CN103060094A - Preparation method of menthol/SiO2 as tobacco flavor sustained-release material - Google Patents
Preparation method of menthol/SiO2 as tobacco flavor sustained-release material Download PDFInfo
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- CN103060094A CN103060094A CN2013100124512A CN201310012451A CN103060094A CN 103060094 A CN103060094 A CN 103060094A CN 2013100124512 A CN2013100124512 A CN 2013100124512A CN 201310012451 A CN201310012451 A CN 201310012451A CN 103060094 A CN103060094 A CN 103060094A
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- menthol
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Abstract
The invention discloses a preparation method of menthol/SiO2 as a tobacco flavor sustained-release material. The preparation method comprises the following steps of: condensing purified CO2 gas to be liquid state, controlling the CO2 temperature to 30-45 DEG C so as to reach a super-critical state through a heat exchanger after the CO2 gas is pressurized to 8-15MPa, and then entering a dissolving kettle (10); dissolving preplaced menthol in the dissolving kettle into supercritical CO2, and entering a loading kettle; adsorbing menthol through particular SiO2 loading material with high pore volume in the loading kettle, then returning the supercritical CO2 into a filter after being separated in the separating kettle, and finishing a complete cycle; and recycling the supercritical CO2 in a complete loop for 8-15 h by dissolving menthol and contacting with the loading material continuously to obtain menthol/SiO2 as the tobacco flavor sustained-release material with higher tobacco flavor capacity. The tobacco flavor sustained-release material prepared by the method greatly improves the defects that the flavor is liable to be lost, and affected with damp and mildewed in process of producing, storing and using cigarettes.
Description
Technical field
The present invention relates to the spice slow-releasing additives production process that a kind of cigarette moistureproof and mildewproof becomes, be specifically related to tobacco spice slow-release material menthol/SiO
2The preparation method.
Background technology
Cigarette is to be widely used the consumer's goods in a kind of daily life, because the cooling effect of menthol, it is a kind of cigarette cold additive commonly used, in cigarette, add in right amount, can relax the pungency of flue gas, remove assorted gas, but because of its extremely strong volatility, so that the maintenance that traditional addition manner that is sprayed directly on the pipe tobacco can't be effectively lasting is mint flavored.
Summary of the invention
The object of the invention provides spice slow-releasing material menthol/SiO that a kind of continuous and effective keeps fragrance in the tobacco, moistureproof and mildewproof to become
2The preparation method, solve spices in the cigarette store and use procedure in the quick loss, the problem of making moist and going mouldy easily that cause because of volatilization, prolong quality guaranteed period of cigarette.
For realizing above purpose, tobacco spice slow-release material menthol/SiO of the present invention
2The preparation method by adopting overcritical load coupling device, menthol is adsorbed on the high pore volume SiO of particulate state
2In, prepare a kind of menthol/SiO
2The spice slow-releasing material, operating process is as follows:
(1), high pore volume silica dioxide granule degree screening
Dried high pore volume silica product is sieved with sub-sieve, and the product of collecting between the 20-60 order is for subsequent use;
(2), get the raw materials ready
High pore volume earth silicon material and powdery menthol after the screening are put into respectively load still and dissolution kettle, and the mass ratio of high pore volume earth silicon material and powdery menthol is 1:(1.5～2.5);
(3), supercritical CO
2Preparation
Open CO
2Cylinder valve, CO
2Gas is removed impurity through filter, enters storage tank after refrigerator is condensed into liquid state again, then is pressurized to 8～15 MPa through pressure liquid pump, by the effect of heat exchanger, makes CO behind surge tank
2Temperature is controlled at 30～45 ℃ and enters in the dissolution kettle after reaching supercritical state;
(4), the supercritical CO of menthol
2Dissolving
Supercritical CO
2After entering dissolution kettle, contact with the menthol that is placed in advance in the dissolution kettle, progressively menthol is dissolved;
(5), the load of menthol
Menthol after the dissolving and supercritical CO
2Enter together in the load still, with the high pore volume SiO of particulate state in the load still
2The support materials contact, support materials is adsorbed menthol, after the absorption, supercritical CO
2Separate last CO through separating still with a small amount of menthol
2Gas comes back to strainer through non-return valve, and a small amount of menthol is collected recycling; Supercritical CO
2In whole loop, the dissolving by menthol with constantly contact with support materials, after 8～15 hours circulation, can obtain the menthol/SiO of higher spices charge capacity
2The spice slow-releasing material product.
The present invention has following characteristics:
1, utilizes high pore volume SiO
2High absorbability and the characteristic of desorption under high temperature, preparation tobacco spice slow-release material.
