CN117989816A - Bear gall powder production method and freeze-drying device - Google Patents

Abstract

The invention belongs to the technical field of bear gall powder production, and provides a bear gall powder production method and a freeze-drying device, wherein the method comprises the following steps: filtering fel Ursi to obtain filtered bile solution; pre-freezing the filtered bile solution at the temperature of minus 40 ℃ to minus 45 ℃ for 1.5 to 2.5 hours, and keeping the pre-frozen bile solution for 1.5 to 2.0 hours; heating to-10 to-15 ℃ and keeping for 1.5-2.5 h; then controlling the temperature rise in stages, controlling the temperature to be kept in stages, and after the temperature is raised to 37-40 ℃ and kept, obtaining a dry material; sieving the dried material to obtain fel Ursi powder. The method can effectively reduce energy consumption and shorten processing time, and the prepared bear gall powder has the advantages of less impurity, low moisture, high purity and stable quality; the device has more uniform heat conduction and more sensitive temperature regulation, and can better meet the regulation and control requirements of temperature rise, temperature reduction, maintenance and the like of the bear gall powder freeze-drying process.

Description

Bear gall powder production method and freeze-drying device

Technical Field

The invention belongs to the technical field of production of bear gall powder, and particularly relates to a production method of bear gall powder and a freeze-drying device.

Background

The bear gall powder is a processed product obtained by processing the bile of the bear, which is a traditional Chinese medicinal material in China, and has the effects of improving eyesight, clearing heat and detoxicating, calming liver, benefiting gall and the like. The production method of the bear gall powder mainly comprises three modes of drying, microwave drying and freeze-drying, wherein the drying and microwave drying are higher in temperature, so that the loss of active ingredients of the bear gall is caused to a certain extent, the appearance color and luster are poor, and the quality phase of a bear gall powder product are influenced; the freeze-drying is to sublimate and dry the water at low temperature, the method has little influence on the active ingredients of the bear bile, the active ingredients of the bear gall powder can be well preserved, and the obtained appearance product of the bear gall powder is better than that of the product of the bear gall powder obtained by drying and microwave drying. However, the existing freeze-drying process has the problems of longer processing time, higher energy consumption and the like, so that the production cost of the freeze-drying process is high.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a production method of bear gall powder and a freeze-drying device, and the method effectively shortens the freeze-drying processing time and reduces the energy consumption through control of pre-freezing treatment, maintenance, heating, maintenance, staged heating, maintenance and the like; the freeze-drying device has more uniform heat conduction and more sensitive temperature regulation, and can better meet the regulation and control requirements of temperature rise, temperature reduction, maintenance and the like of the bear gall powder freeze-drying process.

In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:

The production method of the bear gall powder comprises the following steps:

S1, filtering bear bile to obtain a filtered bile solution;

s2, pre-freezing the filtered bile solution at the temperature of minus 40 ℃ to minus 45 ℃ for 1.5 to 2.5 hours, and keeping the pre-frozen solution for 1.5 to 2.0 hours; heating to-10 to-15 ℃ and keeping for 1.5-2.5 h; then controlling the temperature rise in stages, controlling the temperature to be kept in stages, and after the temperature is raised to 37-40 ℃ and kept, obtaining a dry material;

And S3, sieving the dried material to obtain bear gall powder.

In one embodiment of the present application, in step S1, the filtering includes two times of filtering, the first time of filtering using a filter element having a pore size of 0.45 μm and the second time of filtering using a filter element having a pore size of 0.25 μm.

In one embodiment of the present application, in step S2, the filtered bile solution is sub-packaged into a material tray for pre-freezing treatment, and the depth of the filtered bile solution in the material tray is controlled to be 1.8-2.2 cm.

In one embodiment of the application, in the step S2, the vacuum degree is controlled to be 40-60 Pa when the temperature is raised to-10 ℃ to-15 ℃ and kept; controlling the vacuum degree to be 15-25 Pa when controlling the staged temperature rise and the staged temperature control and keeping;

and/or in the step S2, controlling the cooling speed to be 0.45-0.6 ℃/min when the pre-freezing treatment is carried out; in the process of heating to the temperature ranging from minus 10 ℃ to minus 15 ℃, the heating speed is controlled to be 0.45 ℃ to 0.6 ℃/min; and controlling the temperature rising speed to be 0.4-0.5 ℃/min during the staged temperature rising.

