CN101617854B - Circulation method for preparing expanded cut tobacco - Google Patents
Circulation method for preparing expanded cut tobacco Download PDFInfo
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- CN101617854B CN101617854B CN2008101825256A CN200810182525A CN101617854B CN 101617854 B CN101617854 B CN 101617854B CN 2008101825256 A CN2008101825256 A CN 2008101825256A CN 200810182525 A CN200810182525 A CN 200810182525A CN 101617854 B CN101617854 B CN 101617854B
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Abstract
The invention discloses a circulation method for preparing expanded cut tobacco, comprising the following steps: (1) putting cut tobacco into a preheated impregnating tank, then carrying out vacuum-pumping; (2) spraying liquid expanding agent to the cut tobacco; (3) filling gas expanding agent to the impregnating tank; (4) impregnating; (5) first, recycling the liquid expanding agent, then recycling the gas expanding agent; and (6) expanding the impregnated cut tobacco, and carrying out operations in step (2) or/and step (3) by the liquid expanding agent and the gas expanding agent recycled in step (5). The method of the invention has mild condition and greatly reduced requirement for devices, by fully recycling the expanding agents, the cost is lowered, the complete set of devices has low energy consumption and high automation, continuous mass production can be carried out, all performance indexes of the obtained expanded cut tobacco are high, the expanded efficiency of the cut tobacco is high, and the recycling rate of the expanding agents is high.
Description
Technical field
The present invention relates to tobacco and manufacture field, particularly the pipe tobacco manufacturing process in the production of cigarettes manufacture process.
Background technology
At present in the production of cigarettes manufacture process in the world; For improving the cigarette quality, take kinds of processes to improve quality of tobacco shreds, wherein for reducing the cigarette smoke tar content; Improve sucking quality; Make the cigarette burning homogenising and improve the filling capacity of pipe tobacco, have the producer of certain technical capability all to adopt the tobacco expanding technology, to achieve the above object to cigarette.And in the tobacco expanding technology present stage in the world comparative maturity be carbon dioxide tobacco expanding technology with the technology of popularizing, freon tobacco expanding technology, nitrogen tobacco expanding technology.Wherein use the most general with carbon dioxide tobacco expanding technology again.Carbon dioxide expanded cut tobacco is to begin to drop into industrial tobacco New Machining Technology the seventies.Because this technology has the pipe tobacco of significantly improving filling capacity, saves cigarette consumption silk amount and reduces the tarry matters in smoke amount and CO 2 medium is nontoxic, tasteless, pollution-free and advantage such as low price, thereby receives common concern and the welcome of tobacco circle.In recent years, to this technology to apply and improve research very rapid.But, determined complicated and expensiveization of its technology owing to co 2 liquefaction temperature and pressure and its gaseous state under nature.And carbon dioxide expanded technological attrition is big, equipment repair and maintenance cost is high, production cost is high; The pipe tobacco fragrance loss is big, withered and burnt smell is heavy, flue gas drying, though filling capacity is good, the problem that filament broken rate is high causes the loss in the process of rolling also bigger, and its actual ratio in cigarette props up is lower than the ratio in the prescription.For this reason, a lot of producers have carried out a large amount of research and improvement to the tobacco expanding technology.
As far back as the nineties, several kinds of improved CO have just been proposed
2Expanded cut tobacco technology is (referring to " several kinds of improved CO of Huang Yueyuan, Zhao Tiancheng
2Expanded cut tobacco technology, " tobacco science and technology cigarette process ", 1997 the 3rd phases: 14-16).
Application number is that 01142872.4 one Chinese patent application discloses a kind of improved tobacco shred swelling technology; Be before the tobacco leaf chopping, at first to spray the feed liquid of forming by higher boiling spices and humectant to tobacco leaf; The feed liquid adding proportion is the 0.1%-2% of tobacco leaf weight; After the tobacco leaf chopping is expanded, expanded cut tobacco to be carried out perfuming handle, feed liquid is by CO
2Supercritical extract tobacco essential oil, modification tobacco extract, propane diols, modification inspissated juice, reaction flavor are formed, and the feed liquid ratio of being sprayed is the 0.1%-3% of pipe tobacco weight.The variation of chemical composition was carried out flavoring and casing targetedly and is handled before and after this method expanded according to tobacco leaf, kept and compensated fragrance matter, the perfume quantity of expanded cut tobacco to greatest extent, had improved the inherent quality and the availability of expanded cut tobacco.
Application number is that 200410010347.0 one Chinese patent application discloses a kind of flue-cured tobacco carbon dioxide tobacco thred expansion method; In impregnating autoclave, use the liquid carbon dioxide tobacco shred immersion; The pipe tobacco that drives after flooding with superheated steam then passes through swelling pipeline uniformly, makes tobacco expanding.The flue-cured tobacco raw material content of reducing sugar of selecting for use less than 18%, total volatile alkaline is at least 0.4%, total nitrogen content is at least 5%, nicotine content is minimum is 4%.The width of pipe tobacco can be 0.8～0.9mm.Carbon dioxide content in the pipe tobacco behind the dipping is 3～6%; Initial airflow temperature in the swelling pipeline can be 290～310 ℃, and the air-flow transporting velocity is 29～35m/s.Adopt the method expand the back pipe tobacco and expand before compare, the harmony of chemical composition, inherent quality and smoking quality be improved significantly, the use value of raw tobacco material obviously improves.
But these methods exist still that loss is big, equipment repair and maintenance cost is high, production cost is high and pipe tobacco withered and burnt smell weight, flue gas drying, shortcoming that filament broken rate is high.
