CN115251449A - Process for optimizing near-critical water (NCW) liquefied tobacco stems through orthogonal test - Google Patents
Process for optimizing near-critical water (NCW) liquefied tobacco stems through orthogonal test Download PDFInfo
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- CN115251449A CN115251449A CN202210831743.8A CN202210831743A CN115251449A CN 115251449 A CN115251449 A CN 115251449A CN 202210831743 A CN202210831743 A CN 202210831743A CN 115251449 A CN115251449 A CN 115251449A
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
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Abstract
The invention discloses a process for optimizing near-critical water (NCW) liquefied tobacco stems by an orthogonal test, which comprises the following steps of: step one, placing tobacco stems into an oven at 80 ℃ for drying until the tobacco stems are constant in weight, crushing the tobacco stems by a crusher, sieving the crushed tobacco stems by a 40-mesh sieve, and sealing and storing the crushed tobacco stems for later use; step two, weighing the crushed tobacco stems and deionized water according to a material-liquid ratio, and putting the tobacco stems and the deionized water into a reaction kettle inner container, wherein the total mass of the fed materials is 150g and accounts for about 3/5 of the total volume of the reaction kettle inner container; the invention adopts an orthogonal test method to prepare a series of tobacco stem leaching liquor; the influence of the liquid ratio, the temperature and the time of the NCW reaction material on the tobacco stem liquefaction rate and the content of various nutrients in the leaching solution is researched by a range analysis method, an analysis of variance method and a membership function comprehensive analysis method, the optimal conditions of the NCW treatment on the tobacco stems are determined, the process flow is simple, the operation is convenient, and the maximum comprehensive evaluation value of the T9 treatment can be accurately judged from the graph 2 and the graph 3 and is the optimal treatment combination.
Description
Technical Field
The invention relates to the technical field of near-critical water liquefaction of tobacco stems, in particular to a process for optimizing near-critical water (NCW) liquefaction of tobacco stems by an orthogonal test.
Background
The near-critical water technology is an environment-friendly and efficient solid waste treatment method developed in recent years; the method takes the waste tobacco stems as raw materials, adopts orthogonal test design, optimizes the near-critical water treatment tobacco stem process, and provides theoretical support for developing plant nutrient solution or organic fertilizer by utilizing waste biomass; in recent years, with the development of the production technology of the tobacco industry, the recycling of the waste tobacco stems is improved to a certain extent, and the recycling approaches mainly comprise: the method comprises the steps of producing reconstituted tobacco leaves and tobacco stem extracts, extracting natural active ingredients, preparing organic fertilizers through biological fermentation and the like, however, the existing process ratio for liquefying tobacco stems by near-critical water is complex, the operation is troublesome, the influence of the liquid-to-liquid ratio of reaction materials, temperature and time on the liquefaction rate cannot be accurate, the optimal conditions for treating the tobacco stems by the near-critical water cannot be well judged, and the method is not worthy of wide popularization and application.
Disclosure of Invention
The invention aims to provide an orthogonal test optimized near-critical water (NCW) tobacco stem liquefying process, and a series of tobacco stem leaching liquor is prepared by adopting an orthogonal test method; the influence of the liquid ratio, the temperature and the time of the NCW reaction material on the tobacco stem liquefaction rate and the content of various nutrients in the leaching solution is researched by a range analysis method, an analysis of variance method and a membership function comprehensive analysis method, the optimal conditions of the NCW treatment on the tobacco stems are determined, the process flow is simple, the operation is convenient, and the maximum comprehensive evaluation value of the T9 treatment can be accurately judged from the graph 2 and the graph 3 and is the optimal treatment combination.
