CN109499369B - Tobacco extract concentrating process - Google Patents
Tobacco extract concentrating process Download PDFInfo
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- CN109499369B CN109499369B CN201811476023.4A CN201811476023A CN109499369B CN 109499369 B CN109499369 B CN 109499369B CN 201811476023 A CN201811476023 A CN 201811476023A CN 109499369 B CN109499369 B CN 109499369B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
- B01D61/005—Osmotic agents; Draw solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/422—Electrodialysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
Abstract
The invention relates to a tobacco extract concentration process, and belongs to the technical field of tobacco extract concentration. The process comprises the steps of carrying out primary purification on a tobacco water extracting solution, then carrying out microfiltration, carrying out forward osmosis concentration on a microfiltration permeating solution, and recycling a diluted drawing solution formed by forward osmosis concentration by adopting an electrodialysis or solar salt drying mode. The invention has low process operation pressure and high safety; the concentration temperature is low, the temperature rise during concentration is small, and heat exchange and temperature reduction are not needed; the membrane pollution is light, the cleaning is simple and convenient, and the cleaning frequency is low. Meanwhile, the process has high concentration degree, and the concentration of the concentrated tobacco extract can reach 60 percent; the concentration process of the tobacco extract of the paper-making reconstituted tobacco can completely replace evaporation concentration; and the loss of materials, nicotine and volatile components in the concentration process is small, the energy consumption is low, and the method is easy to popularize and apply.
Description
Technical Field
The invention belongs to the technical field of concentration of tobacco extract, and particularly relates to a concentration process of tobacco extract.
Background
In the production of paper-making reconstituted tobacco, the extraction of tobacco raw materials comprises two modes of stem and leaf mixed extraction and stem and leaf separated extraction, an intermittent or continuous extraction process is adopted, and the concentration of tobacco extract is generally between 6 and 12 percent no matter what extraction method is adopted.
The concentration of the tobacco extract is a procedure of the production of the reconstituted tobacco by a paper-making method, and aims to improve the concentration of the extract to a high-concentration state with the mass percentage concentration of 40-50 percent suitable for coating reconstituted tobacco sheet bases.
In the production of the paper-making reconstituted tobacco, the concentration of the tobacco extract adopts an evaporation concentration mode. The concentration mode has two defects, one is that the volatile components of the tobacco including nicotine are greatly lost, and the loss amount is about 30-50%; and the second is that the concentration process involves phase change of water, and the energy consumption is high.
Patents CN101606748B, CN102823935A and CN103919272A disclose methods for concentrating tobacco extract liquid membrane based on reverse osmosis principle and driven by external pressure, which are different in pore diameter membrane combination (ultrafiltration, nanofiltration and reverse osmosis), and these methods partially or totally replace the evaporation and concentration process of tobacco extract in the production of reconstituted tobacco, so that the loss of tobacco volatile components including nicotine can be reduced to different degrees, and the energy consumption can be reduced to different degrees. However, problems of high-pressure driving, temperature reduction by using heat exchange equipment and the like exist in nanofiltration and reverse osmosis, and the reverse osmosis membrane is seriously polluted and difficult to clean in the using process. Meanwhile, in the preparation process of the tobacco water extract, the modes of evaporation, nanofiltration and reverse osmosis concentration are also adopted, so that the same problems exist. Therefore, how to overcome the defects of the prior art is an urgent problem to be solved in the technical field of tobacco extract concentration.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a tobacco extract concentration process, which comprises the steps of carrying out primary purification on a tobacco extract, filtering by using a microfiltration membrane, carrying out forward osmosis concentration on a permeate, and recycling a diluted draw solution formed by the forward osmosis concentration by adopting an electrodialysis or solar salt drying mode. The process has the advantages of low loss of materials, nicotine and volatile components, low energy consumption and easy popularization and application.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the percentage numbers represent percent by mass unless otherwise specified herein.
