CN104055219A - Tobacco shred additive as well as preparation method and application thereof in cigarette production - Google Patents
Tobacco shred additive as well as preparation method and application thereof in cigarette production Download PDFInfo
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- CN104055219A CN104055219A CN201410276135.0A CN201410276135A CN104055219A CN 104055219 A CN104055219 A CN 104055219A CN 201410276135 A CN201410276135 A CN 201410276135A CN 104055219 A CN104055219 A CN 104055219A
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Abstract
The invention discloses a tobacco shred additive as well as a preparation method and application thereof in cigarette production. The tobacco shred additive is a 0.1-0.3wt% homogeneous-phase solution obtained by performing ultrasonic dispersion on a graphene oxide compound in water by virtue of ultrasonic waves. The preparation method of the tobacco shred additive comprises the following steps: a, low-temperature oxidation reaction; b, middle-temperature oxidation reaction; c, high-temperature oxidation reaction; d, centrifugation; e, ultrasonic dispersion, wherein a liquid tobacco shred additive obtained in the step c is refrigerated and dried so as to obtain the fluffy tobacco shred additive. The application of the tobacco shred additive in the cigarette production comprises the follows steps: uniformly spraying the tobacco shred additive on the surfaces of cigarette tobacco shreds by use of a high-pressure sprayer, and then performing equalization treatment. The tobacco shred additive has a favorable cooling effect; the average reduced temperature is 30-45 DEG C; the maximum temperature for cigarette pumping is reduced by 79 DEG C to the greatest extent; release of harmful substances generated by combustion of cigarettes is effectively reduced, and the combustion and pumping quality of the cigarettes has no change nearly.
Description
Technical field
The present invention relates to cigarette shreds additive technology field, relate in particular to a kind of tobacco shred additive and preparation method thereof and the application for the production of cigarette, particularly a kind of tobacco shred additive mixes with cigarette shreds by solution spray method.
Background technology
Cigarette combustion cone temperature is that impact is main, chemical composition in flow measurement flue gas and content and then affect one of fundamental characteristics parameter of cigarette burning quality.It directly affects the pyrolysis synthetic reaction of tobacco component after burning cone, has affected all kinds of volatilizations in cigarette, half volatile ingredient to the conveying capacity in flue gas, also with harmful substances in flue gas number have very large associated.Along with the rising of cigarette burning temperature, the burst size of CO is almost linear to be increased; In " cigarette shreds thermal cracking products Studies on Analysis of Flavor Constituents " various reports and paper, and scientific experiment confirmation, along with the reduction of burning cone temperature, the reduction amplitude of fragrance matter burst size is very little.In sum, reduce cigarette burning temperature, can reduce the burst size of harmful constituents in cigarette flue gas, fragrance matter burst size is influenced hardly simultaneously.
At present, how reduce in cigarette combustion cone temperature and be still a hang-up, in the time that cigarette burning uses, because the temperature of normal combustion can produce more harmful substance, larger to harm; Because ignition temperature is with the direct ratio that is released into of harmful matter in cigarette, meanwhile, reduce temperature little on the suction quality impact of cigarette, therefore how to reduce the temperature of cigarette burning, the protection to environment and smoker's health are highly beneficial.
Now, cigarette burning thermometry has also obtained develop rapidly, utilizes RM/PLUS one channel smoke sucking machine to coordinate thermal infrared imager high-resolution, quick record effectively to measure the burning cone temperature of cigarette.Wu Jumin has been developed a kind of superfine temperature-sensing thermocouple 2004, measures pipe tobacco burning cone temperature by contact method.As can be seen here, by temperature sensing means accurately, seek the tobacco shred additive of effective reduction cigarette combustion cone temperature, and then reduce the burst size of harmful components in cigarette burning product, finally realize the lowering harm and decreasing coking of cigarette, can solve a difficult problem for cigarette combustion cone temperature.
Summary of the invention
The weak point existing for prior art, the object of the present invention is to provide a kind of tobacco shred additive and preparation method thereof and the application for the production of cigarette, this tobacco shred additive green is harmless, can effectively reduce cigarette combustion cone temperature, and easy being easy to of preparation method controlled.
