CN103131536A - Preparation device and preparation method of essence and flavor powder - Google Patents

Preparation device and preparation method of essence and flavor powder Download PDF

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Publication number
CN103131536A
CN103131536A CN2011103881676A CN201110388167A CN103131536A CN 103131536 A CN103131536 A CN 103131536A CN 2011103881676 A CN2011103881676 A CN 2011103881676A CN 201110388167 A CN201110388167 A CN 201110388167A CN 103131536 A CN103131536 A CN 103131536A
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essence
flavoring agent
preparation
pressure
still
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CN103131536B (en
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蓝洪桥
李斌
陈小明
李军
王宏涛
苏玉忠
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Xiamen University
China Tobacco Fujian Industrial Co Ltd
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Xiamen University
China Tobacco Fujian Industrial Co Ltd
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Abstract

The invention discloses a preparation device and a preparation method of essence and flavor powder. According to the preparation device and the preparation method of the essence and flavor powder, by means of the high diffusivity and the high diffusivity of a supercutical fluid, and with the supercutical fluid as a carrier, the essence and flavor are impregnated or infused into solid powder, wherein the solid powder can be an inorganic polyporous powder material and an organic polyporous powder material, so that the aims that the essence and flavor are protected and the essence and flavor are enabled to have a controlled release function are achieved. Due to the fact that the polyporous material with a carrying capacity takes a long time in reaching saturation at a normal pressure (or in a gas atmosphere of the essence and flavor), the requirement of load of the essence and flavor is hard to meet. With the supercutical fluid as the carrier of the essence and flavor, the essence and flavor are sent into micropores of the polyporous material, and then the supercutical fluid is used to fix the essence and flavor in the polyporous material at a certain decompression speed, namely, the impregnation and infusion of the supercutical fluid, so that the optimal natural state and application effect of the essence and flavor can be achieved.

Description

Preparation facilities of a kind of essence and flavoring agent powder and preparation method thereof
Technical field
The present invention relates to a kind of preparation facilities and preparation method of essence and flavoring agent powder, especially relate to a kind of directly essence and flavoring agent the implantation with supercritical technology take porous material as the wall material and form preparation facilities and the preparation method with essence and flavoring agent powder of controlling release function.
Background technology
Supercritical fluid technology is a green chemical industry technology of just actively researching and developing both at home and abroad in recent ten years.It has been widely applied to many fields, as supercritical fluid extraction, supercritical fluid drying, supercritical fluid dyeing, supercutical fluid micronize, microencapsulant preparation by supercritical fluid technology, supercritical fluid chromatography, supercutical fluid water treatment etc.
In recent years, along with the enhancing of people's environmental consciousness, highlighting of traditional microcapsulary shortcoming comes into one's own with microencapsulant preparation by supercritical fluid technology, and be widely used in chemical industry, the research and practice in a plurality of fields such as medicine.The supercutical fluid microencapsulation technology is based on its Technique for Preparing Fine and grows up.With respect to traditional Micro-Encapsulation Technique, as spraying drying, emulsion method, surface aggregate etc., supercritical fluid technology has some obvious advantages, and as high in the product purity of its preparation, geometrical shape homogeneous, distribution of sizes narrow range, manufacturing process are simple.It is worthy of note, tradition prepares the method for microcapsule generally can use a large amount of organic solvents, has the residue problem of organic solvent; Many method service temperatures are too high, to thermo-sensitivity, structural instability with have bioactive material and have significant limitation.For this reason, the method for microencapsulant preparation by supercritical fluid technology obtains people's common concern.
Summary of the invention
For the deficiencies in the prior art part, the invention provides preparation facilities of a kind of essence and flavoring agent powder and preparation method thereof, these apparatus and method reach the protection essence and flavoring agent, and make essence and flavoring agent have the function of the release controlled.
