CN2921819Y

CN2921819Y - High temperature destructive distillation hot cracking device

Info

Publication number: CN2921819Y
Application number: CN 200620050769
Authority: CN
Inventors: 彭新辉; 易建华; 赵瑜; 李克; 杨华武
Original assignee: China Tobacco Hunan Industrial Co Ltd
Current assignee: China Tobacco Hunan Industrial Co Ltd
Priority date: 2006-04-27
Filing date: 2006-04-27
Publication date: 2007-07-11
Anticipated expiration: 2016-04-27

Abstract

A high temperature destructive distillation hot cracking device comprises a cracking tank, a muffle furnace and a temperature controller, wherein, samples are put in the cracking tank and sealed; the cracking tank is placed in the muffle furnace, and the temperature is controlled by the temperature controller; the cracking tank is communicated with an inert gas steel bottle and a collecting bottle holding absorption solvent respectively through an intake pipe and an outtake pipe. The utility model is simple in structure, large in capacity, good in repeatability and strong in maneuverability, which can be used in the high temperature destructive distillation hot cracking of tobacco, rubber products and other organic compounds and the study on monomer pyrolysis and synthesis of organic compounds, and supplies possible analysis way for elucidating the formation of smoke aroma compositions in tobacco burning and suction process.

Description

A kind of high temperature carbonization thermal cracker

Technical field

The utility model relates to a kind of tobacco or other organism high temperature carbonization thermal cracker of being used for.

Background technology

Cigarette is because the flue gas that the consumer is produced by suction pipe tobacco burning obtains certain satisfies.Smoke components be cigarette shreds by burn, distillation, destructive distillation, pyrolysis and complicated process such as synthetic again form.At present, estimating the traditional method of tobacco quality is to adopt the method for manually smokeing panel test to estimate the quality of fragrant jealous and other index of single-tobacco-typed cigarette or cigarette smoke, and burning and sucking the mode of analyzing flue gas with smoking machine simulation cigarette only is a kind of supplementary means.Cigarette props up when being burnt and sucked, and its fragrance thing not only derives from the combustion zone that cigarette props up, and the more important thing is to derive from its destructive distillation pyrolysis zone.Therefore study thermal cracking, destructive distillation of tobacco and synthetic product again, can systematic analysis other important perfumery that causes except that the aroma substance that directly discharges by high temperature combustion zone, comprise surperficial volatile matter, pyrogen, complex etc. again, can further describe the combustion process that cigarette props up and the mechanism of the fragrant jealous formation of flue gas like this from another side.Up to now, the tobacco chemistry men have utilized the thermal cracking chromatographic technique to measure product and its formation mechanism of prediction of cigarette burning, thereby are that very big contribution has been made in the development that promotes tobacco chemistry.In these researchs, cracker is that gas chromatograph is done the important accessory that pyrolysis chromatography is analyzed.General Study adopts the thermal cracking instrument of CDS series, carries out analyzing and testing in conjunction with GC-MS again.Though this method accuracy of detection is higher, because all being microgram, each sample introduction arrives the milligram level, and samples' representativeness and repeatability just are worth consideration like this, and the reliability of data is also had a greatly reduced quality; And this kind thermal cracking instrument equipment cost height, required funds are more.

The utility model content

The purpose of this utility model aims to provide a kind of simple in structure, and cost is low, and sample size is big, good reproducibility, workable high temperature carbonization thermal cracker.

The purpose of this utility model realizes by following manner:

Device of the present utility model comprises crack tank, muffle furnace, temperature controller, and sample is packed in the crack tank, sealing, and crack tank places muffle furnace, by the temperature controller regulating and controlling temperature; Crack tank is communicated with by draft tube, escape pipe and inert gas steel cylinder, receiving flask that lyosorption is housed respectively.

Described receiving flask places cold-trap, to improve absorption efficiency.

Be connected with air-flow minute adjustment valve on the inert gas steel cylinder.

Because the utility model adopts this important container of crack tank can directly carry out cracking, required cracking apparatus obtains the simplification of maximum possible.Sample is directly put into crack tank, the space of a bigger cracking reaction is provided, and sampling is amplified to more than the gram level fully, can fully, no longer be subjected to the limitation of existing equipment, can do the absorption and the analysis of maximum possible to sample composition, the representativeness of its analysis strengthens widely.And whole device is equipped with the reasonable of ten minutes, effectively.Crack tank directly places can accurately temperature automatically controlled muffle furnace, and receiving flask, cold-trap are made simple, and required cracking collecting device has obtained very big simplification, thereby has greatly reduced equipment cost.In addition, device easy operating of the present utility model is collected completely, not only contains the low temperature volatile compounds that lysate sample itself contains in absorption liquid, also contains products such as the destructive distillation pyrogen of sample under the condition of high temperature and new complex simultaneously.

The utility model has been studied a kind of device that is used for tobacco and other organism destructive distillation thermal cracking research.Apparatus structure of the present utility model is simple, sample-loading amount is big, good reproducibility, workable, the pyrolysis and the study on the synthesis that can be used for tobacco, rubber and other organic high temperature carbonization cracking and organism monomer also provide possible analysis approach for illustrating the formation that tobacco burns and sucks the smoke perfume material in the process.