The purpose of the invention can be realized by the following technical scheme:
an orthogonal test optimization near-critical water (NCW) tobacco stem liquefying process comprises the following steps:
step one, cleaning tobacco stems, placing the tobacco stems in an oven at 80 ℃ for drying to constant weight, crushing the tobacco stems by using a crusher, sieving the crushed tobacco stems by using a 40-mesh sieve, and sealing and storing the crushed tobacco stems for later use;
step two, weighing the crushed tobacco stems and deionized water according to a material-liquid ratio, and putting the tobacco stems and the deionized water into a reaction kettle inner container, wherein the total mass of the fed materials is 150g and accounts for about 3/5 of the total volume of the reaction kettle inner container;
step three, placing the inner container into a high-pressure reaction kettle, adjusting parameters such as temperature and reaction constant temperature time, running a reaction kettle temperature-rising program, and preserving heat for 15-90min according to preset constant temperature time to finish the reaction;
after the reaction is finished, naturally cooling the reaction kettle for 12 hours to below 30 ℃, opening a deflation valve to deflate to enable all gas in the reaction kettle to be released, then opening the reaction kettle, taking out the liner, weighing the total weight of the liner and the reaction product, subtracting the mass of the liner to obtain the total mass of the reaction product, and taking out the reaction product;
fifthly, carrying out liquid-solid separation on the reaction product by using a centrifugal machine, wherein the rotating speed of the centrifugal machine is 6000r/min, the time is 15min, the liquid phase part is the tobacco stem leaching liquor, and the solid phase part is solid residues;
step six, dividing the leaching liquor obtained in the step five into two parts: the first part is dried by a vacuum rotary evaporator at the temperature of 55 ℃, the obtained product is water-soluble oil, the mass of the water-soluble oil is weighed, and the yield of the water-soluble oil is calculated according to the proportion; the second part adopts an inductively coupled plasma mass spectrometer, a total organic carbon analyzer and a full-automatic chemical analyzer to analyze the contents of organic matters, nitrogen, phosphorus, potassium and trace elements in the second part
Step seven, wrapping the obtained solid residues with qualitative filter paper, putting the wrapped solid residues into a Soxhlet extractor, connecting condensed water, adding acetone, repeatedly refluxing, extracting and cleaning for 48 hours until the upper layer acetone is clear, taking out the residues, drying at the drying temperature of 50 ℃, weighing the total mass of the residues, and calculating the residue rate.
As a further scheme of the invention: in the second step, the model of the reaction kettle is YZPR-250, and the specification is 250ml.
As a further scheme of the invention: in the second step, the material-liquid ratio (the mass ratio of the tobacco stalk raw material to the deionized water) is as follows: 1, 6.5, 1:4, and feedstock + water =150g.
As a further scheme of the invention: in the third step, the heating time of the reaction kettle is 70min at the target temperature of 180 ℃, 85min at the target temperature of 220 ℃, and 100min; when the target temperature is reached, the pressure of the reaction system is 0.83 +/-0.20 MPa at 180 ℃, 2.92 +/-0.20 MPa at 220 ℃ and 6.62 +/-0.20 MPa at 260 ℃.
As a further scheme of the invention: and seventhly, evaporating the acetone extracting solution to dryness by using a rotary evaporator at the temperature of 30 ℃, and weighing the mass of the water-insoluble oil to obtain the yield of the water-insoluble oil.
As a further scheme of the invention: the method is characterized in that the feed-liquid ratio, the reaction temperature and the reaction time are taken as factors, each factor is set to be three levels, the test is carried out by adopting an L9 (34) orthogonal test table, the test is carried out by 9 treatments, and each treatment is repeated for 3 times.