For achieving the above object, technical solution of the present invention is:
A kind of preparation facilities of essence and flavoring agent powder is characterized in that: this device comprises:
One supercutical fluid generation device: this device comprises a gas tank or flow container, one strainer A connects this gas tank or flow container, this strainer A is connected with the input terminus of a gas compressor or pressure liquid pump and the backflow output terminal of a pressure valve V1, described gas compressor or highly pressurised liquid delivery side of pump with is connected the backflow input terminus of pressure valve V1 and connects a preheater, the entrance of the outlet of this preheater and a stopping valve joins;
One extraction plant: this device comprises that one is equipped with liquid tank or the gas tank of essence and flavoring agent, one liquor pump or suction port of compressor connect this liquid tank or gas tank, the outlet of liquor pump or compressor is connected with a non-return valve entrance, non-return valve outlet is connected and is connected with the entrance of an extraction kettle with stopping valve outlet in the supercutical fluid generation device, and the entrance of the outlet pressure valve V2 of extraction kettle is connected;
One implanted device: this device comprises the implantation still of being furnished with the material basket, the outlet of the entrance of this implantation still and the pressure valve V2 in extraction plant is joined, this bottom of implanting still connects a blow-off valve, and the top connects a filter B entrance, and the filter B outlet connects pressure valve V3 entrance;
One retrieving arrangement: this device comprises that one connects the recovery still of pressure valve V3 outlet, and this reclaims still bottom and connects a baiting valve, reclaims the still top and sequentially connects a under meter and an interchanger, and this interchanger connects gas tank or the flow container of supercutical fluid generation device.
A kind of preparation method of essence and flavoring agent powder is characterized in that: method comprises the following steps:
Step 1: with liquid essence spices or gas essence and flavoring agent pack into liquid tank or gas grooves;
Step 2: start the supercutical fluid generation device, form supercutical fluid or gas, enter continuously the extraction kettle of extraction plant with certain flow, extraction kettle reaches the temperature and pressure of setting, start liquid pump or compressor are squeezed into extraction kettle with certain flow with essence and flavoring agent; Control the temperature and pressure of the implantation still in implanted device; Control the temperature and pressure that reclaims still in retrieving arrangement, and make supercutical fluid or gas get back to gas tank or flow container after heat exchange;
Step 3: after operation for some time under the condition of upper step 1 and step 2, control the blowdown rate of implanting still, be reduced to normal pressure, take out the material basket of implanting in still, take out powder product.
The usefulness of technique scheme is:
Present technique utilizes supercutical fluid to have high diffusion, penetrating quality; with supercutical fluid as carrier; essence and flavoring agent is implanted (impregnation/infusion) to solid powder (can be inorganic porous powder body material and Porous-Organic powder body material); reach the protection essence and flavoring agent, and make essence and flavoring agent have the function of the release controlled.Because the porous material with carrying capacity need to reach capacity for a long time at (or in atmosphere of essence and flavoring agent) under normal pressure, be difficult to reach the requirement of essence and flavoring agent load.The carrier of the present invention take supercutical fluid as essence and flavoring agent is sent in the micropore of porous material, then supercutical fluid is fixed on (concept of supercutical fluid implantation that Here it is) in porous material with certain decompression rate with essence and flavoring agent, reaches good actual effect.
Description of drawings
Fig. 1 is the preparation facilities process flow diagram of essence and flavoring agent powder of the present invention;
Fig. 2 is the release profiles schematic diagram (N of phenylethyl alcohol from phenylethyl alcohol/silicon-dioxide powdery in the embodiment of the present invention one 2Purge 30 ℃ of temperature, purge pressure 0.102MPa);
Fig. 3 is the release profiles schematic diagram (air purge temperature: 30 ℃, purging pressure be 0.102MPa) of menthol from menthol/silicon-dioxide, menthol/activated carbon, menthol/cyclodextrin powder in the embodiment of the present invention two.
Embodiment
The present invention now is described in conjunction with the accompanying drawings and embodiments.
