CN112858541A - Thermal decomposition tank and method for decomposing and collecting slow-release perfume ingredients by using same - Google Patents
Thermal decomposition tank and method for decomposing and collecting slow-release perfume ingredients by using same Download PDFInfo
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- CN112858541A CN112858541A CN202110231015.9A CN202110231015A CN112858541A CN 112858541 A CN112858541 A CN 112858541A CN 202110231015 A CN202110231015 A CN 202110231015A CN 112858541 A CN112858541 A CN 112858541A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a thermal decomposition tank, which comprises the following components: an outer casing (1); a housing cover (2); an inner housing (3); an inner shell cover (4); an intake pipe (5); an air outlet pipe (6). The invention also discloses a method for decomposing and collecting the slow-release perfume ingredients by using the thermal decomposition tank. The thermal decomposition tank is convenient to assemble and disassemble, and has high convenience and popularization.
Description
Technical Field
The invention belongs to the field of analysis devices, and particularly relates to a thermal decomposition tank and a method for decomposing and collecting slow-release aroma heat release components by using the same.
Background
The slow release perfume is a substance which has stable chemical and physical properties and does not release fragrance at normal temperature, when the temperature is raised to a certain temperature, the fragrance is slowly released, and the fragrance retention time is prolonged compared with that of the common fragrance substance. In order to characterize the thermal sustained-release effect, thermal cracking (PY) and gas chromatography/mass spectrometry (GC/MS) are combined, a sample is decomposed by thermal cracking, the obtained product is analyzed and tested by GC/MS, and the aroma release mechanism and the release mobility of sustained-release aroma are researched by comparing the change of components before and after cracking.
Thermal decomposition is a key link for researching heat release components, and volatile components are fully released through heat energy. As a pretreatment technology of a next test, the release mode is generally as follows, firstly, a macromolecular compound has stable property at normal temperature, when the macromolecular compound is heated to a certain critical point, the chemical bond of the macromolecular compound is broken, and the generated volatile molecules perform random thermal motion and are released, such as glycoside perfume precursors and the like; secondly, the volatile molecules are embedded in the polymer cavity, or attracted by other substances with opposite charges, or kept stable by hydrogen bonds, and when the volatile molecules absorb enough heat, the volatile molecules are released by overcoming van der Waals force, electrostatic attraction or/and hydrogen bond acting force, such as cyclodextrin inclusion complex and the like; thirdly, the volatile molecules absorb heat to change phase, the gas phase diffusion rate is increased, and the volatile molecules are released under the carrying of inert gas.
At present, most of thermal decomposers are used with test equipment, such as a CSD5000 series thermal decomposer developed by American CSD company based on a platinum wire heating mode, an SGE high-temperature thermal decomposer developed by Australia in a gravity heating mode, a JHP-4 thermal decomposer developed by Japan in a Curie point heating method, a thermal decomposer developed by the domestic warrior and used with gas chromatography, and a thermal decomposition test method is established. The cracked products of the thermal decomposer can directly introduce the cracked components into the instrument on line for testing, and the thermal decomposer has the advantages of accurate cracking temperature and time and higher test repeatability. However, the cracker is expensive and has a limited range of applications.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention provides a pyrolysis tank which is simple in parts, easy to assemble and disassemble, good in sealing performance, high in durability, simple to operate when used for decomposing and collecting slow-release aroma heat release components, strong in convenience and easy to popularize.
The technical scheme of the invention is as follows:
the invention discloses a thermal decomposition tank in a first aspect, which comprises the following components:
the outer shell 1 is in a cylindrical shape with a sealed bottom and an opened upper part;
a shell cover 2 which is matched with the upper opening of the shell body 1;
an inner housing 3 having a cylindrical shape with a sealed bottom and an open top, and disposed inside the outer housing 1;
an inner shell cover 4 which is matched with the upper opening of the inner shell 3;
an air inlet pipe 5 which penetrates through the outer shell cover 2 and the inner shell cover 4 and extends into the bottom of the inner shell 3, and is provided with an air inlet valve 51;
and the air outlet pipe 6 penetrates through the outer shell cover 2 and the inner shell cover 4 and is provided with an air outlet valve 61.
Preferably, the pyrolysis tank further comprises an inner top cap 7, the inner top cap 7 being arranged between the outer shell cover 2 and the inner shell cover 4; the inner top cover 7 is connected with the outer shell cover 2 through threads.
