CN109836483B - Production device and production method of zein - Google Patents
Production device and production method of zein Download PDFInfo
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- CN109836483B CN109836483B CN201711217677.0A CN201711217677A CN109836483B CN 109836483 B CN109836483 B CN 109836483B CN 201711217677 A CN201711217677 A CN 201711217677A CN 109836483 B CN109836483 B CN 109836483B
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- 229920002494 Zein Polymers 0.000 title claims abstract description 134
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 78
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- 239000002904 solvent Substances 0.000 claims abstract description 123
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- 238000011084 recovery Methods 0.000 claims abstract description 15
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Abstract
The invention provides a device and a method for producing zein. The production device comprises an extraction unit and a purification unit, wherein the extraction unit is used for dissolving raw materials to obtain an alcoholic solution of zein; the purification unit is communicated with the extraction unit through a solution transmission pipeline and a solvent return pipeline, the solution transmission pipeline transmits the alcohol solution of the zein to the purification unit, the purification unit separates the zein and the alcohol solvent in the alcohol solution of the zein, and the solvent return pipeline returns the alcohol solvent obtained by separation to the extraction unit. A solvent return pipeline is arranged between the extraction unit and the purification unit, and the alcohol solvent obtained by separation in the purification unit is returned to the extraction unit for recycling, so that the utilization efficiency of the alcohol solvent is improved, and the energy consumption of the alcohol solvent in the production process of the zein is reduced. Can realize long-period stable operation, and has the advantages of less equipment investment, simple operation, low energy consumption, high solvent recovery rate, no pollution and the like.
Description
Technical Field
The invention relates to the technical field of deep processing of agricultural products, in particular to a device and a method for producing zein.
Background
Zein (zein) is a natural polymer, is the most important storage protein of corn, is located in zein bodies in corn endosperm cells and accounts for 35-60% of the total content of the zein. Zein, a bioactive carrier, has attracted considerable attention in the food and biopharmaceutical fields due to its unique physicochemical properties.
Firstly, zein has good biocompatibility, biodegradability and the like, is a generally accepted as safe (GRAS) biomaterial, and meets the requirements of people on green, natural and safe bioactive component carriers; secondly, the zein has strong hydrophobicity and unique solubility, is easy to prepare micro-particles or nano-particles, and can be used as an ideal carrier of hydrophobic drugs or functional active ingredients. Compared with other animal and plant proteins, the zein is digested by intestines and stomach for a longer time, and is beneficial to the slow release of functional active ingredients in oral medicaments in vivo; zein is easy to combine with other compounds to form a composite high polymer, and is beneficial to constructing carrier conveying systems with different characteristics according to different requirements. In addition, the zein is the main component of the corn protein powder which is a byproduct in corn starch processing, and has rich resources and low cost. The carrier system which takes zein as a main matrix is developed, so that the corn deep processing industrial chain can be effectively extended, and the comprehensive utilization efficiency of byproducts is improved.
Zein is insoluble in water and anhydrous alcohol, soluble in 60-95% alcohol water solution, and also soluble in strong base (pH >11), Sodium Dodecyl Sulfate (SDS), high-concentration urea, propylene glycol, acetic acid, and other organic solvents. At present, the production process of zein mostly adopts an organic solvent method, usually ethanol is used for extracting the zein, and the ethanol with the volume fraction of 60-95 percent is directly used for extracting the zein. The zein in the extracting solution is mostly precipitated by salting out, adding water, freezing and the like. The volume of the ethanol solution recovered by the methods is obviously increased compared with that before treatment, so that the recovery cost and energy consumption of the solvent are greatly increased, a large amount of wastewater can be generated, great pressure is caused on the environment, and the application and popularization of the zein in the market are hindered.
Therefore, the development of an industrial production route of the zein with less solvent consumption, low energy consumption and high production efficiency is the key for successfully popularizing the zein in the market.
Disclosure of Invention
The invention mainly aims to provide a device and a method for producing zein, which aim to solve the problem of high energy consumption of a zein production solvent in the prior art.
In order to achieve the above object, according to an aspect of the present invention, there is provided a zein production apparatus, comprising: the extraction unit is used for dissolving the raw materials to obtain an alcoholic solution of zein; the purification unit is communicated with the extraction unit through a solution transmission pipeline and a solvent return pipeline, the solution transmission pipeline transmits the alcohol solution of the zein to the purification unit, the purification unit separates the zein and the alcohol solvent in the alcohol solution of the zein, and the solvent return pipeline returns the alcohol solvent obtained by separation to the extraction unit.
Further, the production device further comprises a storage stirring unit, the storage stirring unit comprises a stirring kettle, and the solution transmission pipeline and the solvent return pipeline are communicated with the stirring kettle and penetrate through the stirring kettle.
Further, the solution conveying pipeline comprises a first conveying section and a second conveying section, the solvent returning pipeline comprises a first returning section and a second returning section, the extraction unit comprises an extractor, the extractor is provided with a material inlet and a material outlet, the material outlet is communicated with the stirring kettle through the first conveying section, and the stirring kettle is communicated with the purification unit through the second conveying section; the material import feeds through first returning section with the stirred tank, and the stirred tank feeds through the second returning section with the purification unit, and preferably, the extractor is a plurality of, and a plurality of extractors set up in parallel.
Further, the extraction unit also comprises an alcohol solvent storage tank, the alcohol solvent storage tank is communicated with the first returning section, and the alcohol solvent storage tank is communicated with the material outlet through a backflow pipeline; preferably, the return line is also provided with a return valve.