As shown in Figure 1, the preparation facilities of essence and flavoring agent powder of the present invention comprises a supercutical fluid generation device, an extraction plant, an implanted device and a retrieving arrangement.
The supercutical fluid generation device is for generation of the supercutical fluid that needs temperature and pressure.This part is provided with gas tank, tensimeter P0, strainer A, gas compressor or pressure liquid pump, pressure valve V1 and preheater.When replacing gas compressor with pressure liquid pump, gas tank is flow container (needing supporting water cooler this moment).Pressure valve V1 can use back pressure valve, also can be with other pressure control device (stopping as rotating speed or the fortune of utilizing pressure P 1 to control compressor or pump).Gas under certain pressure P0 (following take carbonic acid gas as example) out is connected with the backflow output terminal of gas compressor input terminus and pressure valve V1 through strainer A from gas tank, the backflow input termination preheater of gas compressor output terminal and pressure valve V1, preheater has the effect of surge tank concurrently.Preheater temperature (T1) can be controlled (jacketed type or electric heating sheets) temperature (carbonic acid gas: 31~100 ℃), the pressure of preheater (P1) be the above temperature of supercutical fluid emergent pressure (carbonic acid gas:>7.3MPa).Preheater outlet connects the stopping valve entrance, and the stopping valve outlet is certain temperature that the supercutical fluid generating portion provides and the supercutical fluid of pressure.
The supercutical fluid that extraction plant provides take the supercutical fluid generating portion is as carrier, obtains the supercutical fluid of essence and flavoring agent saturated the supercutical fluid of certain essence and flavoring agent (or dissolved).This part is provided with extraction kettle, liquid tank, liquor pump, non-return valve, pressure valve V2.The liquid tank outlet that essence and flavoring agent is housed connects the liquor pump entrance, the liquor pump outlet is connected with non-return valve, the non-return valve outlet is connected with the stopping valve outlet of supercutical fluid generation device, and be connected with the entrance of extraction kettle, the extraction kettle outlet is connected with pressure valve V2, and pressure valve V2 can be reducing valve or back pressure valve.Extraction kettle can be controlled (jacketed type or electric heating sheets) temperature (T2) at 31~100 ℃; Its pressure P 2 is equal to or less than P1.If essence and flavoring agent is gas, liquid tank should be changed to gas tank, and liquor pump should be compressor.If essence and flavoring agent is solid and be the solid (as natural phant) that contains essence and flavoring agent, liquid tank and liquor pump all do not need operation, and this moment, extraction kettle will be equipped with the material basket, and solid is packed in material basket and the extraction kettle of packing into.
The saturated supercutical fluid of essence and flavoring agent that implanted device is come with the extraction plant supercutical fluid of certain essence and flavoring agent (or dissolved) the inorganic powder bed of flowing through obtains the inorganic powder product of implanting essence and flavoring agent.This part is provided with implants still, strainer 2, blow-off valve, pressure valve V3.With certain specification (refer to certain size and distribution, certain specific area) the solid powder material basket of packing into, then will expect the basket implantation still of packing into.Implant the still entrance and connect the outlet of extraction plant pressure valve V2, implant the still bottom and connect blow-off valve, the top of implanting still is outlet, takes over the entrance of filter 2, and the outlet of strainer 2 connects the entrance of pressure valve V3.Pressure valve V3 can be reducing valve or back pressure valve.Implant still and can control (jacketed type or electric heating sheets) temperature (T3) at 31~100 ℃; Its pressure P 3 is equal to or less than P2.Blow-off valve can be manual needle valve or cut-off method, can be also the high pressure electric gate that can control emptying speed (bleeding off pressure speed).