Preferably, the outer housing 1 and the outer housing cover 2 are connected by a screw thread.
Preferably, the inner shell 3 and the inner shell cover 4 are made of alumina or graphite material; the shell body 1, the shell cover 2, the air inlet pipe 5, the air outlet pipe 6 and the inner top cover 7 are made of stainless steel materials.
Preferably, the air inlet pipe 5 extends into the inner shell 3 from the bottom 1/5-1/4; the outlet pipe 6 extends into the depth of the mouths 1/5-1/4 of the inner shell 3.
The second aspect of the invention discloses a method for decomposing and collecting slow-release perfume ingredients by using the thermal decomposition tank, which comprises the following steps:
firstly, assembling a thermal decomposition tank, and testing the sealing condition of the thermal decomposition tank at a certain temperature;
secondly, placing a certain mass of slow-release spice into the inner shell 3, then placing the inner shell 3 into the outer shell 1, covering the inner shell cover 4, placing the inner top cover 7, and screwing the outer shell cover 2 and the outer shell 1;
thirdly, opening an air inlet valve 51 and an air outlet valve 61, and introducing inert gas into the pyrolysis tank through an air inlet pipe 5 to replace air in the pyrolysis tank;
closing the air inlet valve 51 and the air outlet valve 61, placing the thermal decomposition tank in a high-temperature furnace, heating to the thermal release temperature of the perfume components, and keeping the temperature for 5-10 min;
fifthly, opening an air inlet valve 51 and an air outlet valve 61, introducing inert gas with the volume 5-10 times of that of the thermal decomposition tank into the thermal decomposition tank, blowing out the thermal decomposition gas from an air outlet pipe 6, absorbing the thermal decomposition gas by using absorption liquid, and then testing.
Preferably, the temperature for testing the sealing condition of the thermal decomposition tank is 500-600 ℃.
Preferably, the inert gas used in step (ii) or (iv) is nitrogen.
Preferably, the slow-release perfume in the step (II) is geraniol glycoside; the heat release temperature of the perfume components is 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃ and 600 ℃; the absorption liquid used in the fifth step is a mixture of ethyl acetate and dichloromethane.
Preferably, the slow-release spice in the step (II) is eugenol/beta-cyclodextrin inclusion compound; the heat release temperature of the perfume components is 100 ℃, 200 ℃, 300 ℃, 400 ℃ and 500 ℃; the absorption liquid used in the fifth step is a mixture of ethyl acetate and dichloromethane.
The invention has the beneficial effects that:
1. the thermal decomposition tank comprises an outer shell and an inner shell, wherein the outer shell cover and the outer shell can be screwed mutually through threads to realize one-time sealing, and the inner shell can be taken out freely by unscrewing. The inner cover can be pressed by screwing or unscrewing the inner cover, thereby avoiding the leakage of the slow-release spice and realizing double sealing. When the heat of the perfume components is released, the thermal decomposition tank does not need to be used together with an instrument, so that the test interference is effectively reduced, and the operation is simple. Has strong convenience and popularization.
2. The outer shell, the outer shell cover, the inner top cover, the air inlet pipe and the air outlet pipe are made of stainless steel, and the inner shell cover are made of alumina or graphite materials, so that the thermal decomposition tank is not easy to damage; and the assembly and disassembly are convenient, the sealing performance is strong, and the testing cost is reduced.
3. The effect of using the thermal decomposition tank of the present invention is substantially the same as that of using the thermal decomposition instrument of the prior art.
Drawings
Fig. 1 is a schematic view of the structure of a pyrolysis tank of the present invention.
FIG. 2 is an exploded view of a thermal decomposition tank according to the present invention
FIG. 3 is a thermogravimetric analysis diagram of the thermal decomposition tank of the present invention for decomposition of geraniol glycoside to collect slow release fragrance components.
FIG. 4 is a total ion flow diagram of gas chromatography mass spectrometry of thermal release of geraniol glycoside at different temperatures.
FIG. 5 is a thermogravimetric analysis diagram of the thermal decomposition tank of the present invention for decomposing and collecting the eugenol/beta-cyclodextrin inclusion compound to collect the slow release perfume components.
