CN106768440B - Method and device that is a kind of while obtaining cigarette burning wimble structure and Temperature Distribution - Google Patents
Method and device that is a kind of while obtaining cigarette burning wimble structure and Temperature Distribution Download PDFInfo
- Publication number
- CN106768440B CN106768440B CN201611126990.9A CN201611126990A CN106768440B CN 106768440 B CN106768440 B CN 106768440B CN 201611126990 A CN201611126990 A CN 201611126990A CN 106768440 B CN106768440 B CN 106768440B
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- Prior art keywords
- cigarette
- embedding
- embedding pipe
- thermocouple
- dodecenylsuccinic anhydride
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
Abstract
The invention discloses a kind of method and devices for obtaining cigarette burning wimble structure and Temperature Distribution simultaneously, this method is by thermo parameters method during thermocouple detection cigarette burning and embeds fixed cigarette combustion cone combination, the deficiency of changing features of cigarette burning process can not be fully described by by avoiding single method, provide more intuitive and reliable foundation for the mechanism that further investigation cigarette burning process and harmful substance generate.
Description
Technical field
The present invention relates to a kind of method and devices for obtaining cigarette burning wimble structure and Temperature Distribution simultaneously, belong to cigarette neck
Domain.
Background technique
The aroma source of cigarette is burnt and also produces a large amount of harmful components simultaneously in combustion process, these it is harmful at
The generation and combustion state divided is closely related, therefore has for the research of combustion state for tobacco business reducing tar and reducing harm important
Directiveness effect.
For a long time, Temperature Distribution variation is limited to for the characterization of cigarette burning process more, and for microcosmic knot therein
Structure Changeement makes little progress, and two kinds of characteristic manners are isolated to come mostly and carry out characterization cigarette burning process.However temperature
It is two particularly important factors in combustion with structure, and influences each other.Therefore the two is effectively combined, for depth
Enter to study a series of physical chemical change during cigarette burning, finding effective reducing tar and reducing harm means from the root has
Highly important meaning.
Summary of the invention
It is simple, efficient, accurate that the object of the present invention is to provide one kind, retains the morphosis of cigarette combustion cone to greatest extent
While obtain cigarette burning wimble structure and Temperature Distribution method.
Simply retain the morphosis of cigarette combustion cone to greatest extent another object of the present invention is to provide a kind of, and
Efficiently, the dress of cigarette burning wimble structure and Temperature Distribution is obtained while accurately original position obtains cigarette combustion cone internal structure
It sets.
A kind of method obtaining cigarette burning wimble structure and Temperature Distribution simultaneously of the present invention, is inserted into heat in cigarette
Then galvanic couple extinguishes rapidly the cigarette of combustion state, go to grey part of exchanging, remove thermocouple, is placed in -10 DEG C~-5 DEG C freezings
It saves；Embedding medium I is slowly added dropwise, stands infiltration, embedding medium II is then further added dropwise, is heated to 40-80 DEG C, solidifies 6-48h,
Cutting, observation；
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol
Acrylamide；
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene
Amide)=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide=0.1-0.5；
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol
Acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol；
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene
Amide)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol third
Acrylamide=0.1-0.5.
The molar ratio of the dodecenylsuccinic anhydride and N hydroxymethyl acrylamide is preferably 0.25-0.45.
The time of penetration is preferably 1-4 hours.
By the way that within the above range, optimal osmotic effect can be reached, reduces the generation of bubble time of penetration control,
And the burning wimble structure of cigarette is not destroyed simultaneously.
The solidification temperature is preferably 60-80 DEG C.
The curing time is preferably 6-12 hours.
By control solidification temperature and curing time, the embedding effect that can have further obtained.
The diameter of the thermocouple is less than 0.2mm；After being inserted into thermocouple, by overlapping glue fill thermocouple and cigarette paper it
Between gap.
Preferably, burning tapered end is placed in embedding pipe in the case where cigarette is vertically fixed.
The method extinguished rapidly is that the cigarette of combustion state is placed in small-sized closed fire-retardant container.
It can not only quickly extinguish in this way, and be conducive to maintain original burning wimble structure.
The small-sized closed container is preferably glass bushing.
By using glass bushing, help quickly to extinguish.
The glass bushing both ends open, one section cracks, and slit width is less than 1mm.
The glass bushing has the structure for adapting to cigarette shape.
Preferably rectangular in shape, square, the round or triangle of the embedding pipe.
The mode of the observation includes directly observing combustion cone cross-section structure, passing through optical microscopy, scanning electron microscopy
Mirror, transmission electron microscope or confocal laser scanning microscope.