Retrieving arrangement is the recovery part essence and flavoring agent, the device of the gas that the backflow supercutical fluid is corresponding.This device is provided with and reclaims still, baiting valve, under meter, interchanger.The outlet of pressure valve V3 takes back receives the still bottom inlet, reclaim still bottom connection one baiting valve, (but also dual-purpose is analyzed the content of exit gas essence and flavoring agent to be used for regular discharging essence and flavoring agent, whether definite implantation is complete), recovery still top is fluid outlet, outlet connects under meter, then connects interchanger, and this interchanger connects the gas tank of supercutical fluid generation device.Reclaim the still temperature according to the character of essence and flavoring agent, can heat or cooling, the gentle pressure tank of pressure is consistent.Heat exchange is carried out according to temperature out, if excess Temperature can be as cold as normal temperature for water.
Operation is front (take liquid essence spices, gas compressor conveyance fluid as example; Operate the liquid essence spices of packing in front liquid tank, implant the solid powder of packing in still), the resistance to air loss of inspection units, each road heat tracing situation and instrument show and control situation, material situation.Confirm no problem after, open supercutical fluid generating portion (this moment, stopping valve was closed), make the supercutical fluid that produces certain temperature and pressure in preheater.Supercutical fluid enters one by one subsequently extraction kettle, implants still and reclaims the still temperature and pressure condition of each still (and reach) with low discharge, and gas is got back to gas tank by under meter and interchanger at last.After each parameter stability, open liquor pump, with certain flow input essence and flavoring agent, and again stablize each operational condition.After stable the implantation for some time (whether jump according to the drain hole essence and flavoring agent and be foundation), V2 and V3 complete shut-down, blow-off valve emptying, controlling and bleeding off pressure speed is normal pressure to implanting still pressure, takes out the material basket and can obtain product.Expect the solid powder of packing in basket, and the implantation still of again packing into, and continue operation, produce the next batch product.
The preparation method of essence and flavoring agent powder of the present invention, its step is as follows:
Step 1: with liquid essence spices or gas essence and flavoring agent pack into liquid tank or gas grooves.
Essence and flavoring agent in above-mentioned steps one is if solid or contain the solid natural material of essence and flavoring agent (as contain) of essence and flavoring agent they are put into extraction kettle, and the essence and flavoring agent still adds entrainment agent according to practical situation.Entrainment agent is generally polar organic solvent, and such as water, ethanol, acetone etc., the mass percent of add-on is the 0.1-20% of the supercritical flow scale of construction.
Essence and flavoring agent in above-mentioned steps one is if gas directly passes into extraction kettle with essence and flavoring agent.
Step 2: start the supercutical fluid generation device, form supercutical fluid or gas, enter continuously extraction kettle with certain flow, extraction kettle reaches temperature (use temperature control system) and the pressure (use pressure valve) of setting, start the essence and flavoring agent pump, with certain flow, essence and flavoring agent is squeezed into extraction kettle; Control temperature (use temperature control system) and the pressure (use reducing valve) of implanting still; Control the temperature (use temperature control system) and the pressure (use reducing valve) that reclaim still, and get back to gas tank or flow container after making supercutical fluid (gas) heat exchange.
Supercutical fluid in step 2 is supercritical co, overcritical alkene, overcritical alkane or their mixture.
In step 2, control the flow of supercutical fluid according to the size of extraction kettle and implantation still.Such as, the extraction kettle of 5L and implantation still, flow is about 2NL/min; The extraction kettle of 50L and implantation still, flow is about 50Nm 3/ h.
In step 2, the flow of essence and flavoring agent determines at supercritical flow temperature, pressure and flow according to it, makes essence and flavoring agent reach in supercutical fluid or near saturated.
In step 2, according to the critical constants of the supercutical fluid that uses, the pressure of extraction kettle is more than emergent pressure, and temperature is more than critical temperature.
In step 2, the pressure of implanting still is normal pressure~40MPa; Temperature is-10 ℃~100 ℃.
In step 2, the pressure that reclaims still is normal pressure~7MPa; Temperature is normal temperature~100 ℃.
In step 2, heat exchange is carried out according to the temperature that reclaims still, and after heat exchange, fluid temperature (F.T.) is near normal temperature.
