阅读说明：本技术 一种机内减压粉碎物料的超临界萃取方法及装置 (Supercritical extraction method and device for crushing material under reduced pressure in machine ) 是由 兰向东 陈海涛 朱林 付亭亭 于 2020-12-25 设计创作，主要内容包括：本发明公开了一种机内减压粉碎物料的超临界萃取方法及装置,属于萃取装置领域,1)先将物料加入萃取釜进行常规萃取；2)步骤1)萃取结束后,快速打开萃取釜快速减压阀门,在60-300秒的时间内,将萃取釜压力减至低于0.1Mpa,开启二氧化碳扰动管通入50-65℃的二氧化碳气体,保持萃取釜压力在0-0.2MPa之间3-5分钟；3)关闭快速减压阀及二氧化碳扰动管阀门,并调整操作参数至常规状态,萃取至终点。本发明可进行分段萃取的,第一段常规超临界萃取,降低物料含油率的同时,保证物料内部充满相同萃取压力的二氧化碳超临界流体,在萃取釜快速减压后,通入加热的二氧化碳气体扰动物料层,使得物料籽粒快速破碎,继续萃取。(The invention discloses a supercritical extraction method and a supercritical extraction device for crushing materials under reduced pressure in a machine, which belong to the field of extraction devices, and 1) adding the materials into an extraction kettle for conventional extraction; 2) after the extraction in the step 1) is finished, quickly opening a quick pressure reduction valve of an extraction kettle, reducing the pressure of the extraction kettle to be lower than 0.1MPa within 60-300 seconds, opening a carbon dioxide disturbing pipe to introduce carbon dioxide gas at 50-65 ℃, and keeping the pressure of the extraction kettle between 0-0.2MPa for 3-5 minutes; 3) and closing the quick pressure reducing valve and the carbon dioxide disturbing pipe valve, adjusting the operating parameters to a conventional state, and extracting to the end point. The method can perform sectional extraction, the first section of conventional supercritical extraction reduces the oil content of the material, ensures that the material is filled with the carbon dioxide supercritical fluid with the same extraction pressure, and introduces the heated carbon dioxide gas to disturb the material layer after the extraction kettle rapidly reduces the pressure, so that the material grains are rapidly crushed and the extraction is continued.)

1. A supercritical extraction method for crushing materials under reduced pressure in an internal machine is characterized by comprising the following steps:

1) adding the material into an extraction kettle for conventional extraction, wherein the filling amount of the material is 80-90%;

2) step 1), opening a quick pressure reduction valve of an extraction kettle after extraction is finished, reducing the pressure of the extraction kettle to be lower than 0.1MPa within 60-300 seconds, opening a carbon dioxide disturbance tube, introducing heated carbon dioxide gas, and keeping the pressure of the extraction kettle between 0-0.2MPa for 3-5 minutes;

3) and closing the quick pressure reducing valve and the carbon dioxide disturbing pipe valve, adjusting the operating parameters to a conventional state, and extracting to the end point.

2. The supercritical extraction process of reduced pressure crushed material in machine of claim 1 wherein the material is seed material.

3. The method of claim 2, wherein the material comprises sesame seeds, flax seeds and/or hemp seeds.

4. The supercritical extraction method of the internal decompression crushed material as claimed in any one of claims 1 to 3, characterized in that the heated carbon dioxide gas is carbon dioxide gas at 50-65 ℃.

5. The supercritical extraction device is characterized by comprising an extraction kettle, a rapid pressure reducing valve and a gas input pipe, wherein the rapid pressure reducing valve and the gas input pipe are connected with the extraction kettle, a carbon dioxide disturbance pipe communicated with the gas input pipe is arranged in the extraction kettle, and a plurality of gas outlets are formed in the carbon dioxide disturbance pipe and used for introducing heated carbon dioxide into the extraction kettle.

6. The apparatus of claim 5, further comprising a heating device connected to the gas inlet pipe for heating the carbon dioxide in the gas inlet pipe.

7. The supercritical extraction apparatus according to claim 6 is characterized in that the heating device is a temperature-controlled heating device for heating the carbon dioxide in the gas input pipe to a specified temperature.

8. The apparatus for supercritical fluid extraction of pulverized material under reduced pressure in machine according to any one of claims 5 to 7, wherein a filter plate is further provided in the reaction vessel for separating the port of the rapid pressure reducing valve from the material in the extraction vessel.

9. The apparatus of any one of claims 5 to 7, wherein the diameter of the air holes is 1.5mm, and the pitch of the air holes is 5 mm.

10. The apparatus of any one of claims 5 to 7, wherein a control valve is provided on the gas inlet pipe.

Technical Field

The invention relates to the field of extraction devices, in particular to a supercritical extraction method and device for crushing materials under reduced pressure in an extraction machine.

