CN1807516A - Method for extracting purple yam red colouring matter using membrane separation method - Google Patents
Method for extracting purple yam red colouring matter using membrane separation method Download PDFInfo
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- CN1807516A CN1807516A CN 200610010637 CN200610010637A CN1807516A CN 1807516 A CN1807516 A CN 1807516A CN 200610010637 CN200610010637 CN 200610010637 CN 200610010637 A CN200610010637 A CN 200610010637A CN 1807516 A CN1807516 A CN 1807516A
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Abstract
This invention is related to a kind of method for barrier separation extrating red colouring matter from sweet potato. It extrat red colouring matter solution from acidificated solution of the purple sweet potato's root tuber and other organs, segregation with purify multi-stage separation film and remove impurities to get concentrating liquid end product. The raw materials used in this invention has extensive source and can be operated at normal temperatureits energy consumption is little and has no hazardous or harmful solvent; it is non-polluted, healthy and safe, low cost; extrating recovery ratio of colouring matter is high, which is up to more than 80%. The stability of colouring matter is good, and the tone of the product is high; the secial resource purple sweet potato can be used to prepare newly drug, daily chemical industry and food stain.
Description
Technical field
The present invention relates to a kind of method of extracting purple yam red colouring matter using membrane separation.
Background technology
Pigment is to be widely used in industry staple products such as medicine industry, food-processing, cosmetics production, but the chemical pigment of producing for synthetic mostly.Now constantly find many kinds in the synthetic colour, human body is had very serious toxic, have many synthetic food colors also human body to be had carinogenicity.Countries in the world are developed country especially, many synthetic colours is deleted from the pigment list of permission to use.In the world wide, originally allow the synthetic food color add in food, existing about 70% is disabled, and the synthetic colour that in May, 1978 promulgation of China Ministry of Health allows to use is only looked for red, carmine, lemon yellow and indigo etc. four kinds of dish, and the use of all limiting the quantity of.Given this plant situation, people have generally recovered the interest to natural pigment, and research, produce, use with farm crop and fruit vegetables natural pigment as raw material, be the emphasis of pigment industry.Often there is the specialized conference discussion world and introduces natural pigment, and carotene wherein, flavonoid, cyanin etc. all have the monograph introduction, and pigment uses and big producing country Japan has also published " natural coloring mattes handbook.In 20 end of the centurys, in developed country, the self colour of U.S.'s permission to use have 29 kinds, and the edible natural pigment of the European Community and Britain permission is respectively 26 and 28 kind.And the maximum country of edible natural pigment kind---Japan in the world, the natural pigment kind of having taken in the foodstuff additive catalogue is 98 kinds.This shows, use natural pigment, has been the emphasis that present world medicine, food, daily-use chemical industry etc. need a large amount of color additive industries.
China is over nearly more than 20 years, work out seven, the edible natural pigment in 80 kind of different material source, the edible natural pigment that allows in " State Standard of the People's Republic of China GB2760-1996 " to use has 48 kinds, as radish red, tomato red, capsanthin and maize etc.But because former thereby very difficult large-scale productions such as resource is few, traditional production technique extraction cost height.
Traditional pigment extraction process adopts old technologies such as lixiviate, evaporation concentration, solvent purification more, has problems such as energy consumption height, the solvent recuperation difficulty is big, production process is complicated, pigment is destroyed, product purity is low.
Summary of the invention
The object of the present invention is to provide a kind of method of extracting purple yam red colouring matter using membrane separation, this method adopts economical, advanced, safe and effective membrane separation technique technology, from Rhizoma Dioscoreae esculentae, extract edible haematochrome, so that make full use of the peculiar resource of Rhizoma Dioscoreae esculentae, produce novel medicinal, daily use chemicals are industrial and the food tinting material, for new way is opened up in purple sweet potato haematochrome production.
The object of the present invention is achieved like this: the piece root of Rhizoma Dioscoreae esculentae and other each organs extract haematochrome solution through souring soln, use the stage trapping membrane separation purification, remove impurity, obtain concentrated solution.
With bright potato is example, and soak solution is the acidizing fluid of water.