In step 2, pressure valve and reducing valve can replace with other pressure control device, such as the mode of the rotating speed of using the pressure-controlling pump.
Step 3: after operation for some time under the condition of upper step 1 and step 2, control the blowdown rate of implanting still, be reduced to normal pressure, take out the material basket of implanting in still, take out powder product.Blowdown rate in this step 3 is less than 1MPa/min.In this step 3 powder product refer to contain the product of implanting essence and flavoring agent; Here the particle diameter of powder arrives between millimeter for nanometer as required.
Embodiment 1: the preparation of phenylethyl alcohol/silicon-dioxide powdery
Phenylethyl alcohol, chemical pure, purity 〉=98%, Chemical Reagent Co., Ltd., Sinopharm Group; Carbonic acid gas, purity 〉=98%, the empty special manufactory in Tongan City; Silicon-dioxide, self-control, 20 microns of median sizes, specific surface area 306m 2/ g.
With the flow process of Fig. 1, this moment, extraction kettle did not fill any material, and phenylethyl alcohol pumps into essence and flavoring agent.Implant the silicon-dioxide powdery of packing in still.Operational condition is: extracting pressure 15MPa, 60 ℃ of extraction temperature, implantable pressure 15MPa, implant temperature 60 C, reclaim still temperature normal temperature, reclaim approximately 5MPa of still pressure, carbon dioxide flow is 2NL/min approximately, phenylethyl alcohol pumps into flow<1mL/min (determining according to the solubleness under 70 ℃ and 15MPa), and working time is 10h approximately.The average content of the phenylethyl alcohol in final product phenylethyl alcohol/silicon-dioxide powdery is: 0.2g/gSiO 2Controlled release curve such as Fig. 2 of this product, this figure show in product>80% phenylethyl alcohol can not discharge under 30 ℃, illustrates that phenylethyl alcohol has obtained good protection.
Embodiment 2: the preparation of menthol/silicon-dioxide powdery
Menthol, chemical pure, the Solution on Chemical Reagents in Shanghai purchasing and supply station provides (bulk); Carbonic acid gas, purity 〉=98%, the empty special manufactory in Tongan City; Silicon-dioxide, self-control, approximately 20 microns of median sizes, specific surface area 336m 2/ g.
With the flow process of Fig. 1, this moment the extraction kettle menthol of packing into, liquor pump and liquid tank are not used.Implant the silicon-dioxide powdery of packing in still.Operational condition is: extracting pressure 10MPa, and 40 ℃ of extraction temperature, implantable pressure 10MPa implants 40 ℃ of temperature, reclaims still temperature normal temperature, reclaims approximately 5MPa of still pressure, and carbon dioxide flow is 2NL/min approximately, and working time is 10h approximately.The average content of the menthol in final product menthol/silicon-dioxide powdery is: 1.4g/gSiO 2Controlled release curve such as Fig. 3 of this product, this figure show that the menthol in product has good control release action under 30 ℃, and approximately have at last 30% can not discharge, and this part menthol has obtained good protection.
Embodiment 3: the preparation of menthol/activated carbon powder
Menthol, chemical pure, the Solution on Chemical Reagents in Shanghai purchasing and supply station provides (bulk); Carbonic acid gas, purity 〉=98%, the empty special manufactory in Tongan City; Activated carbon, China Tobacco Fuzhou Industrial Corporation, 200 microns of median sizes, specific surface area 910m2/g.
With the flow process of Fig. 1, this moment the extraction kettle menthol of packing into, liquor pump and liquid tank are not used.Implant the activated carbon of packing in still.Operational condition is: extracting pressure 10MPa, and 40 ℃ of extraction temperature, implantable pressure 10MPa implants 40 ℃ of temperature, reclaims still temperature normal temperature, reclaims approximately 5MPa of still pressure, and carbon dioxide flow is 2NL/min approximately, and working time is 10h approximately.The average content of the menthol in final product menthol/activated carbon powder is: 0.4g/gSiO 2Controlled release curve such as Fig. 3 of this product, this figure show in product>and 60% menthol can not discharge under 30 ℃, and menthol has obtained good protection in the activated carbon powder.