Background

Sesame, hemp, flax and other small-grain high-oil-content materials, because the oil content is higher and have relatively compact seed coats, when directly utilizing conventional supercritical extraction method to extract, grease and active substances in the materials can not be effectively extracted, the yield is extremely low, so conventional operation adopts the mode of crushing the materials in advance and then entering supercritical equipment to extract to carry out, the heat generated by friction in the mechanical crushing process of the materials can decompose and reduce the content of the active substances, simultaneously, the crushing causes the grease wrapped up in the interior of the seeds to be separated out, the materials to be agglomerated and caked, so that the subsequent supercritical process can not be smoothly carried out, meanwhile, the inevitable contact in the crushing process can be caused with the outside, the probability of causing pollution such as bacteria is increased, and the comprehensive utilization of later-stage material meal is not facilitated.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a supercritical extraction device for crushing materials under reduced pressure in a machine, which is suitable for the sectional extraction of high-oil-content materials such as sesame, flax, hemp seeds and the like under reduced pressure in the machine, improves the extraction efficiency and is beneficial to the comprehensive utilization of material dregs in the later period.

In order to solve the technical problems, the technical scheme provided by the invention is as follows:

on one hand, the invention provides a supercritical extraction method for crushing materials under reduced pressure in a machine, which comprises the following steps:

1) adding the material into an extraction kettle for conventional extraction, wherein the filling amount of the material is 80-90%;

2) step 1), opening a quick pressure reduction valve of an extraction kettle after extraction is finished, reducing the pressure of the extraction kettle to be lower than 0.1MPa within 60-300 seconds, opening a carbon dioxide disturbance tube, introducing heated carbon dioxide gas, and keeping the pressure of the extraction kettle between 0-0.2MPa for 3-5 minutes;

3) and closing the quick pressure reducing valve and the carbon dioxide disturbing pipe valve, adjusting the operating parameters to a conventional state, and extracting to the end point.

Further, the material is a seed material, including but not limited to sesame seeds, flax seeds, and/or hemp seeds.

Further, the heated carbon dioxide gas is carbon dioxide gas at 50-65 ℃.

On the other hand, still provide a supercritical fluid extraction device of material is smashed in built-in decompression, including the extraction cauldron, and the rapid relief valve and the gas input tube be connected with the extraction cauldron, be equipped with the carbon dioxide disturbance pipe with gas input tube intercommunication in the extraction cauldron, be equipped with a plurality of ventholes on the carbon dioxide disturbance pipe for in letting in the extraction cauldron with the carbon dioxide that has heated.

Further, the device also comprises a heating device connected with the gas input pipe and used for heating the carbon dioxide in the gas input pipe.

Further, the heating device is a temperature control heating device and is used for heating the carbon dioxide in the gas input pipe to a specified temperature.

Furthermore, a filter plate is arranged in the reaction kettle and used for separating the port of the rapid pressure reducing valve from materials in the extraction kettle. The filter plate is an 80-mesh filter plate.

Furthermore, the aperture of the air holes is 1.5mm, and the pitch is 5 mm.

Furthermore, a control valve is arranged on the gas input pipe.

After adopting such design, the invention has at least the following advantages:

the method can perform sectional extraction, the first section of conventional supercritical extraction can reduce the oil content of the material and simultaneously ensure that the material is filled with the carbon dioxide supercritical fluid with the same extraction pressure, after the extraction kettle is quickly decompressed (the temperature of the material is reduced after the decompression is quickly carried out), the heated carbon dioxide gas is introduced to disturb the material layer, and the material grains are quickly crushed under the combined action of the internal pressure and the external disturbance of the material grains; and in the second stage, the quick pressure reduction port and the carbon dioxide disturbing pipeline are closed, and system parameters are adjusted to be in a conventional state to carry out second-stage extraction until the operation end point.

Drawings

The foregoing is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and the detailed description.

FIG. 1 is a schematic structural diagram of a supercritical extraction apparatus for pulverizing a material under reduced pressure in a machine according to the present invention;

fig. 2 is a schematic sectional view taken along line a-a of fig. 1.

Detailed Description

Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

The invention provides an embodiment of a supercritical extraction device for reducing pressure and crushing materials in an extraction machine, which comprises an extraction kettle 1, a rapid pressure reducing valve 2 and a gas input pipe 4, wherein the rapid pressure reducing valve 2 and the gas input pipe 4 are connected with the extraction kettle 1, a carbon dioxide disturbing pipe 3 communicated with the gas input pipe 4 is arranged in the extraction kettle 1, and a plurality of gas outlet holes are formed in the carbon dioxide disturbing pipe 3 and are used for introducing heated carbon dioxide into the extraction kettle.

When the extraction kettle is used, the uncrushed material is added into the extraction kettle, the filling rate is 80-90%, the extraction is carried out by a conventional extraction method, then the pressure in the extraction kettle is quickly reduced by a quick pressure reducing valve (the temperature of the material is reduced after the pressure is quickly reduced), heated carbon dioxide gas is introduced to disturb a material layer, and the material grains are quickly crushed under the combined action of the internal pressure and the external disturbance of the material grains; and in the second stage, the quick pressure reduction port and the carbon dioxide disturbing pipeline are closed, and system parameters are adjusted to be in a conventional state to carry out second-stage extraction until the operation end point.