The combustion system is quiet combustion or normal suction.
Device used in the above method, including pedestal, the pedestal are equipped with embedding pipe holder；The embedding pipe holder
On be equipped with embedding pipe；The embedding tube opening is vertically arranged upward；Be also equipped on the pedestal steadily to move up and down
Cigarette clamper；Cigarette is set to be located at the surface of embedding pipe after the cigarette clamper clamping cigarette, and combustion cone is rectified to packet
Pipe laying open end.
The embedding pipe holder can stretch up and down, to adjust cigarette embedding length, meanwhile, in same sample displacement embedding medium
In the process, also facilitate adjusting embedding pipe height or replacement embedding pipe.
The embedding pipe preferably has the structure for adapting to cigarette shape.
Facilitate to agree with cigarette and glass bushing preferably in this way.
The outer shape of the embedding pipe is preferably rectangle, square, circle or triangle.
The internal diameter of the embedding pipe is preferably 8mm~12mm.
It is defined by the internal diameter to embedding pipe, can further match cigarette dimension, while reducing the use of embedding medium
Amount.
Advantages of the present invention essentially consists in:
The present invention for the first time combines thermo parameters method during cigarette burning with microstructure change.On the one hand, hot
Galvanic couple can detect in real time the change of temperature field during cigarette burning；On the other hand, embedding fixation is in situ
Structure during observation cigarette burning inside combustion cone provides feasibility, and it is frangible to overcome the direct cutting process of combustion cone,
Lead to structure determination inaccuracy or the disadvantages of can not be measured completely, during remaining cigarette burning to the maximum extent
Actual physical state.The combination of two kinds of characterization methods avoids the spy that single method can not be fully described by cigarette burning process
Sign variation, for the mechanism that further investigation cigarette burning process and harmful substance generate provide it is more intuitive and reliably according to
According to.
The present invention is by thermo parameters method during thermocouple detection cigarette burning and embeds fixed cigarette combustion cone, cutting
The combination of its structure is observed, while obtaining efficient, accurately temperature profile and the microstructure detection in combustion process, and by
In above-mentioned two process be it is synchronous carry out, the time difference is not present, environmental condition is identical, with carry out respectively thermocouple assay and
The scheme for carrying out structure determination after cutting is compared, and has higher precision, efficiency and realizability.Especially by embedding
The selection of agent, the method for two steps embedding, composition proportion and entire sampling, embedding, solidification process are continued to optimize, and are obtained
Efficiently, accurately original position obtains the effect of cigarette combustion cone internal structure to the present invention.
The device of the invention is simple, and structure is simple and convenient to operate, and is each position during home position observation cigarette burning
Microstructure provides feasibility, avoids the disadvantages of combustion cone cutting process is frangible, remains cigarette burning to the maximum extent
Actual physical state in the process；Meanwhile cigarette and embedding pipe are relatively fixed, avoid since cigarette density is small, can not be complete
Immerse phenomena such as embedding caused by embedding medium is incomplete；Obtained sample can further be sliced, polishing treatment, be transmitted
The means such as Electronic Speculum, scanning electron microscope, laser confocal microscope are observed and are analyzed with carrying out high-resolution, can be from microcosmic angle pair
Cigarette burning process carries out analysis and provides necessary means.
Detailed description of the invention
Fig. 1 is combustion cone center section plan.
Fig. 2 is combustion cone thermo parameters method.
It can be seen from the figure that the present invention can accurately survey the structure of combustion cone and the synchronization of its thermo parameters method
It is fixed.
Fig. 3 is the schematic diagram of device used in the present invention.
Specific embodiment
Following embodiment is intended to illustrate invention, rather than further limits to the scope of the present invention.
Embodiment 1
The method for obtaining cigarette burning wimble structure and Temperature Distribution simultaneously, steps are as follows:
(1) it is implanted into thermocouple: the low-grade fever galvanic couple of 8 diameter 0.1mm is inserted into the surface of cigarette sample pipe tobacco section to be measured extremely
Cigarette center, depth spacing are 0.98mm, and the size of thermocouple is 0.1mm, and will be between thermocouple and cigarette paper with overlapping glue
Gap closing.Cigarette sample is moved into one channel smoke sucking machine, is aspirated using ISO mode, while being acquired in real time by thermocouple
The temperature change of inner cigarette, and export to computer.
(2) it samples: when ISO mode is pumped to third mouth, being inserted in cigarette with glass bushing, guarantee that glass tube cracks alignment
Thermocouple extinguishes cigarette rapidly.Carefully go to grey part of exchanging, and remove thermocouple, by cigarette be placed in refrigerator freezing save to
With.