2, adopt supercritical fluid technology, utilize supercritical CO
2Dissolving and carry menthol flavor secretly fully and support materials (be high pore volume SiO
2) contact, can prepare the slow-release material of high spices charge capacity.
3, utilize high pore volume SiO
2Water-absorbent, be used for tobacco and can play anti-effect of going mouldy, thereby prolong the quality guaranteed period of cigarette.
Preferred by to indexs such as the high pore volume silicon-dioxide of carrier specific surface area, pore volume, granular sizes of the present invention, determine the high pore volume silicon-dioxide of optimum carrier leading indicator, simultaneously by adopting overcritical load coupling device, optimize the processing parameters such as overcritical dissolving and load temperature, pressure, prepare menthol/SiO
2The spice slow-releasing material.Compare with traditional technology, this spice slow-releasing material non-toxic, tasteless mixes with pipe tobacco in cigarette making processes, plays the fragrance slow releasing function, greatly improve the shortcoming that fragrance easily runs off, makes moist easily and go mouldy in production of cigarettes, storage, the use procedure, prolonged the quality guaranteed period of cigarette.
Description of drawings:
Accompanying drawing is overcritical load coupling device synoptic diagram.
Among the figure: 1-CO
2Steel cylinder, 2-strainer, 3-under meter, 4-refrigerator, 5-storage tank, 6-high-pressure pump, 7-non-return valve a, 8-surge tank, 9-heat exchanger, 10-dissolution kettle, 11-load still, 12-separating still, 13-non-return valve b, P-tensimeter, T-thermometer
Embodiment
Preparation method to tobacco spice slow-release material menthol/SiO2 of the present invention is described in further details below in conjunction with the drawings and specific embodiments.
Operation steps shown in the accompanying drawing is: open CO
2Steel cylinder 1, CO
2 Gas process strainer 2 is removed impurity, is condensed into liquid state through refrigerator 4 and enters storage tank 5, then is pressurized to certain pressure through pressure liquid pump 6, and buffering in snubber 8 is passed through the effect of heat exchanger 9, again so that CO
2Enter in the dissolution kettle 10 after reaching supercritical state; The menthol that is placed in advance in the dissolution kettle is dissolved in supercritical CO
2In, with supercritical CO
2Enter together in the load still 11; The high pore volume SiO of particulate state in the load still
2Support materials absorption menthol, then supercritical CO
2Pass through again separating still 12, come back to strainer finally by crossing non-return valve 13, so just finish a whole circulation.Supercritical CO
2In whole loop, the dissolving by spices with constantly contact with support materials, for a long time circulation dissolving and load can obtain the menthol/SiO of higher spices charge capacity
2The spice slow-releasing material product.
Below by two specific embodiment explanation concrete operation steps of the present invention.
Embodiment one
1. high pore volume silica dioxide granule degree screening
The high pore volume silica product of dried 1000 grams is sieved with sub-sieve, collect the product between the 20-60 order, for subsequent use.
2. get the raw materials ready
Take by weighing in the high pore volume earth silicon material 200 gram load stills of screening rear (20-60 order), take by weighing 400 gram menthols and put into dissolution kettle.
3. supercritical CO
2Preparation
Open CO
2Steel cylinder 1 valve, CO
2Gas is removed impurity through filter 2, is condensed into liquid state through refrigerator 4 and enters storage tank 5, then is pressurized to 13 MPa through pressure liquid pump 6, passes through the effect of heat exchanger 9 behind surge tank 8, so that CO again
2Temperature is controlled at 35 ℃ and enters in the dissolution kettle 10 after reaching supercritical state.
4. the supercritical CO of menthol
2Dissolving
Supercritical CO
2After entering dissolution kettle 10, contact with the menthol that is placed in advance in the dissolution kettle, progressively menthol is dissolved.
5. the load of menthol
Menthol after the dissolving and supercritical CO
2Enter together in the load still 11, with support materials in the load still (be the high pore volume SiO of particulate state
2) contact, support materials is adsorbed menthol, the supercritical CO after absorption
2Separate last gas CO through separating still 12 with a small amount of menthol
2Come back to strainer 2 through non-return valve 13, a small amount of menthol reclaims again.Allow supercritical CO
2In whole loop, menthol/SiO is taken out in circulation dissolving and load 15 hours after the pressure release
2The spice slow-releasing material product.
Embodiment two
Operation steps is with embodiment 1, step 3 mesohigh liquor pump is pressurized to circulation dissolving and load time change 10 hours in 10 MPa, the step 5, and other is constant.