Light violet potato washes its surperficial earth, rejects disease and pest qualitative change part, with machine or manual method thinly slice, filament or fritter.Being immersed in temperature in the ratio that was not less than 1: 8 is in 20～40 ℃ the acidizing fluid, concentration is in 5% the aqueous citric acid solution, soak after 1.5 hours, the solution that pumping is soaked filters through pressure filter, the elimination particulate contamination, through the hyperfiltration membrane assembly pre-treatment, enter the thermopnore ion exchange tower, the absorption major part can be to the water-soluble impurity of nanofiltration membrane and reverse osmosis membrane formation contamination and plugging, and then be pumped into nanofiltration membrane component, remove the impurity of molecular weight, the solution of purifying haematochrome less than the haematochrome molecular weight, separate the acid solution that obtains, reuse is soaked, and separates the haematochrome solution that obtains, and concentrates through reverse osmosis membrane assembly, can obtain pigment content at the dope product more than 80%, after adjusting pH value to 3, promptly can be used as additive and use.After dope is adjusted pH value to 3, can obtain the dry powder finished product of haematochrome with corresponding drying process.
If the dry product with Rhizoma Dioscoreae esculentae is made raw material, when the making potato is done, require the nature sun to tan by the sun and surpass four hours time of drying, in order to avoid the pigment loss is too much.
Three kinds of main technical process in the technical scheme of the present invention, the corresponding product that obtains look valency different stage, best with the quality product that technical process one obtains, the extraction yield of pigment can reach more than 80%.
One of main technical process is: Rhizoma Dioscoreae esculentae, clean and crush, acidizing fluid soaks, filtering under pressure, filtrate is through ultrafiltration membrane treatment, the cation-adsorption impurity elimination, the filter membrane separation and purification, reverse osmosis membrane concentrates, behind the adjust pH the concentrated solution finished product.Concentrated solution also can be made the dry powder finished product by the adjust pH after drying.
Two of main technical process is: light violet potato or dried purple potato, clean and crush, and acidizing fluid soaks, filtering under pressure, the cation-adsorption impurity elimination, the nanofiltration membrane separation purifying, reverse osmosis membrane concentrates, and the adjust pH after drying obtains the dry powder finished product.
Three of main technical process is: light violet potato or dried purple potato, clean and crush, and acidizing fluid soaks, filtering under pressure, the cation-adsorption impurity elimination, the nanofiltration membrane separation purifying gets the concentrated solution finished product behind the adjust pH.
Assisting workflows are: potato slag behind the filtering under pressure, and acidizing fluid soaks for the second time, filtering under pressure, filtrate enters main technical process back segment recited above through the ultra-filtration membrane pre-treatment.
Three kinds of main technique flow processs recited above can obtain the pigment solution product of three kinds of grades, can adapt to various other other product needed of different class level.
In described method, acidizing fluid refers to citric acid or the synthetic aqueous solution of alimentary acetic acid or ethanolic soln, immersion refers to souring soln under 20 ℃～40 ℃ temperature condition, soaked 1.5 hours～2 hours, potato slag behind the filtering under pressure still needs uniform temp and time when soaking for the second time for the first time.
In the described method, the various membrane modules of employing are organic materials or inorganic materials is made.
In the described method, the ultra-filtration membrane aperture of employing is 0.01 micron～0.2 micron, and the nanofiltration membrane aperture is 2 nanometers～10 nanometers; The aperture of reverse osmosis membrane is less than 1 nanometer.Ultrafiltration and nanofiltration system operating pressure are 0.3～1.6MPa, and the operating pressure of reverse osmosis membrane is 1.8～3.5MPa.
In the described method, adopt resin cation (R.C.) absorption, should have the resin regeneration flow process.
In the described method, when acidizing fluid was the aqueous solution, configuration proportion was by weight: 3%～6%, and the ratio with 5% is comparatively suitable, and when acidizing fluid was ethanolic soln, configuration proportion is 0.6%～0.8% by weight, and was comparatively suitable with 0.6%.Transferring the pigment solution pH value is with edible soda ash (Na
2CO
3) or sodium hydroxide (NaOH), modulation solution pH value is between 2～3.Residue after purple sweet potato haematochrome extracts can be used for starch and extracts other products productions such as alcohol making, carries out comprehensive development and utilization, improves the comprehensive benefit that pigment is produced.