It is the tobacco expanding process of medium with water that Chinese patent 200510010637.X discloses a kind of, specifically is to make in the process at cigarette shreds, increases leaf silk moisture humidification; Behind the warming and humidifying, carry out hot blast and expand, it is after warming and humidifying that hot blast expands; Make leaf silk that height contains moisture through the high temperature gas flow of temperature at 250-360 ℃; Make the moisture 6-13% of dropping to of leaf silk, dry fast and impel pipe tobacco to produce process and the natural air cooled warm down sequence process that expands.Carbon dioxide expanded technological attrition is big though this method has overcome, equipment repair and maintenance cost is high, production cost is high; The pipe tobacco fragrance loss is big, withered and burnt smell is heavy, flue gas drying, though filling capacity is good, and the problem that filament broken rate is high.But need 250-360 ℃ high temperature gas flow in the whole technology, to the requirement of equipment than higher.
In sum, CO
2The expanded cut tobacco arts demand carries out under cryogenic high pressure, and the broken rate of pipe tobacco is high, and the energy consumption of equipment is big, and CO
2Boiling point lower, although can reclaim, its recovery utilization rate is not high; And above-mentioned be the tobacco expanding technology of medium with water, same very high to the requirement of equipment.In view of this, special proposition the present invention.
Summary of the invention
The object of the present invention is to provide a kind of round-robin method for preparing expanded cut tobacco, it is zero that this method has been used the ODP value, have that the feature of environmental protection is good, material compatibility is good, good penetrability, toxicity are low, moderate boiling point, surface tension is less and infiltrate the pipe tobacco cell more easily and reach the inflating medium of desirable expansion effect, and method mild condition of the present invention; Requirement to equipment reduces greatly; Abundant recycling through swelling agent has reduced cost, package unit low energy consumption, high automation; Can carry out serialization large-scale production; Each item performance indications of the expanded cut tobacco that obtains are all high, and tobacco expanding efficient is high, and the swelling agent recovery utilization rate is high.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of round-robin method for preparing expanded cut tobacco, this method comprises the steps:
(1) pipe tobacco is packed in the impregnating autoclave of preheating, vacuumize then;
(2) the liquid swelling agent of spray on pipe tobacco;
(3) filling gaseous expansion agent in impregnating autoclave;
(4) dipping;
(5) reclaim liquid swelling agent earlier, reclaim the gaseous expansion agent again; And
(6) pipe tobacco behind the dipping is expanded the liquid swelling agent that reclaims in the step (5) the simultaneously and gaseous state swelling agent carries out said step (2) again or/and the operation of step (3).
The basic technology principle of dry-ice expanding pipe tobacco technology is according to CO
2Physical characteristic, use liquid CO
2Pipe tobacco is soaked, form dry ice, it is sucked sublimation pipe rapidly, make CO in the thermal current about 330 ℃ through Venturi tube on the inside and the surface of pipe tobacco
2Distillation impels tobacco expanding rapidly.But there are two defectives in this method: the one, because the liquid CO of input
2So tobacco shred immersion is residual CO on the tobacco shred immersion
2(dry ice) is more, is generally more than 10% of pipe tobacco.Because tobacco shred immersion very easily lumps, must use Mechanical Crushing before going to add thermal expansion, thereby increase the broken rate (generally more than 4%) of pipe tobacco, the while has also increased CO
2Consume; The 2nd, device is in service, pipe tobacco dipping and CO
2Reclaiming is intermittently operated all, and overall efficiency is poor.Therefore, several kinds of improved CO have been proposed in the prior art
2Expanded cut tobacco technology is (referring to " several kinds of improved CO of Huang Yueyuan, Zhao Tiancheng
2Expanded cut tobacco technology ", " tobacco science and technology cigarette process ", 1997 the 3rd phases: 14-16), wherein dry ice impregnation technology process is: the 1. pipe tobacco blending tank of packing into earlier vacuumizes deaeration.Feed a certain amount of liquid CO subsequently
2In jar, expand and form the CO that gas, solid two mixes mutually
2Cold mist stirs cold mist and pipe tobacco is mixed, and the pipe tobacco temperature is reduced to-70～-85 ℃, imports infuser then; 2. feeding pressure to infuser is the saturated CO of 2.5～3.5MPa
2Gas; 3. the infuser explosive decompression draws off pipe tobacco, sends to expansion.
In the said method, vacuumize and add liquid CO earlier though related to
2, add gaseous state CO again
2, but be different with method of the present invention.Vacuumizing in the said method is not impregnating autoclave is vacuumized, and vacuumizes the liquid CO of feeding but pipe tobacco is got into an impregnating autoclave blending tank before
2Need pipe tobacco be soaked the CO that therefore feeds
2Amount many, and dipping process carries out at low temperatures; And the main purpose that vacuumizes of the present invention is to take interior on-condensable gas air of impregnating autoclave and air and the moisture between the pipe tobacco away, and impregnating autoclave is under the certain negative pressure, helps the dipping of swelling agent to pipe tobacco; Improve the dipping effect of pipe tobacco; Thereby make pipe tobacco reach better expansion effect, improve the filling value, better meet the cigarette process demand; For the recycle section decompression, reduce the recovery of unnecessary on-condensable gas simultaneously; And the adding of liquid swelling agent is to adopt the mode of spray to add, and so liquid swelling agent can slowly penetrate pipe tobacco and fall at the bottom of the impregnating autoclave, can be in advance that pipe tobacco is carried out swelling agent is moistening, softening; For next step process gas supercharging is got ready; Can better improve dipping effect, simultaneously liquid swelling agent filling speed is fast, has saved the time on the technology; Improve production efficiency, more reduced the consumption of swelling agent.
In addition, the CO of prior art
2The dipping workshop section of tobacco expanding technology carries out under cryogenic high pressure fully, and the energy consumption consumption rate of equipment is bigger; And dipping of the present invention need not carry out under cryogenic high pressure, and the energy consumption of equipment is little, thereby has reduced operating cost.
The present invention takes the medium dosing method of gas-liquid mixed to realize the filling of medium; After soon pipe tobacco will be put into impregnating autoclave; The liquid medium that directly will be stored in earlier cold jar sprays to pipe tobacco through the nozzle of upper cover in the impregnating autoclave according to a certain percentage; Liquid medium filling finishes, quantitative then liquid medium through evaporimeter rapidly gasification for gas medium from the impregnating autoclave low head to the impregnating autoclave supercharging.
