WO2010063239A1 - 一种制备膨胀烟丝的循环方法 - Google Patents

一种制备膨胀烟丝的循环方法 Download PDF

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Publication number
WO2010063239A1
WO2010063239A1 PCT/CN2009/075332 CN2009075332W WO2010063239A1 WO 2010063239 A1 WO2010063239 A1 WO 2010063239A1 CN 2009075332 W CN2009075332 W CN 2009075332W WO 2010063239 A1 WO2010063239 A1 WO 2010063239A1
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Prior art keywords
tobacco
expansion agent
mpa
pressure
liquid
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PCT/CN2009/075332
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English (en)
French (fr)
Inventor
满鸣
任宏杰
杨继志
何常青
彭黔荣
邓葵
解海鸥
路兰卿
张华�
宋建军
赖东辉
杨大泉
刘晓东
Original Assignee
贵州中烟工业有限责任公司
北京航天试验技术研究所
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Priority claimed from CN2008101825256A external-priority patent/CN101617854B/zh
Application filed by 贵州中烟工业有限责任公司, 北京航天试验技术研究所 filed Critical 贵州中烟工业有限责任公司
Publication of WO2010063239A1 publication Critical patent/WO2010063239A1/zh

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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
    • A24B3/18—Other treatment of leaves, e.g. puffing, crimpling, cleaning
    • A24B3/182—Puffing

Definitions

  • the invention relates to the field of tobacco production and manufacture, in particular to a tobacco manufacturing process in a cigarette manufacturing process. Background technique
  • the technology has the advantages of significantly improving the filling capacity of tobacco, saving cigarettes and reducing the amount of flue gas tar, and the carbon dioxide medium is non-toxic, odorless, non-polluting and inexpensive, it has received widespread attention and welcome from the tobacco industry.
  • research on the promotion, application and improvement of this technology has been extremely rapid.
  • the complexity and high cost of the process are determined.
  • the carbon dioxide expansion technology has large loss, high equipment repair and maintenance cost, and high production cost; the tobacco aroma loss is large, the dry coke gas is heavy, the smoke is dry, and the filling performance is good, but the problem of high breaking rate causes the winding process.
  • the loss in the cigarette is also large, and the actual proportion in the cigarette is lower than the ratio in the formula.
  • many manufacturers have conducted extensive research and improvement on tobacco expansion technology.
  • Chinese Patent Application No. 01142872.4 discloses an improved method for expanding tobacco shreds by first spraying a liquid consisting of a high-boiling point fragrance and a humectant to the tobacco leaf before cutting the tobacco leaf.
  • the ratio of the liquid to the addition is 0.1 - the weight of the tobacco leaf. 2
  • the expanded tobacco is flavored, and the liquid is composed of co 2 supercritical extraction of tobacco essential oil, modified tobacco extract, propylene glycol, modified concentrated juice, reaction flavor, and sprayed material.
  • Liquid ratio is the weight of cut tobacco
  • the method according to the change of the chemical composition before and after the expansion of the tobacco leaves is targeted to the flavoring and feeding treatment, and the aroma and aroma of the expanded tobacco are maximally maintained and compensated, and the intrinsic quality and usability of the expanded tobacco are improved.
  • Chinese Patent Application No. 200410010347.0 discloses a carbon dioxide tobacco expansion method for flue-cured tobacco in which a shredded tobacco is impregnated with liquid carbon dioxide in an impregnation tank, and then the impregnated shredded tobacco is uniformly passed through an expansion pipe with superheated steam to expand the tobacco.
  • the flue-cured tobacco raw materials used have a reducing sugar content of less than 18%, a total volatile base of at least 0.4%, a total nitrogen content of at least 5%, and a nicotine content of at least 4%.
  • the width of the cut tobacco can be 0.8 to 0.9 mm.
  • the carbon dioxide content is 3 to 6%; the initial temperature of the gas flow in the expansion pipe can be 290 to 310 ° C, and the gas flow rate is 29 to 35 m / s.
  • the chemical composition coordination, internal quality and absorption quality of the shredded tobacco were significantly improved by this method, and the use value of the tobacco raw material was significantly improved.
  • Chinese Patent No. 200510010637.X discloses a method for expanding tobacco shreds using water as a medium, in particular, in the process of manufacturing and processing cigarette tobacco, increasing the moisture enrichment of the leaf, and after the warming and humidifying, the hot air is expanded, and the hot air expansion is increasing. After warming and humidifying, the high moisture fraction leaves are passed through a high temperature airflow at a temperature of 250-36 CTC, so that the water content of the filament is reduced to 6-13%, the process of rapidly dehumidifying the tobacco to expand, and the natural air cooling and cooling sequence process.
  • the method overcomes the loss of carbon dioxide expansion technology, high equipment repair and maintenance cost, and high production cost; the tobacco aroma loss is large, the dry coke gas is heavy, the smoke is dry, and the filling performance is good, but the crushing rate is high.
  • the high temperature airflow of 250-36 CTC is required in the whole process, and the requirements for equipment are relatively high.
  • the C0 2 expanded tobacco process needs to be carried out under low temperature and high pressure, the shredded rate of cut tobacco is high, the energy consumption of the equipment is large, and the boiling point of C0 2 is low. Although it can be recycled, its recovery utilization rate is not high;
  • the above-mentioned tobacco-based tobacco expansion process also has high requirements for equipment.
  • the present invention has been specifically proposed. Summary of the invention
  • the object of the present invention is to provide a recycling method for preparing expanded tobacco, which uses zero ODP value, good environmental friendliness, good material compatibility, good permeability, low toxicity, moderate boiling point, and small surface tension. It is easier to infiltrate the tobacco cells and expand the medium to achieve the desired expansion effect, and the method of the invention has mild conditions, greatly reduces the requirements on the equipment, and reduces the cost through the full recycling of the expansion agent, and the whole device has low energy consumption and high automation. Continuous large-scale production can be carried out, and the obtained performance indexes of the expanded tobacco are high, the expansion efficiency of the tobacco is high, and the recovery rate of the expansion agent is high.
  • the present invention adopts the following technical solutions:
  • a recycling method for preparing expanded tobacco comprising the following steps:
  • step (6) Expanding the impregnated shredded tobacco, and simultaneously recovering the liquid expansion agent and the gaseous expansion agent in step (5) The operation of the step (2) or/and the step (3) is performed again.
  • the basic process principle DIET tobacco technology is based on the physical characteristics of C0 2 and of tobacco carried out with liquid C0 2 soaked, is formed of dry ice in the interior and the surface of the thread, tube of rapid inhalation sublimation tube through the venturi, at about 330 ° C In the hot air flow, C0 2 is rapidly sublimated, causing the tobacco to expand.
  • this method has two defects: First, since the input liquid C0 2 is impregnated with shredded tobacco, there is more C0 2 (dry ice) remaining on the impregnated tobacco, which is generally more than 10% of the cut tobacco.
  • a certain amount of liquid C0 2 is introduced to expand in the tank to form a C0 2 cold mist of gas and solid phase mixing, and the mixture is stirred to uniformly mix the cold mist and the tobacco, the temperature of the cut tobacco is lowered to -70 to -85 ° C, and then the impregnation is input. 2; a saturated CO 2 gas having a pressure of 2.5 to 3.5 MPa is supplied to the impregnator; 3 the impregnator is rapidly decompressed, the shredded tobacco is discharged, and the expansion is sent.
  • the vacuuming in the above method is not vacuuming the impregnation tank, but vacuuming a mixing tank before the tobacco enters the impregnation tank, and the liquid C0 2 that is introduced needs to soak the tobacco, so the amount of C0 2 introduced is relatively large.
  • the impregnation process is carried out at a low temperature; and the main purpose of the vacuuming of the present invention is to remove the non-condensable gas air in the impregnation tank and the air and moisture between the shredded tobacco, so that the impregnation tank is under a certain negative pressure.
  • the impregnation of the tobacco by the expansion agent improves the impregnation effect of the tobacco, so that the tobacco can achieve a better expansion effect, increase the filling value, better meet the demand of the cigarette process, and at the same time reduce the pressure of the recycling section and reduce the unnecessary The recovery of the condensable gas; and the addition of the liquid expansion agent is added by spraying, so that the liquid expansion agent can slowly penetrate the tobacco into the bottom of the impregnation tank, and can wet and soften the expansion agent in advance, which is the next process.