FIG. 6 is a total ion flow diagram of gas chromatography mass spectrometry of eugenol/beta-cyclodextrin inclusion compound with different temperature heat release.
The reference signs are: 1. an outer housing; 2. and a housing cover; 3. an inner housing; 4. an inner shell cover; 5. an air inlet pipe; 51. an intake valve; 6. an air outlet pipe; 61. an air outlet valve; 7. an inner top cover;
Detailed Description
The technical solution of the present invention is described below with reference to specific examples. The described embodiments are presented to better illustrate the invention and should not be construed as limiting the claims of the invention. The specific embodiment is as follows:
as shown in fig. 1 and 2, the pyrolysis tank of the present invention comprises the following components: the outer shell 1 is in a cylindrical shape with a sealed bottom and an opened upper part; a shell cover 2 which is matched with the upper opening of the shell body 1; an inner housing 3 having a cylindrical shape with a sealed bottom and an open top, and disposed inside the outer housing 1; an inner shell cover 4 which is matched with the upper opening of the inner shell 3; an air inlet pipe 5 which penetrates through the outer shell cover 2 and the inner shell cover 4 and extends into the bottom of the inner shell 3, and is provided with an air inlet valve 51; and the air outlet pipe 6 penetrates through the outer shell cover 2 and the inner shell cover 4 and is provided with an air outlet valve 61. The pyrolysis tank further comprises an inner top cover 7, the inner top cover 7 being arranged between the outer shell cover 2 and the inner shell cover 4; the inner top cover 7 is connected with the outer shell cover 2 through threads. The outer shell 1 is connected with the outer shell cover 2 through threads. The inner shell 3 and the inner shell cover 4 are made of alumina or graphite materials; the shell body 1, the shell cover 2, the air inlet pipe 5, the air outlet pipe 6 and the inner top cover 7 are made of stainless steel materials. The air inlet pipe 5 extends into the inner shell 3 from the bottom 1/5-1/4; the air outlet pipe 6 extends into the cylinder depth of the mouths 1/5-1/4 of the inner shell 3; so as to be beneficial to the replacement of the gas in the thermal decomposition tank and the complete absorption of the thermal decomposition gas.
The method for collecting and decomposing slow-release perfume ingredients using the thermal decomposition tank of the present invention comprises the steps of:
firstly, assembling a thermal decomposition tank, and testing the sealing condition of the thermal decomposition tank at a certain temperature; the temperature for testing the sealing condition of the thermal decomposition tank is 500-600 ℃;
secondly, placing a certain mass of slow-release spice into the inner shell 3, then placing the inner shell 3 into the outer shell 1, covering the inner shell cover 4, placing the inner top cover 7, and screwing the outer shell cover 2 and the outer shell 1; the inert gas used is nitrogen;
thirdly, opening an air inlet valve 51 and an air outlet valve 61, and introducing inert gas into the pyrolysis tank through an air inlet pipe 5 to replace air in the pyrolysis tank;
closing the air inlet valve 51 and the air outlet valve 61, placing the thermal decomposition tank in a high-temperature furnace, heating to the thermal release temperature of the perfume components, and keeping the temperature for 5-10 min;
opening an air inlet valve 51 and an air outlet valve 61, introducing inert gas with the volume 5-10 times of that of the thermal decomposition tank into the thermal decomposition tank, blowing out the thermal decomposition gas from an air outlet pipe 6, and performing a test after absorbing the thermal decomposition gas by using an absorption liquid; the inert gas used was nitrogen.
Example 1: use of the thermal decomposition tank of the present invention for decomposition of geraniol glycosides
The steps of decomposing geraniol glycoside and collecting slow-release perfume components by using the thermal decomposition tank of the invention are as follows:
wrapping 20mg of geraniol glycoside in tin foil paper, reserving air-permeable holes on the tin foil paper, placing the tin foil paper in an inner shell 3, screwing an inner shell cover 4, and screwing an outer shell cover 2 and an outer shell 1; introducing nitrogen at 500 ℃ to test the sealing performance of the thermal decomposition tank, and performing the following steps under the condition of no air leakage;
placing the thermal decomposition tank in a high-temperature furnace, opening an air inlet valve 51 and an air outlet valve 61, introducing nitrogen at normal temperature for 5min, and closing the air inlet valve 51 and the air outlet valve 61 after air in the thermal decomposition tank is replaced; heating to 100 deg.C, 200 deg.C, 300 deg.C, 400 deg.C, 500 deg.C and 600 deg.C respectively, and keeping at each temperature for 5 min; after cooling, the outlet pipe 6 was inserted into the mixed solution (absorption solution) of ethyl acetate and methylene chloride, the inlet valve 51 and the outlet valve 61 were opened, nitrogen gas of 5 times the volume of the pyrolysis tank was introduced into the decomposition tank, and the pyrolysis gas was completely blown out and absorbed by the absorption solution for future use.