Object of the present invention is achieved through the following technical solutions:
A kind of tobacco shred additive, this tobacco shred additive is be scattered in water by ultrasonic wave and obtained the homogeneous phase solution that graphene oxide concentration is 0.1wt%～0.3wt% by graphene oxide.
A kind of preparation method of tobacco shred additive, this preparation method adopts three step oxidation reactions to produce graphene oxide, then graphene oxide is scattered in and in water, is formed the homogeneous phase solution that graphene oxide mass number is 0.1wt%～0.3wt% by ultrasonic wave; Its preparation method comprises the steps:
A, low-temperature oxidation reaction: to the dense H that adds 255～325 weight portions in the graphite powder of 6～12 weight portions
2sO
4naNO with 2.5～6.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 22.5～37.5 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 8～28 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
The further preferred technical scheme of this tobacco shred additive preparation method is as follows: its preparation method comprises the steps:
A, low-temperature oxidation reaction: to the dense H that adds 260～320 weight portions in the graphite powder of 8～10 weight portions
2sO
4naNO with 3～6 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 24～36 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 10～25 weight portions continues to stir and within 13～17 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 50～60 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 8～12 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
The present invention goes back further preferred technical scheme after completing steps e: after described step e, also carry out step f, step f: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
In the present invention, the further preferred technical scheme of step a is: in described step a, the granularity of graphite powder is controlled at 400 order～800 orders.
In the present invention, the further preferred technical scheme of steps d is: the powdery graphite olefinic oxide after described steps d centrifugal treating, through warm water rinsing repeatedly, until pH value is 6.8～7.2, then is dried processing.
In the present invention, the further preferred technical scheme of step e is: in the liquid tobacco shred additive of described step e, the mass number of graphene oxide in the aqueous solution is 0.1wt%～0.3wt%.
A kind of tobacco shred additive is in the application of producing on cigarette, with high-pressure sprayer, tobacco shred additive is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product.
Better for its effect, the ratio of weight and number of described tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
The present invention compares compared with prior art, has the following advantages and beneficial effect:
(1) pipe tobacco temperature control additive of the present invention belongs to green harmless additive, and its preparation process is easy, be easy to control, and can produce in batches as required.
(2) addition manner of pipe tobacco temperature control additive of the present invention is easy, need not change existing cigarette producing process, and cost of material is cheap, has good industrial application value.
(3) show through test of many times result, tobacco shred additive of the present invention is added in existing many moneys tobacco product pipe tobacco, all have good cooling-down effect, it on average reduces temperature is 30～45 DEG C, and amplitude peak reduces by 79 DEG C of cigarette smoking maximum temperatures; The harmful substance that has effectively reduced cigarette burning discharges, and cigarette is almost unchanged qualitatively in burning suction.
Brief description of the drawings
Fig. 1 is that ESEM characterizes the effect behind the coated pipe tobacco of GO surface;
Fig. 2-1 is blank cigarette combustion cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-2 are sample cigarette a burning cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-3 are sample cigarette b burning cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-4 are sample cigarette c burning cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-5 are sample cigarette d burning cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-6 are sample cigarette e burning cone suction maximum temperature transient temperature distribution audio-visual picture;
Fig. 2-7 are sample cigarette f burning cone suction maximum temperature transient temperature distribution audio-visual picture.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment
A kind of tobacco shred additive, this tobacco shred additive is be scattered in water by ultrasonic wave and obtained the homogeneous phase solution that graphene oxide concentration is 0.1wt%～0.3wt% by graphene oxide.
Shown in as shown in Figure 1, Figure 2-1～Fig. 2-7, a kind of preparation method of tobacco shred additive, this preparation method adopts three step oxidation reaction legal systems to produce graphene oxide, then graphene oxide is scattered in and in water, is formed the homogeneous phase solution that graphene oxide mass number is 0.1wt%～0.3wt% by ultrasonic wave; Its preparation method comprises the steps:
A, low-temperature oxidation reaction: to the dense H that adds 255～325 weight portions in the graphite powder of 6～12 weight portions
2sO
4naNO with 2.5～6.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO4 that adds 22.5～37.5 weight portions in mixed solution, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 8～28 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
According to above-mentioned preparation method's step, the present embodiment is further preferred preparation method comprise the steps:
A, low-temperature oxidation reaction: to the dense H that adds 260～320 weight portions in the graphite powder of 8～10 weight portions
2sO
4naNO with 3～6 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 24～36 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 10～25 weight portions continues to stir and within 13～17 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 50～60 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 8～12 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
The present invention, after having completed step a-e, can also preferably carry out step f, step f: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
A preferred step a embodiment according to the present invention, in step a, the granularity of graphite powder is controlled at 400 order～800 orders.