In one embodiment of the present application, in step S2, the stepwise temperature increase is controlled, and the stepwise temperature control is performed to increase the temperature to 37 ℃ to 40 ℃ and maintain the temperature, which specifically includes:

The first stage, controlling the temperature to be raised to-8 to-5 ℃ and the temperature raising and maintaining time to be 90-120 min;

In the second stage, heating to 2-5 ℃ and keeping the temperature for 90-120 min;

in the third stage, the temperature is controlled to be raised to 12-15 ℃ and the temperature is raised and the holding time is 120-150 min;

A fourth stage, controlling the temperature to be raised to 22-25 ℃ and the temperature raising and maintaining time to be 120-150 min;

in the fifth stage, the temperature is controlled to be raised to 27-30 ℃ and the temperature is raised and the holding time is 300-360 min

A sixth step of controlling the temperature to be raised to 32-35 ℃ and the temperature raising and maintaining time to be 300-360 min;

and seventh, controlling the temperature to be raised to 37-40 ℃ and the temperature raising and maintaining time to be 60-90 min.

In one embodiment of the present application, before step S1, the method further comprises the steps of:

s01, collecting fresh bear bile, quick-freezing at-18 ℃ to-22 ℃ for preservation and transportation, and taking the fresh bear bile as a raw material for freezing bear bile;

S02, thawing the bear bile frozen raw material in a water bath at the temperature of 10-15 ℃ to obtain the bear bile raw material.

In an embodiment of the present application, in step S1, the bear bile is a mixture of a first bear bile raw material and a second bear bile raw material, the first bear bile raw material is bear bile collected from 11 months to 3 months in the next year, the second bear bile raw material is bear bile collected from 4 months to 10 months, and a volume ratio of the first bear bile raw material to the second bear bile raw material is 1:1.8-2.3.

In one embodiment of the application, the moisture content of the bear gall powder is lower than 2%, and the content of tauroursodeoxycholic acid is 40.5% -43.5%.

Bear courage powder production freeze-drying device, including freeze-drying storehouse, a plurality of freeze-drying plywood of interval installation about in the freeze-drying storehouse, the freeze-drying plywood includes:

The upper panel is provided with a smooth heat conduction surface on one side and a groove on the other side, wherein a plurality of division bars are arranged in the groove at intervals in parallel, and divide the groove into continuous serpentine flow channels;

The lower panel is adaptively covered on the groove of the upper panel, and a notch corresponding to the parting bead is arranged on the lower panel;

wherein the upper panel and the parting bead are integrally formed; the lower panel is welded with the parting bead through the notch, and the edge of the lower panel is welded with the edge of the groove.

In one embodiment of the application, a large V-shaped groove is formed in the top of the parting bead along the length direction, the width of the notch is consistent with that of the large V-shaped groove, and the included angle alpha at the bottom of the large V-shaped groove and the included angle beta between the side wall of the large V-shaped groove and the side wall of the notch are 110-140 degrees;

A first groove is formed in the outer side of the edge of the groove of the upper panel, a second groove corresponding to the first groove is formed in the edge of the lower panel, and a large V-shaped welding slot is formed by the first groove and the second groove;

The notch is opened at one end of the edge of the lower panel, and the large V-shaped groove is communicated with the large V-shaped welding slot.

Compared with the prior art, the invention has the beneficial effects that:

1. According to the production method of the bear gall powder, pre-freezing treatment, pre-freezing and maintaining, heating (-10 ℃ to-15 ℃) and maintaining treatment are carried out in the freeze-drying process, wherein the pre-freezing treatment is used for freezing a solution, the solution is changed from a liquid state to a solid state, the solution is maintained after freezing, the freezing is further developed, the gaps between columnar ice crystals in an ice layer are increased, the direct sublimation of a solvent from the solid state to a gaseous state is facilitated, and the freeze-drying process is accelerated; then heating to a relatively high temperature (-10 ℃ to-15 ℃) for maintaining, thereby ensuring sufficient sublimation drying and reducing cold energy consumption; finally, the time and energy consumption for drying are shortened by means of staged temperature rise and temperature control and maintenance, so that the bear gall powder can be dried at a lower temperature. The obtained fel Ursi powder has low water content, good active ingredient retention, uniform crystal grain, bright color Jin Huangjing, rapid dissolution rate, and no insoluble substances. The production method is especially suitable for producing fel Ursi powder from fel Ursi with relatively lower concentration in summer and autumn, and fel Ursi powder with concentration between that of fel Ursi in summer and autumn and fel Ursi in winter.