  • the gas pressurization is prepared to better improve the impregnation effect, and the liquid expansion agent is charged at a high speed, and the process saves time.
  • the production efficiency is improved, and the expansion agent is further reduced.
  • the impregnation section of the prior art C0 2 tobacco expansion process is completely performed under low temperature and high pressure, and the energy consumption of the equipment is relatively large; Under low temperature and high pressure, the energy consumption of the equipment is small, which reduces operating costs.
  • the invention adopts the gas filling method of gas-liquid mixing to realize the filling of the medium, that is, after the tobacco is put into the impregnation tank, the liquid medium stored in the cold tank is directly passed through the nozzle of the upper head of the impregnation tank according to a certain ratio.
  • the tobacco is sprayed, the liquid medium is filled, and then the quantitative liquid medium is rapidly vaporized by the evaporator into a gaseous medium to pressurize the dip tank from the lower head of the impregnation tank.
  • the preheating in the step (1) is preheating the impregnation tank to 65 ° C to 75 ° C.
  • the preheating of the impregnation tank is mainly for providing energy for the gasification of the medium, ensuring that the medium quickly reaches an equilibrium state in a hot space, which is beneficial to improving the impregnation effect of the tobacco.
  • the evacuation described in the step (1) is such that the pressure of the impregnation tank is in the range of 0.05 MPa to 0.005 MPa.
  • the impregnation tank is evacuated to a pressure of 0.05 Mpa ⁇ 0.005 MPa, and the main purpose thereof is to remove the non-condensable gas air in the impregnation tank and the air and moisture between the shredded tobacco, so that the impregnation tank is at a certain negative Pressing, is beneficial to the impregnation of the tobacco by the expansion agent, improving the impregnation effect of the tobacco, so that the tobacco can achieve a better expansion effect, increase the filling value, better meet the demand of the cigarette process, and at the same time decompress the recovery process of the expansion agent. Reduce the recovery of unnecessary non-condensable gases.
  • the mass ratio of the liquid expanding agent to the shredded tobacco sprayed in the step (2) is 0.5 to 1:1.
  • the liquid expansion agent is used to spray the tobacco, the liquid expansion agent can slowly penetrate the tobacco into the bottom of the impregnation tank, and the spraying is mainly to wet and soften the tobacco in advance, and pressurize the next process gas.
  • the liquid expansion agent can be filled faster, the process saves time, and the production efficiency is improved.
  • the amount of the gaseous expansion agent to be charged in the step (3) is such that the pressure in the impregnation tank is increased to 0.1 MPa to 1 MPa.
  • the impregnation tank is pressurized by a gaseous expansion agent, which can enhance the permeability and uniformity of the tobacco, improve the impregnation effect, and prepare the tobacco to have a better expansion effect.
  • the pressure in the impregnation tank is preferably increased to 0.3 MPa to 0.9 MPa, more preferably 0.5 MPa to 0.8 MPa.
  • the immersion described in the step (4) is immersed for 5 minutes to 30 minutes under the conditions of a pressure of 0.1 MPa to 1 MPa and a temperature of 65 to 120 °C.
  • the pressure is preferably 0.3 MPa to 0.9 MPa, and more preferably 0.5 MPa to 0.8 MPa.
  • Tobacco tobacco impregnation is an important step in the whole process.
  • the length of the tobacco immersion time directly affects the impregnation effect of the tobacco, and the tobacco immersion directly affects the expansion effect of the tobacco.
  • liquid expansion agent is used in the industrial prototype process, the liquid expansion agent is vaporized and infiltrated into the tobacco cells, and the pressure of the impregnation tank is completely increased by the heat supplied by the impregnation tank jacket, so that the pressure of the impregnation tank rises slowly, and the time required for pressure balance Growth is not conducive to the improvement of production efficiency;
  • the gas expansion agent is used in the industrial prototype process, the pressure of the impregnation tank rises rapidly, and the medium molecules can quickly penetrate into the tobacco cells, but the gas expansion agent is filled for too long. It is also not conducive to the improvement of production efficiency.
  • the liquid expansion agent is sprayed onto the tobacco, the gaseous expansion agent is added to the impregnation tank, and then the tobacco is impregnated under the condition that the liquid expansion agent and the gaseous expansion agent coexist, so that the liquid expansion agent is used to cut the tobacco.
  • the medium is wetted and softened, ready for the next process gas pressurization, which can better improve the impregnation effect.
  • the liquid expansion agent can be filled faster, the process saves time and the production efficiency is improved; and the gas expansion agent pairs
  • the impregnation tank is pressurized to enhance the permeability and uniformity of the tobacco, improve the impregnation effect, and have a better expansion effect for the tobacco. Prepare.
  • the immersion for 5 min to 30 min under the conditions of a pressure of 0.1 Mpa to 1 Mpa and a temperature of 65 ° C to 120 ° C can make the cut tobacco have a good expansion effect.
  • the recovery of the liquid expansion agent in the step (5) is to reduce the pressure of the liquid expansion agent to the dipping tank to 1 Mpa ⁇ 0.35 MPa; the gaseous expansion agent Recycling includes high pressure recovery, accelerated recovery and ejector recovery.
  • the recovery of the expansion agent can be improved by recovering the gaseous expansion agent by using different recovery methods.
  • the high pressure recovery is such that the pressure of recovering the gaseous expansion agent into the impregnation tank is lowered to 0.8 MPa to 0.35 MPa.
  • the pressure in the impregnation tank slowly drops to lMpa ⁇ 0.35Mpa.
  • the recovery effect is good.
  • the pressure source in the impregnation tank is used first.
  • a certain amount of gaseous expansion agent is driven into the hot tank through a pipeline, and the purification and preliminary cooling effect of the recovery expansion agent is performed by the hot tank.
  • the gaseous expansion agent returns to the condenser condensation, the medium storage tank is stored, and finally enters the medium measuring tank. recycle.
  • the accelerated recovery is that the pressure of recovering the gaseous expansion agent to the impregnation tank drops to 0.35 MPa ⁇ 0.21 MPa; the ejector recovery is that the pressure of recovering the gaseous expansion agent to the immersion tank drops to 0.21 MPa to 0.11 MPa.
  • the main purpose of the ejector recovery is to recover the balance of the gaseous expansion agent in the impregnation tank, to increase the utilization rate of the expansion agent, and to reduce the consumption of the expansion agent.
  • the liquid expansion agent and the gaseous expansion agent are respectively an alcohol of 4 to 12 carbon atoms, a halogenated ether of 2 to 12 carbon atoms, an alkane of 3 to 12 carbon atoms or 2 or more halogens. a component of an atom-substituted alkane of 3 to 12 carbon atoms or a mixture of two or more components;
  • one or a mixture of two or more of tetrafluoroethane, pentafluoropropane, pentafluorobutane, decafluoropentane or methoxy nonafluorobutane is used.
  • the expansion agent of the present invention not only has a moderate boiling point, but also has the advantages of zero or low ozone depletion potential, low toxicity, good safety and chemical stability.
  • the tobacco expansion agent provided by the invention is easy to recover, transport and store, and the energy consumption is small, thereby greatly reducing the running cost.
  • the shredded tobacco expander provided by the present invention is preferably combined as follows:
  • a tobacco filament expander composition of the present invention is: pentafluorobutane (1, 1, 1, 3, 3-pentafluorobutane, HFC-365mfc) 80-90 %, heptafluoropropane (1, 1, 1, 2, 3, 3, 3- heptafluoropropane, R227ca) 10-20%;
  • the second tobacco expander composition of the present invention has a mass percentage composition of: pentafluorobutane 90-99%, hexafluoropropane (HFC-236fa) 1-10%;
  • a third tobacco expander composition of the present invention having a mass percentage composition of: pentafluorobutane 70-90%, pentafluoropropane (1, 1, 1, 3, 3-pentafluoropropane) , HFC-245fa, R245fa) 10-30%;
  • a fourth tobacco expander composition of the present invention having a mass percentage composition of: pentafluorobutane 90-99%, tetrafluoroethane (1, 1, 1, 2-tetrafluoroethane R134a) 1-10%;
  • a fifth tobacco expander composition of the present invention having a mass percentage composition of: pentafluorobutane 80-90%, decafluoropentane (1, 1, 1, 2, 3, 4, 4, 5, 5, 5-Decafluoropentane, HFC-4310, HFC-43-lOmee) 10-20%.