Embodiment 4: the preparation of menthol/cyclodextrin powder
Menthol, chemical pure, the Solution on Chemical Reagents in Shanghai purchasing and supply station provides (bulk); Carbonic acid gas, purity 〉=98%, the empty special manufactory in Tongan City; Cyclodextrin, 200 microns of median sizes, specific surface area 9.9m 2/ g.
With the flow process of Fig. 1, this moment the extraction kettle menthol of packing into, liquor pump and liquid tank are not used.Implant the cyclodextrin of packing in still.Operational condition is: extracting pressure 10MPa, and 40 ℃ of extraction temperature, implantable pressure 10MPa implants 40 ℃ of temperature, reclaims still temperature normal temperature, reclaims approximately 5MPa of still pressure, and carbon dioxide flow is 2NL/min approximately, and working time is 10h approximately.The average content of the menthol in final product menthol/cyclodextrin is: 0.2g/gSiO 2Controlled release curve such as Fig. 3 of this product, this figure show in product that approximately 10% menthol can not discharge under 30 ℃, illustrate that menthol discharges therein substantially, discharge to have certain controlled effect.
Embodiment 5: the preparation of tea perfume (or spice)/silicon-dioxide powdery
Carbonic acid gas, purity 〉=98%, the empty special manufactory in Tongan City; Tealeaves: Wuyi cliff tea, Wuyi Mountain.Silicon-dioxide, self-control, 20 microns of median sizes, specific surface area 306m2/g; Deionized water, self-control.
With the flow process of Fig. 1, this moment the extraction kettle tealeaves of packing into, the liquid tank deionized water of packing into.Implant the tealeaves of packing in still.Operational condition is: extracting pressure 30MPa, and 40 ℃ of extraction temperature, implantable pressure 30MPa implants 40 ℃ of temperature, reclaims still temperature normal temperature, reclaims approximately 6MPa of still pressure, and carbon dioxide flow is 2NL/min approximately, de-ionized water flow rate 1mL/min, working time is 10h approximately.The average content of the tea in final product tea perfume (or spice)/silicon-dioxide inorganic powder fragrant (mixture) is 0.2g/gSiO2 approximately.This product is inhaled in adding cigarette and is commented, and shows that cigarette is continuous soft and fine greasy, and living Feng returns sweet, and sense organ suction quality improves.
Above embodiment only for explanation technological thought of the present invention, can not limit protection scope of the present invention with this, every technological thought that proposes according to the present invention, and any change of doing on the technical scheme basis is within all falling into protection domain of the present invention.

Claims (18)

1. the preparation facilities of an essence and flavoring agent powder, it is characterized in that: this device comprises:
One supercutical fluid generation device: this device comprises a gas tank or flow container, one strainer A connects this gas tank or flow container, this strainer A is connected with the input terminus of a gas compressor or pressure liquid pump and the backflow output terminal of a pressure valve V1, described gas compressor or highly pressurised liquid delivery side of pump with is connected the backflow input terminus of pressure valve V1 and connects a preheater, the entrance of the outlet of this preheater and a stopping valve joins;
One extraction plant: this device comprises that one is equipped with liquid tank or the gas tank of essence and flavoring agent, one liquor pump or suction port of compressor connect this liquid tank or gas tank, the outlet of liquor pump or compressor is connected with a non-return valve entrance, non-return valve outlet is connected and is connected with the entrance of an extraction kettle with stopping valve outlet in the supercutical fluid generation device, and the entrance of the outlet pressure valve V2 of extraction kettle is connected;
One implanted device: this device comprises the implantation still of being furnished with the material basket, the outlet of the entrance of this implantation still and the pressure valve V2 in extraction plant is joined, this bottom of implanting still connects a blow-off valve, and the top connects a filter B entrance, and the filter B outlet connects pressure valve V3 entrance;
One retrieving arrangement: this device comprises that one connects the recovery still of pressure valve V3 outlet, and this reclaims still bottom and connects a baiting valve, reclaims the still top and sequentially connects a under meter and an interchanger, and this interchanger connects gas tank or the flow container of supercutical fluid generation device.