Furthermore, the extraction unit also comprises a power element, the power element is arranged on the first returning section and is positioned between the alcohol solvent storage tank and the extractor, and preferably the power element is a reflux pump; more preferably, the first returning section and the first transmission section are both provided with flow control valves, wherein the flow control valves on the first returning section are positioned between the power element and the material inlet.
Further, the production device comprises a solvent recovery unit, the solvent recovery unit comprises an ultrafiltration membrane assembly, and the ultrafiltration membrane assembly is communicated with and arranged on the first return section and positioned between the alcohol solvent storage tank and the stirring kettle so as to convey the alcohol solvent obtained after ultrafiltration to the alcohol solvent storage tank; preferably, the ultrafiltration membrane module comprises an ultrafiltration membrane, and the ultrafiltration membrane is a polysulfone-based ultrafiltration membrane.
Further, a concentrated solution returning pipeline is arranged between the ultrafiltration membrane component and the stirring kettle, the concentrated solution returning pipeline is used for returning the zein concentrated solution obtained by separating the ultrafiltration membrane component to the stirring kettle, and preferably, a pressure regulating valve is further arranged on the concentrated solution returning pipeline.
Further, the solvent recovery unit also comprises a membrane module feeding pump, and the membrane module feeding pump is communicated with and arranged on the first returning section and is positioned between the stirring kettle and the ultrafiltration membrane module.
Further, the purification unit comprises a rectifying tower, and the rectifying tower is communicated with the stirring kettle through a second transmission section and a second return section; preferably, a rectifying tower feeding pump is arranged on the second transmission section in a communication mode.
Further, the second returning section is communicated with a vacuum pump 23, a condenser and a buffer tank which are sequentially close to the stirring kettle.
Further, a vacuum meter is arranged on the second returning section and is arranged between the rectifying tower and the vacuum pump 23.
According to another aspect of the present application, there is also provided a method for producing zein, comprising: dissolving and extracting the raw materials by adopting an ethanol solution with the volume fraction of 60-95% to obtain an alcohol solution of zein; purifying the alcohol solution of zein to obtain zein and an alcohol solvent; the alcohol solvent is recovered for dissolving and extracting the raw material.
Further, the step of dissolving and extracting the raw materials adopts a reflux mode to dissolve and extract the raw materials for multiple times, more preferably, the dissolution product is extracted while refluxing, and the ratio of the reflux amount to the extraction amount is controlled to be 2-5: 1.
Further, in the step of purifying the alcohol solution of the zein, the alcohol solution of the zein is purified by a rectifying tower, and the absolute pressure of the top of the rectifying tower is controlled to be 5-20 Kpa.
Further, while dissolving and extracting the raw materials and purifying the alcohol solution of zein, the production method also comprises the following steps: filtering and intercepting the alcohol solution of the zein by using an ultrafiltration membrane component to obtain filtrate and intercepted substances, recovering the filtrate for dissolving and extracting raw materials, and purifying the intercepted substances to obtain the zein.
Further, before the production, the production method further comprises the step of driving the production device; preferably, the step of operating the production apparatus includes: s1, adding an ethanol water solution with the volume fraction of 60-95% into an alcohol solvent storage tank; s2, adding the raw materials into the extractor, feeding the ethanol water solution in the alcohol solvent storage tank into the extractor to carry out total reflux extraction on the raw materials for 30-60 min, and then adjusting the ratio of reflux amount to extraction amount of the extractor to be 2-5: 1; s3, keeping for 10-30 min under the condition that the ratio of the backflow amount to the produced amount is controlled to be 2-5: 1, sending the produced liquid into a stirring kettle, then filtering and intercepting the produced liquid by adopting an ultrafiltration membrane assembly to obtain an intercepted substance, and returning the intercepted substance to the stirring kettle, wherein the pressure of the feeding side of the ultrafiltration membrane assembly is controlled within the range of 0.1-0.6 MPa in the filtering and intercepting process; and S4, filtering and retaining for 60-120 min, feeding the mixture of the produced liquid and the retained substance in the stirring kettle into a rectifying tower for rectifying and purifying, and controlling the absolute pressure at the top of the tower to be 5-20 kPa when the liquid level of the kettle of the rectifying tower reaches 50-60% of the volume of the kettle of the tower so as to evaporate alcohol vapor from the top of the tower.
Furthermore, the stirring temperature of the stirring kettle is 40-60 ℃, and the stirring speed is 100-400 r/min.
Further, the step of driving further comprises: alcohol vapor is further condensed into liquid after being evaporated from the tower top, and the liquid is returned to the stirring kettle for reuse.
By applying the technical scheme, the solvent return pipeline is arranged between the extraction unit and the purification unit, the alcohol solvent obtained by separation of the purification unit is returned to the extraction unit for recycling, the utilization efficiency of the alcohol solvent is improved, and the energy consumption of the alcohol solvent in the production process of the zein is reduced. Can realize long-period stable operation, and has the advantages of less equipment investment, simple operation, low energy consumption, high solvent recovery rate, no pollution and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic diagram of a zein production plant in accordance with a preferred embodiment of the present application.