For heating convenience, a heating device 5 connected with the gas input pipe 4 is further included for heating the carbon dioxide in the gas input pipe 4. The heating device 5 may be a temperature-controlled heating device, and the safety is ensured by controlling the heating temperature of the carbon dioxide.

In order to prevent the rapid pressurizing valve from being blocked, a filter plate is also arranged in the reaction kettle 1 and used for separating the port of the rapid pressure reducing valve 2 from materials in the extraction kettle, and the filter plate is an 80-mesh filter plate.

Furthermore, the pore diameter of the pores is 1.5mm, the pitch of the pores is 5mm, and the pores are uniformly distributed.

Further, a control valve is arranged on the gas input pipe 4.

The conventional operation method of the invention is as follows:

1. adding the uncrushed material into an extraction kettle according to a conventional supercritical extraction mode, wherein the filling rate is 80-90%;

2. extracting for 30-45 minutes according to the conventional supercritical extraction pressure, temperature and carbon dioxide flow;

3. opening a rapid decompression valve of the extraction kettle, and reducing the pressure of the extraction kettle to be lower than 0.1Mpa within 60-300 seconds;

4. opening a carbon dioxide disturbing pipe to introduce carbon dioxide gas at 50-65 ℃, and keeping the pressure of the extraction kettle between 0-0.2MPa for 3-5 minutes.

5. And closing the quick pressure reducing valve and the carbon dioxide disturbing pipe valve.

6. Adjusting the operation parameters to a normal state, and extracting to an end point.

The specific embodiment is as follows:

example 1 supercritical extraction of Cannabis sativa seeds by means of an extraction apparatus according to the invention

Charging fructus Cannabis seed into extraction kettle with filling rate of 85%, adjusting temperature of the extraction kettle to 37 deg.C, pressure of 30MPa, and separation pressure of the separation kettle of 6.5 MPa. Separating temperature is 32 ℃, carbon dioxide flow pump is 23HZ, extracting time is 45 minutes, a quick decompression electric valve is opened, pressure of an extraction kettle is reduced to 0.1MPa, air inlet temperature of a carbon dioxide disturbance pipe is set to be 60 ℃, pressure of the extraction kettle is kept to be not more than 0.2MPa, ventilation is carried out for 5 minutes, the disturbance pipe and the quick decompression valve are closed, system parameters are adjusted to be in a conventional state, extraction is continued for 100 minutes, and oil content of the extracted hemp seed meal is measured to be 0.23%.

Comparative example 1 conventional supercritical extraction of hemp seed

Charging fructus Cannabis seed into extraction kettle with filling rate of 85%, adjusting temperature of the extraction kettle to 37 deg.C, pressure of 30MPa, and separation pressure of the separation kettle of 6.5 MPa. The separation temperature is 32 ℃, the carbon dioxide flow pump is 23HZ, the extraction time is 150 minutes, and the oil content of the extracted hemp seed meal is measured to be 18.7 percent.

EXAMPLE 2 supercritical extraction of flaxseed by means of the extraction apparatus of the invention

The flaxseed is loaded into an extraction kettle, the filling rate is 80%, the temperature of the extraction kettle is adjusted to 40 ℃, the pressure is 27MPa, and the separation pressure of the separation kettle is 7 MPa. Separating temperature is 35 ℃, carbon dioxide flow pump is 23HZ, extracting time is 45 minutes, a quick pressure reduction electric valve is opened, pressure of an extraction kettle is reduced to 0.1MPa, air inlet temperature of a carbon dioxide disturbance pipe is set to be 50 ℃, pressure of the extraction kettle is kept to be not more than 0.2MPa, ventilation is carried out for 3 minutes, the disturbance pipe and the quick pressure reduction valve are closed, system parameters are adjusted to be in a conventional state, extraction is continued for 100 minutes, and oil content of the extracted flaxseed meal is measured to be 0.31%.

Comparative example 2-conventional supercritical extraction of flaxseed

The flaxseed is loaded into an extraction kettle, the filling rate is 80%, the temperature of the extraction kettle is adjusted to 40 ℃, the pressure is 27MPa, and the separation pressure of the separation kettle is 7 MPa. The separation temperature is 35 ℃, the carbon dioxide flow pump is 23HZ, the extraction time is 150 minutes, and the oil content of the extracted linseed meal is measured to be 20.2 percent.

From the above examples 1 and 2 and comparative examples 1 and 2, it is clear that the efficiency of the staged extraction of the present invention is higher.

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 present invention in any way, and it will be apparent to those skilled in the art that the above description of the present invention can be applied to various modifications, equivalent variations or modifications without departing from the spirit and scope of the present invention.