  • the tobacco expansion agent of the present invention and the preparation method of the above-mentioned five kinds of tobacco expansion agent compositions are prepared according to the method disclosed in the patent application No. 200510008577.8, specifically: the raw materials used are all first-grade products.
  • the above five compositions can be weighed and placed in a preparation tank according to the above ratio, stirred, uniformly mixed, and then subjected to pressure filtration using a 600-mesh filter to obtain the shredded expander combination of the present invention. Things.
  • the gaseous expansion agent and the liquid expansion agent are two different substances or two different combinations, and may be two identical substances or two identical combinations.
  • the expansion agent has a moderate boiling point, and the present invention can also be realized when the gaseous expansion agent or the liquid expansion agent is used.
  • the gaseous expansion agent is formed by evaporation of a corresponding liquid expansion agent. That is, in the present invention, the gaseous expansion agent and the liquid expansion agent are the same substance or the same combination, but only in two different forms. This reduces some equipment and reduces the cost of running.
  • the liquid expansion agent is recovered, gasified, purified, condensed and recycled, and the gaseous expansion agent is recovered, purified, condensed and recycled. use.
  • the liquid expansion agent and the gaseous expansion agent can be sufficiently recovered and reused.
  • the method of expanding the tobacco shred of the present invention is a method commonly used in the prior art, such as microwave expansion or the like. However, the expansion method of the present invention is preferred.
  • the tobacco expansion process of the present invention mainly occurs in an industrial microwave generator chamber, and the medium vapor forms a force pushing outward against the tobacco cell wall to expand the tobacco.
  • the present invention has the following advantages:
  • the filling value is 6.8, the moisture content of the expanded tobacco (12.5 ⁇ 1)%, the whole silk rate is 80%, the water-cured tobacco is zero, and the expanded tobacco has good resilience. High silk rate, no water stains, agglomeration.
  • a padding value is higher than 7.5, the moisture content of the expanded tobacco 12.5 Disabled 0.5%, greater than 90% of the entire wire. It can be seen that with the method of the invention, the expansion effect of the tobacco is obviously superior to the prior art;
  • the recycling method for preparing the expanded tobacco of the present invention can be carried out without using low temperature and high pressure, and the energy consumption of the device is small, thereby reducing the running cost;
  • the recycling method for preparing the expanded tobacco of the present invention adopts a spray method to add a liquid expansion agent, so that the amount of the liquid expansion agent is small, thereby reducing the amount of the expansion agent required for the entire process, thereby reducing the cost.
  • the expansion effect is not reduced by the decrease in the amount of the expansion agent, but the expansion effect is better;
  • the recycling method for preparing expanded tobacco of the present invention adopts zero ODP value, good environmental friendliness, good material compatibility, good permeability, low toxicity, moderate boiling point, small surface tension and easier penetration into cut tobacco.
  • the cells and the expansion medium which achieve the desired expansion effect, and the method of the invention has mild conditions, the requirements on the equipment are greatly reduced, the cost is reduced by the full recycling of the expansion agent, and the whole device is low in energy consumption and high in automation, and can be continuously In large-scale production, the obtained performance indexes of the expanded tobacco are high, the expansion efficiency of the tobacco is high, and the recovery rate of the expansion agent is high.
  • the mass percentage composition of a shredded tobacco expander of this example is: pentafluorobutane 87%, heptafluoropropane 13%.
  • the preparation method is as follows: the raw materials are weighed according to the mass percentage of pentafluorobutane 87% and heptafluoropropane, and then placed in a preparation tank, stirred and uniformly mixed, and then filtered under pressure with a 600-mesh filter to prepare a cost example.
  • the tobacco filament expander composition, the technical index data is shown in Table 1.
  • the liquid tobacco expansion agent is recovered first, and the recovery is completed.
  • the pressure in the impregnation tank is lowered to 0.9 MPa, and then the pressure of the high-pressure recovery gas-fired tobacco expansion agent to the impregnation tank is lowered to 0.8 MPa, and then the gaseous tobacco is accelerated.
  • the pressure of the expansion agent to the impregnation tank drops to 0.35 MPa, and finally the pressure of the remaining gas in the immersion tank is reduced to 0.21 MPa after the effluent is recovered; after the recovered liquid tobacco expansion agent is vaporized, purified and condensed Recycling, the recovered gaseous tobacco expansion agent is purified and condensed and recycled;
  • the tobacco is discharged and sent to the microwave expander at a microwave frequency of 2450HZ, a power of 10KW, and the time for the tobacco to pass through the microwave cavity is half a minute.
  • continuous passage of about 10 minutes to 15 minutes yielded expanded tobacco having a filling value of 7.6, a moisture content of expanded tobacco of 12.6%, and a whole yarn rate of 91%.
  • the mass percentage composition of a shredded tobacco expander of this embodiment is: pentafluorobutane 91.8%, hexafluoropropane 8.2%.
  • the preparation method comprises the following steps:: weighing raw materials according to pentafluorobutane 91.8% and hexafluoropropane 8.2% by mass, and then placing them in a preparation tank, stirring and mixing uniformly, and then filtering and filtering with a 600-mesh filter to make a cost.
  • the tobacco filament expander composition of the examples, the technical index data thereof is shown in Table 2.
  • the liquid tobacco expansion agent is recovered first, and the recovery is completed.
  • the pressure in the impregnation tank is lowered to 0.6 MPa, and then the pressure of the high-pressure recovery gas-fired tobacco expansion agent to the impregnation tank is lowered to 0.35 MPa, and the gaseous tobacco is accelerated.
  • the pressure of the expansion agent to the impregnation tank drops to 0.21Mpa, and finally the pressure of the remaining gas in the impregnation tank is reduced to O.11Mpa; the recovered liquid tobacco expansion agent is vaporized, purified and condensed. After recycling, the recovered gaseous tobacco expansion agent is purified and condensed and recycled;
  • the tobacco is discharged and sent to the microwave expander at a microwave frequency of 2450HZ, a power of 10KW, and the time for the tobacco to pass through the microwave cavity is half a minute.
  • the continuous passage of about 10 minutes to 15 minutes gave an expanded cut tobacco having a filling value of 7.7, a moisture content of the expanded tobacco of 12.6%, and a whole yarn rate of 91%.
  • the mass percentage composition of a shredded tobacco expander of this example is: pentafluorobutane 83%, pentafluoropropane 17%.
  • the preparation method comprises the following steps: weighing raw materials according to pentafluorobutane 83% and pentafluoropropane 17% by mass, and then placing them in a preparation tank, stirring and mixing uniformly, and then filtering and filtering with a 600-mesh filter to produce a cost.
  • the tobacco filament expander composition of the examples, the technical index data thereof is shown in Table 3.
  • the liquid tobacco expansion agent is recovered first, and the recovery is completed.
  • the pressure in the impregnation tank is lowered to 0.6 MPa, and then the pressure of the high-pressure recovery gas-fired tobacco expansion agent to the impregnation tank is lowered to 0.35 MPa, and the gaseous tobacco is accelerated.
  • the pressure of the expansion agent to the impregnation tank drops to 0.21Mpa, and finally the pressure of the remaining gas in the impregnation tank is reduced to O.11Mpa; the recovered liquid tobacco expansion agent is vaporized, purified and condensed.
  • the recovered gaseous tobacco expansion agent is purified and condensed and recycled; (6) After the liquid tobacco expansion agent and the gaseous tobacco expansion agent are recovered, the tobacco is discharged and sent to the microwave expander at a microwave frequency of 2450HZ, a power of 10KW, and the time for the tobacco to pass through the microwave cavity is half a minute. However, the continuous passage of about 10 minutes to 15 minutes gave an expanded cut tobacco having a filling value of 8.5, a moisture content of the poulted tobacco of 12.0%, and a whole yarn rate of 92%.
  • the mass percentage composition of a tobacco filler of this embodiment is 93% pentafluorobutane and 7% tetrafluoropropane.
  • the preparation method comprises the following steps:: weighing the raw material according to 93% of pentafluorobutane and 7% by mass of tetrafluoropropane, and then placing it in a preparation tank, stirring and mixing uniformly, and then filtering and filtering with a 600-mesh filter to make a cost.