In the round-robin method of preparation expanded cut tobacco of the present invention, wherein, the preheating described in the step (1) is for to be preheated to 65 ℃～75 ℃ with impregnating autoclave.Among the present invention, the impregnating autoclave preheating mainly is for the medium gasification provides energy, guarantees that medium reaches poised state rapidly in the space of a heat, helps improving the dipping effect of pipe tobacco.
In the above-mentioned round-robin method, the pressure that vacuumizes to making impregnating autoclave described in the step (1) is in 0.05Mpa～0.005Mpa.Among the present invention, impregnating autoclave is evacuated to pressure is in 0.05Mpa～0.005Mpa, its main purpose is to take interior on-condensable gas air of impregnating autoclave and air and the moisture between the pipe tobacco away; Impregnating autoclave is under the certain negative pressure; Help the dipping of swelling agent, improve the dipping effect of pipe tobacco, thereby make pipe tobacco reach better expansion effect pipe tobacco; Improve the filling value; Better meeting the cigarette process demand, is the recovery technology decompression of swelling agent simultaneously, reduces the recovery of unnecessary on-condensable gas.
In the above-mentioned round-robin method, the liquid swelling agent of spray and the mass ratio of pipe tobacco are 0.5～1:1 in the step (2).Among the present invention, will adopt liquid swelling agent that pipe tobacco is sprayed, liquid swelling agent can slowly penetrate pipe tobacco and fall at the bottom of the impregnating autoclave; Adopting spray mainly is that in advance pipe tobacco to be carried out medium moistening, softening; Get ready for next step process gas supercharging, can better improve dipping effect, simultaneously liquid swelling agent filling speed is fast; Save the time on the technology, improved production efficiency.
In the above-mentioned round-robin method, the adding amount of gaseous expansion agent described in the step (3) is to make the pressure in the impregnating autoclave increase to 0.1Mpa～1Mpa.Among the present invention, adopt the gaseous expansion agent that impregnating autoclave is carried out supercharging, can strengthen the impregnability and the uniformity of pipe tobacco, improve dipping effect, prepare for pipe tobacco has preferably expansion effect.
Preferably the pressure in the impregnating autoclave is increased to 0.3Mpa～0.9Mpa, more preferably 0.5Mpa～0.8Mpa.
In the above-mentioned round-robin method, the dipping described in the step (4) is for flooding 5min～30min under the condition of 65 ℃～120 ℃ of pressure 0.1Mpa～1Mpa, temperature.Wherein, the preferred 0.3Mpa～0.9Mpa of said pressure, preferred again 0.5Mpa～0.8Mpa.
The pipe tobacco dipping is a step very important in the whole technology, and in certain pressure limit, the length of pipe tobacco dip time directly influences the dipping effect of pipe tobacco, and pipe tobacco dipping quality directly has influence on the expansion effect of pipe tobacco.
If in industrial model machine technology, take liquid swelling agent filling; The pipe tobacco cell is infiltrated in liquid swelling agent gasification, the heat that the raising of impregnating autoclave pressure leans on the impregnating autoclave chuck to provide fully, and impregnating autoclave pressure raises slowly like this; The pressure balance required time increases, and is unfavorable for the raising of production efficiency; Equally, if in industrial model machine technology, take gaseous expansion agent filling, impregnating autoclave pressure rises very fast, and medium molecule can infiltrate rapidly in the pipe tobacco cell, but gaseous expansion agent filling overlong time is unfavorable for the raising of production efficiency equally.Among the present invention, on pipe tobacco, spray liquid swelling agent earlier, filling gaseous expansion agent in impregnating autoclave again; And then under the condition of liquid swelling agent and gaseous state swelling agent coexistence, pipe tobacco is flooded, it is moistening, softening that so liquid swelling agent carries out medium to pipe tobacco; Get ready for next step process gas supercharging, can better improve dipping effect, simultaneously liquid swelling agent filling speed is fast; Save the time on the technology, improved production efficiency; And the gaseous expansion agent is carried out supercharging to impregnating autoclave, strengthens the permeability and the uniformity of pipe tobacco, improves dipping effect, prepares for pipe tobacco has preferably expansion effect.
Among the present invention, under the condition of 65 ℃～120 ℃ of pressure 0.1Mpa～1Mpa, temperature, flood 5min～30min and can make pipe tobacco have good expansion effect.
In the round-robin method of preparation expanded cut tobacco of the present invention, wherein the recovery of liquid swelling agent described in the step (5) is that the pressure that reclaims in liquid swelling agent to the impregnating autoclave drops to 1Mpa～0.35Mpa; The recovery of said gaseous expansion agent comprises that high pressure reclaims, quickens to reclaim and injection reclaims.Among the present invention, adopt different ways of recycling to reclaim the gaseous expansion agent, can improve the recovery utilization rate of swelling agent.
Among the present invention, it is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.8Mpa～0.35Mpa that described high pressure reclaims.
After liquid swelling agent recovery finished, the pressure in the impregnating autoclave slowly descended, and drops to 1Mpa～0.35Mpa; For guaranteeing that condenser can be to reclaiming the timely condensation of swelling agent, recovering effect is good, utilizes the pressure source in the impregnating autoclave earlier; Rapidly a certain amount of gaseous expansion agent is driven into the heat jar through a pipeline; Through the heat jar purification to the recovery swelling agent, preliminary cooling effect, condenser condenses is got back in the gaseous expansion agent, the medium basin is stored, and enters into the medium measuring tank at last and recycles.
It is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.35Mpa～0.21Mpa that described acceleration is reclaimed;
It is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.21Mpa～0.11Mpa that described injection reclaims.Among the present invention, the main purpose that injection reclaims is the surplus gaseous expansion agent of reclaiming in the impregnating autoclave, improves the utilization rate of swelling agent, reduces swelling agent consumption.