2. the preparation method of an essence and flavoring agent powder, it is characterized in that: method comprises the following steps:
Step 1: with liquid essence spices or gas essence and flavoring agent pack into liquid tank or gas grooves;
Step 2: start the supercutical fluid generation device, form supercutical fluid or gas, enter continuously the extraction kettle of extraction plant with certain flow, extraction kettle reaches the temperature and pressure of setting, start liquid pump or compressor are squeezed into extraction kettle with certain flow with essence and flavoring agent; Control the temperature and pressure of the implantation still in implanted device; Control the temperature and pressure that reclaims still in retrieving arrangement, and make supercutical fluid or gas get back to gas tank or flow container after heat exchange;
Step 3: after operation for some time under the condition of upper step 1 and step 2, control the blowdown rate of implanting still, be reduced to normal pressure, take out the material basket of implanting in still, take out powder product.
3. as the preparation method of a kind of essence and flavoring agent powder in claim 2, it is characterized in that: the essence and flavoring agent in step 1 is gas, essence and flavoring agent is directly passed into extraction kettle; Essence and flavoring agent in step 1 is solid or the solid that contains essence and flavoring agent, essence and flavoring agent is put into extraction kettle, and adds entrainment agent; Entrainment agent is polar organic solvent, and mass percent is the 0.1-20% of the supercritical flow scale of construction.
4. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: the supercutical fluid in step 2 is supercritical co, overcritical alkene, overcritical alkane or their mixture.
5. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, control the flow of supercutical fluid according to the size of extraction kettle and implantation still.
6. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, the flow of essence and flavoring agent determines at supercritical flow temperature, pressure and flow according to it, makes essence and flavoring agent reach in supercutical fluid or near saturated.
7. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, according to the critical constants of the supercutical fluid that uses, the pressure of extraction kettle is more than emergent pressure, and temperature is more than critical temperature.
8. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, the pressure of implanting still is normal pressure~40MPa; Temperature is-10 ℃~100 ℃.
9. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, the pressure that reclaims still is normal pressure~7MPa; Temperature is normal temperature~100 ℃.
10. as the preparation method of a kind of essence and flavoring agent powder in claim 2 or 3, it is characterized in that: in step 2, heat exchange is carried out according to the temperature that reclaims still, and after heat exchange, fluid temperature (F.T.) is near normal temperature.
11. the preparation method as a kind of essence and flavoring agent powder in claim 2 or 3 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
12. the preparation method as a kind of essence and flavoring agent powder in claim 4 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
13. the preparation method as a kind of essence and flavoring agent powder in claim 5 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
14. the preparation method as a kind of essence and flavoring agent powder in claim 6 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
15. the preparation method as a kind of essence and flavoring agent powder in claim 7 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
16. the preparation method as a kind of essence and flavoring agent powder in claim 8 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
17. the preparation method as a kind of essence and flavoring agent powder in claim 9 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
18. the preparation method as a kind of essence and flavoring agent powder in claim 10 is characterized in that: in step 3, blowdown rate is less than 1MPa/min.
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CN106905570A (en) * 2017-04-17 2017-06-30 中国热带农业科学院农产品加工研究所 Distribute latex product of fragrance and preparation method thereof
CN106995539A (en) * 2017-04-17 2017-08-01 中国热带农业科学院农产品加工研究所 Distribute latex product of fragrance and preparation method thereof
CN113340759A (en) * 2021-06-03 2021-09-03 福建兴隆香业有限公司 Laterite agilawood preparation device and method
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

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