A preferred steps d embodiment according to the present invention, the powdery graphite olefinic oxide after steps d centrifugal treating, through warm water rinsing repeatedly, until pH value is 6.8～7.2, then is dried processing.
A preferred step e embodiment according to the present invention, in the liquid tobacco shred additive of step e, the mass number of graphene oxide in the aqueous solution is 0.1wt%～0.3wt%.
A kind of tobacco shred additive is in the application of producing on cigarette, with high-pressure sprayer, tobacco shred additive is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product.
In order to make tobacco shred additive apply get Geng Jia on cigarette, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
The application specific embodiment of tobacco shred additive of the present invention on production cigarette is as follows:
Embodiment 1
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 255 weight portions in the graphite powder of 6 weight portions
2sO
4naNO with 2.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 22.5 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 8～28 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As shown in Fig. 2-2, obtain sample cigarette a by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette a is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
Embodiment 2
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 260 weight portions in the graphite powder of 8 weight portions
2sO
4naNO with 3 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 24 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 10 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO4 unnecessary in reaction solution;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As Figure 2-3, obtain sample cigarette b by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette b is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
Embodiment 3
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 290 weight portions in the graphite powder of 9 weight portions
2sO
4naNO with 4.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 24 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to temperature 45 C is stirred 35 minutes, then the deionized water of adding 17.5 weight portions continues to stir and within 20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7 minutes under 7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As in Figure 2-4, obtain sample cigarette c by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette c is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65 hours that 22 DEG C of temperature and relative humidity are 60%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001.
Embodiment 4
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 290 weight portions in the graphite powder of 12 weight portions
2sO
4naNO with 4.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 30 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35 DEG C of temperature is stirred 35 minutes, then the deionized water of adding 10 weight portions continues to stir and within 20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 15 minutes under 7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As shown in Figure 2-5, obtain sample cigarette d by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette d is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65 hours that 20 DEG C of temperature and relative humidity are 55%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.003.
Embodiment 5
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 325 weight portions in the graphite powder of 28 weight portions
2sO
4naNO with 6.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 37.5 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to temperature 45 C is stirred 25 minutes, then the deionized water of adding 25 weight portions continues to stir and within 20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under temperature 70 C condition and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 8 minutes under 7200rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.07W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As shown in Fig. 2-6, obtain sample cigarette e by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette e is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 72 hours that 24 DEG C of temperature and relative humidity are 65%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.002.
Embodiment 6
First prepare tobacco shred additive, its preparation method is as follows:
A, low-temperature oxidation reaction: to the dense H that adds 320 weight portions in the graphite powder of 18 weight portions
2sO
4naNO with 6 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 30 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 4.5 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water;
F: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
As shown in Fig. 2-7, obtain sample cigarette f by above-mentioned steps, then in the time producing cigarette, by high-pressure sprayer, sample cigarette f is evenly sprayed to the pipe tobacco surface of cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product, the ratio of weight and number of its tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
The sample cigarette of above-described embodiment 1-6 is carried out respectively to cigarette burning, measure the temperature value of its cigarette burning in the time of cigarette burning, the assay method of cigarette burning temperature of the present invention comprises the steps:
Maximum temperature while utilizing RM1/PLUS one channel smoke sucking machine to coordinate infrared heat image instrument measuring cigarette high-resolution, quick record glow and aspirate.The distance of adjusting thermal imaging system and object is 0.1m, the temperature-measuring range of Infrared Detectors is selected 300～1500 DEG C, bring into focus, infrared emittance is set to 0.87, with burning cone solid-state temperature in the speed record cigarette smoking process of 50Hz, to aspirate maximum temperature and to glow maximum temperature value parameter as a comparison.The cigarette of each kind carries out ten times to be measured, results averaged.