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: removing impurities from the tobacco extract to obtain a primary purified tobacco extract with a suspended matter content of 1-3%;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 0-100 ℃ by adopting a membrane with the aperture of 50-400nm, and stopping filtering when the operating pressure is increased to 0.3MPa to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution;
the adopted drawing agent in the concentration process is inorganic acid salt and/or organic acid salt; the cation of the inorganic acid salt is Na+、K+、Mg2+、Ca2+Or NH4 +The anion is Cl-、SO4 2-，HSO4 -、PO4 3-、HPO4 2-、H2PO4 −、CO3 2-、HCO3 -(ii) a The organic acid salt is potassium, sodium or ammonium salt of malic acid, sorbic acid, benzoic acid, lactic acid and citric acid; concentrating at 5-45 deg.C under 0.1-0.3 MPa; the concentration adopts a single-stage concentration or multi-stage concentration mode of gradual concentration;
step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in an electrodialysis or solar salt mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3).
Further, preferably, the impurity removal mode in the step (1) is one or a combination of several of sedimentation, centrifugation and filtration.
Further, it is preferable that the sedimentation includes natural sedimentation and chemical sedimentation; the centrifugation comprises butterfly centrifugation and horizontal screw centrifugation; the filtration is plate-frame filter pressing, filter screen filtration and filter cloth filtration.
Further, it is preferable that the membrane used in the step (2) is an inorganic membrane or an organic membrane.
Further, it is preferable that the membrane used in the step (2) is a ceramic membrane, a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane.
Further, it is preferable that the membrane used in the step (2) has a pore diameter of 200nm and a concentration temperature of 10 to 40 ℃.
Further, it is preferable that an equal volume of water is added to the retentate obtained in step (2), the microfiltration step is performed again, an equal volume of water and the microfiltration step are repeated again for 1 to 2 times, and the permeate is combined for forward osmosis concentration.
Further, preferably, the drawing agent is NaCl, CaCl2、NH4HCO3And (NH)4)2HPO4One or a combination of more of the above; the concentration temperature is 15-35 ℃; the membrane adopted for forward osmosis concentration is a hollow fiber forward osmosis membrane.
Further, preferably, in the step (3), a three-stage concentration mode of step-by-step concentration is adopted for concentration, and the dehydration amount of the first-stage, second-stage and third-stage concentration is respectively 55-60%, 25-30% and 10-15% of the total dehydration amount and is 100% in total; the membrane adopted for forward osmosis concentration is a hollow fiber forward osmosis membrane with aquaporin, acetate fiber, triacetate fiber or polyamide as a separation layer.
Further, it is preferable that in the step (4), the electrodialysis temperature is 20 to 35 ℃ and the pressure is 0.1 to 0.3MPa, and a homogeneous membrane is used.
The invention has no special limitation on the acquisition mode of the tobacco extract, and can be a product obtained by tobacco according to a conventional extraction process.
The primary purification step and the microfiltration and filtration step are abbreviated as MF process, because the extracting solution obtained by solid-liquid separation after the extraction of the tobacco raw material has impurities such as silt, tiny tobacco raw material fragments and the like, the primary purification is firstly needed, but the primarily purified tobacco extracting solution is still not clear and is in a suspension emulsion state, and the content of suspended matters is limited to be within the range of 1-3 percent.
For the microfiltration and filtration step, the invention preferably selects a ceramic membrane, a polyvinylidene fluoride membrane and a polytetrafluoroethylene membrane which have strong pollution resistance, easy cleaning and weak adsorption capacity to the effective components of the tobacco. The pore size of the membrane is in the range of 50-400nm, preferably 200nm, to ensure proper flux during microfiltration, lactic acid bacteria are retained, and the filtered permeate is clarified to true solution. Meanwhile, the effective components in the trapped fluid are recovered by adding water for dilution and then continuing to filter.