Two embodiment effect comparison
1. the mensuration of charge capacity
Adopt the menthol charge capacity of gas chromatograph for determination products obtained therefrom, embodiment 1 and embodiment 2 results are respectively: 1.67g menthol/gSiO
2With 1.55 g menthol/gSiO
2
2. the mensuration of menthol retention rate
The product pressure that the present invention is obtained be 0.01Mpa nitrogen temperature be respectively 25 ℃, 40 ℃, 90 ℃ respectively purge 120min, measure its menthol retention rate, two embodiment are basic identical for test result, are respectively: 84.3%, 66.2%, 27.6%.
Can draw from above two embodiment: adopt supercritical fluid technology, with high pore volume SiO
2Menthol for more than adsorbable its quality of carrier in the lower situation of temperature, can effectively keep the menthol flavor composition, in the higher situation of temperature, has and discharges preferably effect.High pore volume SiO of while
2Itself has hygroscopic properties, therefore, product of the present invention is used in tobacco has fabulous spice slow-releasing effect, in tobacco storage and use procedure, continue to keep fragrance, has simultaneously the anti-effect of going mouldy of certain moisture absorption, prolong the quality guaranteed period of tobacco, thereby product of the present invention have wide market outlook.
Claims (1)
1. tobacco spice slow-release material menthol/SiO
2The preparation method, it is characterized in that: by adopting overcritical load coupling device, menthol is adsorbed on the high pore volume SiO of particulate state
2In, prepare a kind of menthol/SiO
2The spice slow-releasing material, operating process is as follows:
(1), high pore volume silica dioxide granule degree screening
Dried high pore volume silica product is sieved with sub-sieve, and the product of collecting between the 20-60 order is for subsequent use;
(2), get the raw materials ready
High pore volume earth silicon material and powdery menthol after the screening are put into respectively load still (11) and dissolution kettle (10), and the mass ratio of high pore volume earth silicon material and powdery menthol is 1:(1.5～2.5);
(3), supercritical CO
2Preparation
Open CO
2Steel cylinder (1) valve, CO
2Gas is removed impurity through filter (2), enters storage tank (5) after refrigerator (4) is condensed into liquid state again, then is pressurized to 8～15 MPa through pressure liquid pump (6), by the effect of heat exchanger (9), makes CO behind surge tank (8)
2Temperature is controlled at 30～45 ℃ and enters in the dissolution kettle (10) after reaching supercritical state;
(4), the supercritical CO of menthol
2Dissolving
Supercritical CO
2After entering dissolution kettle (10), contact with the menthol that is placed in advance in the dissolution kettle, progressively menthol is dissolved;
(5), the load of menthol
Menthol after the dissolving and supercritical CO
2Enter together in the load still (11), with the high pore volume SiO of particulate state in the load still
2The support materials contact, support materials is adsorbed menthol, after the absorption, supercritical CO
2Separate last CO through separating still (12) with a small amount of menthol
2Gas comes back to strainer (1) through non-return valve (13), and a small amount of menthol is collected recycling; Supercritical CO
2In whole loop, the dissolving by menthol with constantly contact with support materials, after 8～15 hours circulation, can obtain the menthol/SiO of higher spices charge capacity
2The spice slow-releasing material product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234270A (en) * | 2020-03-18 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Mint terylene master batch and preparation method thereof |
| CN111440499A (en) * | 2020-05-30 | 2020-07-24 | 青岛盈海涂料科技有限责任公司 | Water-based antifouling paint and preparation method thereof |
| CN112931934A (en) * | 2021-03-24 | 2021-06-11 | 湖北中烟工业有限责任公司 | Fragrance-holding and cooling additive and preparation method and application thereof |
| CN113951538A (en) * | 2021-11-18 | 2022-01-21 | 湖北中烟工业有限责任公司 | Heating non-combustion menthol sustained-release material and preparation method and application thereof |
| US11766067B2 (en) | 2017-05-15 | 2023-09-26 | Nicoventures Trading Limited | Ground tobacco composition |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11766067B2 (en) | 2017-05-15 | 2023-09-26 | Nicoventures Trading Limited | Ground tobacco composition |
| CN111234270A (en) * | 2020-03-18 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Mint terylene master batch and preparation method thereof |
| CN111440499A (en) * | 2020-05-30 | 2020-07-24 | 青岛盈海涂料科技有限责任公司 | Water-based antifouling paint and preparation method thereof |
| CN112931934A (en) * | 2021-03-24 | 2021-06-11 | 湖北中烟工业有限责任公司 | Fragrance-holding and cooling additive and preparation method and application thereof |
| CN113951538A (en) * | 2021-11-18 | 2022-01-21 | 湖北中烟工业有限责任公司 | Heating non-combustion menthol sustained-release material and preparation method and application thereof |
| CN113951538B (en) * | 2021-11-18 | 2023-02-07 | 湖北中烟工业有限责任公司 | Heating non-combustion menthol sustained-release material and preparation method and application thereof |
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Application publication date: 20130424 |