2. According to the production method of the bear gall powder, the filter elements with different pore diameters are adopted for filtering twice, and the filter element with the pore diameter of 0.45 mu m is adopted for the first filtering, so that the filtering speed is high, and impurities such as large-particle tissues and fat can be effectively removed; the filter element with the aperture of 0.25 μm is selected for the second filtering, which is beneficial to effectively filtering out microorganisms such as bacteria; the filter elements with different apertures are adopted for twice filtration, so that the filtration treatment time can be effectively shortened, the loss of active ingredients is reduced, the filtration effects of impurities, microorganisms and the like are good, and the fishy smell of the obtained product is reduced.

3. Because the bile of the black bear has low and thick yield in winter (about 11 to 3 months of the next year), and has high and thin yield in summer and autumn (about 4 to 10 months); when the bear bile in different seasons is subjected to freeze-drying treatment independently, the quality difference of the obtained bear bile powder is large, the temperature of the freeze-drying process of the universal freeze-drying process is maintained in a lower range, and the problem of certain energy consumption waste exists when the freeze-drying treatment of the bear bile in summer and autumn is carried out; according to the invention, the winter bear bile and the summer bear bile are mixed in proportion to obtain the mixed bear bile raw material with proper concentration, and the freezing point/co-melting point of the mixed bear bile raw material is higher than that of the winter bear bile (thick), so that the temperature can be raised to a relatively high temperature (-10 ℃ to-15 ℃) for freeze-drying and maintaining, the energy consumption is reduced while the freeze-drying effect is achieved, and the quality stability of the obtained bear bile powder product is good.

4. According to the freeze-drying device, the grooves and the parting strips are formed in the upper panel of the freeze-drying laminate, the parting strips and the upper panel are integrally formed, and a welding structure is not adopted (the parting strips, the upper panel and the lower panel of the traditional freeze-drying laminate are of split structures and are respectively connected through welding, namely, the parting strips are welded with the upper panel and the lower panel, so that heat conduction between a heat conduction medium and a heat conduction surface is more uniform, temperature adjustment is more sensitive, and further, the temperature distribution of materials contacted with the heat conduction surface is more uniform; when the method is used for controlling the freeze-drying process of the bear gall powder production method, the control requirement of cooling/heating can be effectively met, and the freeze-drying process is controlled more accurately; in addition, the freeze-drying laminate of the application has the advantages that the notch corresponding to the parting bead is arranged on the lower panel, the parting bead is welded with the lower panel through the notch, and the edge is welded, so that the welding part of the freeze-drying laminate is reduced, the welding difficulty is reduced, the operation is simpler, the manufacturing cost is effectively reduced, the heat conduction surface of the upper panel is not deformed due to welding, the quality is easier to control,

5. Set up big V type groove, big V type welding slot (first groove, second groove), and make big V type groove and big V type welding slot intercommunication, can effectively guarantee the welding quality of welding seam, avoid not fusing the condition of thoroughly welding, further guarantee the quality of freeze-drying plywood.

Drawings

In order to more clearly illustrate the embodiments of the application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.

FIG. 1 is a flow chart of a production method of bear gall powder in the invention.

FIG. 2 is a comparative photograph of bear gall powder prepared in example 1 and comparative example 1.

FIG. 3 is a photograph showing the comparison of bear gall powder of example 1 with bear gall powder prepared by a commercially available drying process.

Fig. 4 is a schematic structural diagram of a freeze-drying bin and a freeze-drying layer plate in the freeze-drying device for producing bear gall powder.

Fig. 5 is a schematic perspective view of a lyophilization laminate according to the present invention.

FIG. 6 is a schematic view of the structure of the upper panel with a groove.

Fig. 7 is a schematic structural diagram of a mating surface of a lower panel and an upper panel in the present invention.

FIG. 8 is a schematic cross-sectional view of the portion B-B in FIG. 6.

FIG. 9 is a schematic cross-sectional view of the portion A-A in FIG. 5.

Fig. 10 is an enlarged schematic view of the C portion in fig. 9.

Fig. 11 is an enlarged view of the portion D in fig. 10.