Among the present invention, described liquid swelling agent and gaseous state swelling agent be respectively alcohol, a 2-12 carbon atom of 4-12 carbon atom halogen ether, a 3-12 carbon atom alkane or by the mixture of a kind of component in the alkane of 2 the substituted 3-12 of above halogen atom carbon atoms or two or more component;
The mixture of one or more of alcohol, pentane, isopentane, hexane, cyclohexane, heptane, octane, Difluoroethane, HFC-134a, tetrafluoropropane, pentafluoropropane, HFC-236fa, heptafluoro-propane, 3-pentafluorobutane, Decafluoropentane or the MSX 4518 of its preferred 4-12 carbon atom;
One or more mixture of preferred again Difluoroethane, HFC-134a, tetrafluoropropane, pentafluoropropane, HFC-236fa, heptafluoro-propane, 3-pentafluorobutane, Decafluoropentane or MSX 4518;
More preferably one or more mixture of HFC-134a, pentafluoropropane, 3-pentafluorobutane, Decafluoropentane or MSX 4518.
If the boiling point of swelling agent is too low, then be difficult for reclaiming, transporting and store; If the too high capacity that then need increase equipment of boiling point, energy consumption become big, operating cost increases.And swelling agent of the present invention moderate boiling point not only, and have ODP be zero or very low, toxicity is little, safety and good chemical stability.Adopt tobacco expanding agent easy recovery provided by the present invention, transportation and storage, energy consumes little, greatly reduces operating cost.
" several kinds of improved CO
2Expanded cut tobacco technology " (referring to " several kinds of improved CO of Huang Yueyuan, Zhao Tiancheng
2Expanded cut tobacco technology ", " tobacco science and technology cigarette process ", 1997 the 3rd phases: 14-16) though in the dry ice impregnation technology process introduced related to and vacuumize and add liquid CO earlier
2, add gaseous state CO again
2But used swelling agent CO in this method
2Boiling point be-78.5 ℃, and its character and the used tobacco expanding agent of the present invention also have very big difference, when using tobacco expanding agent provided by the present invention and prepare expanded cut tobacco, can not simply apply mechanically CO
2Expanded cut tobacco technology.
The preferred following compound mode of tobacco expanding agent provided by the present invention:
A kind of composition of tobacco shred puffing agent of the present invention, the mass percent of this composition of tobacco shred puffing agent consists of: 3-pentafluorobutane (1,1,1,3; The 3-3-pentafluorobutane, HFC-365mfc) 80-90%, heptafluoro-propane (1,1,1; 2,3,3,3-heptafluoro-propane, R227ca) 10-20%;
Second kind of composition of tobacco shred puffing agent of the present invention, the mass percent of this composition of tobacco shred puffing agent consists of: 3-pentafluorobutane 90-99%, HFC-236fa (HFC-236fa) 1-10%;
The third composition of tobacco shred puffing agent of the present invention, the mass percent of this composition of tobacco shred puffing agent consists of: 3-pentafluorobutane 70-90%, pentafluoropropane (1,1,1,3,3-pentafluoropropane, HFC-245fa, R245fa) 10-30%;
The 4th kind of composition of tobacco shred puffing agent of the present invention, the mass percent of this composition of tobacco shred puffing agent consists of: 3-pentafluorobutane 90-99%, HFC-134a (1,1,1,2-HFC-134a R134a) 1-10%;
The 5th kind of composition of tobacco shred puffing agent of the present invention, the mass percent of this composition of tobacco shred puffing agent consists of: 3-pentafluorobutane 80-90%, Decafluoropentane (1,1,1,2,3,4,4,5,5,5-Decafluoropentane, HFC-4310, HFC-43-10mee) 10-20%.
The preparation method of tobacco expanding agent of the present invention and above-mentioned five kinds of composition of tobacco shred puffing agent is the disclosed method preparation of 200510008577.8 patent application according to application number, and be specially: used raw material all adopts primes.Five kinds of above-mentioned compositions all can be through pressing said ratio, and weighing is placed in the preparing tank, stirs, and makes it to mix, and carries out pressure filtration with 600 purpose filters then, and obtains composition of tobacco shred puffing agent of the present invention.
Among the present invention, described gaseous expansion agent is two kinds of different materials or two kinds of different combinations with liquid swelling agent, also can be two kinds of identical materials or two kinds of identical combinations.Among the present invention, described swelling agent moderate boiling point, when the gaseous expansion agent of adopting or liquid swelling agent not simultaneously, also can realize the present invention.
Preferably, described gaseous expansion agent is that corresponding liquid swelling agent forms after evaporating.Be among the present invention, described gaseous expansion agent and liquid swelling agent are with a kind of material or with a kind of combination, just two kinds of different forms.Can reduce some equipment like this, thereby reduce the cost of operation.
In the round-robin method of preparation expanded cut tobacco of the present invention, after described liquid swelling agent reclaims, recycling after gasification, purification, condensation, after described gaseous expansion agent is reclaimed, recycling after purification, condensation.
Among the present invention, liquid swelling agent and the recycling fully of gaseous state swelling agent.
The method of tobacco expanding of the present invention is a method commonly used in the prior art, like microwave expansion etc.But preferred expanding method of the present invention.Tobacco expanding process of the present invention mainly occurs in the industrial microwave generator cavity, and medium steam forms the power of pipe tobacco cell membrane to extrapolation, makes tobacco expanding.