The forward osmosis concentration step is abbreviated as FO process, and is preferably a hollow fiber forward osmosis membrane taking aquaporin, acetate fiber, triacetate fiber or polyamide as a separation layer, and more preferably an aquaporin hollow fiber forward osmosis membrane. Preferably, the concentration adopts a three-stage concentration mode of step-by-step concentration, the dehydration amount of the first-stage concentration, the dehydration amount of the second-stage concentration and the dehydration amount of the third-stage concentration are respectively 55-60%, 25-30% and 10-15% of the total dehydration amount and 100% of the total dehydration amount, the draw solution formed by the third-stage concentration and with reduced concentration is used as the draw solution of the second-stage concentration, and the draw solution further diluted by the second-stage concentration is used as the draw solution of the first-stage concentration. When the draw solution is not required to be recycled (for example, NaCl is used as a draw agent and can be discharged into sea and salt lake), a multi-stage concentration mode is preferably adopted, and the principle of the lowest use amount of the draw agent is followed. The temperature for concentration is suitably 5-45 deg.C, preferably 15-35 deg.C; the operation pressure is 0.1-0.3 MPa.
When the tobacco extract is subjected to forward osmosis concentration, the dosage of the drawing agent is not particularly limited as long as the concentration of the prepared tobacco extract concentrated solution is not more than 60%.
The step of drawing liquid post-treatment electrodialysis is abbreviated as ED process. The electrodialysis ion exchange membrane can be used for recycling forward osmosis concentrated draw solution, membrane selection is carried out according to the principle of lowest energy consumption, a homogeneous membrane and a semi-homogeneous membrane are preferably selected, and a heterogeneous membrane is carefully selected. The electrodialysis is suitably carried out at a temperature of from 5 to 45 deg.C, preferably from 20 to 35 deg.C; the operation pressure is 0.1-0.3 MPa.
Drying salt in the sun: the diluted draw solution generated in the concentration process is concentrated to a concentration not lower than that required by the last stage of concentration by using solar energy and wind energy as power.
The method and the process can completely replace the preparation process (such as evaporation concentration and the like) of the concentrated solution of the tobacco extract in the production of the paper-making reconstituted tobacco, and the concentrated solution of the tobacco extract concentrated to the concentration of not less than 40 percent can be coated, and the concentration can reach 60 percent at most. Similarly, the process can partially or completely replace the existing preparation process of the tobacco water extract, can be completely replaced when the concentration requirement of the water extract does not exceed 60 percent, and can be concentrated to the concentration of 40 to 60 percent by forward osmosis and then evaporated and concentrated when the concentration requirement of the water extract exceeds 60 percent, so that the denaturation of a large amount of heat-sensitive substances can be avoided, the loss of materials and the like can be reduced, and the energy consumption can be reduced.
Compared with the prior art, the invention has the beneficial effects that:
(1) the operation pressure is low (0.1-0.3 MPa), and the safety is high;
(2) the concentration temperature is low (5-45 ℃), the temperature rise is small during concentration, and heat exchange is not needed;
(3) the membrane pollution is light, the cleaning is simple and convenient, and the cleaning frequency is low;
(4) the concentration degree is high, and the concentration of the tobacco extract of the extractum after concentration can reach 60 percent;
(5) the material, nicotine and volatile components are slightly lost (all less than 1%) in the forward osmosis concentration process;
(6) the concentration energy consumption in the forward osmosis concentration process is low, 1 ton of water is removed by concentration, and the power consumption is less than 30 ℃.
The forward osmosis concentration method based on the forward osmosis principle and driven by the osmotic pressure difference of a separation system is not reported to be applied to the concentration of tobacco extract.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
Example 1
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: removing impurities from the tobacco extract to obtain a primary purified tobacco extract with a suspended matter content of 1-1.5%;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 90-100 ℃ by adopting a membrane with the pore diameter of 400nm, wherein the operating pressure is increased to 0.3MPa during microfiltration, and stopping filtration to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution;
the adopted drawing agent in the concentration process is NaCl; concentrating at 5-20 deg.C under 0.1-0.3 MPa; the concentration adopts a single-stage concentration mode; the membrane adopted for forward osmosis concentration is a polyamide forward osmosis membrane;
step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in an electrodialysis mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3).