Reference numerals:

1. A freeze-drying bin;

2. Lyophilizing the laminate;

3. an upper panel; 31. a heat transfer surface; 32. a groove; 33. a parting bead; 331. a large V-groove; 34. a first groove;

4. a lower panel; 41. a notch; 42. and a second groove.

Detailed Description

Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.

Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

The embodiment of the invention provides a production method of bear gall powder, which adopts a freeze-drying method to produce bear gall into bear gall powder. As shown in fig. 1, the production method of the bear gall powder comprises the following steps:

S1, filtering bear bile, and obtaining a filtered bile solution after filtering.

Preferably, the filtering is carried out by adopting a twice filtering mode, and a filter element with the pore diameter of 0.45 μm is selected for the first filtering so as to rapidly filter and remove large-particle impurities such as tissue fragments, fat and the like in the bear bile. The filter element with the aperture of 0.25 μm is selected for the second filtering to ensure that fine microorganism impurities in bile solution are filtered effectively, reduce loss of active ingredients and shorten the filtering treatment time.

S2, sub-packaging the filtered bile solution obtained in the step S1, then placing the sub-packaged filtered bile solution into a freeze-drying device for freeze-drying treatment, firstly, pre-freezing the solution for 1.5-2.5 hours at-40 to-45 ℃, keeping the temperature after the pre-freezing treatment time reaches, and keeping the pre-frozen solution for 1.5-2.0 hours; after the holding time is up, controlling the temperature to rise relatively at a constant speed until the temperature rises to-10 ℃ to-15 ℃, and maintaining the temperature for 1.5-2.5 h; and then controlling the temperature rise in a staged manner, and controlling the temperature to be kept in a staged manner, so that the temperature is finally raised to 37-40 ℃ and kept, and then the dried material is obtained.

Wherein, split charging the filtered bile solution into a material tray for pre-freezing treatment, preferably controlling the depth of the filtered bile solution in the material tray to be 1.8-2.2 cm.

The pre-freezing treatment and the pre-freezing after-holding are carried out under normal pressure without vacuumizing treatment; and when the temperature is controlled to be increased to-10 ℃ to-15 ℃ at a relatively constant speed and maintained, vacuumizing treatment is needed, and the vacuum degree is controlled to be 40-60 Pa. When the staged temperature rise and the staged temperature control and maintenance are controlled, the vacuum degree is controlled within 15-25 Pa, and the combined moisture can be well removed.

When the pre-freezing treatment is carried out, the temperature reduction speed is preferably controlled to be about 0.45-0.6 ℃/min; the temperature is increased from-40 ℃ to-45 ℃ to-10 ℃ to-15 ℃ and the temperature increasing speed is controlled to be 0.45 ℃ to 0.6 ℃/min; when the temperature is raised in stages, the temperature raising speed is controlled to be 0.4-0.5 ℃/min. The size of crystal grains formed in the freezing process can be controlled to a certain extent by controlling the cooling speed of the pre-freezing treatment, and the quick sublimation drying speed and the quick combined water removal speed can be obtained by combining the pre-freezing treatment and the maintaining treatment, so that the effect of shortening the freeze-drying time is achieved.

The method comprises the steps of controlling stepwise temperature rise, and controlling and maintaining stepwise temperature to finally rise the temperature to 37-40 ℃, and specifically comprises the following seven steps:

The first stage, controlling the temperature to be raised from-10 ℃ to-15 ℃ to-8 ℃ to-5 ℃, controlling the temperature raising speed, and controlling the total time length for keeping after the temperature is raised to-8 ℃ to-5 ℃ to be 90-120 min;

the second stage, controlling the temperature to be raised to 2-5 ℃ from-8 ℃ to-5 ℃, controlling the temperature raising speed, and controlling the temperature raising process and the total duration of holding after the temperature is raised to 2-5 ℃ to be 90-120 min;

In the third stage, the temperature is controlled to be increased from 2 ℃ to 5 ℃ to 12 ℃ to 15 ℃, the temperature increasing speed is controlled, and the total duration of the temperature increasing process and the maintenance after the temperature is increased to 12 ℃ to 15 ℃ is 120 to 150min;

A fourth stage, namely controlling the temperature to be raised from 12 ℃ to 15 ℃ to 22 ℃ to 25 ℃, controlling the temperature raising speed, and controlling the temperature raising process and the total duration of maintaining after the temperature is raised to 22 ℃ to 25 ℃ to be 120 min to 150min;