Injecting the final absorption liquid into a gas chromatography-mass spectrometer under the following instrument conditions: the chromatographic column is DB-5MS (30m multiplied by 0.25 mu m), high-purity helium is used as carrier gas, the flow rate is 1ml/min, the injection port temperature is 280 ℃, the temperature rise program is 50 ℃ for 3min, the temperature rise rate is 3 ℃/min at 50 → 280 ℃, the temperature rise rate is 10min at 280 ℃, an EI ion source is used for full scanning, the scanning range is 45-500amu, a total ion flow diagram is collected, and the ion source temperature and the four-level bar temperature are 230 ℃ and 150 ℃ respectively. The total ion flow pattern is shown in figure 3.
The test analysis shows that the released geraniol component is 95.8% of the theoretical amount of geraniol in the geraniol glycoside. The thermogravimetric analysis diagram of geraniol glycoside is shown in fig. 2; the composition and content of geraniol glycosides released at different temperatures are shown in table 1 below.
TABLE 1 composition and content of geraniol glycosides released at different temperatures
Example 2: the thermal decomposition tank can also be used for decomposing eugenol/beta-cyclodextrin inclusion compound
The thermal decomposition tank can also be used for decomposing eugenol/beta-cyclodextrin inclusion compound and collecting slow-release perfume ingredients, and the steps are as follows:
wrapping 100mg of eugenol/beta-cyclodextrin inclusion compound in tin foil paper, leaving air-permeable holes on the tin foil paper, placing the tin foil paper in an inner shell 3, screwing an inner shell cover 4, and screwing an outer shell cover 2 and an outer shell 1; introducing nitrogen at 550 ℃ to test the sealing performance of the pyrolysis tank, and performing the following steps under the condition of no air leakage;
placing the thermal decomposition tank in a high-temperature furnace, opening an air inlet valve 51 and an air outlet valve 61, introducing nitrogen at normal temperature for 5min, and closing the air inlet valve 51 and the air outlet valve 61 after air in the thermal decomposition tank is replaced; heating to 100 deg.C, 300 deg.C, 400 deg.C and 500 deg.C respectively, and maintaining at each temperature for 5 min; after cooling, the outlet pipe 6 was inserted into the mixed solution (absorption solution) of ethyl acetate and methylene chloride, the inlet valve 51 and the outlet valve 61 were opened, nitrogen gas of 5 times the volume of the pyrolysis tank was introduced into the decomposition tank, and the pyrolysis gas was completely blown out and absorbed by the absorption solution for future use.
Injecting the final absorption liquid into a gas chromatography-mass spectrometer under the following instrument conditions: the chromatographic column is DB-5MS (30m multiplied by 0.25 mu m), high-purity helium is used as carrier gas, the flow rate is 1.2ml/min, the injection port temperature is 280 ℃, the temperature rising program is 70 ℃ for 4min, the temperature rising speed is 7 ℃/min for 70 → 290 ℃, the temperature rising speed is 10min for 300 ℃, EI ion sources are fully scanned, the scanning range is 45-500amu, a total ion flow diagram is collected, and the ion source temperature and the four-level bar temperature are 230 ℃ and 150 ℃ respectively. The total ion flow pattern is shown in figure 6.
The test analysis shows that the released eugenol is 93.1 percent of the theoretical amount of the eugenol in the eugenol/beta-cyclodextrin inclusion compound. A thermogravimetric analysis chart of the eugenol which is the eugenol/beta-cyclodextrin inclusion compound is shown in figure 5; the components and contents of the eugenol/beta-cyclodextrin inclusion compound released at different temperatures are shown in table 2 below.
