CN101962485A - Later-stage pulverizing process for water-soluble gardenia yellow pigment stock solution and device used thereby - Google Patents
Later-stage pulverizing process for water-soluble gardenia yellow pigment stock solution and device used thereby Download PDFInfo
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- CN101962485A CN101962485A CN2010102646299A CN201010264629A CN101962485A CN 101962485 A CN101962485 A CN 101962485A CN 2010102646299 A CN2010102646299 A CN 2010102646299A CN 201010264629 A CN201010264629 A CN 201010264629A CN 101962485 A CN101962485 A CN 101962485A
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Abstract
The invention discloses a later-stage pulverizing process for water-soluble gardenia yellow pigment stock solution and a device used thereby. In the process, the gardenia yellow pigment stock solution is pulverized by a method of dehydrating at the temperature of between 35 and 60 DEG C in vacuum, wherein the concentration of the gardenia yellow pigment stock solution is between 15 and 30 weight percent in vacuum dehydration, the thickness is controlled to be between 5 and 15mm, the vacuum degree is controlled to be between 0.05MPa and 0.09MPa, and the water-soluble gardenia yellow natural pigment powder with water content of between 3 and 5 weight percent is obtained. In the gardenia yellow pigment powder, the water content is below 5 percent, the product colority and the colority of vacuum freeze drying are equivalent, the colority is 8 colority higher than the conventional spray drying, and the OD ratio is less than 0.4. The process has the advantages of simple process and low cost, the whole later-stage process is performed in a low-temperature vacuum environment, and the original quality of the pigment is well maintained, so the later-stage pulverizing process has large-scale industrial value.
Description
Technical field:
The present invention relates to a kind of later stage preparation technology's, particularly Gardenia Yellow of natural food pigment later stage dehydration flouring technology.
Background technology:
Gardenia Yellow is the rare water-soluble carotenoid of a class, have that raw material is easy to get, inexpensive, product safety, strong coloring force and advantage such as easy to use, and possess and reduce myocardial contraction and prevent health-care effect such as arteriosclerosis, therefore be widely used in food service industry and cosmetic industries such as beverage, cake, candy, flour products, drinks and milk-product, have good development space and vast market prospect.
Yet in the production and application process of Gardenia Yellow, but exist easy oxidized decomposition and the shortcoming of fading.Cause that the reason that Gardenia Yellow fades is because trans-crocetin and trans-crocetin molecule itself contain the shortcomings such as quality guaranteed period weak point of unsaturated double-bond and liquid state product, make it be subject to light, heat, H
+, destruction such as acid, metal ion, oxygenant, gradually become stable hydrocarbon by unsaturated hydrocarbons, thereby the absorption peak of pigment solution drifted about to the ultraviolet region, promptly fade; Chlorogenic acid in the pigment is very easily oxidized in addition, and makes painted food deepening, has had a strong impact on the product quality of natural gardenia yellow pigment, has reduced economic benefit.
Problem is hereto extracted in earlier stage at Gardenia Yellow, the separation and purification stage, and scientific research personnel's research has both at home and abroad also proposed the multiple extraction of Gardenia Yellow and the optimization technology of separation and purification, has guaranteed that to greatest extent Gardenia Yellow effective constituent is not destroyed.But the stage of powder process in the end, the present industrial spraying drying that mostly adopts, the spraying drying that adopts in last dehydration powder process stage in the CN 1847323 A patents for example, inlet temperature is 175-195 ℃, air outlet temperature has reached 85-105 ℃, this makes Gardenia Yellow be exposed in the environment of high temperature, oxygen enrichment, oxygenolysis has taken place and causes the reduction of unit product look valency, has influenced the quality of product.Vacuum lyophilization is a kind of milling method, in the CN 101165104 A patents, has proposed to adopt the mode of spraying drying or vacuum lyophilization.Though vacuum lyophilization can keep the quality of Gardenia Yellow well, but its energy consumption is big, the cost height, and the production cycle is long, be suitable for producing high value-added product, this makes that vacuum lyophilization can not popularization and application in the Gardenia Yellow industrial production more; In the CN 101077940 A patents, introduced a kind of extracting method of Gardenia Yellow, for last Gardenia Yellow powder process mode, also mentioned vacuum drying method, but the material of its processing is the xln of Gardenia Yellow, and do not offer some clarification on vacuum lyophilization or other vacuum-drying in the patent yet, more do not mention relevant dewatering process.
