
Embodiment 1
The solid-to-liquid ratio of safflower silk and deionized water is 1: 8 times during lixiviate, and soak time is 2.5 hours, 25 ℃ of extraction temperatures, and extraction time 2 hours, lixiviate number of times are 2 times; Filter just adopts 120 order stainless steel filtering nets just to filter, and filters by plate filter then, reaches the effect except that particulate, ash content, sterilization;
Selection HB type resin absorption need to adopt 80% alcohol-pickled 48 hours, after water cleans, injects filtrate just; Upper prop adsorption volume flow is 2BV/h, and adsorption time is 1.5 hours; Cleaning and elution volume flow are 4BV/h, and adsorption time is 2.5 hours, promptly gets yellow pigment; Upper prop soup and scavenging solution pH value are 3; Select the high 140cm of resin column for use, blade diameter length ratio 1: 5cm;
Nanofiltration separation: adopt microfiltration membrane to remove macromole, controlling pressure is 0.1MPa, temperature be room temperature ± 5 ℃; Use the nanofiltration membrane thickening: controlling pressure is 1MPa, and temperature is 20 ℃, 5 times of concentration rates;
The outer circulation vacuum decompression concentrates: nanofiltration liquid concentrates through the outer circulation vacuum decompression, and temperature is 50 ℃, and vacuum tightness is 2Pa, recovered alcohol;
Spraying drying: 40% solid content material is implemented drying, and feeding temperature is 60 ℃, and inlet temperature is 160 ℃, and air outlet temperature is 80 ℃; Obtain the yellow pigment product, extraction rate reached to 80% makes the look valency of pigment reach 150.
Embodiment 2
The solid-to-liquid ratio of safflower silk and deionized water is 1: 12 during lixiviate, soaks 50 ℃ of extraction temperatures, extraction time 2.5 hours 1.5 hours; The lixiviate number of times is 3 times; Filter just adopts 100 order stainless steel filtering nets just to filter, and filters by plate filter then, reaches the effect except that particulate, ash content, sterilization;
Selection HB type resin absorption need to adopt 90% alcohol-pickled 50 hours, after water cleans, injects filtrate just; Upper prop adsorption volume flow is 3BV/h, and adsorption time is 2.0 hours; Cleaning and elution volume flow are 5BV/h, and adsorption time is 2.8 hours, promptly gets yellow pigment; Upper prop soup and scavenging solution pH value are 4; Select the high 130cm of resin column for use, blade diameter length ratio 1: 6cm;
Nanofiltration separation: remove macromole with microfiltration membrane, controlling pressure is 0.2MPa, temperature be room temperature ± 5 ℃; Use the nanofiltration membrane thickening: controlling pressure is 4MPa, and temperature is 50 ℃, 10 times of concentration rates;
The outer circulation vacuum decompression concentrates: nanofiltration liquid concentrates through the outer circulation vacuum decompression, and temperature is 80 ℃, and vacuum tightness is 6Pa, recovered alcohol;
Spraying drying: 60% solid content material is implemented drying, and feeding temperature is 80 ℃, and inlet temperature is 190 ℃, and air outlet temperature is 90 ℃, obtains the yellow pigment product, and extraction rate reached to 95% makes the look valency of pigment reach 160.
Embodiment 3
The solid-to-liquid ratio of safflower silk and deionized water is 1: 10 times during lixiviate, and soak time is 2.0 hours, 40 ℃ of extraction temperatures, and extraction time 3 hours, lixiviate number of times are 2 times; Filter just adopts 110 order stainless steel filtering nets just to filter, and filters by plate filter then, reaches the effect except that particulate, ash content, sterilization;
The macroporous resin adsorption of selection AB-8 type also need adopt 95% alcohol-pickled 49 hours, after water cleans, injects filtrate just; Upper prop adsorption volume flow is 4BV/h, and adsorption time is 1.8 hours; Cleaning and elution volume flow are 6BV/h, and adsorption time is 2.8 hours, promptly gets yellow pigment; Upper prop soup and scavenging solution pH value are 4; The resin column of selecting for use is high to be 120cm, blade diameter length ratio 1: 6cm;
Nanofiltration separation: remove macromole with microfiltration membrane, controlling pressure is 0.15MPa, temperature be room temperature ± 5 ℃; Use the nanofiltration membrane thickening: controlling pressure is 2.5MPa, and temperature is 45 ℃, 7 times of concentration rates;
The outer circulation vacuum decompression concentrates: nanofiltration liquid concentrates through the outer circulation vacuum decompression, and temperature is 60 ℃, and vacuum tightness is 4Pa, recovered alcohol;
Spraying drying: 50% solid content material is implemented drying, and feeding temperature is 70 ℃, and inlet temperature is 175 ℃, and air outlet temperature is 85 ℃; Obtain the yellow pigment product, extraction rate reached to 90% makes the look valency of pigment reach 170.