Rhizoma Dioscoreae esculentae is the peculiar variety type of sweet potato.Because of containing haematochrome, its yellowish pink is purplish red, and beautiful appearance is tempting, also because of containing haematochrome, makes it become a kind of important natural pigment source.The contained pigment of Rhizoma Dioscoreae esculentae belongs to anthocyanin class pigment, this pigment that is present in the cell vacuole, and its main component is Cyanidin and peonidin.It can be that bright potato also can be siccatives such as potato dry plate that technical scheme of the present invention adopts the Rhizoma Dioscoreae esculentae raw material, must not change technology because of bright potato material of employing or dried potato material.Except piece root from sweet potato, the pigment that other organs such as its stem, leaf contain, also available technical solution of the present invention is extracted pigment wherein.Therefore its raw material sources of technology of the present invention are extensive, and the most of areas of China all are fit to the sweet potato plantation, and area is big, the output height.At home, the beginning of the eighties, China introduced " mountains and rivers purple " and " purple rugose rose " waits some Rhizoma Dioscoreae esculentae germplasms, through improvement for many years, had now selected the higher Rhizoma Dioscoreae esculentae new lines of many output, can satisfy industrialization and extract the sweet potato haematochrome requirement.Mainly contain Rhizoma Dioscoreae esculentae No. 18, No. 135, wide potato, No. 4, peaceful potato.For the extraction pigment, " mountains and rivers purple ", " American Black potato " two kind pigment content height of the U.S. of Japan, higher more than 2 times than the anthocyanidin content of common purple potato, be the first-selected kind of technical solution of the present invention.
Technology of the present invention is owing to adopt membrane technique separation and purification and concentrated purple sweet potato haematochrome, and in whole process, pigment does not undergo phase transition, and is to operate under normal temperature condition, and energy consumption is low, does not destroy the molecular structure of purple sweet potato haematochrome; Can not adopt other solvent extractions and only use aqueous solution lixiviate, not use any poisonous and harmful solvent in the production process, pollution-free, safety and sanitation, safe, cost is low; Pigment extraction recovery height can reach more than 80%.Pigment stability is good: do not destroy the phthalidyl structure that the sweet potato anthocyanin contains in the membrane technique leaching process, help the stability to light, thermal response.Product look valency height: use this technology and extract the look valency that purified pigment product look valency is higher than other extraction processes.Pigment with method of the present invention is produced is mainly used in food color, the medicine industry product are painted, also can be used as the additive of features healthcare products.
Embodiment
Embodiment 1
According to one of technical process, get 200 kilograms of light violet sweet potatoes, clean the back section, put into volume 2m
3Steeping tank in, implantation concentration is 5% aqueous citric acid solution, adjusts soaking temperature to 40 ℃, 1.5 after hour, extract red pigments solution out from steeping tank, filter the elimination particulate contamination with the pumping pressure filter, pigment liquid after the filtration, with the pressure of 0.4MPa, the cross-current type hyperfiltration membrane assembly is advanced in pumping, after pre-treatment separates, obtain containing the acid solution of partial pigment, utilize remaining pump pressure to return steeping tank and use again; The enrichment haematochrome solution that obtains still under remaining pump function, enters cation exchange tower, the water-soluble impurity that the removal meeting pollutes and stops up to nanofiltration and reverse osmosis membrane; With the pressure of 0.6MPa, the cross-current type nanofiltration membrane component is advanced in pumping, isolates the non-pigmented part more than 95% in the solution, and the pigment solution concentration of this moment is about 20%～30%, separates the remaining acid solution in back, turns to steeping tank and recycles; The haematochrome solution that nanofiltration separation obtains under the effect of pump, by concentrating of reverse osmosis membrane, obtains concentration and is 90% pigment solution, and after suitably adjusting pH value, its look valency can reach 100 (E1%).Pigment solution after the reverse osmosis membrane separation, further drying obtains the dry powder finished product, and the look valency is higher than 100 (E1%), and every index meets the foodstuff additive national standard fully.
