CN107744710B - Method for selectively adsorbing aroma components in tobacco pyrolysis smoke and application - Google Patents
Method for selectively adsorbing aroma components in tobacco pyrolysis smoke and application Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D50/60—Combinations of devices covered by groups B01D46/00 and B01D47/00
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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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The invention discloses a method for selectively adsorbing aroma components in tobacco pyrolysis flue gas by using a solid adsorption material and application thereof, wherein (1) cut tobacco is filled in a tube body of a quartz reaction tube, the solid adsorption material is respectively added into a straight sand core tube and a sand core funnel, an absorption liquid is added into an absorption bottle, an ice block and water are added into an ice bath kettle, and a thermometer is inserted; (2) opening a heating device, introducing cracking atmosphere into a quartz reaction tube, controlling the flow rate to be 30-50 ml/min, introducing condensed water, setting the temperature rise program of the heating device to 600-800 ℃ within 1-2 min, keeping the temperature of 600-800 ℃ for 1.5-2.5 min, cooling to room temperature, and taking out the solid adsorption material which adsorbs aroma components in the tobacco pyrolysis smoke in the straight sand core tube and the sand core funnel. The invention can be used for treating tobacco to obtain the solid phase material adsorbed with smoke components, is applied to novel tobacco products, improves the sensory characteristics of the novel tobacco products, increases the market acceptance of the novel tobacco products and promotes the transformation of consumption forms.
Description
Technical Field
The invention relates to the field of novel tobacco, in particular to a method for selectively adsorbing aroma components in tobacco pyrolysis smoke by using a solid adsorption material.
Background
The enactment of the ban of the regulation in the tobacco control frame convention formulated by the world health organization forbids the diffusion of tobacco smoke in public places, and brings strong impact on the development of the traditional cigarette; on the other hand, new tobacco products have significant advantages in terms of reducing environmental pollution and reducing the potential risk of smoking. In addition, with the change of consumption concept and life style of people, the rapid development of scientific technology and the continuous acceleration of the upgrading and updating speed of commodities, the demand and the focus of tobacco consumers are continuously changed, and under the background of the times, the tobacco industry of all countries around the world is a significant way for the development of the future industry through the research and the development of novel tobacco products.
A small amount of research on tobacco high-temperature treatment technology in China before, mainly aims at a heating device, a process flow and a nicotine extraction technology. For example, the invention application with publication number CN1609104A discloses a method for extracting nicotine from tobacco stem and tobacco stubble by dry distillation, which comprises extracting nicotine from tobacco stem and tobacco stubble by dry distillation, heating the pulverized tobacco stem and tobacco stubble in isolation of air, and absorbing aerosol with water; the raw materials are heated, condensed and seasoned to prepare the liquid cigarette, and the heating temperature is below 550 ℃; the invention application document of CN1050540A discloses a process for preparing nicotine products from tobacco by a dry distillation method, wherein, the tobacco is put into caustic soda for dry distillation and then nicotine is extracted; the invention application document of CN101061888A discloses a high-temperature dry distillation thermal cracking device and a cracking method, wherein tobacco powder is treated at the temperature below 300 ℃ in an inert environment, is absorbed by an organic solvent for analyzing and reading the quality of tobacco leaves, and tobacco waste is treated by adopting a high-temperature treatment technology; the invention application document of CN103315395A discloses a pollution-free low-tar cigarette and a manufacturing method thereof, which is characterized in that tobacco leaves are treated at high temperature, dedusted and condensed, then are flavored, and are added into an inert carrier to prepare the cigarette, wherein the amount of harmful substances such as carbon monoxide, tar, benzopyrene, nitrosamine and the like is obviously reduced compared with the traditional cigarette. Of all the studies, there have been few studies on the collection of smoke with solid materials and the separation of smoke constituents, and they have not been applied to new tobacco products.
Disclosure of Invention
The invention aims to provide a method for selectively adsorbing aroma components in tobacco pyrolysis smoke by using a solid adsorption material, which can be used for treating tobacco to obtain a solid phase material adsorbed with smoke components, is applied to novel tobacco products, improves the sensory characteristics of the novel tobacco products, increases the market acceptance of the novel tobacco products and promotes the transformation of consumption forms.