Summary of the invention:
In order to solve the easy oxidation of high temperature that exists in the existing Gardenia Yellow production, the shortcoming that the vacuum lyophilization cost is high, the invention provides the device of a kind of water-soluble Gardenia Yellow stoste later stage flouring technology and use thereof, have that cost is low, pigment stability good, not oxidized advantage.
Technical scheme of the present invention is: a kind of water-soluble Gardenia Yellow stoste later stage flouring technology, employing is carried out powder process in the method for 35 ℃～60 ℃ of vacuum hydro-extractions to Gardenia Yellow stoste, during vacuum hydro-extraction, the concentration of described Gardenia Yellow stoste is between 15%wt～30%wt, gauge control is between 5mm～15mm, vacuum degree control is between 0.05MPa～0.09MPa, dewatered with this understanding 20～30 hours, and obtained the water-soluble Gardenia Yellow natural pigment dry powder of water content between 3%wt～5%wt.
The employed device of described water-soluble Gardenia Yellow stoste later stage flouring technology, by dewatering box, formed by charging tray, heated constant temperature plate, water vapor condenser, vacuum pump, be provided with in the dewatering box and be subjected to charging tray and heated constant temperature plate, be subjected to charging tray on the heated constant temperature plate, dewatering box has water vapor condenser, the external vacuum pump of dewatering box.
Be provided with bypass control valve between vacuum pump and the dewatering box.
Water vapor condenser is connected with refrigerating unit.
The heated constant temperature plate is connected with heating unit.
Described device is controlled by controller.
Beneficial effect:
1. method of the present invention is in the cryogenic vacuum dehydration, and the temperature of hot-plate is controlled in 35 ℃～60 ℃ scopes, has solved Gardenia Yellow and has reduced problem owing to being in the look valency that causes under the high-temperature condition for a long time.
2. in the cryogenic vacuum dehydration, need not cryogenic freezing, dewatering time is shortened to 20～30 hours, energy-conservation about 30%.
3. owing to adopt vacuum condition, make be in all the time in low temperature, the vacuum environment natural gardenia xanthan liquid stage of powder process in the end, Gardenia Yellow is finished dehydration in low-oxygen environment, reduce Gardenia Yellow owing to the oxidized quality decline problem that causes, has guaranteed the quality of product.
4. adopt the low temperature flouring technology that really dewaters to obtain Gardenia Yellow powder-product with the vacuum lyophilization equal quality, and the powder process cost significantly reduce.
5. the vacuum dewatering system of Cai Yonging directly produces vacuum tightness in the dewatering box by vacuum pump, but controls vacuum tightness in the dewatering box by bypass control valve.
6. be provided with a water vapor condenser in the dewatering box bottom, thereby guaranteed the useful effect of vacuum pump.
7. adopt the resulting Gardenia Yellow powder of Gardenia Yellow preparation method of the present invention, the final water content of its product and look valency and vacuum lyophilization product basically identical, high 8 the look valencys of more conventional spraying drying, realized pigment product look valency height, good in economic efficiency, and technology is simple, and low, the simple operation and other advantages of cost has large-scale industrialization and is worth.
Description of drawings
Fig. 1 is the present invention: cryogenic vacuum dewatering unit work synoptic diagram.
1 is dewatering box, and 2 for being subjected to charging tray, and 3 is the heated constant temperature plate, and 4 is condenser, and 5 is vacuum pump, and 6 is that bypass control valve 7 is heating unit, and 8 is refrigerating unit.
Embodiment:
Below in conjunction with embodiment the present invention is described further.
A kind of water-soluble Gardenia Yellow stoste later stage flouring technology, with through the Gardenia Yellow stoste of separation and purification as raw material, put it into and carry out powder process in the cryogenic vacuum dewatering unit.Its stock solution quality concentration is controlled at 15%～30%, and the feed liquid gauge control is at 5mm～15mm, and vacuum degree control is between 0.05MPa～0.09MPa in the dewatering box, and Heating temperature is 35 ℃～60 ℃.Dewatered with this understanding 20～30 hours, and obtained the high colour-value water-soluble natural gardenia yellow pigment dry powder of water content between 3%wt-5%wt.
Described cryogenic vacuum dehydration preparation Gardenia Yellow powder: the temperature of heating plate of natural gardenia yellow pigment stoste is controlled between 35 ℃-60 ℃, Heating temperature is lower than 60 ℃ and has solved natural pigment owing to being in the destroyed problem of look valency that causes under the high-temperature condition for a long time, and has improved production efficiency of products.