Description of drawings

Fig. 1 is the structural representation of the utility model device.

Fig. 2 is the structural drawing of the utility model crack tank.

Fig. 3 be among the embodiment tobacco powder in 100 ℃ handle 2 hours after the total ion current figure (TIC) that detect with GC/MS of absorption liquid.

Fig. 4 is that tobacco powder rises to 200 ℃ again and handles the total ion current figure (TIC) that new absorption liquid detects with GC/MS after 2 hours after above-mentioned 100 ℃ of processing was changed absorption liquid in 2 hours among the embodiment.

Fig. 5 for tobacco powder among the embodiment in above-mentioned 100 ℃ and 200 ℃ respectively handle changed absorption liquid in 2 hours after, rise to 300 ℃ again and handled 2 hours, its new absorption liquid is with the total ion current figure (TIC) of GC/MS detection.

Fig. 6 be among the embodiment tobacco powder directly in 300 ℃ handle 2 hours after the total ion current figure (TIC) that detect with GC/MS of its absorption liquid.

Embodiment

Embodiment 1

Device of the present utility model comprises crack tank 6, muffle furnace 5,

temperature controller

4, and 7 li samples of packing into of surface plate are placed in the crack tank 6, sealing, and crack tank 6 places muffle furnace 5, by temperature controller 4 regulating and controlling temperatures; The bottom of crack tank 6 is connected with inert gas steel cylinder 1 by draft tube 3, connects an accurate barometric damper 2 on the draft tube 3, enters the gas flow rate of crack tank in order to control; The top of crack tank 6 is connected with the receiving flask 9,10 that lyosorption is housed by escape pipe 8.Receiving flask is put into cold-trap 11.

Specifically connect referring to Fig. 1.In advance tobacco leaf is worn into powder, and cross the 80-100 mesh sieve.Earlier temperature controller 4 is set in a certain temperature, muffle furnace 5 is heated to this assigned temperature.Take by weighing the above-mentioned tobacco powder of 10 grams, put into crack tank, cover completely and connect the inert gas steel cylinder, water is checked its impermeability in advance.After installing collection solvent (as methylene chloride, absolute ethyl alcohol or acetone etc.) in first order receiving flask and the second level receiving flask respectively, connect with crack tank again.Immediately crack tank is inserted the muffle furnace centre and also close the door immediately, control air-flow minute adjustment valve makes pyrolysis gas bubbling speed in first order receiving flask moderate.After cracking 2-3 hour, go in the first order receiving flask, after again two-stage being absorbed liquid mixing and concentrating, adopt GC-MS or Other Instruments to detect compound in the absorption liquid with absorption liquid washing crack tank and escape pipe identical in an amount of and the first order receiving flask.

Referring to Fig. 3,4,5,6.As seen from the figure, classes of compounds and content all change in the absorption liquid of tobacco under the treatment of different temperature condition.Under 100 ℃ of conditions, nicotine content is lower, does not just overflow but pyrolysis almost takes place for neophytadiene and some low-boiling point materials, so the higher (see figure 3) of content.But in the time of 200 ℃, nicotine content increases more, because carbonization decomposition is inviolent yet, so neophytadiene and other content of material reduce very fast (see figure 4).Be raised to 300 ℃, except nicotine continued to increase, the higher material of some boiling points was also overflowed rapidly, adds possible pyrogenation and carbonization gas, and some materials that can detect are obviously handled (see figure 5) more than preceding two.In addition, from figure, also can find out, contain Megastigmatrienone, 2 in the pyrogenation and carbonization gas of tobacco, 3-dihydro-3, flavor matters such as 5-dihydroxy-6-methyl-4 (H) pyrans-4-ketone (DDMP), furans and pyrazine, thereby the part of soluble these materials source.And directly sample is placed under 300 ℃ of conditions, in the absorption liquid detectable material abundance many, not only contain the low temperature volatile compounds that lysate sample itself contains, also contain simultaneously products such as the destructive distillation pyrogen of sample under the condition of high temperature and new complex.(see figure 6).

Therefore adopting this method to carry out series heats up, can not only detect the kind and the content of easy volatile matter in the tobacco leaf, correlationship in the time of also further studying the tobacco leaf carbonization decomposition between the generation of other material and they and the temperature, thus new analysis platform provided for understanding quality of tobacco.

Claims

1, a kind of high temperature carbonization thermal cracker, it is characterized in that: comprise crack tank (6), muffle furnace (5), temperature controller (4), sample is packed in the crack tank (6), sealing, crack tank (6) places muffle furnace (5), by temperature controller (4) regulating and controlling temperature; Crack tank (6) is communicated with by draft tube (3), escape pipe (8) and inert gas steel cylinder (1), receiving flask (9,10) that lyosorption is housed respectively.

2, a kind of high temperature carbonization thermal cracker according to claim 1 is characterized in that: described receiving flask (9,10) places cold-trap (11).

3, a kind of high temperature carbonization thermal cracker according to claim 1 is characterized in that: be connected with air-flow minute adjustment valve (2) on the inert gas steel cylinder.