With respect to prior art, the present invention has following advantage:
(1) adopt round-robin method provided by the invention, filling value >=6.8, swollen back moisture in cut tobacco content (12.5 ± 1) %, whole cut rate >=80%, water stain pipe tobacco are zero, and swollen back pipe tobacco resilience is good, and whole cut rate is high, no water stain, clustering phenomena.And employing CO
2Etc. other tobacco thred expansion methods of prior art, the filling value is higher than 7.5, the back moisture in cut tobacco content 12.5 ± 0.5% that expands, and whole cut rate is greater than 90%.It is thus clear that, adopting method of the present invention, the expansion effect of pipe tobacco obviously is superior to prior art;
(2) round-robin method of preparation expanded cut tobacco of the present invention need not under cryogenic high pressure, can carry out, and the energy consumption of equipment is little, thereby reduces operating cost;
(3) round-robin method of preparation expanded cut tobacco of the present invention; Adopt the mode of spray to add liquid swelling agent; Thereby the consumption of liquid swelling agent is less, thereby makes the consumption of the swelling agent that whole technology is required reduce, and then has reduced cost; Do not reduce because of the minimizing of the consumption of swelling agent and expansion effect has, expansion effect is better on the contrary;
(4) round-robin method of preparation expanded cut tobacco of the present invention, to have adopted the ODP value be zero, have that the feature of environmental protection is good, material compatibility is good, good penetrability, toxicity are low, moderate boiling point, surface tension is less and infiltrate the pipe tobacco cell more easily and reach the inflating medium of desirable expansion effect, and method mild condition of the present invention; Requirement to equipment reduces greatly; Abundant recycling through swelling agent has reduced cost, package unit low energy consumption, high automation; Can carry out serialization large-scale production; Each item performance indications of the expanded cut tobacco that obtains are all high, and tobacco expanding efficient is high, and the swelling agent recovery utilization rate is high.
The specific embodiment
Below be the specific embodiment of the present invention, described embodiment is in order to further describe the present invention, rather than restriction the present invention.
Embodiment 1
(1) preparation of tobacco expanding agent
The mass percent of a kind of tobacco expanding agent of present embodiment consists of: 3-pentafluorobutane 87%, heptafluoro-propane 13%.
Its preparation method is: press 3-pentafluorobutane 87%, the mass percent of heptafluoro-propane 13% takes by weighing raw material, then; Place preparing tank, mix, use 600 purpose filter pressure filtrations again; Process the composition of tobacco shred puffing agent of present embodiment, its technology index data is seen table 1.
The technical indicator of the tobacco expanding agent of table 1. embodiment 1
| Test event | Unit | CFC-11 | Tobacco expanding agent of the present invention |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid | |
| Boiling point | ℃ | 24 | 24 |
| Freezing point | ℃ | -111 | -35 |
| Density | g/cm 3(20℃) | 1.476 | 1.29 |
| ODP | 1.0 | 0 | |
| Vaporization potential | KJ/Kg | 180.3 | 171 |
| Viscosity | Mpas(20℃) | 0.43 | |
| Residual quantity | Ppm | After 7 days, 5-7 | |
| Toxicity/LD50 | mg/kg | 1436.4 |
(2) use (one) prepared tobacco expanding agent and prepare expanded cut tobacco
(1) the pipe tobacco 100kg of the moisture content of weighing 19% is packed in the impregnating autoclave that is preheated to 75 ℃, then impregnating autoclave is vacuumized, make its pressure be in 0.05Mpa;
(2) spray (one) prepared tobacco expanding agent 100kg on the pipe tobacco in impregnating autoclave;
(3) get (one) prepared tobacco expanding agent 100kg, be filled into after the gasification in the impregnating autoclave, make the pressure in the impregnating autoclave increase to 1Mpa;
(4) the impregnating autoclave external jacket continues to be heated to 120 ℃, and pipe tobacco floods 20min under the condition of 120 ℃ of pressure 1Mpa, temperature;
(5) after dipping finishes; Reclaim liquid tobacco expanding agent earlier; Recovery finishes, and the pressure in the impregnating autoclave drops to 0.9Mpa, and high pressure recovery gaseous state tobacco expanding agent to the pressure in the impregnating autoclave drops to 0.8Mpa then; Quicken to reclaim gaseous state tobacco expanding agent to the pressure in the impregnating autoclave again and drop to 0.35Mpa, the pressure in balance gas to the impregnating autoclave in injection reclaims impregnating autoclave drops to 0.21Mpa at last; Liquid tobacco expanding agent recycling after gasification, purification and condensation of reclaiming, the recycling after purification and condensation of the gaseous state tobacco expanding agent of recovery;
(6) after liquid tobacco expanding agent and gaseous state tobacco expanding agent reclaim and finish; Draw off pipe tobacco; And it is sent to the inherent microwave frequency of microwave expansion device is that 2450HZ, power are 10KW; Pipe tobacco is half a minute through the time of microwave cavity, but continuously through about 10 minutes～15 minutes, obtains the filling value and be 7.6, the expanded cut tobacco of swollen back moisture in cut tobacco content 12.6%, whole cut rate 91%.
In the process that pipe tobacco expands, the next group pipe tobacco is encased in again and carries out step (1) and later operation in the impregnating autoclave, thereby realizes the continuous impregnating process.
Embodiment 2
(1) preparation of tobacco expanding agent
The mass percent of a kind of tobacco expanding agent of present embodiment consists of: 3-pentafluorobutane 91.8%, HFC-236fa 8.2%.
Its preparation method is: press 3-pentafluorobutane 91.8%, the mass percent of HFC-236fa 8.2% takes by weighing raw material, then; Place preparing tank, mix, use 600 purpose filter pressure filtrations again; Process the composition of tobacco shred puffing agent of present embodiment, its technology index data is seen table 2.