Wherein the figures include the following reference numerals:
10. an extraction unit; 20. a purification unit; 30. a storage stirring unit;
11. an extractor; 12. an alcohol solvent storage tank; 13. a power element;
21. a rectifying tower; 22. a rectifying tower feed pump; 23. a vacuum pump; 24. a condenser; 25. a buffer tank; 26. a vacuum gauge;
01. a solution delivery line; 02. a solvent return line; 03. a concentrated solution return line;
011. a first transmission section; 012. a second transmission segment; 021. a first return section; 022. a second returning section;
1. a reflux valve; 2. a flow control valve; 3. a pressure regulating valve; 4. a production valve;
31. stirring the mixture in a kettle;
41. an ultrafiltration membrane module; 42. a membrane module feed pump.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As mentioned in the background, the prior art zein production has a problem of high solvent consumption, and in order to improve the current situation, in an exemplary embodiment of the present application, a zein production apparatus is provided, as shown in fig. 1, the zein production apparatus includes: an extraction unit 10 and a purification unit 20, wherein the extraction unit 10 is used for dissolving raw materials to obtain an alcoholic solution of zein; the purification unit 20 is communicated with the extraction unit 10 through a solution transmission pipeline 01 and a solvent return pipeline 02, the solution transmission pipeline 01 transmits the alcohol solution of zein to the purification unit 20, the purification unit 20 separates the zein and the alcohol solvent in the alcohol solution of zein, and the solvent return pipeline 02 returns the alcohol solvent obtained by separation to the extraction unit 10.
The utility model provides an above-mentioned zein's apparatus for producing, through set up the solvent between extraction element 10 and purification unit 20 and return pipeline 02, the alcoholic solvent that obtains the separation of purification unit 20 returns extraction element 10 reuse, has improved the utilization efficiency of alcoholic solvent, has reduced the energy consumption of alcoholic solvent in zein's the production process.
In order to further improve the effect of the purification unit 20 on the alcohol solution of zein delivered by the extraction unit 10, in a preferred embodiment of the present application, the production apparatus further includes a storage stirring unit 30, the storage stirring unit 30 includes a stirring tank 31, and the solution delivery line 01 and the solvent return line 02 are both communicated with the stirring tank 31 and disposed through the stirring tank 31.
The storage stirring unit 30 is communicated between the extraction unit 10 and the purification unit 20, and the storage stirring unit 30 is arranged by passing through the solution conveying pipeline 01 and the solvent return pipeline 02, so that the alcohol solution of zein conveyed by the extraction unit 10 can be conveniently stored, uniformly mixed and stirred, and the purification effect of the purification unit 20 on the alcohol solution is better.
Specifically, the solution transfer line 01 and the solvent return line 02 may be appropriately arranged according to the positional relationship between the specific devices of the extraction unit 10 and the purification unit 20 in actual production. In a preferred embodiment of the present application, as shown in fig. 1, the solution conveying line 01 includes a first conveying section 011 and a second conveying section 012, the solvent returning line 02 includes a first returning section 021 and a second returning section 022, the extraction unit 10 includes an extractor 11, the extractor 11 has a material inlet and a material outlet, the material outlet is communicated with the stirred tank 31 through the first conveying section 011, and the stirred tank 31 is communicated with the purification unit 20 through the second conveying section 012; the material inlet is communicated with the stirred tank 31 through the first return segment 021, and the stirred tank 31 is communicated with the purification unit 20 through the second return segment 022.
In the preferred embodiment, the specific separation process is as follows: after the raw material containing zein enters the extractor 11 from the material inlet to extract the zein, the alcoholic solution containing zein enters the first transmission section 011 of the solution transmission pipeline 01 through the material outlet, and then enters the stirring kettle 31 to be stirred, the stirred alcoholic solution containing zein enters the purification unit 20 through the second transmission section 012 to be purified of the zein and separated of the alcohol solvent, the separated alcohol solvent returns to the stirring kettle 31 through the second returning section 022, and then returns to the extractor 11 through the material inlet through the first returning section 021 to extract the zein.
Preferably, the extractor 11 is provided in plurality, and the plurality of extractors 11 are arranged in parallel to improve the extraction efficiency and maintain the stable operation of the whole system. More preferably, the extractor 11 is provided with two extractors, one for extraction and the other for unloading, reloading and standby, the two extractors 11 being switchable with respect to each other, the whole process being continuously operated. The discharge of the extractor 11 is divided into two parts, one part returns to the solvent storage tank, the other part returns to the stirring kettle 31, and the proportion of the two parts is adjustable.
In order to further improve the extraction stability and extraction efficiency of the zein in the extraction process. In a preferred embodiment of the present application, the extraction unit 10 further includes an alcohol solvent storage tank 12, the alcohol solvent storage tank 12 is disposed in the first returning section 021 in a communicating manner, and the alcohol solvent storage tank 12 is in communication with the material outlet through a return line.
An alcohol solvent storage tank 12 is arranged on the first returning section 021 to communicate the stirring kettle 31 with the extractor 11, so that the alcohol solvent can be reasonably added according to the requirement of the extractor 11 on the alcohol solvent amount; the alcohol solvent storage tank 12 is communicated with the material outlet through a backflow pipeline, so that the extraction rate of the extractor 11 on the zein is improved, the mixed solution in the extractor 11 enters the alcohol solvent storage tank 12 through the backflow pipeline, and then returns to the extractor 11 through the first returning section 021 for extraction, so that the zein alcohol solution is extracted for multiple times, and the improvement of the extraction rate is facilitated.
In order to more conveniently select the number of times and the flow rate of the reflux extraction according to the needs, the reflux line is preferably further provided with a reflux valve 1.