Embodiment 2
According to two of technical process, 200 kilograms of light violet sweet potatoes are cleaned the back section, put into volume 2m
3Steeping tank in, implantation concentration is 5% aqueous citric acid solution, adjust soaking temperature to 40 ℃, after 1.5 hours, extract red pigments solution out from steeping tank, filter with the pumping pressure filter, the elimination particulate contamination, the pigment liquid after the filtration is with the pressure of 0.1MPa, pumping enters cation exchange tower, the impurity that the removal meeting pollutes and stops up to nanofiltration and reverse osmosis membrane; With the pressure of 0.6MPa, cross-current type nanofiltration membrane (NF) assembly is advanced in pumping, isolates the non-pigmented part more than 95% in the solution, and the pigment solution concentration of this moment is about 20%～30%, separates the remaining acid solution in back, turns to steeping tank and recycles; The haematochrome solution that nanofiltration separation obtains under the effect of 2.0MPa pump pressure, by concentrating of reverse osmosis membrane, obtains concentration and is 90% pigment solution, and after suitably adjusting pH value, its look valency can reach 100 (E1%).Pigment solution after the reverse osmosis membrane separation, further drying obtains the dry powder finished product, and the look valency is higher than 100 (E1%), and every index meets the foodstuff additive national standard fully.
Embodiment 3
According to one of technical process, 200 kilograms of light violet sweet potatoes are cleaned the back section, put into volume 2m
3Steeping tank in, implantation concentration is 5% aqueous citric acid solution, adjust soaking temperature to 40 ℃, after 1.5 hours, extract red pigments solution out from steeping tank, filter with the pumping pressure filter, the elimination particulate contamination, the pigment liquid after the filtration is with the pressure of 0.1MPa, pumping enters thermopnore type cation exchange tower, the impurity that the removal meeting pollutes and stops up to nanofiltration and reverse osmosis membrane; With the pressure of 0.6MPa, cross-current type nanofiltration membrane (NF) assembly is advanced in pumping, isolates the non-pigmented part more than 95% in the solution, and the pigment solution concentration of this moment is about 50%～60%, separates the remaining acid solution in back, turns to steeping tank and recycles; The haematochrome solution that nanofiltration separation obtains, look valency can reach more than 60 (E1%), and other every indexs meet the foodstuff additive standard fully.
Embodiment 4
According to two of technical process, 100 kilograms on light violet sweet potato stem, leaf, cleaning and chopping is put into volume 2m
3Steeping tank in, implantation concentration is 5% aqueous citric acid solution, adjust soaking temperature to 40 ℃, after 2 hours, extract red pigments solution out from steeping tank, filter with the pumping pressure filter, the elimination particulate contamination, the pigment liquid after the filtration is with the pressure of 0.1MPa, pumping enters cation exchange tower, the impurity that the removal meeting pollutes and stops up to nanofiltration membrane and reverse osmosis membrane; With the pressure of 0.6MPa, cross-current type nanofiltration membrane (NF) assembly is advanced in pumping, isolates the non-pigmented part more than 95% in the solution, and the pigment solution concentration of this moment is about 30%～40%, separates the remaining acid solution in back, turns to steeping tank and recycles; The haematochrome solution that nanofiltration separation obtains under the effect of pump, by concentrating of reverse osmosis membrane, obtains concentration and is 90% pigment solution, and after suitably adjusting pH value, its look valency can reach 100 (El%) (GB).Pigment solution after the reverse osmosis membrane separation, further drying obtains the dry powder finished product, and the look valency is higher than 100 (E1%), and every index meets the foodstuff additive national standard fully.
By the liquid product that above-mentioned technical process production obtains, the important structure through checking its anthocyanogen is not destroyed, can be used as foodstuff additive and uses.
Claims (10)
1, a kind of method of extracting purple yam red colouring matter using membrane separation is characterized in that this method is: the piece root of Rhizoma Dioscoreae esculentae and other each organs extract haematochrome solution through souring soln, use the stage trapping membrane separation purification, remove impurity, obtain concentrated solution.
2, the method for the described extracting purple yam red colouring matter using membrane separation of root a tree name claim 1, it is characterized in that: in the described method, concentrate, obtain concentrated solution behind the adjust pH through ultrafiltration membrane treatment, cation-adsorption impurity elimination, nanofiltration membrane separation purifying, reverse osmosis membrane through haematochrome solution that souring soln extracts.
3, a kind of method of extracting purple yam red colouring matter using membrane separation is characterized in that: light violet potato or dried purple potato clean and crush, and acidizing fluid soaks, filtering under pressure, and the cation-adsorption impurity elimination through the nanofiltration membrane separation purifying, concentrates through reverse osmosis membrane, gets concentrated solution behind the adjust pH.
4, a kind of method of extracting purple yam red colouring matter using membrane separation is characterized in that: light violet potato or dried purple potato, clean and crush, and acidizing fluid soaks, filtering under pressure, the cation-adsorption impurity elimination through the nanofiltration membrane separation purifying, transfers the pH final vacuum to concentrate, and gets concentrated solution behind the adjust pH.