Example 2
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: removing impurities from an extracting solution obtained by solid-liquid separation after extracting a tobacco raw material to obtain a primary tobacco purification extracting solution with the suspended matter content of 1.8-3%; the impurity removal mode is natural sedimentation;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 10-20 ℃ by adopting a ceramic membrane with the aperture of 50nm, wherein the operating pressure is increased to 0.3MPa during microfiltration, and stopping filtration to obtain trapped liquid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution;
the adopted drawing agent in the concentration process is potassium citrate; concentrating at 25-45 deg.C under 0.1-0.3 MPa; the concentration adopts a single-stage concentration mode; the forward osmosis membrane is aquaporins hollow fiber forward osmosis membrane
Step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in a solar salt drying mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3).
Example 3
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: removing impurities from an extracting solution obtained by solid-liquid separation after extracting a tobacco raw material to obtain a primary tobacco purification extracting solution with the suspended matter content of 1.8-2.5%; removing impurities by horizontal screw centrifugation;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 0-40 ℃ by adopting a polyvinylidene fluoride membrane with the pore diameter of 200nm, increasing the operating pressure to 0.3MPa during microfiltration, and stopping filtering to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution; the forward osmosis concentration adopts a membrane of an acetate fiber hollow fiber forward osmosis membrane;
the adopted drawing agents in the concentration process are potassium malate, potassium sorbate, potassium benzoate and potassium lactate (the mass ratio is 1: 1: 1: 1); the concentration temperature is 15-35 deg.C, and the pressure is 0.1-0.3 MPa; the concentration adopts a three-stage concentration mode of gradual concentration; the first-stage, second-stage and third-stage concentration dehydration amounts are respectively 55%, 30% and 15% of the total dehydration amount, and the total dehydration amount is 100%;
step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in an electrodialysis mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3); the electrodialysis temperature is 20-35 deg.C, the pressure is 0.1-0.3MPa, and homogeneous membrane is adopted.
Adding water with the same volume to the trapped fluid obtained in the step (2), performing the microfiltration step again, repeating the step of adding water with the same volume to the trapped fluid obtained in the step (2) and performing the microfiltration step for 1 time, combining the permeate and performing forward osmosis concentration.
Example 4
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: removing impurities from an extracting solution obtained by solid-liquid separation after extracting a tobacco raw material to obtain a primary tobacco purification extracting solution with the suspended matter content of 1-3%; the impurity removal mode is plate-frame filter pressing;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 20-30 ℃ by adopting a polytetrafluoroethylene membrane with the aperture of 100nm, wherein the operating pressure is increased to 0.3MPa during microfiltration, and stopping filtration to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution; the forward osmosis concentration adopts a membrane of a triacetyl cellulose hollow fiber forward osmosis membrane;
the drawing agent adopted in the concentration process is NaCl, KCl and NH4HCO3And (NH)4)2HPO4The mixture of (1: 1: 1: 1); concentrating at 20-30 deg.C under 0.1-0.3 MPa; the concentration adopts a single-stage concentration or a multi-stage concentration mode of three-stage concentration; the dehydration amount of the first-stage, second-stage and third-stage concentration is respectively 58%, 28% and 14% of the total dehydration amount, and the total dehydration amount is 100%.
Step (4), post-treatment of the drawing liquid: concentrating the diluted solution formed in the step (3) by adopting an electrodialysis mode, and recycling the concentrated solution to the forward osmosis concentration process in the step (3); the electrodialysis temperature is 5-45 deg.C, the pressure is 0.1-0.3MPa, and a semi-homogeneous membrane is adopted.
Adding water with the same volume into the trapped fluid obtained in the step (2), performing the microfiltration step again, repeating the water with the same volume and the microfiltration step for 2 times, combining the permeate and performing forward osmosis concentration.
Example 5
A tobacco extract concentrating process comprises the following steps:
step (1), primary purification: extracting tobacco raw materials, and then carrying out solid-liquid separation to obtain an extracting solution for removing impurities to obtain a primary purified tobacco extracting solution with the suspended matter content of 2-2.4%; the impurity removal mode is sedimentation and centrifugation; the sedimentation is chemical sedimentation, and the centrifugation is butterfly centrifugation;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 10-40 ℃ by adopting a polytetrafluoroethylene membrane with the pore diameter of 200nm, increasing the operating pressure to 0.3MPa during microfiltration, and stopping filtering to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution;
the drawing agent adopted in the concentration process is NaH2PO4And sodium citrate (in a mass ratio of 1: 1); the concentration temperature is 18-22 deg.C, and the pressure is 0.1-0.3 MPa; the concentration adopts a three-stage concentration mode of gradual concentration; the dehydration amount of the first-stage, second-stage and third-stage concentration is 60%, 30% and 10% of the total dehydration amount respectively, and the total dehydration amount is 100%.