(3) embedding is fixed: by embedding medium I:1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- hydroxyl first
Base acrylamide is uniformly mixed according to molar ratio for 1:0.2:0.49, and cigarette is vertically fixed, and burning tapered end is placed in embedding pipe.
It is slowly dropped into embedding medium I, is permeated 2 hours under room temperature, is then slowly dropped into embedding medium II, each formula and ratio are as follows: 1,2,3-
Means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N hydroxymethyl acrylamide and 2,4,6- tri- (dimethylamino methyl)
The molar ratio of phenol is 1:0.2:0.49:1.It is placed in baking oven, solidifies 12 hours at 60 DEG C.
(4) it cuts: the cigarette sample after solidification being taken out from embedding pipe, removes and does not embed part.Use precision slicer
Plane cutting is punched along cigarette, obtains combustion cone centre section.
The microscope observation analysis of cigarette combustion cone
The cigarette combustion cone embedded samples of acquisition are subjected to axially cutting, slice thickness 0.1mm.It is placed under optical microscopy
Combustion cone internal structure is observed, its combustion state and distribution are distinguished by pipe tobacco color.Combustion cone length is measured simultaneously
11.58mm, area of section 56.22mm2, and the volume for calculating combustion cone is about 512.36mm3.Pass through the images such as Image J
Processing software, the Areal porosity for calculating the cigarette sample combustion cone is 33.2%, significantly less than the Areal porosity of unburned part
50.1%.
(5) data processing: the temperature data that thermocouple acquires is depicted as thermoisopleth, obtains thermo parameters method.Simultaneously will
Thermo parameters method under cigarette combustion cone cross-section structure is corresponding with the structure compares and analyzes, and analyzes the mutual of temperature and structure
Relationship (Fig. 1 and Fig. 2).
Embodiment 2
As shown in figure 3, the fixed device of cigarette combustion cone of the invention, including pedestal 1, the pedestal 1 are equipped with embedding pipe
Bracket 6；Outer shape is installed for round, square or triangle on the embedding pipe holder 6, internal diameter is 8mm~12mm's
Embed pipe 5；The embedding pipe 5 is opening up to be vertically arranged；The cigarette folder that can steadily move up and down is also equipped on the pedestal 1
Holder 2；The cigarette clamper clamps the surface for making cigarette 3 be located at embedding pipe after cigarette 3, and combustion cone is rectified to embedding pipe
5 open ends.
In use, a cigarette sample is taken to light first, it is pumped to third mouth under mode standard, cigarette is put into circle rapidly
In shape glass bushing, extinguish cigarette rapidly；Grey part of exchanging carefully is gone to, cigarette 3 is fixed on vertically in cigarette clamper 2,
And height is regulated, protrude into combustion cone 4 integrally in embedding pipe 5；It is slowly dropped into the embedding medium for being not added with curing agent, is seeped under room temperature
Saturating 2 hours；Then the height of embedding pipe holder 6 is adjusted, the embedding pipe more renewed makes combustion cone 4 integrally protrude into the packet after replacement
In pipe laying, and fill the embedding medium containing curing agent of brand-new；After standing eliminates bubble, whole device is placed in baking oven, 60
Solidify 24 hours at DEG C；The cigarette sample after solidification is taken out from embedding pipe finally, removes and does not embed part；Use precision slicing
Machine carries out cutting, obtains the axial cross section of cigarette combustion cone, and carry out subsequent analysis.
Comparative example 1
It in step (3), is directly handled with embedding medium II, is not used embedding medium I, remaining operation is the same as embodiment 1.
As a result a large amount of bubbles are generated, can not accurate observation combustion cone structure.
Claims (9)
1. a kind of method for obtaining cigarette burning wimble structure and Temperature Distribution simultaneously, which is characterized in that be inserted into thermoelectricity in cigarette
It is even, the cigarette of combustion state is extinguished rapidly, grey part of exchanging is gone to, removes thermocouple, -10 DEG C~-5 DEG C freezings is subsequently placed in and protects
It deposits；Embedding medium I is slowly added dropwise, stands infiltration, embedding medium II is then further added dropwise, is heated to 40-80 DEG C, solidifies 6-48h, cuts open
It cuts, observes；Its combustion state and distribution are distinguished by pipe tobacco color；
The temperature data that thermocouple acquires is depicted as thermoisopleth, obtains thermo parameters method；Simultaneously by cigarette combustion cone section knot
Thermo parameters method under structure is corresponding with the structure compares and analyzes, and analyzes the correlation of temperature and structure；
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene
Amide；
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N hydroxymethyl acrylamide)
=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide=0.1-0.5；
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene
Amide and 2,4,6- tri- (dimethylamino methyl) phenol；
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol acryloyl
Amine)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol propylene
Amide=0.1-0.5.