A tobacco shred pyrolysis and smoke absorption device comprises;
the device comprises a quartz reaction tube, a gas inlet and a gas outlet, wherein one end of the quartz reaction tube is provided with the gas inlet, and the other end of the quartz reaction tube is provided with the gas outlet;
the heating device is sleeved outside the quartz reaction tube;
a thermocouple arranged in the quartz reaction tube;
the device comprises a straight sand core pipe, a sand core funnel and an absorption bottle which are connected in sequence, wherein an air inlet of the straight sand core pipe is connected with an air outlet of a quartz reaction pipe;
the straight condenser pipe is sleeved outside the straight sand core pipe;
and the absorption bottle is arranged in the ice bath kettle.
Preferably, a rotameter is arranged on a pipeline connecting the high-pressure gas source and the quartz reaction tube.
Preferably, the heating means comprises:
a steel heating pipe sleeved outside the quartz reaction pipe;
a copper hollow coil wound on the steel heating pipe;
and the all-solid induction heater is connected with the copper hollow coil through a transformer.
Further preferably, an intelligent regulator connected with the all-solid induction heater is further arranged, and the thermocouple is connected into the intelligent regulator.
Preferably, the straight core tubes are arranged in two stages in series. The product separation can be carried out, and the first stage has a filtering effect, removes part of tar-like heavy component substances and contains most of aromatic hydrocarbon substances, so that the aromatic hydrocarbon substance content in the later extract is reduced.
Preferably, the quartz reaction tube, the straight sand core tube and the sand core funnel are all vertically arranged. Since the extract is mostly in liquid phase, the product can be fully collected in the vertical arrangement.
Preferably, the absorption bottles are connected in series.
The invention also provides a method for selectively adsorbing aroma components in the high-temperature pyrolysis flue gas of tobacco by using the solid adsorption material, and the device for pyrolyzing and absorbing the tobacco shreds and the flue gas comprises the following steps:
(1) filling tobacco shreds into a tube body of a quartz reaction tube, respectively adding a solid adsorption material into a straight sand core tube and a sand core funnel, adding an absorption liquid into an absorption bottle, adding ice blocks and water into an ice bath kettle, and inserting a thermometer;
(2) opening a heating device, introducing cracking atmosphere into a quartz reaction tube, controlling the flow rate to be 30-50 ml/min, introducing condensed water, setting the temperature rise program of the heating device to 600-800 ℃ within 1-2 min, keeping the temperature of 600-800 ℃ for 1.5-2.5 min, cooling to room temperature, and taking out the solid adsorption material which adsorbs aroma components in the tobacco pyrolysis smoke in the straight sand core tube and the sand core funnel.
Preferably, the absorption liquid is propylene glycol.
Preferably, the solid adsorption material is one of alumina, a ZSM-5 molecular sieve and an MCM-41 molecular sieve. Further, the silicon-aluminum ratio of the ZSM-5 molecular sieve is 25-360; the silicon-aluminum ratio of the MCM-41 molecular sieve is full silicon.
Preferably, the cracking atmosphere is nitrogen or air-nitrogen mixed gas with 10-20% of oxygen content.
The temperature raising procedure is as follows: the initial temperature is 20 ℃, the temperature reaches 500-600 ℃ after 1.5min, the temperature reaches 600-800 ℃ after 0.5min, and the temperature is maintained at 600-800 ℃ for 2 min.
Further preferably, the initial temperature is 20 ℃ over 1.5min to 550 ℃, over 0.5min to 600 ℃, and maintained at 600 ℃ for 2 min.
Preferably, the filling height of the cut tobacco in the quartz reaction tube is 8-12 cm, most preferably 10cm, and the tail end of the thermocouple is inserted to a half of the filling height of the cut tobacco.
Preferably, the mass ratio of the tobacco shreds in each reaction to each part of the solid adsorption material is 10: 0.8-1.2; more preferably 10: 1. One part of solid adsorption material is arranged in each straight sand core pipe, and one part of solid adsorption material is arranged in the sand core funnel.
Weighing 10g of tobacco shreds, filling the tobacco shreds into a quartz reaction tube body, controlling the filling height to be 10cm, and inserting the tail end of a thermal electrode of a thermocouple into half of the tobacco shred filling height to ensure the accuracy of temperature measurement. Weighing 3 parts of 1g solid adsorption material, respectively adding the solid adsorption material into two straight sand core tubes and sand core funnels, weighing 2 parts of 25ml absorption liquid, adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice cubes and water into an ice bath kettle to provide an ice water bath, and inserting a thermometer to observe the temperature of the ice water bath. Vacuum silicone grease is coated at an instrument interface to ensure the sealing performance of a reaction system, after the instrument is installed, condensed water of the all-solid-state induction heating instrument, a transformer, a copper hollow coil and a straight condenser pipe is turned on, a high-pressure air source switch is turned on to provide a cracking atmosphere, a certain gas flow is controlled to be 30-50 ml/min, then power switches of the intelligent regulator and the all-solid-state induction heating instrument are turned on, and a temperature rise program is set to reach 600-800 ℃ within 1-2 min.