Each sample cigarette is first carried out the sorting of weight and resistance to suction before experiment, ensures that it has comparativity as far as possible.Then 22 ± 10 DEG C of temperature, balance 72h under humidity 60 ± 2%RH condition.According to international standard, the single port suction capacity setting of smoking machine is that 35cm3, suction time are that 2s, suction are spaced apart 60s.And obtain the blank cigarette of table 1, table 2 and the ignition temperature of each sample cigarette and measure situation.
Table 1 tobacco shred additive is to the cigarette cooling-down effect of high suction temperatures:
| Cigarette sample | Suction peak-peak temperature (DEG C) | Suction peak temperature mean value (DEG C) | The range of decrease (DEG C) |
| Blank cigarette | 934 | 930 | — |
| Sample cigarette a | 905 | 902 | 28 |
| Sample cigarette b | 868 | 865 | 65 |
| Sample cigarette c | 855 | 854 | 76 |
| Sample cigarette d | 904 | 897 | 33 |
| Sample cigarette e | 863 | 860 | 70 |
| Sample cigarette f | 854 | 851 | 79 |
The cooling-down effect of table 2 tobacco shred additive to the highest temperature of glowing of cigarette:
| Cigarette sample | The peak-peak of glowing temperature (DEG C) | Glow peak temperature mean value (DEG C) | The range of decrease (DEG C) |
| Blank cigarette | 643 | 641 | — |
| Sample cigarette a | 615 | 610 | 31 |
| Sample cigarette b | 608 | 605 | 36 |
| Sample cigarette c | 601 | 598 | 43 |
| Sample cigarette d | 614 | 609 | 32 |
| Sample cigarette e | 603 | 600 | 41 |
| Sample cigarette f | 601 | 597 | 44 |
The table 3 cigarette paper combustionregulator trial-production Sensory Quality of Cigarette table (judging panel's number 7 people) of smokeing panel test
Table 1 draws the following conclusions: by add cigarette that tobacco shred additive that this preparation method obtains produces to cigarette the cooling value scope of high suction temperatures be 30～45 DEG C, table 2 draws the following conclusions: be 30～45 DEG C by adding the cigarette that tobacco shred additive that this preparation method obtains produces to the cooling value scope of the highest temperature of glowing of cigarette; Table 3 draws the following conclusions: almost consistent with blank cigarette on Sensory Quality of Cigarette by adding the cigarette that tobacco shred additive that this preparation method obtains produces, the suction quality that cigarette under 30～45 DEG C of scopes of cooling is described reduces less, almost without affecting.
To sum up correction data draws, the addition manner of the tobacco shred additive that the present invention obtains is easy, need not change existing cigarette producing process, and cost of material is cheap, has good industrial application value.Test of many times result shows, tobacco shred additive of the present invention is added in existing many moneys tobacco product pipe tobacco, all there is good cooling-down effect, amplitude peak reduces by 79 DEG C of cigarette smoking maximum temperatures, average cooling is 30～45 DEG C, the harmful substance that has effectively reduced cigarette burning discharges, and cigarette is almost unchanged qualitatively in burning suction.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. a tobacco shred additive, is characterized in that: this tobacco shred additive is be scattered in water by ultrasonic wave and obtained the homogeneous phase solution that graphene oxide concentration is 0.1wt%～0.3wt% by graphene oxide.