  • the technical index data is shown in Table 4.
  • the liquid tobacco expansion agent is recovered first, and the recovery is completed, and the pressure in the impregnation tank is lowered to 0.9 Mpa. Then, the pressure of the high-pressure recovery of the gaseous tobacco expansion agent to the impregnation tank is lowered to 0.8 MPa, and then the pressure of the recovery of the gaseous tobacco expansion agent to the impregnation tank is lowered to 0.35 MPa, and finally the remaining gas in the impregnation tank is recovered by ejector to the impregnation. The pressure in the tank drops to 0.21Mpa; the recovered liquid tobacco expansion agent is recycled after being gasified, purified and condensed, and the recovered gaseous tobacco expansion agent is purified and condensed and recycled;
  • the tobacco is discharged and sent to the microwave expander at a microwave frequency of 2450HZ, a power of 10KW, and the time for the tobacco to pass through the microwave cavity is half a minute.
  • continuous passage of about 10 minutes to 15 minutes gave an expanded cut tobacco having a filling value of 8.0, a moisture content of expanded tobacco of 12.6%, and a total yarn rate of 93%.
  • the mass percentage composition of a tobacco filler of this embodiment is: pentafluorobutane 82%, decafluoropentane 18%.
  • the preparation method comprises the following steps:: weighing the raw material according to 93% of pentafluorobutane and 7% by mass of tetrafluoropropane, and then placing it in a preparation tank, stirring and mixing uniformly, and then filtering and filtering with a 600-mesh filter to make a cost.
  • the technical index data is shown in Table 5.
  • the liquid tobacco expansion agent is recovered first, and the recovery is completed.
  • the pressure in the impregnation tank is lowered to 0.9 MPa, and then the pressure of the high-pressure recovery gas-fired tobacco expansion agent to the impregnation tank is lowered to 0.8 MPa, and then the gaseous tobacco is accelerated.
  • the pressure of the expansion agent to the impregnation tank drops to 0.35 MPa, and finally the pressure of the remaining gas in the immersion tank is reduced to 0.21 MPa after the effluent is recovered; after the recovered liquid tobacco expansion agent is vaporized, purified and condensed Recycling, the recovered gaseous tobacco expansion agent is purified and condensed and recycled;
  • the tobacco is discharged and sent to the microwave expander at a microwave frequency of 2450HZ, a power of 10KW, and the time for the tobacco to pass through the microwave cavity is half a minute.
  • continuous passage of about 10 minutes to 15 minutes gave an expanded cut tobacco having a filling value of 8.5, a moisture content of the expanded tobacco of 12.6%, and a whole yarn rate of 95%.
  • the inventors conducted a screening test on the filling method of the expanding agent, and the results are shown in the following table:

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Description

一种制备膨胀烟丝的循环方法
技术领域
本发明涉及烟草生产制造领域， 特别涉及卷烟生产制造过程中的烟丝制造工艺。 背景技术
目前在世界的卷烟生产制造过程中，为能提高卷烟品质，采取多种工艺提高烟丝品质， 其中为减少卷烟烟气焦油量， 提高吸食品质， 使卷烟燃烧均匀化和提高烟丝对卷烟的填充 能力， 有一定技术能力的厂家均采用烟丝膨胀技术， 以达到上述目的。 而在烟丝膨胀技术 中现阶段在世界上比较成熟和普及的技术是二氧化碳烟丝膨胀技术， 氟利昂烟丝膨胀技 术， 氮气烟丝膨胀技术。 其中又以二氧化碳烟丝膨胀技术使用最为普遍。 二氧化碳膨胀烟 丝是 70年代开始投入工业生产的烟草加工新技术。 由于该技术具有显著提高烟丝填充能 力、 节省卷烟耗丝量和减少烟气焦油量以及二氧化碳介质无毒、 无味、 无污染且价格便宜 等优点， 因而受到烟草界的普遍关注和欢迎。 近年来， 对该技术的推广应用和改进研究极 为迅速。 但是由于二氧化碳液化温度和压力和其在自然状态下的气态状态， 决定了其工艺 的复杂化和高成本化。 并且二氧化碳膨胀技术损耗大、 设备修理和维护费用高、 生产成本 高； 烟丝香气损失较大、 枯焦气重、 烟气干燥， 填充性能虽好， 但碎丝率高的问题， 致使 在卷制过程中的损耗也较大， 其在烟支中的实际比例低于配方中的比例。 为此， 很多厂家 对烟丝膨胀技术进行了大量的研究和改进。