After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, the heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, the high-pressure gas source and the condensed water are turned off. The solid adsorption material was taken out and placed in a constant temperature and humidity chamber with 60% humidity and 24 ℃ for equilibration for 48 hours.
The solid adsorption material adsorbed with the smoke aroma components obtained by the steps can release the special aroma components during high-temperature combustion of cigarettes under the heating condition of lower temperature, and can improve the sensory quality of the cigarettes when being added into a novel cigarette product, and the sensory enjoyment close to the special sensory enjoyment of the traditional cigarettes can be obtained by consumers while the tar and the harm are reduced.
The invention also provides the solid adsorption material which is prepared by the method and adsorbs the aroma components in the smoke.
The invention also provides application of the solid adsorption material adsorbed with the smoke aroma components in tobacco products.
The invention provides a method for selectively adsorbing aroma components in tobacco pyrolysis smoke by using a solid adsorption material from the aspect of improving the sensory enjoyment of novel tobacco, namely, the smoke released by the pyrolysis of the tobacco is collected by using the solid material, and when the solid material is heated at a low temperature, aroma substances which are not contained in the tobacco and can only be generated by the pyrolysis of the tobacco can be released. The solid material obtained by the method can be added into novel tobacco products, so that the defect of insufficient aroma components is overcome, the sensory quality of the novel tobacco products is improved, consumers can obtain sensory enjoyment close to the special sensory enjoyment of the traditional cigarettes, the market acceptance of the novel tobacco products is further increased, and the change of consumption forms is promoted.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for selectively adsorbing aroma components in tobacco pyrolysis smoke by using a solid adsorption material, wherein the solid adsorption material after smoke adsorption can release aroma substances which are not contained in the tobacco and only generated through pyrolysis under the condition of low temperature heating, and can be added into a novel tobacco product to make up for the defect of insufficient aroma components and improve the sensory quality of the novel tobacco product.
The method has simple treatment process, can obviously improve the sensory quality of the novel tobacco products, increases the market acceptance of the novel tobacco products, promotes the transformation of consumption forms, and has good industrial application prospect.
Drawings
Fig. 1 is a schematic structural diagram of a tobacco shred pyrolysis and smoke absorption device.
In the figure: 1 is the intelligent regulation appearance, 2 is full solid induction heater, 3 is the transformer, 4 is quartz reaction tube, 5 is flowmeter, 6 is high pressurized air source, 7 is copper hollow coil, 8 is the thermocouple, 9 is the steel heating pipe, 10 is straight shape sand core pipe, 11 is straight shape condenser pipe, 12 is the psammitolite funnel, 13 is the wide-necked bottle, 14 is the ice bath pot.
FIG. 2 is a bar graph of the relative released smoke content of the solid adsorbent material of example 1.
FIG. 3 is a bar graph of the relative released smoke content of the solid adsorbent material of example 2.
FIG. 4 is a bar graph of the relative released smoke content of the solid adsorbent material of example 3.
FIG. 5 is a bar graph of the relative released smoke content of the solid adsorbent material of example 4.
FIG. 6 is a bar graph of the relative released smoke content of the solid adsorbent material of example 5.
FIG. 7 is a bar graph of the relative released smoke content of the solid adsorbent material of example 6.
FIG. 8 is a bar graph of the relative released smoke content of the solid adsorbent material of example 7.
FIG. 9 is a bar graph of the relative released smoke of the solid adsorbent material of example 8.
FIG. 10 is a bar graph of the relative released smoke of the solid adsorbent material of example 9.
Detailed Description
The present invention is further described in detail by the following examples, which are not intended to limit the present invention.
As shown in fig. 1, the device for tobacco shred pyrolysis and flue gas absorption comprises an intelligent regulator 1, a heating device, a quartz reaction tube 4, a straight sand core tube 10, a sand core funnel 12, a wide-mouth bottle 12, an ice bath pot 14 and a high-pressure gas source 6.