TABLE 2 eugenol/beta-cyclodextrin inclusion complex released ingredients and contents at different temperatures
As can be seen from the examples, the thermal decomposition tank of the present invention is used to substantially achieve the same effect as the thermal decomposition instrument of the related art. But the pyrolysis tank is convenient to assemble and disassemble, strong in sealing performance, low in cost and more convenient to use.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A pyrolysis tank, characterized in that it comprises the following components:
the outer shell (1) is in a cylinder shape with a sealed bottom and an opened upper part;
the shell cover (2) is matched with an upper opening of the shell body (1);
an inner housing (3) having a cylindrical shape with a sealed bottom and an open upper portion, and disposed inside the outer housing (1);
an inner shell cover (4) which is matched with an upper opening of the inner shell (3);
the air inlet pipe (5) penetrates through the outer shell cover (2) and the inner shell cover (4) and extends into the bottom of the inner shell (3), and an air inlet valve (51) is arranged on the air inlet pipe;
and the air outlet pipe (6) penetrates through the outer shell cover (2) and the inner shell cover (4) and is provided with an air outlet valve (61).
2. The pyrolysis tank of claim 1, further comprising an inner top cover (7), the inner top cover (7) being arranged between the outer shell cover (2) and the inner shell cover (4); the inner top cover (7) is connected with the outer shell cover (2) through threads.
3. The pyrolysis tank according to claim 1, characterized in that the outer shell (1) and the outer shell cover (2) are connected by a screw thread.
4. The pyrolysis tank according to claim 2, characterized in that the inner shell (3) and the inner shell cover (4) are made of alumina or graphite material; the shell body (1), the shell cover (2), the air inlet pipe (5), the air outlet pipe (6) and the inner top cover (7) are made of stainless steel materials.
5. The pyrolysis tank of claim 1, wherein the intake pipe (5) is extended into a depth of a cylinder from a bottom 1/5-1/4 inside the inner case (3); the air outlet pipe (6) extends into the cylinder depth of the mouth part 1/5-1/4 of the inner shell (3).
6. A method for disaggregating collection of slow-release perfume ingredients by means of a thermal disintegration tank according to any of claims 1 to 5, comprising the steps of:
firstly, assembling a thermal decomposition tank, and testing the sealing condition of the thermal decomposition tank at a certain temperature;
secondly, placing a certain mass of slow-release spice in the inner shell (3), then placing the inner shell (3) in the outer shell (1), covering the inner shell cover (4), placing the inner top cover (7), and screwing the outer shell cover (2) and the outer shell (1);
thirdly, opening an air inlet valve (51) and an air outlet valve (61), and introducing inert gas into the pyrolysis tank through an air inlet pipe (5) to replace air in the pyrolysis tank;
closing the air inlet valve (51) and the air outlet valve (61), placing the thermal decomposition tank in a high-temperature furnace, heating to the thermal release temperature of the perfume components, and keeping the temperature for 5-10 min;
opening an air inlet valve (51) and an air outlet valve (61), introducing inert gas with the volume 5-10 times of that of the thermal decomposition tank into the thermal decomposition tank, blowing out the thermal decomposition gas from an air outlet pipe (6), absorbing by using absorption liquid, and then testing.
7. The method for decomposition collection of sustained-release perfume ingredients using a pyrolysis tank as claimed in claim 6, wherein the temperature of the test (i) for the sealing condition of the pyrolysis tank is 500-600 ℃.
8. The method for decomposition collecting slow-release perfume ingredients according to claim 6, wherein the inert gas used in step (ii) or (iv) is nitrogen.
9. The method for decomposing and collecting slow-release flavor components according to claim 6, wherein the slow-release flavor of step (ii) is geraniol glycoside; the heat release temperature of the perfume components is 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃ and 600 ℃; the absorption liquid used in the fifth step is a mixture of ethyl acetate and dichloromethane.
10. The method for decomposing and collecting slow-release perfume ingredients by using a pyrolysis tank as recited in claim 6, wherein the slow-release perfume of step (ii) is eugenol/β -cyclodextrin inclusion compound; the heat release temperature of the perfume components is 100 ℃, 200 ℃, 300 ℃, 400 ℃ and 500 ℃; the absorption liquid used in the fifth step is a mixture of ethyl acetate and dichloromethane.
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| US20140119995A1 (en) * | 2011-04-06 | 2014-05-01 | Vivacta Limited | Device for detecting an analyte |
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