早在 90年代， 就提出了几种改进的 C02膨胀烟丝工艺 （参见黄岳元、 赵天成的 "几 种改进的 C02膨胀烟丝工艺， 《烟草科技 ·卷烟工艺》， 1997年第 3期： 14一 16)。
申请号为 01142872.4的中国专利申请公开了一种膨胀烟丝改良技术，是在烟叶切丝前 首先向烟叶喷洒由高沸点香料和保润剂组成的料液， 料液添加比例为烟叶重量的 0.1 -2
% , 在烟叶切丝膨胀后， 对膨胀烟丝进行加香处理， 料液由 co2超临界萃取烟草精油、 改 性烟草提取物、 丙二醇、 改性浓縮果汁、 反应香料组成， 所喷洒的料液比例为烟丝重量的
0.1 %-3 %。 该方法根据烟叶膨胀前后化学成分的变化， 有针对性地进行加香加料处理， 最 大限度地保持和补偿了膨胀烟丝的香气质、香气量，提高了膨胀烟丝的内在质量和可用性。
申请号为 200410010347.0的中国专利申请公开了一种烤烟二氧化碳烟丝膨胀方法，在 浸渍罐中用液态二氧化碳浸渍烟丝， 然后以过热蒸汽带动浸渍后的烟丝均匀的通过膨胀管 道， 使烟丝膨胀。 选用的烤烟原料还原糖含量小于 18 %、 总挥发碱至少为 0.4%、 总氮含 量至少为 5 %、 烟碱含量最低为 4%。 烟丝的宽度可以为 0.8〜0.9mm。 浸渍后的烟丝中的 二氧化碳含量为 3〜6%； 膨胀管道中的气流初始温度可为 290〜310°C， 气流输送速度为 29〜35m/s。采用此方法膨胀后烟丝与膨胀前相比， 化学成分的协调性、 内在质量和吸味品 质得到明显改善， 烟叶原料的使用价值明显提高。
但是， 这些方法仍然存在着损耗大、 设备修理和维护费用高、 生产成本高以及烟丝枯 焦气重、 烟气干燥、 碎丝率高的缺点。
中国专利 200510010637.X公开了一种以水为介质的烟丝膨胀工艺方法，具体是在卷烟 烟丝制造加工过程中， 增加叶丝水分加湿， 增温增湿后， 进行热风膨胀， 热风膨胀是在增 温增湿之后，使高含水分的叶丝通过温度在 250-36CTC的高温气流，使叶丝含水降到 6-13%， 进行快速去湿促使烟丝产生膨胀的过程， 和自然风冷降温顺序过程。 该方法虽然克服了二 氧化碳膨胀技术损耗大、 设备修理和维护费用高、 生产成本高； 烟丝香气损失较大、 枯焦 气重、 烟气干燥， 填充性能虽好， 但碎丝率高的问题。 但整个工艺中需要 250-36CTC的高 温气流， 对设备的要求比较高。
综上所述， C02膨胀烟丝工艺需要在低温高压下进行， 烟丝的造碎率高， 设备的能耗 大， 且 C02的沸点较低， 尽管能够回收， 但其回收利用率不高； 而上述以水为介质的烟丝 膨胀工艺， 同样对设备的要求很高。 有鉴于此， 特提出本发明。 发明内容
本发明的目的在于提供一种制备膨胀烟丝的循环方法， 该方法使用了 ODP值为零、 具有环保性好、 材料相容性好、 渗透性好、 毒性低、 沸点适中、 表面张力较小以及更容易 渗入烟丝细胞和达到理想的膨胀效果的膨胀介质， 而且本发明的方法条件温和， 对设备的 要求大大降低， 通过膨胀剂的充分回收利用， 降低了成本， 整套装置低能耗、 高自动化， 可以进行连续化大规模生产， 得到的膨胀烟丝的各项性能指标均高， 烟丝膨胀效率高， 膨 胀剂回收利用率高。
为实现上述目的， 本发明采用如下技术方案：
一种制备膨胀烟丝的循环方法， 该方法包括如下步骤：
( 1 ) 将烟丝装入预热的浸渍罐中， 然后抽真空；
(2) 向烟丝上喷淋液态膨胀剂；
(3) 向浸渍罐中加注气态膨胀剂；
(4) 浸渍；
(5) 先回收液态膨胀剂， 再回收气态膨胀剂； 及
(6) 对浸渍后的烟丝进行膨胀， 同时步骤 （5 ) 中回收的液态膨胀剂和气态膨胀剂 再进行所述步骤 （2) 或 /和步骤 （3) 的操作。
干冰膨胀烟丝技术的基本工艺原理是根据 C02的物理特性，用液态 C02对烟丝进行浸 泡， 在烟丝的内部及表面形成干冰， 通过文丘里管将之迅速吸入升华管， 在 330°C左右的 热气流中使 C02迅速升华， 促使烟丝膨胀。 但是该方法存在两个缺陷： 一是由于输入液态 C02浸渍烟丝， 故浸渍烟丝上残留的 C02 (干冰） 较多， 一般为烟丝的 10%以上。 由于浸 渍烟丝极易结块， 去加热膨胀前必须用机械破碎， 从而增大了烟丝的造碎率 （一般在 4% 以上）， 同时也增大了 C02消耗； 二是装置运行中， 烟丝浸渍和 C02回收都为间歇操作， 整机效率差。 因此， 现有技术中提出了几种改进的 C02膨胀烟丝工艺 （参见黄岳元、 赵天 成的"几种改进的 C02膨胀烟丝工艺"， 《烟草科技 ·卷烟工艺》， 1997年第 3期： 14一 16)， 其中干冰浸渍工艺过程是： ①烟丝先装入一混合罐， 抽真空排除空气。 随后通入一定量液 态 C02在罐中膨胀形成气、 固两相混合的 C02冷雾， 进行搅拌使冷雾与烟丝混合均匀， 烟 丝温度降至 -70〜- 85°C，然后输入浸渍器；②向浸渍器通入压力为 2.5〜3.5MPa的饱和 C02 气体； ③浸渍器迅速减压， 卸出烟丝， 送去膨胀。
上述方法中， 虽然涉及到了抽真空以及先加液态 C02， 再加气态 C02， 但与本发明的 方法是不同的。 上述方法中的抽真空不是对浸渍罐抽真空， 而是对烟丝进入浸渍罐之前的 一混合罐抽真空， 通入的液态 C02需要将烟丝浸泡， 因此通入的 C02的量比较多， 且浸渍 过程是在低温下进行的； 而本发明的抽真空的主要目的是抽走浸渍罐内的不冷凝性气体空 气以及烟丝之间的空气和湿气，使浸渍罐处于一定的负压下，有利于膨胀剂对烟丝的浸渍， 提高烟丝的浸渍效果， 从而使烟丝达到更好的膨胀效果， 提高填充值， 更好的满足卷烟工 艺需求， 同时为回收工段减压， 减少不必要的不冷凝性气体的回收； 而液态膨胀剂的加入 是采用喷淋的方式加入， 这样液态膨胀剂能够缓慢穿透烟丝落入浸渍罐底， 能够提前对烟 丝进行膨胀剂湿润、 软化， 为下一步工艺气体增压作好准备， 能够更好的提高浸渍效果， 同时液态膨胀剂加注速度快， 工艺上节省了时间， 提高了生产效率， 更减少了膨胀剂的用 此外， 现有技术的 C02烟丝膨胀工艺的浸渍工段完全是在低温高压下进行的， 设备的 能耗消耗比较大； 而本发明的浸渍不需要在低温高压下进行， 设备的能耗小， 从而降低了 运行成本。
本发明采取气液混合的介质加注方式来实现介质的加注， 即将烟丝放入浸渍罐后， 先 直接将存贮在冷罐的液体介质按照一定比例通过浸渍罐内上封头的喷嘴向烟丝喷洒， 液体 介质加注完毕， 然后定量的液体介质通过蒸发器迅速气化为气体介质从浸渍罐下封头向浸 渍罐增压。 本发明所述的制备膨胀烟丝的循环方法中， 其中， 步骤 （1 ) 中所述的预热为将浸渍 罐预热至 65°C〜75°C。 本发明中， 浸渍罐预热主要是为了介质气化提供能量， 保证介质在 一个热的空间内迅速达到平衡状态， 有利于提高烟丝的浸渍效果。
上述循环方法中， 步骤 （1 ) 中所述的抽真空为使浸渍罐的压力处于 0.05Mpa〜 0.005Mpa。 本发明中， 将浸渍罐抽真空至压力处于 0.05Mpa〜0.005Mpa， 其主要目的是抽 走浸渍罐内的不冷凝性气体空气以及烟丝之间的空气和湿气， 使浸渍罐处于一定的负压 下， 有利于膨胀剂对烟丝的浸渍， 提高烟丝的浸渍效果， 从而使烟丝达到更好的膨胀效果， 提高填充值， 更好的满足卷烟工艺需求， 同时为膨胀剂的回收工艺减压， 减少不必要的不 冷凝性气体的回收。
上述循环方法中， 步骤 （2) 中喷淋的液态膨胀剂与烟丝的质量比为 0.5〜1： 1。 本发 明中， 将采用液态膨胀剂对烟丝进行喷淋， 液态膨胀剂能够缓慢穿透烟丝落入浸渍罐底， 采用喷淋主要是提前对烟丝进行介质湿润、 软化， 为下一步工艺气体增压作好准备， 能够 更好的提高浸渍效果， 同时液态膨胀剂加注速度快， 工艺上节省了时间， 提高了生产效率。