The technical indicator of the tobacco expanding agent of table 2. embodiment 2
| Test event | Unit | CFC-11 | Tobacco expanding agent of the present invention |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid | |
| Boiling point | ℃ | 24 | 24 |
| Freezing point | ℃ | -111 | -36 |
| Density | g/cm 3(20℃) | 1.476 | 1.26 |
| ODP | 1.0 | 0 | |
| Vaporization potential | KJ/Kg | 180.3 | 168 |
| Viscosity | Mpas(20℃) | 0.43 | |
| Residual quantity | Ppm | After 7 days, 5-7 | |
| Toxicity/LD50 | mg/kg | 1436.4 |
(2) use (one) prepared tobacco expanding agent and prepare expanded cut tobacco
(1) the pipe tobacco 200kg of the moisture content of weighing 20% is packed in the impregnating autoclave that is preheated to 65 ℃, then impregnating autoclave is vacuumized, make its pressure be in 0.005Mpa;
(2) spray (one) prepared tobacco expanding agent 120kg on the pipe tobacco in impregnating autoclave;
(3) be filled in the impregnating autoclave after getting (one) prepared tobacco expanding agent 80kg gasification, make the pressure in the impregnating autoclave increase to 0.8Mpa;
(4) the impregnating autoclave external jacket continues to be heated to 100 ℃, and the pipe tobacco in the impregnating autoclave floods 25min under the condition of 100 ℃ of pressure 0.8Mpa, temperature;
(5) after dipping finishes; Reclaim liquid tobacco expanding agent earlier; Recovery finishes, and the pressure in the impregnating autoclave drops to 0.6Mpa, and high pressure recovery gaseous state tobacco expanding agent to the pressure in the impregnating autoclave drops to 0.35Mpa then; Quicken to reclaim gaseous state tobacco expanding agent to the pressure in the impregnating autoclave again and drop to 0.21Mpa, the pressure in balance gas to the impregnating autoclave in injection reclaims impregnating autoclave drops to 0.11Mpa at last; Liquid tobacco expanding agent recycling after gasification, purification and condensation of reclaiming, the recycling after purification and condensation of the gaseous state tobacco expanding agent of recovery;
(6) after liquid tobacco expanding agent and gaseous state tobacco expanding agent reclaim and finish; Draw off pipe tobacco; And it is sent to the inherent microwave frequency of microwave expansion device is that 2450HZ, power are 10KW; Pipe tobacco is half a minute through the time of microwave cavity, but continuously through about 10 minutes～15 minutes, obtains the filling value and be 7.7, the expanded cut tobacco of swollen back moisture in cut tobacco content 12.6%, whole cut rate 91%.
Embodiment 3
(1) preparation of tobacco expanding agent
The mass percent of a kind of tobacco expanding agent of present embodiment consists of: 3-pentafluorobutane 83%, pentafluoropropane 17%.
Its preparation method is: press 3-pentafluorobutane 83%, the mass percent of pentafluoropropane 17% takes by weighing raw material, then; Place preparing tank, mix, use 600 purpose filter pressure filtrations again; Process the composition of tobacco shred puffing agent of present embodiment, its technology index data is seen table 3.
The technical indicator of the tobacco expanding agent of table 3. embodiment 3
| Test event | Unit | CFC-11 | Tobacco expanding agent of the present invention |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid | |
| Boiling point | ℃ | 24 | 24 |
| Freezing point | ℃ | -111 | -34 |
| Density | g/cm 3(20℃) | 1.476 | 1.28 |
| ODP | 1.0 | 0 | |
| Vaporization potential | KJ/Kg | 180.3 | 178 |
| Viscosity | Mpas(20℃) | 0.43 | |
| Residual quantity | Ppm | After 7 days, 5-7 | |
| Toxicity/LD50 | mg/kg | 1436.4 |
(2) use (one) prepared tobacco expanding agent and prepare expanded cut tobacco
(1) the pipe tobacco 200kg of the moisture content of weighing 21% is packed in the impregnating autoclave that is preheated to 70 ℃, then impregnating autoclave is vacuumized, make its pressure be in 0.01Mpa;
(2) spray (one) prepared tobacco expanding agent 200kg on the pipe tobacco in impregnating autoclave;
(3) after getting (one) prepared tobacco expanding agent 100kg gasification, be filled in the impregnating autoclave, make the pressure in the impregnating autoclave increase to 0.8Mpa;
(4) the impregnating autoclave external jacket continues to be heated to 100 ℃, and the pipe tobacco in the impregnating autoclave floods 25min under the condition of 100 ℃ of pressure 0.8Mpa, temperature;
(5) after dipping finishes; Reclaim liquid tobacco expanding agent earlier; Recovery finishes, and the pressure in the impregnating autoclave drops to 0.6Mpa, and high pressure recovery gaseous state tobacco expanding agent to the pressure in the impregnating autoclave drops to 0.35Mpa then; Quicken to reclaim gaseous state tobacco expanding agent to the pressure in the impregnating autoclave again and drop to 0.21Mpa, the pressure in balance gas to the impregnating autoclave in injection reclaims impregnating autoclave drops to 0.11Mpa at last; Liquid tobacco expanding agent recycling after gasification, purification and condensation of reclaiming, the recycling after purification and condensation of the gaseous state tobacco expanding agent of recovery;
(6) after liquid tobacco expanding agent and gaseous state tobacco expanding agent reclaim and finish; Draw off pipe tobacco; And it is sent to the inherent microwave frequency of microwave expansion device is that 2450HZ, power are 10KW; Pipe tobacco is half a minute through the time of microwave cavity, but continuously through about 10 minutes～15 minutes, obtains the filling value and be 8.5, the expanded cut tobacco of swollen back moisture in cut tobacco content 12.0%, whole cut rate 92%.
Embodiment 4
(1) preparation of tobacco expanding agent
The mass percent of a kind of tobacco expanding agent of present embodiment consists of: 3-pentafluorobutane 93%, tetrafluoropropane 7%.
Its preparation method is: press 3-pentafluorobutane 93%, the mass percent of tetrafluoropropane 7% takes by weighing raw material, then; Place preparing tank, mix, use 600 purpose filter pressure filtrations again; Process the composition of tobacco shred puffing agent of present embodiment, its technology index data is seen table 4.