The invention has the beneficial effects that: the invention adopts an orthogonal test method to prepare a series of tobacco stem leaching liquor; the influence of the liquid ratio, the temperature and the time of the NCW reaction material on the tobacco stem liquefaction rate and the content of various nutrients in the leaching solution is researched by a range analysis method, an analysis of variance method and a membership function comprehensive analysis method, the optimal conditions for processing the tobacco stems by the NCW are determined, the process flow is simple, the operation is convenient, the maximum comprehensive evaluation value of T9 processing can be accurately judged from the graph 2 and the graph 3, the optimal processing combination is realized, the nutrient content of the liquefied product is high, and the liquefied product can be used as a formula matrix of plant nutrient solution and liquid organic fertilizer.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a table of levels of orthogonality test factors according to the present invention;
FIG. 2 is a trial design of the present invention L9 (34);
FIG. 3 shows the nutrient content of the liquid part of the tobacco stem after liquefaction.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1-3, the orthogonal test optimizes the Near Critical Water (NCW) liquefied stem process, comprising the following steps:
step one, placing tobacco stems into an oven at 80 ℃ for drying until the tobacco stems are constant in weight, crushing the tobacco stems by a crusher, sieving the crushed tobacco stems by a 40-mesh sieve, and sealing and storing the crushed tobacco stems for later use;
step two, taking a material-liquid ratio, a reaction temperature and reaction time as factors, setting three levels for each factor, carrying out the test by adopting an L9 (34) orthogonal test table, carrying out 9 treatments in the test, repeating the treatment for 3 times, weighing the crushed tobacco stems and deionized water according to the material-liquid ratio, putting the crushed tobacco stems and the deionized water into a reaction kettle inner container, and adding 150g of the total mass of the materials to be about 3/5 of the total volume of the reaction kettle inner container; the model of the reaction kettle is YZPR-250, and the specification is 250ml; the material-liquid ratio (mass ratio of tobacco stem raw materials to deionized water) is as follows: 1, 6.5, 1:4, and feedstock + water =150g;
step three, placing the liner into a high-pressure reaction kettle, adjusting parameters such as temperature, reaction constant temperature time and the like, operating a reaction kettle temperature-raising program, preserving heat for 15-90min according to preset constant temperature time, and finishing the reaction; the heating time of the reaction kettle is 70min at the target temperature of 180 ℃, 85min at 220 ℃, and 100min at 260 ℃; when the target temperature is reached, the pressure of the reaction system is 0.83 +/-0.20 MPa at 180 ℃, 2.92 +/-0.20 MPa at 220 ℃ and 6.62 +/-0.20 MPa at 260 ℃;
naturally cooling the reaction product at room temperature for 12h to below 30 ℃ after the reaction is finished, opening a deflation valve to deflate, opening the reaction kettle after all gas in the reaction kettle is released, taking out the liner, weighing the total weight of the liner and the reaction product, subtracting the mass of the liner to obtain the total mass of the reaction product, and taking out the reaction product;
fifthly, carrying out liquid-solid separation on the reaction product by using a centrifugal machine, wherein the rotating speed of the centrifugal machine is 6000r/min, the time is 15min, the liquid phase part is the tobacco stem leaching liquor, and the solid phase part is solid residues;
step six, dividing the leaching liquor obtained in the step five into two parts: the first part is dried in a rotary vacuum evaporator at the temperature of 55 ℃, the obtained product is water-soluble oil, the mass of the water-soluble oil is weighed, and the yield of the water-soluble oil is calculated according to the proportion; the second part adopts an inductively coupled plasma mass spectrometer, a total organic carbon analyzer and a full-automatic chemical analyzer to analyze the contents of organic matters, nitrogen, phosphorus, potassium and trace elements in the second part
And seventhly, wrapping the obtained solid residues with qualitative filter paper, putting the wrapped solid residues into a Soxhlet extractor, connecting condensed water, adding acetone, repeatedly refluxing, extracting and cleaning for 48 hours until the upper layer of acetone is clear, taking out the residues, drying at the drying temperature of 50 ℃, weighing the total mass of the residues, and calculating the residue rate.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. The process for optimizing the near-critical water (NCW) liquefied tobacco stems by using the orthogonal test is characterized by comprising the following steps of:
step one, placing tobacco stems into an oven at 80 ℃ for drying until the tobacco stems are constant in weight, crushing the tobacco stems by a crusher, sieving the crushed tobacco stems by a 40-mesh sieve, and sealing and storing the crushed tobacco stems for later use;
step two, weighing the crushed tobacco stems and deionized water according to a material-liquid ratio, and putting the tobacco stems and the deionized water into a reaction kettle inner container, wherein the total mass of the fed materials is 150g and accounts for about 3/5 of the total volume of the reaction kettle inner container;
step three, placing the liner into a high-pressure reaction kettle, adjusting parameters such as temperature, reaction constant temperature time and the like, operating a reaction kettle temperature-raising program, preserving heat for 15-90min according to preset constant temperature time, and finishing the reaction;
after the reaction is finished, naturally cooling the reaction kettle for 12 hours to below 30 ℃, opening a deflation valve to deflate, opening the reaction kettle after all gas in the reaction kettle is released, taking out the liner, weighing the total weight of the liner and the reaction product, subtracting the mass of the liner to obtain the total mass of the reaction product, and taking out the reaction product;
fifthly, carrying out liquid-solid separation on the reaction product by using a centrifugal machine, wherein the rotating speed of the centrifugal machine is 6000r/min, the time is 15min, the liquid phase part is the tobacco stem leaching liquor, and the solid phase part is solid residue;
step six, dividing the leaching solution obtained in the step five into two parts: the first part is dried by a vacuum rotary evaporator at the temperature of 55 ℃, the obtained product is water-soluble oil, the mass of the water-soluble oil is weighed, and the yield of the water-soluble oil is calculated according to the proportion; the second part adopts an inductively coupled plasma mass spectrometer, a total organic carbon analyzer and a full-automatic chemical analyzer to analyze the contents of organic matters, nitrogen, phosphorus, potassium and trace elements in the second part
Step seven, wrapping the obtained solid residues with qualitative filter paper, putting the wrapped solid residues into a Soxhlet extractor, connecting condensed water, adding acetone, repeatedly refluxing, extracting and cleaning for 48 hours until the upper layer acetone is clear, taking out the residues, drying at the drying temperature of 50 ℃, weighing the total mass of the residues, and calculating the residue rate.