上述循环方法中， 步骤 （3) 中所述气态膨胀剂的加注量为使浸渍罐中的压力增加至 0.1Mpa〜lMpa。本发明中， 采用气态膨胀剂对浸渍罐进行增压， 可以加强烟丝的浸透性和 均匀性， 提高浸渍效果， 为烟丝有较好的膨胀效果作准备。
优选将浸渍罐中的压力增加至 0.3Mpa〜0.9Mpa， 更优选 0.5Mpa〜0.8Mpa。
上述循环方法中，步骤（4)中所述的浸渍为在压力 0.1Mpa〜lMpa、温度 65°C〜120°C 的条件下浸渍 5min〜30min。 其中， 所述压力优选 0.3Mpa~0.9Mpa, 再优选 0.5Mpa〜 0.8Mpa。
烟丝浸渍是整个工艺中很重要的一步， 在一定的压力范围内， 烟丝浸渍时间的长短直 接影响烟丝的浸渍效果， 而烟丝浸渍好坏直接影响到烟丝的膨胀效果。
如果在工业样机工艺中采取液态膨胀剂加注， 液态膨胀剂气化渗入烟丝细胞， 浸渍罐 压力的提高完全靠浸渍罐夹套提供的热量， 这样浸渍罐压力升高缓慢， 压力平衡所需时间 增长， 不利于生产效率的提高； 同样， 如果在工业样机工艺中采取气态膨胀剂加注， 浸渍 罐压力上升较快， 介质分子能够迅速渗入烟丝细胞中， 但气态膨胀剂加注时间过长， 同样 不利于生产效率的提高。 本发明中， 先向烟丝上喷淋液态膨胀剂， 再向浸渍罐中加注气态 膨胀剂， 然后再在液态膨胀剂和气态膨胀剂共存的条件下对烟丝进行浸渍， 这样液态膨胀 剂对烟丝进行介质湿润， 软化， 为下一步工艺气体增压作好准备， 能够更好的提高浸渍效 果， 同时液态膨胀剂加注速度快， 工艺上节省了时间， 提高了生产效率； 而气态膨胀剂对 浸渍罐进行增压， 加强烟丝的渗透性和均匀性， 提高浸渍效果， 为烟丝有较好的膨胀效果 作准备。
本发明中， 在压力 0.1Mpa〜lMpa、 温度 65°C〜120°C的条件下浸渍 5min〜30min能 够使烟丝具有很好的膨胀效果。
本发明所述的制备膨胀烟丝的循环方法中， 其中步骤 （5 ) 中所述液态膨胀剂的回收 是回收液态膨胀剂至浸渍罐内的压力下降至 lMpa〜0.35Mpa; 所述气态膨胀剂的回收包括 高压回收、 加速回收和引射回收。 本发明中， 采用不同的回收方式回收气态膨胀剂， 可以 提高膨胀剂的回收利用率。
本发明中， 所述的高压回收是回收气态膨胀剂至浸渍罐内的压力下降至 0.8Mpa〜 0.35Mpa。
当液态膨胀剂回收完毕后， 浸渍罐内的压力缓慢下降， 下降至 lMpa〜0.35Mpa， 为保 证冷凝器能够对回收膨胀剂及时冷凝， 回收效果良好， 先利用浸渍罐内的压力源， 迅速将 一定量的气态膨胀剂通过一管路打入到热罐， 通过热罐对回收膨胀剂的提纯、 初步降温作 用， 气态膨胀剂回到冷凝器冷凝、 介质贮罐贮存， 最后进入到介质计量罐循环使用。
所述的加速回收是回收气态膨胀剂至浸渍罐内的压力下降至 0.35Mpa〜0.21Mpa; 所述的引射回收是回收气态膨胀剂至浸渍罐内的压力下降至 0.21Mpa~0.11Mpa。 本发 明中， 引射回收的主要目的是回收浸渍罐内的余量气态膨胀剂， 提高膨胀剂的利用率， 减 少膨胀剂消耗。
本发明中， 所述的液态膨胀剂和气态膨胀剂分别为 4-12个碳原子的醇、 2-12个碳原 子的卤代醚、 3-12个碳原子的烷烃或被 2个以上卤原子取代的 3-12个碳原子的烷烃中的 一种组分或者两种以上的组分的混合物；
其优选 4-12 个碳原子的醇、 正戊烷、 异戊烷、 己烷、 环己烷、 庚烷、 辛烷、 二氟乙 烷、 四氟乙烷、 四氟丙烷、 五氟丙烷、 六氟丙烷、 七氟丙烷、 五氟丁烷、 十氟戊烷或甲氧 基九氟丁烷的一种或两种以上的混合物；
再优选二氟乙烷、 四氟乙烷、 四氟丙烷、 五氟丙烷、 六氟丙烷、 七氟丙烷、 五氟丁烷、 十氟戊烷或甲氧基九氟丁烷一种或两种以上的混合物；
更优选四氟乙烷、 五氟丙烷、 五氟丁烷、 十氟戊烷或甲氧基九氟丁烷一种或两种以上 的混合物。
若膨胀剂的沸点太低， 则不易回收、 运输及储存； 若沸点太高则需增加设备的容量， 能量消耗变大， 运行成本增加。 而本发明所述的膨胀剂不仅沸点适中， 而且具有臭氧消耗 潜能值为零或很低、 毒性小、 安全及化学稳定性好等优点。 采用本发明所提供的烟丝膨胀 剂容易回收、 运输及储存， 能量消耗小， 大大降低了运行成本。 "几种改进的 co2膨胀烟丝工艺"（参见黄岳元、 赵天成的 "几种改进的 co2膨胀烟 丝工艺"， 《烟草科技 ·卷烟工艺》， 1997年第 3期： 14一 16) 中介绍的干冰浸渍工艺过程 虽然涉及到了抽真空以及先加液态 C02， 再加气态 C02。 但是该方法中所用的膨胀剂 C02 的沸点是 -78.5°C， 且其性质与本发明所用的烟丝膨胀剂也有很大的差异， 在应用本发明所 提供的烟丝膨胀剂制备膨胀烟丝时， 不能简单的套用 C02的膨胀烟丝工艺。
本发明所提供的烟丝膨胀剂优选如下组合方式：
本发明的一种烟丝膨胀剂组合物， 该烟丝膨胀剂组合物的质量百分比组成为： 五氟丁 烷 （1， 1， 1， 3， 3-五氟丁烷， HFC-365mfc) 80-90%, 七氟丙烷 （1， 1， 1， 2， 3， 3， 3- 七氟丙烷， R227ca) 10-20%；
本发明的第二种烟丝膨胀剂组合物， 该烟丝膨胀剂组合物的质量百分比组成为： 五氟 丁烷 90-99%， 六氟丙烷 (HFC-236fa) 1-10%；
本发明的第三种烟丝膨胀剂组合物， 该烟丝膨胀剂组合物的质量百分比组成为： 五氟 丁烷 70-90%， 五氟丙烷 （1， 1， 1， 3， 3-五氟丙烷， HFC-245fa， R245fa) 10-30%；
本发明的第四种烟丝膨胀剂组合物， 该烟丝膨胀剂组合物的质量百分比组成为： 五氟 丁烷 90-99%， 四氟乙烷 （1， 1， 1， 2-四氟乙烷 R134a) 1-10%；
本发明的第五种烟丝膨胀剂组合物， 该烟丝膨胀剂组合物的质量百分比组成为： 五氟 丁烷 80-90%，十氟戊烷（1， 1， 1， 2， 3， 4， 4， 5， 5， 5-十氟戊烷， HFC-4310, HFC-43-lOmee) 10-20%。
本发明的烟丝膨胀剂以及上述五种烟丝膨胀剂组合物的制备方法按照申请号为 200510008577.8的专利申请所公开的方法制备， 具体为： 所用的原料均采用一级品。 上述 的五种组合物均可以通过按上述配比， 称重后置于配制罐中， 搅拌， 使之混合均匀， 然后 用 600目的过滤器进行加压过滤， 而得到本发明的烟丝膨胀剂组合物。
本发明中， 所述的气态膨胀剂和液态膨胀剂为两种不同的物质或两种不同的组合， 也 可以为两种相同的物质或两种相同的组合。 本发明中， 所述的膨胀剂沸点适中， 当采用的 气态膨胀剂或液态膨胀剂不同时， 也能实现本发明。
优选， 所述的气态膨胀剂为相应的液态膨胀剂经蒸发后形成的。 即本发明中， 所述的 气态膨胀剂和液态膨胀剂为同一种物质或同一种组合， 只是两种不同的形态。 这样可以减 少一些设备， 从而降低运行的成本。
本发明所述的制备膨胀烟丝的循环方法中， 所述的液态膨胀剂回收后， 经气化、提纯、 冷凝后再循环利用， 所述的气态膨胀剂回收后， 经提纯、 冷凝后再循环利用。
本发明中， 液态膨胀剂和气态膨胀剂能够充分地回收再利用。 本发明的烟丝膨胀的方法为现有技术中常用的方法， 如微波膨胀等。 但优选本发明的 膨胀方法。 本发明的烟丝膨胀过程主要发生在工业微波发生器腔体内， 介质蒸汽形成对烟 丝细胞壁向外推的力， 使烟丝膨胀。
相对于现有技术， 本发明具有如下优点：
( 1 ) 采用本发明提供的循环方法， 填充值 6. 8， 膨后烟丝水分含量 （12. 5 ± 1 ) %， 整丝率 80%， 水渍烟丝为零， 膨后烟丝回弹性好， 整丝率高， 无水渍、 结团现象。 而采 用 C02等现有技术的其他烟丝膨胀方法， 填充值高于 7. 5， 膨胀后烟丝水分含量 12. 5士 0. 5%， 整丝率大于 90%。 可见， 采用本发明的方法， 烟丝的膨胀效果明显优于现有技术；