Described cryogenic vacuum dehydration preparation Gardenia Yellow powder: the thickness of natural gardenia yellow pigment stoste is preferably between the 5mm-15mm.
Described cryogenic vacuum dehydration preparation Gardenia Yellow powder: the mass concentration of natural gardenia yellow pigment stoste preferably is controlled in the 15%-30% scope.
Described cryogenic vacuum dehydration preparation Gardenia Yellow powder: the vacuum tightness in the vacuum chamber preferably is controlled between the 0.05MPa-0.09MPa.
The employed device synoptic diagram of water-soluble Gardenia Yellow stoste later stage flouring technology of the present invention is seen accompanying drawing 1.Mainly by dewatering box, formed by charging tray, heated constant temperature plate, water vapor condenser, vacuum pump, be provided with in the dewatering box and be subjected to charging tray and heated constant temperature plate, be subjected to charging tray on the heated constant temperature plate, dewatering box has water vapor condenser, the external vacuum pump of dewatering box.Be provided with the bypass vacuum control valve between vacuum pump and the dewatering box.Water vapor condenser is connected with refrigerating unit.The heated constant temperature plate is connected with heating unit.Whole device is provided with microcomputer controller and is used for work such as electrical equipment control and data acquiring and recording.Heated constant temperature plate in the dewatering box can thermostatically heating, and enough heats is provided for the top charging tray that is subjected to, and dewatering box has the low temperature water vapor condenser, is used for the moisture that the condensation upper strata removes, and guarantees the pumping efficiency of vacuum pump.
The cryogenic vacuum dewatering unit of described preparation Gardenia Yellow powder: its principle of work is material to be dried to be placed be subjected on the charging tray, the decompression dehumidification that under vacuum condition, carries out, dehumidification institute heat requirement is provided by the heated constant temperature plate, the heated constant temperature plate is connected with heating unit, adopts the heating of outer circulation constant temperature fluid.Utilize vacuum pump to bleeding in the dewatering box, the wet branch of extracting out carries out the wet branch of cryogenic condensation by the water vapor condenser under the dewatering box earlier, remaining wet branch and non-condensable gas are discharged through vacuum pump, thereby guarantee that vacuum tightness can be stablized in the dewatering box, and the dehumidification efficient of material is constant.Condenser adopts circulation low temperature freonll-11 to obtain to be low to moderate-50 ℃ cryotron surface temperature.Whole drying and dehydrating process need not the mode dehumidification by freezing and sublimation again because decompression reduces the boiling point of water, makes at a lower temperature, have higher drying rate, and the quality of thermo-sensitivity product is not destroyed by pyritous substantially.
The cryogenic vacuum dewatering unit of described preparation Gardenia Yellow powder: directly produce vacuum tightness in the dewatering box by vacuum pump, and the vacuum tightness in the dewatering box is by vacuum pump with bypass valve aperture size is common regulates.In order to control the vacuum tightness in the dewatering box, between vacuum pump and dewatering box, be provided with the bypass vacuum control valve, at the initial stage of dehydration beginning, this valve is opened to certain aperture, made that the vacuum tightness in the dewatering box reduces, guarantee to be subjected to the feed liquid in the charging tray to be unlikely to bubble because of crossing low pressure moment dehumidification, influence carrying out smoothly of whole dehydration, along with the carrying out of dehydration, this valve can progressively be turned aperture down, until closing at last.
Because the boiling point lowering of water and the heat of giving of constant temperature hot-plate is arranged under the low pressure, speed was very fast when the initial stage dewatered, water evaporation quantity is bigger, the water vapour of in time being taken away by vacuum pump can not make the pounds per square inch absolute (psia) in the dewatering box become big, vacuum tightness reduces, thereby cause vacuum tightness can accurately not maintain a definite value, and in the present invention, owing to below dewatering box, be provided with water vapor condenser, well solved this problem, the device that just is not condensed that vacuum pump is taken away is caught that sub-fraction water vapour of agglomerative and residual non-condensable gas, thereby can guarantee the vacustat in the dewatering box, guarantees the dehydration of system.