The quartz reaction tube 4 is vertically arranged, the upper end of the quartz reaction tube is provided with an air inlet, the lower end of the quartz reaction tube is provided with an air outlet, the air inlet is connected with a high-pressure air source 6 through a pipeline, and a rotor flow meter 5 is arranged on the connecting pipeline; two sections of straight shape sand core pipes 10 and a sand core funnel 12 connect gradually and all vertical settings, and the upper port of the straight shape sand core pipe of top section links to each other with the gas outlet of quartz reaction tube, and every straight shape sand core pipe overcoat establishes straight shape condenser tube 11, and during the export of sand core funnel 12 inserted the wide-necked bottle 12, the wide-necked bottle can set up to a plurality ofly that concatenates, and the ice bath 14 is arranged in to the wide-necked bottle.
The quartz reaction tube is sleeved with a heating device, the heating device comprises an all-solid induction heater 2, a transformer 3, a copper hollow coil 7 and a steel heating tube 9, the steel heating tube 9 is sleeved outside the quartz reaction tube, the copper hollow coil 7 is wound on the steel heating tube, the copper hollow coil is connected with the low-voltage output end of the transformer, and the high-voltage input end of the transformer is connected with the all-solid induction heater.
The intelligent regulator 1 is connected with the all-solid induction heater 2, the thermocouple 8 is inserted into the quartz reaction tube, and the thermocouple is connected into the intelligent regulator 1.
The equipment or parts required in the apparatus of the present invention are commercially available.
Example 1
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube 4, weighing 3 parts of 1g of alumina and respectively adding the alumina into two straight sand core tubes 10 and a sand core funnel 12, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouthed bottle 13, adding a proper amount of ice blocks and water into an ice bath pot 14, and inserting a thermometer to observe the temperature of the ice blocks and water. At instrument kneck coating vacuum silicone grease, the instrument installation back that finishes, opens the comdenstion water of all solid induction heating appearance 2, transformer 3, copper hollow coil 7 and straight condenser pipe 11, opens 6 switches of high pressurized air source and provides schizolysis atmosphere nitrogen gas, and gas flow is 50ml/min, then opens intelligent regulation appearance 1, the switch of all solid induction heating appearance 2 to set up the intensification procedure and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorbing materials in the two straight sand core pipes 10 and the sand core funnel 12.
Example 2
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of ZSM-5 molecular sieve (the silica-alumina ratio is 25) and respectively adding the ZSM-5 molecular sieve into two straight sand core tubes and a sand core funnel, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the wide-mouth bottle. Coating vacuum silicone grease at instrument kneck, instrument installation finishes the back, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure gas source switch and provides schizolysis atmosphere nitrogen gas, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the procedure of rising temperature and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 3
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of ZSM-5 molecular sieve (the silica-alumina ratio is 117) and respectively adding the ZSM-5 molecular sieve into two straight sand core tubes and a sand core funnel, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the wide-mouth bottle. Coating vacuum silicone grease at instrument kneck, instrument installation finishes the back, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure gas source switch and provides schizolysis atmosphere nitrogen gas, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the procedure of rising temperature and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 4
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of ZSM-5 molecular sieve (the silica-alumina ratio is 360) and respectively adding the ZSM-5 molecular sieve into two straight sand core tubes and a sand core funnel, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the wide-mouth bottle. Coating vacuum silicone grease at instrument kneck, instrument installation finishes the back, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure gas source switch and provides schizolysis atmosphere nitrogen gas, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the procedure of rising temperature and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 5
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of MCM-41 molecular sieve (the silica-alumina ratio is 25) and respectively adding the molecular sieve into two straight sand core tubes and a sand core funnel, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the wide-mouth bottle. Vacuum silicone grease is coated at the instrument interface, after the instrument is installed, the full-solid induction heating instrument, the transformer and the copper hollow coil) and the condensed water of the straight condenser tube are opened, the high-pressure gas source switch is opened to provide cracking atmosphere nitrogen, the gas flow is 50ml/min, then the power switch of the intelligent regulating instrument and the full-solid induction heating instrument is opened, and the temperature rise program is set as follows: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 6
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of MCM-41 molecular sieve (the silica-alumina ratio is full silicon) and respectively adding the molecular sieve into two straight sand core tubes and sand core funnels, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouth bottle, adding a proper amount of ice blocks and water into an ice bath kettle, and inserting a thermometer to observe the temperature of the wide-mouth bottle. Coating vacuum silicone grease at instrument kneck, instrument installation finishes the back, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure gas source switch and provides schizolysis atmosphere nitrogen gas, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the procedure of rising temperature and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 7