( 2 ) 本发明的制备膨胀烟丝的循环方法， 无需在低温高压下即可进行， 设备的能耗 小， 从而降低运行成本；
( 3 ) 本发明的制备膨胀烟丝的循环方法， 采用喷淋的方式加入液态膨胀剂， 从而液 态膨胀剂的用量较小， 从而使得整个工艺所需的膨胀剂的用量降低， 进而减少了成本， 而 膨胀效果却没有因为膨胀剂的用量的减少而降低， 反而膨胀效果更好了；
(4) 本发明的制备膨胀烟丝的循环方法， 采用了 ODP值为零、 具有环保性好、 材料 相容性好、 渗透性好、 毒性低、 沸点适中、 表面张力较小以及更容易渗入烟丝细胞和达到 理想的膨胀效果的膨胀介质， 而且本发明的方法条件温和， 对设备的要求大大降低， 通过 膨胀剂的充分回收利用， 降低了成本， 整套装置低能耗、 高自动化， 可以进行连续化大规 模生产， 得到的膨胀烟丝的各项性能指标均高， 烟丝膨胀效率高， 膨胀剂回收利用率高。 具体实施方式
以下为本发明的具体实施方式， 所述的实施例是为了进一步描述本发明， 而不是限制 本发明。
实施例 1
(一） 烟丝膨胀剂的制备
本实施例的一种烟丝膨胀剂的质量百分比组成为： 五氟丁烷 87%， 七氟丙烷 13%。 其制备方法是： 按五氟丁烷 87%， 七氟丙烷 13%的质量百分比称取原料， 然后， 置于 配制罐中， 搅拌混合均匀， 再用 600目的过滤器加压过滤， 制成本实施例的烟丝膨胀剂组 合物， 其技术指标数据见表 1。
表 1.实施例 1的烟丝膨胀剂的技术指标
Figure imgf000009_0001
沸点 °C 24 24
冰点 °C -111 -35
密度 g/cm3 (20°C) 1.476 1.29
ODP 1.0 0
汽化潜能 KJ/Kg 180.3 171
粘度 Mpas (20°C) 0.43
残留量 Ppm 7天后， 5-7
毒性/ LD50 mg/kg 1436.4
(二） 应用 （一） 所制备的烟丝膨胀剂制备膨胀烟丝
( 1 ) 将称重的含水率 19%的烟丝 100kg装入预热至 75°C的浸渍罐内， 然后对浸渍罐 抽真空， 使其压力处于 0.05Mpa;
(2) 向浸渍罐内的烟丝上喷淋 （一） 所制备的烟丝膨胀剂 100kg;
(3)取 （一）所制备的烟丝膨胀剂 100kg, 气化后加注到浸渍罐中， 使浸渍罐中的压 力增加至 IMpa;
(4) 浸渍罐外夹套持续加热至 120°C， 烟丝在压力 lMpa、 温度 120°C的条件下浸渍 20min;
(5)浸渍完毕后，先回收液态烟丝膨胀剂，回收完毕，浸渍罐内的压力下降至 0.9Mpa， 然后高压回收气态烟丝膨胀剂至浸渍罐内的压力下降至 0.8Mpa，再加速回收气态烟丝膨胀 剂至浸渍罐内的压力下降至 0.35Mpa， 最后在引射回收浸渍罐内的余量气体至浸渍罐内的 压力下降至 0.21Mpa; 回收的液态烟丝膨胀剂经气化、 提纯和冷凝后再循环利用， 回收的 气态烟丝膨胀剂经提纯和冷凝后再循环利用；
(6) 液态烟丝膨胀剂和气态烟丝膨胀剂回收完毕后， 卸出烟丝， 并将其送入到微波 膨胀器内在微波频率为 2450HZ、 功率为 10KW, 烟丝通过微波腔体的时间为半分钟， 但 连续通过约 10分钟〜 15分钟， 得到填充值为 7.6、 膨后烟丝水分含量 12.6%、 整丝率 91% 的膨胀烟丝。
在烟丝进行膨胀的过程中， 下一批烟丝又装入到浸渍罐中进行步骤 （1 ) 及以后的工 序， 从而实现连续浸渍过程。 实施例 2
(一） 烟丝膨胀剂的制备
本实施例的一种烟丝膨胀剂的质量百分比组成为： 五氟丁烷 91.8%， 六氟丙烷 8.2%。 其制备方法是： 按五氟丁烷 91.8%， 六氟丙烷 8.2%的质量百分比称取原料， 然后， 置 于配制罐中， 搅拌混合均匀， 再用 600目的过滤器加压过滤， 制成本实施例的烟丝膨胀剂 组合物， 其技术指标数据见表 2。
表 2.实施例 2的烟丝膨胀剂的技术指标
Figure imgf000011_0001
(二） 应用 （一） 所制备的烟丝膨胀剂制备膨胀烟丝
( 1 ) 将称重的含水率 20%的烟丝 200kg装入预热至 65°C的浸渍罐内， 然后对浸渍罐 抽真空， 使其压力处于 0.005Mpa;
(2) 向浸渍罐内的烟丝上喷淋 （一） 所制备的烟丝膨胀剂 120kg;
( 3 ) 取 （一） 所制备的烟丝膨胀剂 80kg气化后加注到浸渍罐中， 使浸渍罐中的压力 增加至 0.8Mpa;
(4)浸渍罐外夹套持续加热至 100°C， 浸渍罐内的烟丝在压力 0.8Mpa、温度 100°C的 条件下浸渍 25min;
( 5 )浸渍完毕后，先回收液态烟丝膨胀剂，回收完毕，浸渍罐内的压力下降至 0.6Mpa， 然后高压回收气态烟丝膨胀剂至浸渍罐内的压力下降至 0.35Mpa， 再加速回收气态烟丝膨 胀剂至浸渍罐内的压力下降至 0.21Mpa， 最后在引射回收浸渍罐内的余量气体至浸渍罐内 的压力下降至 O.llMpa; 回收的液态烟丝膨胀剂经气化、 提纯和冷凝后再循环利用， 回收 的气态烟丝膨胀剂经提纯和冷凝后再循环利用；
( 6 ) 液态烟丝膨胀剂和气态烟丝膨胀剂回收完毕后， 卸出烟丝， 并将其送入到微波 膨胀器内在微波频率为 2450HZ、 功率为 10KW, 烟丝通过微波腔体的时间为半分钟， 但 连续通过约 10分钟〜 15分钟， 得到填充值为 7.7、 膨后烟丝水分含量 12.6%、 整丝率 91% 的膨胀烟丝。 实施例 3
(一） 烟丝膨胀剂的制备
本实施例的一种烟丝膨胀剂的质量百分比组成为： 五氟丁烷 83%， 五氟丙烷 17%。 其制备方法是： 按五氟丁烷 83%， 五氟丙烷 17%的质量百分比称取原料， 然后， 置于 配制罐中， 搅拌混合均匀， 再用 600目的过滤器加压过滤， 制成本实施例的烟丝膨胀剂组 合物， 其技术指标数据见表 3。
表 3.实施例 3的烟丝膨胀剂的技术指标
Figure imgf000012_0001
(二） 应用 （一） 所制备的烟丝膨胀剂制备膨胀烟丝
( 1 ) 将称重的含水率 21%的烟丝 200kg装入预热至 70°C的浸渍罐内， 然后对浸渍罐 抽真空， 使其压力处于 O.OlMpa;
(2) 向浸渍罐内的烟丝上喷淋 （一） 所制备的烟丝膨胀剂 200kg;
(3) 取 （一） 所制备的烟丝膨胀剂 100kg气化后， 加注到浸渍罐中， 使浸渍罐中的 压力增加至 0.8Mpa;
(4)浸渍罐外夹套持续加热至 100°C， 浸渍罐内的烟丝在压力 0.8Mpa、温度 100°C的 条件下浸渍 25min;
(5)浸渍完毕后，先回收液态烟丝膨胀剂，回收完毕，浸渍罐内的压力下降至 0.6Mpa， 然后高压回收气态烟丝膨胀剂至浸渍罐内的压力下降至 0.35Mpa， 再加速回收气态烟丝膨 胀剂至浸渍罐内的压力下降至 0.21Mpa， 最后在引射回收浸渍罐内的余量气体至浸渍罐内 的压力下降至 O.llMpa; 回收的液态烟丝膨胀剂经气化、 提纯和冷凝后再循环利用， 回收 的气态烟丝膨胀剂经提纯和冷凝后再循环利用； (6) 液态烟丝膨胀剂和气态烟丝膨胀剂回收完毕后， 卸出烟丝， 并将其送入到微波 膨胀器内在微波频率为 2450HZ、 功率为 10KW, 烟丝通过微波腔体的时间为半分钟， 但 连续通过约 10分钟〜 15分钟， 得到填充值为 8.5、 膨后烟丝水分含量 12.0%、 整丝率 92% 的膨胀烟丝。 实施例 4
(一） 烟丝膨胀剂的制备
本实施例的一种烟丝膨胀剂的质量百分比组成为： 五氟丁烷 93%， 四氟丙烷 7%。 其制备方法是： 按五氟丁烷 93%， 四氟丙烷 7%的质量百分比称取原料， 然后， 置于 配制罐中， 搅拌混合均匀， 再用 600目的过滤器加压过滤， 制成本实施例的烟丝膨胀剂组 合物， 其技术指标数据见表 4。
表 4.实施例 4的烟丝膨胀剂的技术指标
Figure imgf000013_0001
(二） 应用 （一） 所制备的烟丝膨胀剂制备膨胀烟丝