2. The orthogonal test optimized near-critical water (NCW) liquefied tobacco stem process according to claim 1, wherein in the second step, the model of the reaction kettle is YZPR-250, and the specification is 250ml.
3. The orthogonal test optimization near-critical water (NCW) liquefied tobacco stem process according to claim 1, wherein in the second step, the material-liquid ratio (mass ratio of tobacco stem raw material to deionized water) is as follows: 1, 1.
4. The orthogonal test optimized near-critical water (NCW) liquefied tobacco stem process according to claim 1, wherein in the third step, the heating time of the reaction kettle is 70min at a target temperature of 180 ℃, 85min at 220 ℃, and 100min; when the target temperature is reached, the pressure of the reaction system is 0.83 +/-0.20 MPa at 180 ℃, 2.92 +/-0.20 MPa at 220 ℃ and 6.62 +/-0.20 MPa at 260 ℃.
5. The orthogonal test optimized near-critical water (NCW) liquefied tobacco stem process according to claim 1, wherein in the seventh step, the acetone extracting solution is evaporated to dryness through a rotary evaporator at the temperature of 30 ℃, and the mass of the water-insoluble oil is weighed to obtain the yield of the water-insoluble oil.
6. The orthogonal test optimized Near Critical Water (NCW) liquefied tobacco stem process according to claim 1, wherein three horizontal tests are set for each factor, based on the feed-to-liquid ratio, the reaction temperature and the reaction time, and are performed by using an L9 (34) orthogonal test table, wherein the tests are performed for 9 treatments and each treatment is repeated for 3 times.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3043723A (en) * | 1959-09-17 | 1962-07-10 | Gen Cigar Co | Process and product utilizing tobacco stems |
| CN1682613A (en) * | 2004-04-12 | 2005-10-19 | 侯金荣 | Method extracting waste tobacco at subcritical DMC |
| CN105246359A (en) * | 2013-05-07 | 2016-01-13 | 泰顿生物科学有限公司 | Green process to hydrolyze carbohydrates from tobacco biomass using subcritical water |
| CN113876023A (en) * | 2021-09-20 | 2022-01-04 | 河南中烟工业有限责任公司 | Method for preparing tobacco flavor by utilizing tobacco leaf residues and application of tobacco flavor |
-
2022
- 2022-07-14 CN CN202210831743.8A patent/CN115251449A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3043723A (en) * | 1959-09-17 | 1962-07-10 | Gen Cigar Co | Process and product utilizing tobacco stems |
| CN1682613A (en) * | 2004-04-12 | 2005-10-19 | 侯金荣 | Method extracting waste tobacco at subcritical DMC |
| CN105246359A (en) * | 2013-05-07 | 2016-01-13 | 泰顿生物科学有限公司 | Green process to hydrolyze carbohydrates from tobacco biomass using subcritical water |
| CN113876023A (en) * | 2021-09-20 | 2022-01-04 | 河南中烟工业有限责任公司 | Method for preparing tobacco flavor by utilizing tobacco leaf residues and application of tobacco flavor |
Non-Patent Citations (1)
| Title |
|---|
| 朱克明等: "亚临界条件下水相液化烟草工艺及产物的研究", 《广州化工》 * |
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