In order to return the alcoholic solvent more conveniently and quickly, in a preferred embodiment of the present application, the extraction unit 10 further comprises a power element 13, the power element 13 is disposed on the first return section 021 and is located between the alcoholic solvent storage tank 12 and the extractor 11, and the power element 13 is preferably a reflux pump; more preferably, a flow control valve 2 is arranged on both the first returning section 021 and the first conveying section, wherein the flow control valve 2 on the first returning section 021 is located between the power element 13 and the material inlet.
The power element 13 can provide power with corresponding magnitude according to actual needs, and the flow control valve 2 is arranged to reasonably adjust the flow of the returned alcohol solvent according to actual needs. Correspondingly, the power element 13 for returning can also set the power with corresponding magnitude according to the flow magnitude of the returned alcohol solvent.
In order to further mention the purity of the returned alcohol solvent, in a preferred embodiment of the present application, the production apparatus comprises a solvent recovery unit, the solvent recovery unit comprises an ultrafiltration membrane assembly 41, and the ultrafiltration membrane assembly 41 is communicatively disposed on the first returning section 021 and located between the alcohol solvent storage tank 12 and the stirring tank 31, so as to convey the alcohol solvent obtained after ultrafiltration to the alcohol solvent storage tank 12.
The ultrafiltration membrane component 41 can intercept proteins in zein-containing materials in the stirring kettle 31, and the alcohol solvent passing through the ultrafiltration membrane component 41 is returned to the alcohol solvent storage tank 12, so that the purity of the alcohol solvent is relatively pure, and the recycling efficiency of the alcohol solvent is improved.
The ultrafiltration membrane material specifically used in the ultrafiltration membrane module 41 can be selected from existing ultrafiltration membrane materials. Preferably, the ultrafiltration membrane module 41 includes an ultrafiltration membrane, and the ultrafiltration membrane is a polysulfone-based ultrafiltration membrane. The polysulfone ultrafiltration membrane has good chemical stability, excellent acid and alkali resistance, good water permeability, high strength, long service life and stable interception performance.
In order to further facilitate the purification of the zein retained by the ultrafiltration membrane module 41, in a preferred embodiment of the present application, as shown in fig. 1, a concentrated solution returning line 03 is further disposed between the ultrafiltration membrane module 41 and the stirring tank 31, the concentrated solution returning line 03 is used for returning the zein concentrated solution separated by the ultrafiltration membrane module 41 to the stirring tank 31, and preferably, a pressure regulating valve 3 is further disposed on the concentrated solution returning line 03.
The arrangement of the concentrated solution return pipeline 03 facilitates direct return of the zein concentrated solution separated by the ultrafiltration membrane module 41 to the stirring kettle 31, and after the zein concentrated solution is uniformly mixed with the zein-containing alcoholic solution conveyed by the first conveying section, the zein concentrated solution and the zein-containing alcoholic solution are conveyed by the second conveying section and enter the purification unit 20 for purification.
In a preferred embodiment of the present application, as shown in fig. 1, the solvent recovery unit further comprises a membrane module feed pump 42, the membrane module feed pump 42 being disposed in communication with the first return section 021 and between the stirred tank 31 and the ultrafiltration membrane module 41. The arrangement of the feeding pump improves the circulation efficiency between the alcohol solution in the stirring tank 31 and the ultrafiltration membrane module 41.
The purification unit 20 can be used for purification in existing purification facilities as long as purification of zein can be achieved. In a preferred embodiment of the present application, purification unit 20 includes a rectification column 21, and rectification column 21 is in communication with stirred tank 31 via second transfer section 012 and second return section 022.
The target protein can be purified by adopting the rectifying tower 21 according to the difference of the boiling points of the zein in the alcoholic solution, the alcoholic solvent and other components, and the purity is high. Specifically, the rectifying tower 21 is a vacuum rectifying tower, the number of theoretical plates is 20-30, a tower kettle is not heated, and the tower top does not reflux.
Preferably, the second transmission section 012 is connected to a rectifying tower feeding pump 22, so that a power with a proper magnitude is required to be provided for feeding.
In order to further improve the recovery rate of the alcohol solvent in the zein production process, in a preferred embodiment of the present application, as shown in fig. 1, a vacuum pump 23, a condenser 24 and a buffer tank 25 are connected to the second returning section 022, and are sequentially close to the stirring tank 31.
The top of the rectifying tower 21 is vacuumized by a vacuum pump 23, which is beneficial to the volatilization of the alcohol solvent with lower boiling point. The condenser 24 is arranged to condense the volatilized alcohol solvent into liquid again, and the buffer tank 25 is arranged to temporarily store the condensed alcohol solvent for recycling as required.
In a preferred embodiment of the present application, as shown in fig. 1, a vacuum gauge 26 is further disposed on the second return section 022, and the vacuum gauge 26 is disposed between the rectifying tower 21 and the vacuum pump 23. The vacuum gauge 26 can display the vacuum condition of the top of the rectifying tower in real time.
In another exemplary embodiment of the present application, there is provided a method for producing zein, comprising: dissolving and extracting the raw materials by adopting an ethanol solution with the volume fraction of 60-95% to obtain an alcohol solution of zein; purifying the alcohol solution of zein to obtain zein and an alcohol solvent; and recovering the alcohol solvent for dissolving and extracting the raw material.
According to the production method of the zein, the alcohol solvent after purification and separation is recycled, so that the utilization efficiency of the alcohol solvent in the zein production process is improved, the loss of the alcohol solvent is reduced, the energy consumption is reduced, and the finally obtained zein product has high purity.