Step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in an electrodialysis mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3). The electrodialysis temperature is 25-30 deg.C, the pressure is 0.1-0.3MPa, and homogeneous membrane is adopted.
Adding water with the same volume to the trapped fluid obtained in the step (2), performing the microfiltration step again, repeating the step of adding water with the same volume to the trapped fluid obtained in the step (2) and performing the microfiltration step for 1 time, combining the permeate and performing forward osmosis concentration.
Application example 1: forward osmosis concentration of tobacco leaf extract in MF + FO + ED mode
MF process: cooling 100L of leaf extract with mass percent concentration of 8.2% obtained by natural sedimentation primary purification to 26 ℃, filtering through a 100nm polyvinylidene fluoride microfiltration membrane, when the operation pressure is increased to 0.3MPa, adding equal volume of tap water (5.6L) into the trapped fluid, continuing to filter until the operation pressure is increased to 0.3MPa, adding equal volume of tap water (5.2L) into the trapped fluid, continuing to filter until the operation pressure is increased to 0.3MPa, and ending the filtration to obtain 105L of permeate with mass percent concentration of 7.1%.
FO process:
primary concentration: 10L of 7.1% permeation solution (27 ℃) is placed in a forward osmosis concentration chamber, a aquaporin hollow fiber forward osmosis membrane is a concentration membrane, 7.1L of NaCl solution (25 ℃) with the mass percent concentration of 8.5% is added into a drawing liquid chamber, a circulating pump is started for concentration, when the water absorption capacity of the drawing liquid is basically lost (the liquid level change is observed or determined from the conductivity change of the drawing liquid and the concentration liquid), the concentration is finished, and a primary concentrated solution with the mass percent concentration of 14.5% is obtained. In the first-stage concentration process, the pressure is between 0.1 and 0.15MPa, and the temperature of the concentrated solution and the temperature of the liquid extract are gradually close to each other due to heat exchange and are lower than 27 ℃.
Secondary concentration: after the first-stage concentration is finished, the diluted Draw Solution (DS) is replaced by 5L of NaCl solution (25 ℃) with the mass percent concentration of 12%, and second-stage concentration is carried out according to the first-stage concentration mode to obtain second-stage concentrated solution with the mass percent concentration of 28.6%. In the process of secondary concentration operation, the pressure is between 0.1 and 0.2 MPa, and the temperatures of the concentrated solution and the liquid drawing solution are basically consistent and are lower than 26 ℃.
And (3) third-stage concentration: after the second-stage concentration is finished, the diluted Draw Solution (DS) is replaced by 4L of NaCl solution (25 ℃) with the mass percent concentration of 15%, and third-stage concentration is carried out according to a first-stage concentration mode to obtain third-stage concentrated solution with the mass percent concentration of 48.5%. In the process of three-stage concentration operation, the pressure is between 0.1 and 0.3MPa, and the temperatures of the concentrated solution and the liquid drawing solution are basically consistent and are lower than 26 ℃.
An ED process:
12.5L of the diluted draw solution with the mass percent concentration of 4.8 percent formed by the first-stage forward osmosis in the FO process is injected into a dilute chamber and a concentrated chamber of electrodialysis taking a homogeneous membrane as an ion exchange membrane according to the proportion of 2.5-3:1, and the concentration of NaCl solution in the concentrated chamber is increased to 15 percent by mass percent at the temperature of 25-27 ℃ under the operation pressure of 0.1-0.3 MPa.