2. a preparation method for tobacco shred additive, is characterized in that: its preparation method comprises the steps:
A, low-temperature oxidation reaction: to the dense H that adds 255～325 weight portions in the graphite powder of 6～12 weight portions
2sO
4naNO with 2.5～6.5 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 22.5～37.5 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 8～28 weight portions continues to stir and within 12～20 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 48～70 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 7～15 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
3. according to the preparation method of tobacco shred additive claimed in claim 2, it is characterized in that: its preparation method comprises the steps:
A, low-temperature oxidation reaction: to the dense H that adds 260～320 weight portions in the graphite powder of 8～10 weight portions
2sO
4naNO with 3～6 weight portions
3, then in ice-water bath, stir and obtain mixed solution, to the KMnO that adds 24～36 weight portions in mixed solution
4, reaction obtains low-temperature oxidation solution under lower than 20 DEG C of temperature conditions;
B, middle temperature oxidation reaction: the water bath with thermostatic control that the low-temperature oxidation solution of step a is placed in to 35～45 DEG C of temperature is stirred 25～35 minutes, then the deionized water of adding 10～25 weight portions continues to stir and within 13～17 minutes, obtains middle temperature oxidation reaction solution;
C, high-temperature oxydation reaction: the middle temperature oxidation reaction solution of step b is placed under 50～60 DEG C of conditions of temperature and adds H
2o
2, until remove KMnO unnecessary in reaction solution
4till;
D, centrifugal treating: the reaction solution that step c is obtained is centrifugal treating 8～12 minutes under 7000～7400rpm condition at the rotating speed of centrifuge, obtains powdery graphite olefinic oxide;
E, ultrasonic wave disperse: the powdery graphite olefinic oxide that steps d is obtained is 0.06～0.08W/cm by ultrasonic frequency
3ultrasonic wave be scattered in water.
4. according to the preparation method of tobacco shred additive claimed in claim 3, it is characterized in that: after described step e, also carry out step f,
Step f: the liquid tobacco shred additive that step c is obtained obtains the tobacco shred additive of puffy after freezing, dry processing.
5. according to the preparation method of tobacco shred additive claimed in claim 3, it is characterized in that: in described step a, the granularity of graphite powder is controlled at 400 order～800 orders.
6. according to the preparation method of tobacco shred additive claimed in claim 3, it is characterized in that: the powdery graphite olefinic oxide after described steps d centrifugal treating, through warm water rinsing repeatedly, until pH value is 6.8～7.2, then is dried processing.
7. according to the preparation method of tobacco shred additive claimed in claim 3, it is characterized in that: in the liquid tobacco shred additive of described step e, the mass number of graphene oxide in the aqueous solution is 0.1wt%～0.3wt%.
One kind according to claim 1 tobacco shred additive or the tobacco shred additive that obtains according to preparation method described in claim 2～7 any one in the application of producing on cigarette, it is characterized in that: the pipe tobacco surface that with high-pressure sprayer, tobacco shred additive is evenly sprayed to cigarette, again pipe tobacco is placed in to the tandem-driving bogie balance 65～79 hours that 22 ± 2 DEG C of temperature and relative humidity are 60 ± 5%RH, finally with factory's cigarette machine, the tobacco cartridge after balance is made to cigarette finished product.
9. according to the preparation method of tobacco shred additive claimed in claim 8, it is characterized in that: the ratio of weight and number of described tobacco shred additive homogeneous phase solution and pipe tobacco is 0.001～0.003.
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| CN106690404A (en) * | 2015-11-18 | 2017-05-24 | 中国烟草总公司郑州烟草研究院 | Cut tobacco additive based on graphene nanocomposite and preparation method and application thereof |
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| US5551451A (en) * | 1993-04-07 | 1996-09-03 | R. J. Reynolds Tobacco Company | Fuel element composition |
| US20100065075A1 (en) * | 2008-09-18 | 2010-03-18 | R.J. Reynoldds Tobacco Company | Method for Preparing Fuel Element For Smoking Article |
| CN103005712A (en) * | 2013-01-04 | 2013-04-03 | 江苏中烟工业有限责任公司 | Grapheme type fiber cigarette filter and preparation method thereof |
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| CN106690404B (en) * | 2015-11-18 | 2018-07-27 | 中国烟草总公司郑州烟草研究院 | Tobacco shred additive and its preparation method and application based on graphene nanocomposite material |
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Effective date of registration: 20161219 Address after: 610000, Sichuan, Chengdu, Longquanyi economic and Technological Development Zone, Jackie Chan Road, Longquan, No. 2, paragraph Patentee after: CHINA TOBACCO SICHUAN INDUSTRIAL CO., LTD. Patentee after: CHONGQING CHINA TOBACCO INDUSTRIAL CO., LTD. Address before: 610000 Jackie Chan Road, Chengdu economic and Technological Development Zone, Longquanyi District, Sichuan, China, No. 2, No. Patentee before: China Tobacco Chuanyu Industry Co., Ltd. |