In order to further improve the dissolving efficiency and the extraction efficiency of zein, in a preferred embodiment of the present application, the step of dissolving and extracting the raw material is performed by dissolving and extracting the raw material for multiple times in a reflux manner, more preferably, a dissolution product is extracted while refluxing, and the ratio of the reflux amount to the extraction amount is controlled to be 2-5: 1.
The larger the amount of reflux, the more sufficient the dissolution and the higher the dissolution efficiency, and accordingly, the extraction efficiency is relatively lowered. The more the extraction amount is, the higher the extraction efficiency is, the higher the production efficiency is, but the dissolving times are relatively less. The ratio of the reflux amount to the extraction amount is controlled within the range of 2-5: 1, and the dissolution degree and the production efficiency can be considered.
In the step of purifying the alcohol solution of zein, the purity of the target protein can be improved by adopting the rectifying tower 21 for purification. The specific column top absolute pressure of the rectifying column 21 can be optimally adjusted according to the production conditions. In a preferred embodiment of the present application, in the step of purifying the alcohol solution of zein, the alcohol solution of zein is purified by using a rectifying tower 21, and the absolute pressure at the top of the rectifying tower 21 is controlled to be 5 to 20 Kpa.
In order to further improve the purification effect, in a preferred embodiment of the present application, the production method further comprises, while performing dissolution extraction on the raw material and purifying the zein alcohol solution: filtering and intercepting the alcohol solution of the zein by using an ultrafiltration membrane component to obtain filtrate and intercepted substances, recovering the filtrate for dissolving and extracting raw materials, and purifying the intercepted substances to obtain the zein.
The zein is produced by combining membrane separation and purification with reduced pressure rectification and purification, so that the purity of zein products can reach 85% -90%, the cyclic utilization of alcohol solvents is realized, the loss of the solvents is reduced, and the production efficiency is improved.
The ultrafiltration membrane in the ultrafiltration membrane component can be used by selecting the ultrafiltration membrane suitable for intercepting zein according to the interception performance in the existing ultrafiltration membrane component. In a preferred embodiment of the application, an ultrafiltration membrane in an ultrafiltration membrane component is a polysulfone ultrafiltration membrane, and the ultrafiltration pressure of the ultrafiltration membrane is 0.1-0.6 MPa. The polysulfone ultrafiltration membrane has good chemical stability, excellent acid and alkali resistance, good water permeability, high strength, long service life and stable interception performance. The ultrafiltration pressure is within the range of 0.1-0.6 MPa, the permeation side is normal pressure, and the zein molecules of 25000 Da-45000 Da can be intercepted.
In a preferred embodiment of the present application, before the production, the production method further includes a step of starting the production apparatus; preferably, the step of operating the production apparatus includes: s1, adding an ethanol water solution with the volume fraction of 60-95% into an alcohol solvent storage tank; s2, adding the raw materials into the extractor, feeding the ethanol water solution in the alcohol solvent storage tank into the extractor to carry out total reflux extraction on the raw materials for 30-60 min, and then adjusting the ratio of reflux amount to extraction amount of the extractor to be 2-5: 1; s3, keeping for 10-30 min under the condition that the ratio of the backflow amount to the produced amount is controlled to be 2-5: 1, sending the produced liquid into a stirring kettle, then filtering and intercepting the produced liquid by adopting an ultrafiltration membrane assembly to obtain an intercepted substance, and returning the intercepted substance to the stirring kettle, wherein the pressure of the feeding side of the ultrafiltration membrane assembly is controlled within the range of 0.1-0.6 MPa in the filtering and intercepting process; and S4, filtering and retaining for 60-120 min, feeding the mixture of the produced liquid and the retained substance in the stirring kettle into a rectifying tower for rectifying and purifying, and controlling the absolute pressure at the top of the tower to be 5-20 kPa when the liquid level of the kettle of the rectifying tower reaches 50-60% of the volume of the kettle of the tower so as to evaporate alcohol vapor from the top of the tower.
In the step of starting, the alcohol solvent is added into the alcohol solvent storage tank and is in a usable state, the alcohol solvent in the alcohol solvent storage tank is fed into the extractor for total reflux extraction while the raw materials are added into the extractor, after the zein extracted by the total reflux is fully dissolved, the proper reflux amount and extraction amount ratio is set, and the specific time is kept, so that the extraction liquid enters the stirring kettle. And then, delivering the produced liquid in the stirring kettle into an ultrafiltration membrane component for ultrafiltration interception, returning the zein to the stirring kettle, and returning the alcohol solvent penetrating through the ultrafiltration membrane to the alcohol solvent storage tank and the extractor for reutilization. And the liquid after ultrafiltration by the ultrafiltration membrane component returns to the stirring kettle, which is equivalent to concentrating the produced liquid in the stirring kettle, so that the concentration of the zein in the stirring kettle is improved, and convenience is provided for subsequent purification. And finally, mixing and stirring the intercepted substances and the produced liquid, and then sending the mixture into a rectifying tower, starting a rectifying mode until the liquid level in the rectifying tower reaches 50-60% of the volume of a tower kettle, and enabling the absolute pressure of the tower top to be in the range so as to enable the alcohol solvent to be evaporated from the tower top in a steam mode. And filtering and drying the residue at the bottom of the kettle to obtain a zein product with the purity of 85-90 percent.