The technical indicator of the tobacco expanding agent of table 4. embodiment 4
| Test event | Unit | CFC-11 | Tobacco expanding agent of the present invention |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid | |
| Boiling point | ℃ | 24 | 24 |
| Freezing point | ℃ | -111 | -35 |
| Density | g/cm 3(20℃) | 1.476 | 1.28 |
| ODP | 1.0 | 0 | |
| Vaporization potential | KJ/Kg | 180.3 | 176 |
| Viscosity | Mpas(20℃) | 0.43 | |
| Residual quantity | Ppm | After 7 days, 5-7 | |
| Toxicity/LD50 | mg/kg | 1436.4 |
(2) use (one) prepared tobacco expanding agent and prepare expanded cut tobacco
(1) the pipe tobacco 100kg of the moisture content of weighing 19% is packed in the impregnating autoclave that is preheated to 75 ℃, then impregnating autoclave is vacuumized, make its pressure be in 0.05Mpa;
(2) spray (one) prepared tobacco expanding agent 100kg on the pipe tobacco in impregnating autoclave;
(3) get (one) prepared tobacco expanding agent 100kg, be filled into after the gasification in the impregnating autoclave, make the pressure in the impregnating autoclave increase to 1Mpa;
(4) the impregnating autoclave external jacket continues to be heated to 120 ℃, and pipe tobacco floods 20min under the condition of 120 ℃ of pressure 1Mpa, temperature;
(5) after dipping finishes; Reclaim liquid tobacco expanding agent earlier; Recovery finishes, and the pressure in the impregnating autoclave drops to 0.9Mpa, and high pressure recovery gaseous state tobacco expanding agent to the pressure in the impregnating autoclave drops to 0.8Mpa then; Quicken to reclaim gaseous state tobacco expanding agent to the pressure in the impregnating autoclave again and drop to 0.35Mpa, the pressure in balance gas to the impregnating autoclave in injection reclaims impregnating autoclave drops to 0.21Mpa at last; Liquid tobacco expanding agent recycling after gasification, purification and condensation of reclaiming, the recycling after purification and condensation of the gaseous state tobacco expanding agent of recovery;
(6) after liquid tobacco expanding agent and gaseous state tobacco expanding agent reclaim and finish; Draw off pipe tobacco; And it is sent to the inherent microwave frequency of microwave expansion device is that 2450HZ, power are 10KW; Pipe tobacco is half a minute through the time of microwave cavity, but continuously through about 10 minutes～15 minutes, obtains the filling value and be 8.0, the expanded cut tobacco of swollen back moisture in cut tobacco content 12.6%, whole cut rate 93%.
Embodiment 5
(2) preparation of tobacco expanding agent
The mass percent of a kind of tobacco expanding agent of present embodiment consists of: 3-pentafluorobutane 82%, Decafluoropentane 18%.
Its preparation method is: press 3-pentafluorobutane 93%, the mass percent of tetrafluoropropane 7% takes by weighing raw material, then; Place preparing tank, mix, use 600 purpose filter pressure filtrations again; Process the composition of tobacco shred puffing agent of present embodiment, its technology index data is seen table 5.
The technical indicator of the tobacco expanding agent of table 5. embodiment 5
| Test event | Unit | CFC-11 | Tobacco expanding agent of the present invention |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid | |
| Boiling point | ℃ | 24 | 39 |
| Freezing point | ℃ | -111 | -35 |
| Density | g/cm 3(20℃) | 1.476 | 1.29 |
| ODP | 1.0 | 0 | |
| Vaporization potential | KJ/Kg | 180.3 | 170 |
| Viscosity | Mpas(20℃) | 0.43 | |
| Residual quantity | Ppm | After 7 days, 5-7 | |
| Toxicity/LD50 | mg/kg | 1436.4 |
(2) use (one) prepared tobacco expanding agent and prepare expanded cut tobacco
(1) the pipe tobacco 100kg of the moisture content of weighing 19% is packed in the impregnating autoclave that is preheated to 75 ℃, then impregnating autoclave is vacuumized, make its pressure be in 0.05Mpa;
(2) spray (one) prepared tobacco expanding agent 100kg on the pipe tobacco in impregnating autoclave;
(3) get (one) prepared tobacco expanding agent 100kg, be filled into after the gasification in the impregnating autoclave, make the pressure in the impregnating autoclave increase to 1Mpa;
(4) the impregnating autoclave external jacket continues to be heated to 120 ℃, and pipe tobacco floods 20min under the condition of 120 ℃ of pressure 1Mpa, temperature;
(5) after dipping finishes; Reclaim liquid tobacco expanding agent earlier; Recovery finishes, and the pressure in the impregnating autoclave drops to 0.9Mpa, and high pressure recovery gaseous state tobacco expanding agent to the pressure in the impregnating autoclave drops to 0.8Mpa then; Quicken to reclaim gaseous state tobacco expanding agent to the pressure in the impregnating autoclave again and drop to 0.35Mpa, the pressure in balance gas to the impregnating autoclave in injection reclaims impregnating autoclave drops to 0.21Mpa at last; Liquid tobacco expanding agent recycling after gasification, purification and condensation of reclaiming, the recycling after purification and condensation of the gaseous state tobacco expanding agent of recovery;
(6) after liquid tobacco expanding agent and gaseous state tobacco expanding agent reclaim and finish; Draw off pipe tobacco; And it is sent to the inherent microwave frequency of microwave expansion device is that 2450HZ, power are 10KW; Pipe tobacco is half a minute through the time of microwave cavity, but continuously through about 10 minutes～15 minutes, obtains the filling value and be 8.5, the expanded cut tobacco of swollen back moisture in cut tobacco content 12.6%, whole cut rate 95%.
Embodiment 6-9
Embodiment 6-9 is different except used swelling agent, and other parameters all adopt embodiment 1, and concrete data are following:
| Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | |
| Swelling agent | The mixture that isopentane, tetrafluoropropane, 3-pentafluorobutane are formed | The mixture that n-amyl alcohol, heptane, MSX 4518 are formed | The mixture that HFC-236fa, Decafluoropentane are formed | The mixture that butanone, dichloro one fluoroethane are formed |
| The filling value | 8.2 | 7.5 | 7.9 | 8.4 |
| Moisture | 12.8％ | 12.3％ | 12.8％ | 12.2％ |
| Whole cut rate | 92％ | 93.4％ | 94％ | 92.6％ |
Test Example 1
The inventor has carried out screening test to the dosing method of swelling agent, and the result sees the following form:
Swelling agent dosing method difference is to the influence of expansion effect
| The swelling agent dosing method | Moisture (%) before swollen | Swollen back moisture (%) | Filling value (cm 3/g) |
| Pipe tobacco is with criticizing quantitatively, and liquid state is annotated, and pipe tobacco is 1:2, dip time with medium filling ratio | 18.79 | 12.30 | 7.82 |
| 15 minutes, time 23S expanded | |||
| Pipe tobacco is quantitative with criticizing, the gaseous state filling, and pipe tobacco is annotated than being 1:2, dip time 15 minutes, expansion time 23S with medium | 18.79 | 11.90 | 6.99 |
| Pipe tobacco is with criticizing quantitatively, and liquid state is annotated, the gaseous state supercharging, and pipe tobacco is 1:2 with medium filling ratio, dip time 15 minutes, expansion time 23S | 18.79 | 12.15 | 7.96 |
Can find out that from last table when the liquid filling of employing, during the mode of gaseous state supercharging, expansion effect is better.