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of aluminum oxide and respectively adding the aluminum oxide into two straight sand core tubes and sand core funnels, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouthed bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the ice blocks and water. Coating vacuum silicone grease at instrument kneck, instrument installation back that finishes, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure air source switch and provides the schizolysis atmosphere for the nitrogen gas air mixture that the oxygen content is 10%, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the intensification procedure and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 8
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of aluminum oxide and respectively adding the aluminum oxide into two straight sand core tubes and sand core funnels, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouthed bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the ice blocks and water. Coating vacuum silicone grease at instrument kneck, instrument installation back that finishes, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure air source switch and provides the schizolysis atmosphere for the nitrogen gas air mixture that the oxygen content is 15%, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the intensification procedure and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
Example 9
Weighing 10g of tobacco shreds and filling the tobacco shreds into a quartz reaction tube body, weighing 3 parts of 1g of aluminum oxide and respectively adding the aluminum oxide into two straight sand core tubes and sand core funnels, weighing 2 parts of 25ml of absorption liquid and adding the absorption liquid into a wide-mouthed bottle, adding a proper amount of ice blocks and water into an ice bath pot, and inserting a thermometer to observe the temperature of the ice blocks and water. Coating vacuum silicone grease at instrument kneck, instrument installation back that finishes, opens the comdenstion water of full solid induction heating appearance, transformer, copper hollow coil and straight condenser pipe, opens high-pressure air source switch and provides the schizolysis atmosphere for the nitrogen gas air mixture that the oxygen content is 20%, and gas flow is 50ml/min, then opens the switch of intelligent regulation appearance, full solid induction heating appearance to set up the intensification procedure and do: the initial temperature is 20 deg.C, and reaches 550 deg.C after 1.5min, and reaches 600 deg.C after 0.5min, and the temperature is maintained at 600 deg.C for 2min, and the process is finished. After the instrument is preheated and the gas and the condensed water are stabilized for a period of time, a heating switch is turned on to start heating until the reaction is finished, the temperature of the system is reduced to the room temperature, and all power supplies, high-pressure gas sources and the condensed water are turned off. And respectively taking out the solid adsorption materials in the two straight sand core pipes and the sand core funnel.
The adsorbing materials obtained in the above examples 1 to 9 after adsorbing the flavor components of the smoke are placed in a constant temperature and humidity chamber with 60% humidity and 24 ℃ for balancing 48 hours, and then subjected to headspace mass spectrometry detection and analysis, and the histogram of the relative content of the released smoke of the solid adsorbing materials is shown in fig. 2 to 10, wherein three parts of the solid adsorbing materials filled in two straight sand core tubes and a sand core funnel are respectively marked as C1, C2 and C3 from top to bottom. According to the result of headspace analysis, most of aromatic hydrocarbons and phenolic substances are adsorbed by the first layer of solid material C1; and the solid material of the first layer of the molecular sieve has obvious adsorption on heterocyclic substances.
The method for selectively adsorbing the aroma components in the tobacco pyrolysis smoke by using the solid adsorbing material is described above for helping understanding of the present invention, but the embodiment of the present invention is not limited by the above examples, and any changes, modifications, substitutions, combinations, and simplifications which do not depart from the principle of the present invention should be equivalent replacement ways, and are included in the protection scope of the present invention.
Claims (6)
1. A method for selectively adsorbing aroma components in tobacco pyrolysis flue gas by using a solid adsorption material, which utilizes a tobacco shred pyrolysis and flue gas absorption device, and comprises the following steps:
the device comprises a quartz reaction tube, a gas inlet and a gas outlet, wherein one end of the quartz reaction tube is provided with the gas inlet, and the other end of the quartz reaction tube is provided with the gas outlet;
the heating device is sleeved outside the quartz reaction tube;
a thermocouple arranged in the quartz reaction tube;
the device comprises a straight sand core pipe, a sand core funnel and an absorption bottle which are connected in sequence, wherein an air inlet of the straight sand core pipe is connected with an air outlet of a quartz reaction pipe;
the straight condenser pipe is sleeved outside the straight sand core pipe;
the absorption bottle is arranged in the ice bath pot;
a rotor flowmeter is arranged on a pipeline connecting the high-pressure gas source and the quartz reaction tube;
a steel heating pipe sleeved outside the quartz reaction pipe;
a copper hollow coil wound on the steel heating pipe;
the all-solid induction heater is connected with the copper hollow coil through a transformer;
an intelligent regulator connected with the all-solid induction heater, wherein the thermocouple is connected into the intelligent regulator
The method comprises the following steps:
(1) filling tobacco shreds into a tube body of a quartz reaction tube, respectively adding a solid adsorption material into a straight sand core tube and a sand core funnel, adding an absorption liquid into an absorption bottle, adding ice blocks and water into an ice bath kettle, and inserting a thermometer; the mass ratio of the tobacco shreds to each part of the solid adsorption material in each reaction is 10: 0.8-1.2; one part of solid adsorption material in each straight sand core pipe and one part of solid adsorption material in the sand core funnel;
(2) introducing cracking atmosphere into the quartz reaction tube, controlling the flow to be 30-50 ml/min, introducing condensed water, setting the temperature rise program of a heating device to 600-800 ℃ within 1-2 min, keeping the temperature of 600-800 ℃ for 1.5-2.5 min, cooling to room temperature, and taking out the solid adsorption material which adsorbs aroma components in tobacco pyrolysis smoke in the straight sand core tube and the sand core funnel.