In the preferred embodiment, the specific stirring temperature and the stirring speed of the stirring kettle can be optimally adjusted according to actual needs. In a preferred embodiment of the application, the stirring temperature of the stirring kettle is 40-60 ℃, and the stirring speed is 100-400 r/min. The stirring effect can be more uniform under the stirring condition.
In a preferred embodiment of the present application, the driving step further includes: alcohol vapor is further condensed into liquid after being evaporated from the tower top and then returns to the stirring kettle for reuse, so that the utilization efficiency of the alcohol solvent is improved.
In a most preferred embodiment of the present application, a method for producing zein is provided, which comprises the following specific steps:
(1) respectively adding water solution with the mass fraction of ethanol of 60-95% into a stirring kettle and a buffer tank, wherein the adding amount is 40-60% of the volume of the stirring kettle and the buffer tank, the temperature of the stirring kettle is 40-60 ℃, and the stirring speed is 100-400 r/min;
(2) opening an upper end socket of the extractor, adding a proper amount of corn protein powder into the extractor, installing the upper end socket, screwing a bolt, starting a feed pump of the extractor, carrying out total reflux extraction for 30-60 min, adjusting the ratio of reflux amount to extraction amount of the extractor to be 2: 1-5: 1, and keeping for 10-30 min;
(3) opening a membrane component feeding pump, setting the feeding side pressure to be 0.1-0.6 MPa, opening a rectifying tower feeding pump 22 after 60-120 min, and starting a vacuum pump 23 when the liquid level of a tower kettle reaches 50-60% to control the absolute pressure of the tower top to be 5-20 kPa;
(4) condensing the ethanol steam at the tower top by a vacuum pump 23, and then feeding the condensed ethanol steam into a stirring tank through a buffer tank; and filtering and drying the liquid extracted from the tower kettle to obtain a zein product.
According to the zein production method provided by the application, the solvent loss is reduced, the energy consumption is reduced, the production efficiency is improved, and the zein product with higher purity is finally obtained.
The method is not only suitable for producing zein by using corn protein powder as a raw material, but also suitable for producing zein by using crops such as corn, wheat, soybean, coconut and the like as raw materials.
The advantageous effects of the present application will be further described with reference to specific examples.
Example 1
Respectively adding an aqueous solution with the mass fraction of ethanol of 60% into a stirring kettle and a buffer tank, wherein the adding amount of the stirring kettle and the buffer tank is 40% of the volume, the temperature of the stirring kettle is set to be 40 ℃, and the stirring speed is set to be 100 r/min. Adding 2kg of corn protein powder into an extractor, opening a reflux valve 1, closing a production valve 4, starting an extractor feed pump, carrying out total reflux extraction for 30min, adjusting the opening degrees of the reflux valve 1 and the production valve 4 to ensure that the ratio of the reflux amount of the extractor to the production amount is 2:1, and keeping for 10 min; and (3) opening a membrane component feeding pump, setting the feeding side pressure to be 0.1MPa through a pressure regulating valve 3, opening a rectifying tower feeding pump 22 after 60min, setting the theoretical plate number of the rectifying tower to be 20, feeding the 12 th plate, and starting a tower top vacuum pump 23 to vacuumize when the liquid level of the tower kettle reaches 50%, and controlling the tower top pressure to be 5 kPa. After the system is stable, the temperature of the top of the tower is 21.8 ℃, the temperature of the bottom of the tower is 35.6 ℃, the mass fraction of ethanol in gas extracted from the top of the tower is 90.2%, the gas is condensed into liquid by a condenser after passing through a vacuum pump 23 and enters a buffer tank 25, the mass fraction of ethanol in liquid extracted from the bottom of the tower is 0.2%, and the liquid is filtered and dried to obtain 0.6kg of crude zein, wherein the purity of the zein is 89.4% and the yield of the zein is 30.3%.
Example 2
Respectively adding an aqueous solution with the ethanol mass fraction of 95% into a stirring kettle and a buffer tank, wherein the adding amount of the stirring kettle and the buffer tank is 60% of the volume, the temperature of the stirring kettle is set to be 60 ℃, and the stirring speed is set to be 400 r/min. Adding 3kg of corn protein powder into the extractor; opening a reflux valve 1, closing a production valve 4, starting an extractor feed pump, performing total reflux extraction for 60min, adjusting the opening degrees of the reflux valve 1 and the production valve 4 to ensure that the ratio of the reflux amount of the extractor to the production amount is 5:1, and keeping for 30 min; and (3) opening a membrane component feeding pump, setting the feeding side pressure to be 0.6MPa through a pressure regulating valve 3, opening a rectifying tower feeding pump 22 after 120min, setting the theoretical plate number of the rectifying tower to be 20, feeding the 12 th plate, and starting a tower top vacuum pump 23 to vacuumize when the liquid level of the tower kettle reaches 60%, and controlling the tower top pressure to be 20 kPa. After the system is stable, the temperature of the top of the tower is 48.8 ℃, the temperature of the bottom of the tower is 58.6 ℃, the mass fraction of ethanol in gas extracted from the top of the tower is 94.2%, the gas is condensed into liquid by a condenser after passing through a vacuum pump 23 and enters a buffer tank 25, the mass fraction of ethanol in liquid extracted from the bottom of the tower is 0.5%, and the liquid is filtered and dried to obtain 0.95kg of crude zein, wherein the purity of the zein is 84.7% and the yield of the zein is 31.6%.