2. method according to claim 1, it is characterised in that: the dodecenylsuccinic anhydride and N- methylol propylene
The molar ratio of amide is 0.25-0.45.
3. method according to claim 1, it is characterised in that: the time of penetration is 1-4 hours.
4. method according to claim 1, it is characterised in that: the solidification temperature is 60-80 DEG C, curing time 6-
12 hours.
5. according to the described in any item methods of claims 1-4, it is characterised in that: the diameter of the thermocouple is less than 0.2mm；
After being inserted into thermocouple, the gap between thermocouple and cigarette paper is filled by overlapping glue.
6. according to the described in any item methods of claims 1-4, it is characterised in that: will combustion in the case where cigarette is vertically fixed
Tapered end is burnt to be placed in embedding pipe.
7. according to the described in any item methods of claims 1-4, it is characterised in that: the method extinguished rapidly is by combustion state
Cigarette be placed in small-sized closed fire-retardant container；The small-sized closed container is glass bushing；It opens at the glass bushing both ends
Mouthful, one section cracks, and slit width is less than 1mm；The glass bushing has the structure for adapting to cigarette shape.
8. device used in any one of claim 1-7 method, it is characterised in that: including pedestal (1), on the pedestal (1)
Equipped with embedding pipe holder (6)；Embedding pipe (5) is installed on the embedding pipe holder (6)；The embedding pipe (5) is opening up perpendicular
Straight setting；The cigarette clamper (2) that can steadily move up and down is also equipped on the pedestal (1)；Cigarette clamper (2) folder
Hold the surface for making cigarette (3) to be located at embedding pipe (5) after cigarette (3), and combustion cone (4) face embedding pipe (5) open end.
9. device according to claim 8, it is characterised in that: the embedding pipe (5) has the knot for adapting to cigarette shape
Structure；
The embedding pipe holder (6) can stretch up and down；
The outer shape of the embedding pipe (5) is rectangle, square, circle or triangle；
The internal diameter of the embedding pipe (5) is 8mm~12mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611126990.9A CN106768440B (en) | 2016-12-09 | 2016-12-09 | Method and device that is a kind of while obtaining cigarette burning wimble structure and Temperature Distribution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611126990.9A CN106768440B (en) | 2016-12-09 | 2016-12-09 | Method and device that is a kind of while obtaining cigarette burning wimble structure and Temperature Distribution |
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| Publication Number | Publication Date |
|---|---|
| CN106768440A CN106768440A (en) | 2017-05-31 |
| CN106768440B true CN106768440B (en) | 2019-04-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4854332A (en) * | 1986-07-03 | 1989-08-08 | Sakura Color Products Corp. | Cigarette having thermochromogenic portions thereon |
| CN101769733A (en) * | 2010-01-12 | 2010-07-07 | 湖北中烟工业有限责任公司 | Method for measuring dimension of cigarette burning cone shape |
| CN101922979A (en) * | 2009-06-15 | 2010-12-22 | 湖北中烟工业有限责任公司 | Device and method for measuring gas phase temperature of a cigarette combustion cone |
| CN105158142A (en) * | 2015-09-16 | 2015-12-16 | 中国烟草总公司郑州烟草研究院 | Detection method for permeability of cigarette burning cone |
-
2016
- 2016-12-09 CN CN201611126990.9A patent/CN106768440B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4854332A (en) * | 1986-07-03 | 1989-08-08 | Sakura Color Products Corp. | Cigarette having thermochromogenic portions thereon |
| CN101922979A (en) * | 2009-06-15 | 2010-12-22 | 湖北中烟工业有限责任公司 | Device and method for measuring gas phase temperature of a cigarette combustion cone |
| CN101769733A (en) * | 2010-01-12 | 2010-07-07 | 湖北中烟工业有限责任公司 | Method for measuring dimension of cigarette burning cone shape |
| CN105158142A (en) * | 2015-09-16 | 2015-12-16 | 中国烟草总公司郑州烟草研究院 | Detection method for permeability of cigarette burning cone |
Non-Patent Citations (1)
| Title |
|---|
| 卷烟燃烧锥温度分布的表征方法;刘民昌 等;《烟草科技》;20121231(第12期);9-13 |
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