Claims (13)
1. round-robin method for preparing expanded cut tobacco, this method comprises the steps:
(1) pipe tobacco is packed in the impregnating autoclave of preheating, vacuumize then;
(2) the liquid swelling agent of spray on pipe tobacco;
(3) filling gaseous expansion agent in impregnating autoclave;
(4) dipping;
(5) reclaim liquid swelling agent earlier, reclaim the gaseous expansion agent again; And
(6) pipe tobacco behind the dipping is expanded, after the liquid swelling agent described in the step (5) reclaims simultaneously, recycling after gasification, purification, condensation, after described gaseous expansion agent is reclaimed, recycling after purification, condensation.
2. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: the preheating described in the step (1) is for to be preheated to 65 ℃～75 ℃ with impregnating autoclave; The pressure that vacuumizes to making impregnating autoclave described in the step (1) is in 0.05Mpa～0.005Mpa.
3. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: the liquid swelling agent of spray and the mass ratio of pipe tobacco are 0.5～1: 1 in the step (2).
4. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: the adding amount of gaseous expansion agent described in the step (3) is to make the pressure in the impregnating autoclave increase to 0.1Mpa～1Mpa.
5. the round-robin method of preparation expanded cut tobacco according to claim 4 is characterized in that: the adding amount of gaseous expansion agent described in the step (3) is to make the pressure in the impregnating autoclave increase to 0.3Mpa～0.9Mpa.
6. the round-robin method of preparation expanded cut tobacco according to claim 5 is characterized in that: the adding amount of gaseous expansion agent described in the step (3) is to make the pressure in the impregnating autoclave increase to 0.5Mpa～0.8Mpa.
7. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: the dipping described in the step (4) floods 5min～30min at pressure 0.1Mpa～1Mpa under the condition that temperature is 65 ℃～120 ℃.
8. according to the round-robin method of right 7 described preparation expanded cut tobaccos, it is characterized in that: described pressure is 0.3Mpa～0.9Mpa.
9. the round-robin method of preparation expanded cut tobacco according to claim 8 is characterized in that: described pressure is 0.5Mpa～0.8Mpa.
10. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: the recovery of liquid swelling agent described in the step (5) is that the pressure that reclaims in liquid swelling agent to the impregnating autoclave drops to 1Mpa～0.35Mpa; The recovery of said gaseous expansion agent comprises that high pressure reclaims, quickens to reclaim and injection reclaims.
11. the round-robin method of preparation expanded cut tobacco according to claim 10 is characterized in that: it is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.8Mpa～0.35Mpa that described high pressure reclaims; It is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.35Mpa～0.21Mpa that described acceleration is reclaimed; It is to reclaim gaseous expansion agent to the pressure in the impregnating autoclave to drop to 0.21Mpa～0.11Mpa that described injection reclaims.
12. the round-robin method of preparation expanded cut tobacco according to claim 1 is characterized in that: described liquid swelling agent and gaseous state swelling agent are respectively one or several in the halogenated alkane of alkane or 2-12 carbon atom of halogen ether, a 2-12 carbon atom of ketone, a 2-12 carbon atom of alcohol, a 2-12 carbon atom of 2-12 carbon atom.
13. the round-robin method of preparation expanded cut tobacco according to claim 12 is characterized in that: described gaseous expansion agent is that corresponding liquid swelling agent forms after evaporating.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101825256A CN101617854B (en) | 2008-07-03 | 2008-12-05 | Circulation method for preparing expanded cut tobacco |
| PCT/CN2009/075332 WO2010063239A1 (en) | 2008-12-05 | 2009-12-04 | Recycling method for making expanded tobacco shred |
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| CN200810132971.6 | 2008-07-03 | ||
| CN200810132971 | 2008-07-03 | ||
| CN2008101825256A CN101617854B (en) | 2008-07-03 | 2008-12-05 | Circulation method for preparing expanded cut tobacco |
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| CN101617854B true CN101617854B (en) | 2012-06-27 |
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| WO2010063238A1 (en) * | 2008-12-05 | 2010-06-10 | 贵州中烟工业有限责任公司 | Method for continuously puffing tobacco shred with microwave |
| CN101744359B (en) * | 2008-12-19 | 2012-07-25 | 北京航天试验技术研究所 | Tobacco shred immersion method and device |
| CN106031525A (en) * | 2015-03-18 | 2016-10-19 | 北京航天试验技术研究所 | Cut tobacco expansion technology which can reduce medium loss |
| CN109275940A (en) * | 2018-08-02 | 2019-01-29 | 河南中烟工业有限责任公司 | It is a kind of using water as the tobacco expanding technique of medium |
| CN110973684A (en) * | 2019-12-02 | 2020-04-10 | 北京航天试验技术研究所 | Tobacco shred expanding agent and tobacco shred expanding method |
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Non-Patent Citations (2)
| Title |
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| 黄岳元等.几种改进的CO2膨胀烟丝工艺.《烟草科技.卷烟工艺》.1997,(第124期),第14页. * |
| 黄岳元等.几种改进的CO2膨胀烟丝工艺.《烟草科技。卷烟工艺》.1997,(第124期),第14页. |
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