Embodiment 1:
Through sophisticated cape jasmine fresh fruit that selecting through air-dry, pulverizing, cross Gardenia Yellow stoste behind mesh sieve, ethanol lixiviate, filtration, the recovery ethanol, to be mixed with concentration be 20% mother liquor (surveying its look valency is 120), adopts spraying drying and cryogenic vacuum dehydration dual mode to carry out powder process respectively.At first carry out spraying drying according to parameter shown in the CN 1847323 A patents, adopting inlet temperature is 175-195 ℃, and air outlet temperature is controlled at 85-105 ℃, and air quantity is 40m
3/ h, the gained powder carries out look valency and moisture determination; Get same feed liquid and carry out the cryogenic vacuum dehydration, feed liquid is put into the dish of long 350mm, wide 250mm, high 50mm, controlling its thickness is 7mm, temperature of heating plate is adjusted to 45 ℃, begins simultaneously to vacuumize to dewater, vacuum tightness is set at 0.08Mpa, whole dehydration continues about 24 hours, with the gained powder grind get final product water content at the powder-product of 3%-5%, measure its look valency respectively, and compare with mother liquor look valency.The result shows: the look valency of the powder that obtains through vacuum hydro-extraction is than the mother liquor look valency 32 look valencys that descended, but than high 8 the look valencys of spraying drying.
Embodiment 2:
Directly buy from the market and do mother liquor (the look valency is 120), adopt two kinds of methods of vacuum lyophilization and cryogenic vacuum dehydration to carry out powder process respectively through the Gardenia Yellow stoste of separation and purification.Adopt the material disc of long 350mm, wide 250mm, high 50mm, put into a certain amount of feed liquid, controlling its thickness is 7mm, at first at-45 ℃ of following pre-freeze 2-3 hours, at pounds per square inch absolute (psia) is about 35 hours of dehydration in the vacuum environment of 400mTorr, and the gained powder is ground its water content and the look valency measured.Secondly the pigment feed liquid of same thickness is carried out cryogenic vacuum dehydration powder process, regulate temperature of heating plate to 45 ℃, vacuum tightness is set at 0.08Mpa, and whole dehydration continues 24 hours.The gained powder is ground mensuration water content and look valency, and the result shows: the final water content of its product and vacuum lyophilization product are respectively 4.09% and 4.43% (moisture wet basis), and the look valency is respectively 87.6 and 88.5, differ less than 1 look valency.And through calculating, vacuum lyophilization energy-conservation about 30% is compared in the cryogenic vacuum dehydration.
Claims (6)
1. water-soluble Gardenia Yellow stoste later stage flouring technology, it is characterized in that: Gardenia Yellow stoste is adopted carry out powder process in the method for 35 ℃～60 ℃ of vacuum hydro-extractions, during vacuum hydro-extraction, the concentration of described Gardenia Yellow stoste is between 15%wt～30%wt, gauge control is between 5mm～15mm, vacuum degree control was dewatered 20～30 hours between 0.05MPa～0.09MPa with this understanding, obtained the water-soluble Gardenia Yellow natural pigment dry powder of water content between 3%wt～5%wt.
2. the employed device of the described water-soluble Gardenia Yellow stoste later stage flouring technology of claim 1, it is characterized in that: by dewatering box, formed by charging tray, heated constant temperature plate, water vapor condenser, vacuum pump, be provided with in the dewatering box and be subjected to charging tray and heated constant temperature plate, be subjected to charging tray on the heated constant temperature plate, dewatering box has water vapor condenser, the external vacuum pump of dewatering box.
3. the employed device of water-soluble Gardenia Yellow stoste later stage flouring technology as claimed in claim 2 is characterized in that: be provided with bypass control valve between vacuum pump and the dewatering box.
4. the employed device of water-soluble Gardenia Yellow stoste later stage flouring technology as claimed in claim 2, it is characterized in that: water vapor condenser is connected with refrigerating unit.
5. the employed device of water-soluble Gardenia Yellow stoste later stage flouring technology as claimed in claim 2, it is characterized in that: the heated constant temperature plate is connected with heating unit.
6. the employed device of water-soluble Gardenia Yellow stoste later stage flouring technology as claimed in claim 2, it is characterized in that: described device is controlled by controller.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104018353A (en) * | 2014-06-23 | 2014-09-03 | 陈引发 | Pulp for environment-friendly packaging decoration artificial leather coatings |
| CN105086506A (en) * | 2015-09-24 | 2015-11-25 | 云南麦瑞科生物科技有限公司 | Preparation device and method of high-quality gardenia yellow pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104018353A (en) * | 2014-06-23 | 2014-09-03 | 陈引发 | Pulp for environment-friendly packaging decoration artificial leather coatings |
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Application publication date: 20110202 |