Example 3
Respectively adding 55% of water solution of ethanol by mass into a stirring kettle and a buffer tank, wherein the adding amount of the stirring kettle and the buffer tank is 40% of the volume, the temperature of the stirring kettle is set to be 40 ℃, and the stirring speed is set to be 100 r/min. Adding 2kg of corn protein powder into an extractor, opening a reflux valve 1, closing a production valve 4, starting an extractor feed pump, carrying out total reflux extraction for 30min, adjusting the opening degrees of the reflux valve 1 and the production valve 4 to ensure that the ratio of the reflux amount of the extractor to the production amount is 2:1, and keeping for 10 min; and (3) opening a membrane component feeding pump, setting the feeding side pressure to be 0.08MPa through a pressure regulating valve 3, opening a rectifying tower feeding pump 22 after 60min, setting the theoretical plate number of the rectifying tower to be 20, feeding the 12 th plate, and starting a tower top vacuum pump 23 to vacuumize when the liquid level of the tower kettle reaches 50%, and controlling the tower top pressure to be 25 kPa. After the system is stable, the temperature of the top of the tower is 51.6 ℃, the temperature of the bottom of the tower is 63.7 ℃, the mass fraction of ethanol in gas extracted from the top of the tower is 87.4%, the gas is condensed into liquid by a condenser after passing through a vacuum pump 23 and enters a buffer tank 25, the mass fraction of ethanol in liquid extracted from the bottom of the tower is 2.4%, and the liquid is filtered and dried to obtain 0.12kg of crude zein, wherein the purity of the zein is 80.2% and the yield of the zein is 11.3%.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the application provides a method for producing zein by combining a membrane separation technology and reduced pressure rectification, so that zein products with the purity of 85% -90% can be obtained, the recycling of an alcohol solvent is realized, the loss of the solvent is reduced, and the production efficiency is improved. The device for producing the zein can realize long-period stable operation, and also has the advantages of low equipment investment, simplicity in operation, low energy consumption, high solvent recovery rate, no pollution and the like.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (16)
1. A zein production apparatus, comprising:
an extraction unit (10), the extraction unit (10) being configured to dissolve a raw material to obtain an alcoholic solution of zein;
a refining unit (20) in communication with the extraction unit (10) via a solution transfer line (01) and a solvent return line (02), the solution transfer line (01) conveying the zein alcohol solution to the refining unit (20), the refining unit (20) separating the zein and alcohol solvent in the zein alcohol solution, the solvent return line (02) returning the separated alcohol solvent to the extraction unit (10);
the storage stirring unit (30) comprises a stirring kettle (31), and the solution transmission pipeline (01) and the solvent return pipeline (02) are communicated with the stirring kettle (31) and arranged to penetrate through the stirring kettle (31);
wherein the solution transfer line (01) comprises a first transfer section (011) and a second transfer section (012), the solvent return line (02) comprises a first return section (021) and a second return section (022), the extraction unit (10) comprises an extractor (11), the extractor (11) has a material inlet and a material outlet, the material outlet is communicated with the stirred tank (31) through the first transfer section (011), and the stirred tank (31) is communicated with the purification unit (20) through the second transfer section (012); the material inlet is communicated with the stirred tank (31) through the first return section (021), and the stirred tank (31) is communicated with the purification unit (20) through the second return section (022); the extraction unit (10) further comprises an alcohol solvent storage tank (12), the alcohol solvent storage tank (12) is communicated with the first returning section (021), and the alcohol solvent storage tank (12) is communicated with the material outlet through a return line; the production device comprises a solvent recovery unit, the solvent recovery unit comprises an ultrafiltration membrane assembly (41), the ultrafiltration membrane assembly (41) is communicated with and arranged on the first return section (021) and positioned between the alcohol solvent storage tank (12) and the stirring kettle (31), so that the alcohol solvent obtained after ultrafiltration is conveyed to the alcohol solvent storage tank (12);
the ultrafiltration membrane component (41) comprises an ultrafiltration membrane, and the ultrafiltration membrane is a polysulfone ultrafiltration membrane; a concentrated solution returning pipeline (03) is further arranged between the ultrafiltration membrane assembly (41) and the stirring kettle (31), the concentrated solution returning pipeline (03) is used for returning the zein concentrated solution obtained by separating the ultrafiltration membrane assembly (41) to the stirring kettle (31), and a pressure regulating valve (3) is further arranged on the concentrated solution returning pipeline (03); the solvent recovery unit further comprises a membrane component feeding pump (42), and the membrane component feeding pump (42) is communicated with the first returning section (021) and is positioned between the stirring kettle (31) and the ultrafiltration membrane component (41);
the purification unit (20) comprises a rectifying tower (21), and the rectifying tower (21) is communicated with the stirring kettle (31) through the second transmission section (012) and the second return section (022).
2. The production device according to claim 1, wherein the extractor (11) is provided in plurality, and a plurality of the extractors (11) are provided in parallel.
3. A production device according to claim 2, characterized in that a return valve (1) is also arranged on the return line.
4. The production plant according to claim 3, characterized in that said extraction unit (10) further comprises a power element (13), said power element (13) being arranged on said first return section (021) and between said alcoholic solvent tank (12) and said extractor (11).
5. A production device according to claim 4, characterized in that the power element (13) is a reflux pump.
6. The production device according to claim 4,
the first returning section (021) and the first transmission section (011) are both provided with a flow control valve (2), wherein the flow control valve on the first returning section (021) is positioned between the power element (13) and the material inlet.