Application example 2: forward osmosis concentration of stem extract in MF + FO + sun salt
MF process: 100L of stalk extract with the mass percentage concentration of 9.8 percent at 65 ℃ obtained by a primary purification mode of horizontal screw centrifugation and sedimentation is filtered by a ceramic microfiltration membrane with the thickness of 200nm, and the filtration is finished when the operating pressure is increased to 0.3MPa, so that 94L of permeate with the mass percentage concentration of 9.7 percent is obtained, and the temperature is 30 ℃.
FO process:
the first-stage concentration mode: 10L of 9.7% permeate (30 ℃) was placed in a forward osmosis concentration chamber, the polyamide forward osmosis membrane was a concentration membrane, 15L of saturated NaCl solution (30 ℃) was added to the draw solution chamber, and the circulating pump was started to concentrate. The operating pressure is controlled to be 0.1-0.3MPa, and when the electrical conductivity of the material in the concentration chamber and the solution in the drawing liquid chamber is basically constant, the concentration is stopped, so that the tobacco stem concentrated solution with the mass percentage concentration of 51.7% is obtained. The amount of the draw solution in the concentration mode is 3950 g.
A third-stage concentration mode:
the three-stage concentration mode is characterized in that: the draw solution formed by the third-stage forward osmosis and reduced in concentration is used as the draw solution of the second-stage forward osmosis, and the draw solution formed by the second-stage forward osmosis and reduced in concentration is used as the draw solution of the first-stage forward osmosis. The dosage of the penetrant is determined by the draw solution used in the three-stage forward osmosis.
(1) 10L of MF (30 ℃) penetrating fluid with the concentration of 9.7 percent is placed in a forward osmosis concentration chamber, the polyamide forward osmosis membrane is a concentration membrane, 7.2L of NaCl solution with the percentage concentration of 14.3 percent (30 ℃) is added into a drawing liquid chamber during primary concentration, and a circulating pump is started for concentration. The operating pressure is controlled to be 0.1-0.15MPa, and when the electrical conductivity of the material in the concentration chamber and the solution in the drawing liquid chamber is basically constant, the concentration is stopped, and a primary forward osmosis concentrated solution with the mass percentage concentration of 20.7% is obtained.
(2) After the first-stage concentration is finished, the diluted Draw Solution (DS) is replaced by 5.1L of NaCl solution (30 ℃) with the mass percent concentration of 15.1%, second-stage concentration is carried out according to the first-stage concentration mode, the operation pressure is controlled to be 0.1-0.3MPa, and second-stage forward osmosis concentrated solution with the mass percent concentration of 31.5% is obtained.
(3) And (3) third-stage concentration: and after the second-stage concentration is finished, replacing the diluted Draw Solution (DS) with 4L of saturated NaCl solution (30 ℃), and performing third-stage concentration in a first-stage concentration mode, wherein the operation pressure is controlled to be 0.1-0.3MPa, so that a third-stage forward osmosis concentrated solution with the mass percent concentration of 51.3% is obtained.
The amount of the drawing agent in the three-stage concentration mode is 1050 g.
The salt drying process: in the salt-solarizing pond, the low-concentration absorption liquid is evaporated and concentrated to a high-concentration absorption liquid state by solar energy and wind energy, and the best effect is to precipitate crystals.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A tobacco extract concentrating process is characterized by comprising the following steps:
step (1), primary purification: removing impurities from the tobacco extract to obtain a primary purified tobacco extract with a suspended matter content of 1-3%;
step (2), microfiltration and filtration: carrying out microfiltration on the primary purified extracting solution of the tobacco obtained in the step (1) at 0-100 ℃ by adopting a membrane with the aperture of 50-400nm, and stopping filtering when the operating pressure is increased to 0.3MPa to obtain trapped fluid and permeate;
and (3) forward osmosis concentration: carrying out forward osmosis concentration on the permeate obtained in the step (2) to obtain a concentrated solution of a tobacco extract and a diluted draw solution;
the adopted drawing agent in the concentration process is inorganic acid salt and/or organic acid salt; the cation of the inorganic acid salt is Na+、K+、Mg2+、Ca2+Or NH4 +The anion is Cl-、SO4 2-，HSO4 -、PO4 3-、HPO4 2-、H2PO4 −、CO3 2-、HCO3 -(ii) a The organic acid salt is potassium, sodium or ammonium salt of malic acid, sorbic acid, benzoic acid, lactic acid and citric acid; concentrating at 5-45 deg.C under 0.1-0.3 MPa; the concentration adopts a single-stage concentration or multi-stage concentration mode of gradual concentration;
step (4), post-treatment of the drawing liquid: concentrating the diluted draw solution formed in the step (3) in an electrodialysis or solar salt mode, and recycling the concentrated draw solution to the forward osmosis concentration process in the step (3).