5, the method for root a tree name claim 1,2,3 or 4 described extracting purple yam red colouring matter using membrane separations, it is characterized in that: in the described method, potato slag behind the filtering under pressure, acidizing fluid soaks for the second time, filtering under pressure once more, filtrate enters the back segment of the technical process of method recited above through the ultra-filtration membrane pre-treatment.
6, the method for root a tree name claim 1,2,3 or 4 described extracting purple yam red colouring matter using membrane separations, it is characterized in that: in the described method, acidizing fluid refers to citric acid or the synthetic aqueous solution of alimentary acetic acid or ethanolic soln, immersion refers to souring soln under 20 ℃～40 ℃ temperature condition, soaked 1.5 hours～2 hours, potato slag behind the filtering under pressure still needs uniform temp and time when soaking for the second time for the first time.
7, the method for root a tree name claim 1,2,3 or 4 described extracting purple yam red colouring matter using membrane separations is characterized in that: in the described method, the various membrane modules of employing are organic materials or inorganic materials is made.
8, the method for the described extracting purple yam red colouring matter using membrane separation of root a tree name claim 2 is characterized in that: in the described method, the ultra-filtration membrane aperture of employing is 0.01 micron～0.2 micron, and the nanofiltration membrane aperture is 2 nanometers～10 nanometers; The aperture of reverse osmosis membrane is less than 1 nanometer.Ultrafiltration and nanofiltration system operating pressure are 0.3～1.6MPa, and the operating pressure of reverse osmosis membrane is 1.8～3.5MPa.
9, the method for root a tree name claim 3 or 4 described extracting purple yam red colouring matter using membrane separations is characterized in that: in the described method, the nanofiltration membrane aperture is 2 nanometers～10 nanometers, and the nanofiltration system operating pressure is 0.3～1.6MPa.
10, the method for the described extracting purple yam red colouring matter using membrane separation of root a tree name claim 3 is characterized in that: in the described method, the aperture of reverse osmosis membrane is less than 1 nanometer, and the operating pressure of reverse osmosis membrane is 1.8～3.5MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460470C (en) * | 2006-11-10 | 2009-02-11 | 华南师范大学 | Process for extracting purple sweep potato pigment |
| CN101186757B (en) * | 2007-12-24 | 2010-10-06 | 钱生球 | Method for producing purple sweet potato haematochrome |
| CN101962486A (en) * | 2010-08-26 | 2011-02-02 | 永康市毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN102206426A (en) * | 2011-03-23 | 2011-10-05 | 武汉普赛特膜技术循环利用有限公司 | Comprehensive utilization of pigment of purple sweet potato in purple sweet potato and method for comprehensively utilizing component thereof |
| CN102391667A (en) * | 2011-08-30 | 2012-03-28 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102516807A (en) * | 2011-12-29 | 2012-06-27 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN102604424A (en) * | 2012-02-27 | 2012-07-25 | 河北科技大学 | Method for extracting anthocyanins from purple sweet potato |
-
2006
- 2006-01-17 CN CN 200610010637 patent/CN1807516A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460470C (en) * | 2006-11-10 | 2009-02-11 | 华南师范大学 | Process for extracting purple sweep potato pigment |
| CN101186757B (en) * | 2007-12-24 | 2010-10-06 | 钱生球 | Method for producing purple sweet potato haematochrome |
| CN101962486A (en) * | 2010-08-26 | 2011-02-02 | 永康市毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN101962486B (en) * | 2010-08-26 | 2013-06-26 | 浙江毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN102206426A (en) * | 2011-03-23 | 2011-10-05 | 武汉普赛特膜技术循环利用有限公司 | Comprehensive utilization of pigment of purple sweet potato in purple sweet potato and method for comprehensively utilizing component thereof |
| CN102391667A (en) * | 2011-08-30 | 2012-03-28 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102391667B (en) * | 2011-08-30 | 2014-02-12 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102516807A (en) * | 2011-12-29 | 2012-06-27 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN102516807B (en) * | 2011-12-29 | 2014-03-19 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN102604424A (en) * | 2012-02-27 | 2012-07-25 | 河北科技大学 | Method for extracting anthocyanins from purple sweet potato |
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