7. The production device according to any one of claims 1 to 6,
and a rectifying tower feeding pump (22) is communicated with the second transmission section (012).
8. The production device according to claim 7, wherein the second return section (022) is communicated with a vacuum pump (23), a condenser (24) and a buffer tank (25) which are sequentially close to the stirred tank (31).
9. The production device according to claim 8, characterized in that a vacuum gauge (26) is also arranged on the second return stretch (022), and the vacuum gauge (26) is arranged between the rectification column (21) and the vacuum pump (23).
10. A method for producing zein, characterized in that the zein is produced by the production apparatus according to any one of claims 1 to 9; the production method comprises the following steps:
dissolving and extracting the raw materials by adopting an ethanol solution with the volume fraction of 60-95% to obtain an alcohol solution of zein;
purifying the alcohol solution of the zein to obtain zein and an alcohol solvent;
recovering the alcohol solvent for dissolving and extracting the raw material;
in the step of purifying the alcohol solution of the zein, a rectifying tower (21) is adopted to purify the alcohol solution of the zein, and the absolute pressure of the top of the rectifying tower (21) is controlled to be 5-20 Kpa;
while the raw material is subjected to dissolution extraction and the zein alcoholic solution is purified, the production method further comprises the following steps: filtering and intercepting the alcohol solution of the zein by using an ultrafiltration membrane component (41) to obtain filtrate and an intercepted substance, recovering the filtrate for dissolving and extracting the raw materials, and purifying the intercepted substance to obtain the zein; the ultrafiltration membrane in the ultrafiltration membrane component (41) is a polysulfone ultrafiltration membrane, and the ultrafiltration pressure of the ultrafiltration membrane is 0.1-0.6 MPa.
11. The production method according to claim 10, wherein the step of subjecting the raw material to dissolution extraction is performed by subjecting the raw material to multiple dissolution extractions by refluxing.
12. The production method according to claim 11, wherein the dissolution product is recovered while refluxing, and the ratio of the amount of reflux to the amount of recovery is controlled to 2-5: 1.
13. The method of claim 10, further comprising the step of starting the production device prior to production.
14. The method of claim 13, wherein the step of operating the production device comprises:
s1, adding an ethanol water solution with the volume fraction of 60-95% into the alcohol solvent storage tank (12);
s2, adding raw materials into an extractor (11), feeding the ethanol water solution in the alcohol solvent storage tank (12) into the extractor (11) to carry out total reflux extraction on the raw materials for 30-60 min, and then adjusting the ratio of the reflux amount to the extraction amount of the extractor (11) to be 2-5: 1;
s3, keeping for 10-30 min under the condition that the ratio of the reflux amount to the produced amount is controlled to be 2-5: 1, sending the produced liquid into a stirring kettle (31), then filtering and intercepting the produced liquid by using an ultrafiltration membrane component (41) to obtain an intercepted substance, and returning the intercepted substance to the stirring kettle (31), wherein the pressure of the feed side of the ultrafiltration membrane component (41) is controlled within the range of 0.1-0.6 MPa in the filtering and intercepting process;
and S4, keeping the filtration and interception for 60-120 min, sending the mixture of the produced liquid and the intercepted substances in the stirring kettle (31) into a rectifying tower (21) for rectification and purification, and controlling the absolute pressure of the tower top to be 5-20 kPa when the liquid level of the tower kettle of the rectifying tower (21) reaches 50-60% of the volume of the tower kettle so as to evaporate alcohol vapor from the tower top.
15. The production method according to claim 14, wherein the stirring temperature of the stirring tank (31) is 40 ℃ to 60 ℃ and the stirring speed is 100r/min to 400 r/min.
16. The method of claim 14, wherein the step of starting further comprises: the alcohol vapor is further condensed into liquid after being evaporated from the tower top, and the liquid returns to the stirring kettle (31) for reuse.
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| CN104774253A (en) * | 2015-03-06 | 2015-07-15 | 广东省食品工业研究所 | Preparation method for zein |
| CN106009766A (en) * | 2016-05-26 | 2016-10-12 | 中国科学院兰州化学物理研究所 | Method for continuously extracting maize yellow pigment and zein from maize protein meal |
| CN106366171A (en) * | 2016-12-05 | 2017-02-01 | 中国科学院兰州化学物理研究所 | Pilot scale production process and production line of white zein |
| CN206359453U (en) * | 2016-12-05 | 2017-07-28 | 中国科学院兰州化学物理研究所 | A kind of pilot production line of white zein |
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| US7045607B2 (en) * | 1999-05-18 | 2006-05-16 | The Board Of Trustees Of The University Of Illinois | Method and system for extraction of zein from corn |
| US7569671B2 (en) * | 2005-01-06 | 2009-08-04 | The Board Of Trustees Of The University Of Illinois | Method and system for corn fractionation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104774253A (en) * | 2015-03-06 | 2015-07-15 | 广东省食品工业研究所 | Preparation method for zein |
| CN106009766A (en) * | 2016-05-26 | 2016-10-12 | 中国科学院兰州化学物理研究所 | Method for continuously extracting maize yellow pigment and zein from maize protein meal |
| CN106366171A (en) * | 2016-12-05 | 2017-02-01 | 中国科学院兰州化学物理研究所 | Pilot scale production process and production line of white zein |
| CN206359453U (en) * | 2016-12-05 | 2017-07-28 | 中国科学院兰州化学物理研究所 | A kind of pilot production line of white zein |
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