Claims (4)
1. method of from safflower, extracting refined yellow pigment, it is characterized in that: comprise that filigree is selected, filter is just mentioned in water logging, the refining employing resin absorption of its vat liquor, nanofiltration separation, outer circulation vacuum decompression concentrate, spray-dired step:
Filter is just mentioned in water logging: the filigree of lixiviate and the solid-to-liquid ratio of deionized water are 1: 8-12, and soak time is 1.5-2.5 hour, extraction temperature 25--50 ℃, extraction time 2-4 hour, the lixiviate number of times was 2-3 time; Filter just adopts tripodia strainer, plate filter to remove particulate, ash content and sterilization, and wherein said tripodia strainer is a 100-120 order stainless steel filtering net;
Resin absorption: macroporous resin need adopt alcohol-pickled 45-50 hour of 80-95%, clean clean alcohol with treating water then after, inject filtrate absorption just; The upper prop absorption flow is 1-4BV/h, and adsorption time is 1.5-2.0 hour; With the alcohol wash-out of 50-80%, the wash-out flow is 2-6BV/h, and elution time is 2.5-3.0 hour, collects the elutriant that is rich in carthamin yellow;
Nanofiltration separation: remove macromole with microfiltration membrane, controlling pressure is 0.1-0.2MPa, temperature be room temperature ± 5 ℃; Use the nanofiltration membrane thickening: controlling pressure is 1-4MPa, and temperature is 20-50 ℃, and concentration rate 5-10 doubly;
The outer circulation vacuum decompression concentrates: nanofiltration liquid concentrates through the outer circulation vacuum decompression, and temperature is 50-80 ℃, and vacuum tightness is 2-6Pa, recovered alcohol;
Spraying drying: solid content is implemented drying for the 40%-60% material, and feeding temperature is 60-80 ℃, and inlet temperature is 160-190 ℃, and air outlet temperature is 80-90 ℃.
2. in accordance with the method for claim 1, it is characterized in that: the higher primary school that selects resin column for use is in 150cm, blade diameter length ratio 1: 4-1: 6.
3. it is characterized in that in accordance with the method for claim 1: the pH value of modulation upper prop soup and scavenging solution is 2-5.
4. it is characterized in that in accordance with the method for claim 1: removing molecular weight with membrane filtration is material more than 6000.
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| CN102584529A (en) * | 2011-12-28 | 2012-07-18 | 浙江赛特膜技术有限公司 | Alcohol recovering and concentrating process method of adsorption resin desorption solutions of plant extracts in membrane method |
| CN103478891B (en) * | 2013-09-11 | 2016-08-24 | 上海聚华科技股份有限公司 | The preparation method of Nicotiana tabacum L. pigment |
| CN108498550A (en) * | 2018-03-07 | 2018-09-07 | 浙江亚林生物科技股份有限公司 | The preparation method of uranidin in a kind of extraction pollen pini |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1307076A (en) * | 2000-01-21 | 2001-08-08 | 浙江大学 | Method for extracting natural edible pigment safflor yellow |
| CN1600817A (en) * | 2003-09-22 | 2005-03-30 | 浙江永宁制药厂 | Yellow pigment of safflower preparation method and application |
| CN101007828A (en) * | 2006-01-25 | 2007-08-01 | 天津天士力制药股份有限公司 | Process for extracting carthamus tinctorius yellow pigment |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1307076A (en) * | 2000-01-21 | 2001-08-08 | 浙江大学 | Method for extracting natural edible pigment safflor yellow |
| CN1600817A (en) * | 2003-09-22 | 2005-03-30 | 浙江永宁制药厂 | Yellow pigment of safflower preparation method and application |
| CN101007828A (en) * | 2006-01-25 | 2007-08-01 | 天津天士力制药股份有限公司 | Process for extracting carthamus tinctorius yellow pigment |
Non-Patent Citations (1)
| Title |
|---|
| 张浩勤等.红花黄、红花红色素提取新技术.《河南化工》.2006,第23卷(第2期),第5-7页. * |
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Effective date of registration: 20121225 Address after: 834800 the Xinjiang Uygur Autonomous Region Tacheng Yumin County District Road Patentee after: Xinjiang horngjaan characteristics of agricultural science and Technology Development Co. Ltd. Address before: 834800 the Xinjiang Uygur Autonomous Region Yumin County Baerlukelu No. 18 Patentee before: Wang Laizhong |
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