( 1 ) 将称重的含水率 19%的烟丝 100kg装入预热至 75°C的浸渍罐内， 然后对浸渍罐 抽真空， 使其压力处于 0.05Mpa;
(2) 向浸渍罐内的烟丝上喷淋 （一） 所制备的烟丝膨胀剂 100kg;
(3)取 （一）所制备的烟丝膨胀剂 100kg, 气化后加注到浸渍罐中， 使浸渍罐中的压 力增加至 IMpa;
(4) 浸渍罐外夹套持续加热至 120°C， 烟丝在压力 lMpa、 温度 120°C的条件下浸渍 20min;
(5)浸渍完毕后，先回收液态烟丝膨胀剂，回收完毕，浸渍罐内的压力下降至 0.9Mpa， 然后高压回收气态烟丝膨胀剂至浸渍罐内的压力下降至 0.8Mpa，再加速回收气态烟丝膨胀 剂至浸渍罐内的压力下降至 0.35Mpa， 最后在引射回收浸渍罐内的余量气体至浸渍罐内的 压力下降至 0.21Mpa; 回收的液态烟丝膨胀剂经气化、 提纯和冷凝后再循环利用， 回收的 气态烟丝膨胀剂经提纯和冷凝后再循环利用；
( 6 ) 液态烟丝膨胀剂和气态烟丝膨胀剂回收完毕后， 卸出烟丝， 并将其送入到微波 膨胀器内在微波频率为 2450HZ、 功率为 10KW, 烟丝通过微波腔体的时间为半分钟， 但 连续通过约 10分钟〜 15分钟， 得到填充值为 8.0、 膨后烟丝水分含量 12.6%、 整丝率 93% 的膨胀烟丝。 实施例 5
(二） 烟丝膨胀剂的制备
本实施例的一种烟丝膨胀剂的质量百分比组成为： 五氟丁烷 82%， 十氟戊烷 18%。 其制备方法是： 按五氟丁烷 93%， 四氟丙烷 7%的质量百分比称取原料， 然后， 置于 配制罐中， 搅拌混合均匀， 再用 600目的过滤器加压过滤， 制成本实施例的烟丝膨胀剂组 合物， 其技术指标数据见表 5。
表 5.实施例 5的烟丝膨胀剂的技术指标
Figure imgf000014_0001
(二） 应用 （一） 所制备的烟丝膨胀剂制备膨胀烟丝
( 1 ) 将称重的含水率 19%的烟丝 100kg装入预热至 75°C的浸渍罐内， 然后对浸渍罐 抽真空， 使其压力处于 0.05Mpa;
(2) 向浸渍罐内的烟丝上喷淋 （一） 所制备的烟丝膨胀剂 100kg;
( 3 )取 （一）所制备的烟丝膨胀剂 100kg, 气化后加注到浸渍罐中， 使浸渍罐中的压 力增加至 IMpa;
(4) 浸渍罐外夹套持续加热至 120°C， 烟丝在压力 lMpa、 温度 120°C的条件下浸渍 20min;
(5)浸渍完毕后，先回收液态烟丝膨胀剂，回收完毕，浸渍罐内的压力下降至 0.9Mpa， 然后高压回收气态烟丝膨胀剂至浸渍罐内的压力下降至 0.8Mpa，再加速回收气态烟丝膨胀 剂至浸渍罐内的压力下降至 0.35Mpa， 最后在引射回收浸渍罐内的余量气体至浸渍罐内的 压力下降至 0.21Mpa; 回收的液态烟丝膨胀剂经气化、 提纯和冷凝后再循环利用， 回收的 气态烟丝膨胀剂经提纯和冷凝后再循环利用；
(6) 液态烟丝膨胀剂和气态烟丝膨胀剂回收完毕后， 卸出烟丝， 并将其送入到微波 膨胀器内在微波频率为 2450HZ、 功率为 10KW, 烟丝通过微波腔体的时间为半分钟， 但 连续通过约 10分钟〜 15分钟， 得到填充值为 8.5、 膨后烟丝水分含量 12.6%、 整丝率 95% 的膨胀烟丝。 实施例 6-9
实施例 6-9除了所用的膨胀剂不同， 其他参数均采用实施例 1， 具体数据如下:
Figure imgf000015_0001
试验例 1
本发明人对膨胀剂的加注方式进行了筛选试验， 结果见下表:
膨胀剂加注方式不同对膨胀效果的影响
Figure imgf000015_0002
Figure imgf000016_0001
从上表可以看出， 当采用液态加注， 气态增压的方式时， 膨胀效果较好。

Claims

权利要求书
1、 一种制备膨胀烟丝的循环方法， 该方法包括如下步骤：
(1) 将烟丝装入预热的浸渍罐中， 然后抽真空；
(2) 向烟丝上喷淋液态膨胀剂；
(3) 向浸渍罐中加注气态膨胀剂；
(4) 浸渍；
(5) 先回收液态膨胀剂， 再回收气态膨胀剂； 及
(6) 对浸渍后的烟丝进行膨胀， 同时步骤 （5) 中回收的液态膨胀剂和气态膨胀剂 再进行所述步骤 （2) 或 /和步骤 （3) 的操作。
2、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 步骤（1) 中所述的预 热为将浸渍罐预热至 65°C 75°C; 步骤 （1) 中所述的抽真空为使浸渍罐的压力处于 0.05Mpa 5Mpa
3、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 步骤（2) 中喷淋的液 态膨胀剂与烟丝的质量比为 0.5 1 1
4、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 步骤（3) 中所述气态 膨胀剂的加注量为使浸渍罐中的压力增加至 0.1Mpa lMpa， 优选 0.3Mpa 0.9Mpa， 再优 选 0.5Mpa 0.8Mpa
5、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 步骤（4) 中所述的浸 渍为在压力 0.1Mpa lMpa，优选 0.3Mpa 0.9Mpa，再优选 0.5Mpa 0.8Mpa;温度 65°C 120 °C的条件下浸渍 5min 30min
6、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 步骤（5) 中所述液态 膨胀剂的回收是回收液态膨胀剂至浸渍罐内的压力下降至 lMpa 0.35Mpa;所述气态膨胀 剂的回收包括高压回收、 加速回收和引射回收。
7、 根据权利要求 6所述的制备膨胀烟丝的循环方法， 其特征在于： 所述的高压回收是回 收气态膨胀剂至浸渍罐内的压力下降至 0.8Mpa 0.35Mpa; 所述的加速回收是
回收气态膨胀剂至浸渍罐内的压力下降至 0.35Mpa 0.21Mpa; 所述的引射回收是回收气 态膨胀剂至浸渍罐内的压力下降至 0.21Mpa~0.11Mpa
8、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 所述的液态膨胀剂和 气态膨胀剂分别为 2-12个碳原子的醇、 2-12个碳原子的酮、 2-12个碳原子的卤代醚、 2-12 个碳原子的烷烃或 2-12个碳原子的卤代烷烃中的一种或者几种。
9、 根据权利要求 8所述的制备膨胀烟丝的循环方法， 其特征在于： 所述的气态膨胀剂为 相应的液态膨胀剂经蒸发后形成的。
10、 根据权利要求 1所述的制备膨胀烟丝的循环方法， 其特征在于： 所述的液态膨胀剂回 收后， 经气化、 提纯、 冷凝后再循环利用， 所述的气态膨胀剂回收后， 经提纯、 冷凝后再 循环利用。
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CN101513272A (zh) * 2009-04-03 2009-08-26 云南瑞升烟草技术（集团）有限公司 一种膨胀烟丝的方法

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US5065774A (en) * 1989-08-18 1991-11-19 R. J. Reynolds Tobacco Company Process for expanding tobacco under moderate conditions
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JPH067138A (ja) * 1992-03-18 1994-01-18 R J Reynolds Tobacco Co タバコ材刻み補充料を膨脹させるための方法及び装置
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