2. The tobacco extract concentrating process according to claim 1, wherein the impurity removal manner in the step (1) is one or more of sedimentation, centrifugation and filtration.
3. The tobacco extract concentrating process according to claim 2, wherein the sedimentation comprises natural sedimentation and chemical sedimentation; the centrifugation comprises butterfly centrifugation and horizontal screw centrifugation; the filtration is plate-frame filter pressing, filter screen filtration and filter cloth filtration.
4. The process for concentrating a tobacco extract according to claim 1, wherein the membrane used in the step (2) is an inorganic membrane or an organic membrane.
5. The process for concentrating a tobacco extract according to claim 1, wherein the membrane used in the step (2) is a ceramic membrane, a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane.
6. The process for concentrating tobacco extract according to claim 1, wherein the membrane used in step (2) has a pore size of 100-200nm and a concentration temperature of 10-40 ℃.
7. The tobacco extract concentrating process according to claim 1, wherein an equal volume of water is added to the retentate obtained in step (2), the microfiltration step is performed again, an equal volume of water and the microfiltration step are repeated for 1-2 times to obtain a retentate, and the permeate is combined for forward osmosis concentration.
8. The tobacco extract concentrating process according to claim 1, wherein in the step (3), the extracting agent is NaCl, CaCl2、NH4HCO3And (NH)4)2HPO4One or a combination of more of the above; the concentration temperature is 15-35 ℃; the membrane adopted for forward osmosis concentration is a hollow fiber forward osmosis membrane.
9. The tobacco extract concentrating process according to claim 1, wherein in the step (3), the concentration adopts a three-stage concentration mode of gradual concentration, and the dehydration amount of the first-stage, second-stage and third-stage concentration is respectively 55-60%, 25-30%, 10-15% and 100% of the total dehydration amount; the membrane adopted for forward osmosis concentration is a hollow fiber forward osmosis membrane with aquaporin, acetate fiber, triacetate fiber or polyamide as a separation layer.
10. The tobacco extract concentrating process according to claim 1, wherein in the step (4), the electrodialysis temperature is 20-35 ℃, the pressure is 0.1-0.3MPa, and a homogeneous membrane is adopted.
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| CN109938389B (en) * | 2019-04-28 | 2021-08-31 | 河南卷烟工业烟草薄片有限公司 | Purification method capable of removing small particle suspended matters in tobacco extract |
| CN111040879A (en) * | 2019-12-31 | 2020-04-21 | 云南中烟新材料科技有限公司 | Preparation method and application of grape concentrated juice for preparing tobacco flavor |
| CN111170989B (en) * | 2020-01-15 | 2023-07-25 | 云南中烟新材料科技有限公司 | Method for preparing nicotine sulfate |
| CN111495192A (en) * | 2020-06-09 | 2020-08-07 | 云南中烟再造烟叶有限责任公司 | Concentration method for extracting nicotine condensate by steam distillation |
| CN112094694A (en) * | 2020-09-19 | 2020-12-18 | 云南中烟新材料科技有限公司 | Drawing agent for forward osmosis concentration of tobacco flavor and application thereof |
| CN114684956B (en) * | 2020-12-31 | 2023-10-17 | 南通醋酸化工股份有限公司 | Membrane separation method for recycling sorbic acid in sorbic acid wastewater |
| CN112998310B (en) * | 2021-03-08 | 2023-01-24 | 山东瑞博斯烟草有限公司 | Concentrated solution of tobacco water extract, concentration method and application |
| CN113180284B (en) * | 2021-03-18 | 2022-07-29 | 云南中烟新材料科技有限公司 | Method for extracting and concentrating tobacco water extract |
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