2. The method of claim 1, wherein the absorption liquid is propylene glycol.
3. The method of claim 1, wherein the solid adsorbent material is one of alumina, ZSM-5 molecular sieve, MCM-41 molecular sieve.
4. The method of claim 1, wherein the temperature-raising procedure is: the initial temperature is 20 ℃, the temperature reaches 500-600 ℃ after 1.5min, the temperature reaches 600-800 ℃ after 0.5min, and the temperature is maintained at 600-800 ℃ for 2 min.
5. A solid adsorbing material with smoke aroma components adsorbed, which is prepared by the method of any one of claims 1 to 4.
6. Use of a solid adsorbent material according to claim 5 having a smoke aroma constituent adsorbed thereon in a smoking article.
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| CN110959892A (en) * | 2018-09-26 | 2020-04-07 | 浙江中烟工业有限责任公司 | Method for preparing functional tobacco shred fragrance raw material through soaking high-pressure low-temperature reaction |
| CN111358034A (en) * | 2020-03-31 | 2020-07-03 | 佛山市高明曦逻科技有限公司 | Tobacco curing barn recovery device and using method thereof |
| CN113812668B (en) * | 2021-09-27 | 2023-03-21 | 浙江中烟工业有限责任公司 | Method for extracting rectified aroma substances by dry distillation of tobacco leaves |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3908160A1 (en) * | 1989-03-13 | 1990-09-27 | Bat Cigarettenfab Gmbh | Smokable article |
| CN101329232A (en) * | 2008-07-28 | 2008-12-24 | 中国烟草总公司郑州烟草研究院 | Method for screening fragrant raw material for cigarette based on thermal cracking - gas chromatograph mass spectrogram multiple techniques |
| CN104921287A (en) * | 2015-06-05 | 2015-09-23 | 浙江中烟工业有限责任公司 | Tobacco extract and preparing method and application thereof |
| CN104928026A (en) * | 2015-05-14 | 2015-09-23 | 安徽中烟工业有限责任公司 | Flavoring enhancing electronic cigarette sensory quality, and electronic cigarette liquid |
| CN104983064A (en) * | 2015-06-05 | 2015-10-21 | 浙江中烟工业有限责任公司 | Electronic cigarette liquid and preparation method thereof |
| CN105167170A (en) * | 2015-09-14 | 2015-12-23 | 浙江中烟工业有限责任公司 | Method for preparing electronic cigarette nicotine liquid by means of tobacco subjected to dry distillation pyrolysis |
-
2017
- 2017-09-07 CN CN201710801378.5A patent/CN107744710B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3908160A1 (en) * | 1989-03-13 | 1990-09-27 | Bat Cigarettenfab Gmbh | Smokable article |
| CN101329232A (en) * | 2008-07-28 | 2008-12-24 | 中国烟草总公司郑州烟草研究院 | Method for screening fragrant raw material for cigarette based on thermal cracking - gas chromatograph mass spectrogram multiple techniques |
| CN104928026A (en) * | 2015-05-14 | 2015-09-23 | 安徽中烟工业有限责任公司 | Flavoring enhancing electronic cigarette sensory quality, and electronic cigarette liquid |
| CN104921287A (en) * | 2015-06-05 | 2015-09-23 | 浙江中烟工业有限责任公司 | Tobacco extract and preparing method and application thereof |
| CN104983064A (en) * | 2015-06-05 | 2015-10-21 | 浙江中烟工业有限责任公司 | Electronic cigarette liquid and preparation method thereof |
| CN105167170A (en) * | 2015-09-14 | 2015-12-23 | 浙江中烟工业有限责任公司 | Method for preparing electronic cigarette nicotine liquid by means of tobacco subjected to dry distillation pyrolysis |
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