A fifth stage, namely controlling the temperature to be raised from 22-25 ℃ to 27-30 ℃, controlling the temperature raising speed, and controlling the temperature raising process and the total duration of holding after the temperature is raised to 27-30 ℃ to be 300-360 min;

a sixth step of controlling the temperature to be raised from 27 ℃ to 30 ℃ to 32 ℃ to 35 ℃, controlling the temperature raising speed, and controlling the temperature raising process and the total duration of holding after the temperature is raised to 32 ℃ to 35 ℃ to 300 min to 360min;

And in the seventh stage, the temperature is controlled to be increased from 32-35 ℃ to 37-40 ℃, the temperature increasing speed is controlled, and the total duration of the temperature increasing process and the maintaining process after the temperature is increased to 37-40 ℃ is controlled to be 60-90 min.

By controlling the staged temperature rise and carrying out the staged temperature control and maintenance, the combined moisture in the material can be effectively removed, the energy consumption is saved, and the influence on the effective components in the material is reduced.

In step S2, the pre-freezing treatment is performed to quickly freeze the solution, the solution is changed from a liquid state to a solid state, the temperature is maintained unchanged and continuously maintained after freezing, and the sublimation drying is performed, and simultaneously, the freezing is further developed, so that the gaps between columnar ice crystals in the ice layer are increased, and the direct sublimation of the solvent from the solid state to the gas state is facilitated, thereby accelerating the freeze-drying process. And then heating to-10 ℃ to-15 ℃, wherein the temperature range is close to but lower than the co-dissolution point/solidification point of the filtered bile solution, and maintaining at the temperature, and continuously performing sublimation drying, so that the sublimation drying effect can be effectively ensured, and the cold energy consumption is reduced. Finally, through the mode of staged temperature rising and temperature control and maintenance, the water adsorption with stronger combination is better removed, the drying temperature is reduced, and the time required by drying is shortened.

S3, the dried material obtained in the step S2 is a fluffy block material, and the dried material is screened by adopting a screen after sterilization treatment in a clean environment to obtain a bear gall powder product with uniform particles.

Preferably, a 60 mesh screen is employed for vibratory screening. The sieved fel Ursi powder can be sterilized by ozone or ultraviolet.

Steps S1 to S3 are all operated in a clean environment, and the used appliances are all sterilized, wherein the environment and the appliances can be sterilized by ultraviolet rays, ozone, alcohol, high-temperature damp heat and the like.

In one embodiment, the method further comprises a pretreatment step of bear bile before performing the operation of step S1, specifically comprising the steps of:

s01, collecting bear bile of a healthy black bear aged 4-6 years in a culturing farm in a drainage tube mode, packaging after collection, rapidly quick-freezing at-18 ℃ to-22 ℃, storing and transporting at-18 ℃ to-22 ℃, and taking the quick-frozen fresh bear bile as a bear bile freezing raw material for standby. The freezing time of the bear bile freezing raw material is preferably controlled within 24 months.

S02, before the operation of the step S1, the raw materials for freezing the bear bile are taken and placed in a water bath with the temperature of 10-15 ℃ for quick thawing, and the required raw materials for the bear bile are obtained after thawing.

The quick-freezing preservation and transportation of the fresh bear bile can effectively solve the problems that the collection amount of the bear bile in a farm is unstable and has larger fluctuation, and the transportation and the subsequent freeze-drying processing treatment can be carried out after the collection are carried out for many times, so that the transportation and the maintenance of active ingredients of the bear bile are convenient, the control of the production amount of each batch of the freeze-drying process is convenient, and the stability of the quality of each batch of products is further ensured. Before freeze-drying processing, a proper amount of bear bile frozen raw material is taken according to the batch production to defrost, and the raw material is quickly defrosted through a water bath at 10-15 ℃, so that the problems that the temperature is unstable and the effective components are damaged in natural defrosting can be effectively avoided, and the problem that insoluble matters are formed by precipitation of the effective components of the bear bile in the natural defrosting process can be effectively avoided, and the quality of the obtained bear bile can be better ensured.

Preferably, in step S1, the adopted bear bile is a mixture of a first bear bile raw material and a second bear bile raw material, wherein the first bear bile raw material is bear bile collected from 11 months to 3 months in the next year, namely winter bear bile; the second bear bile is collected from 4 months to 10 months each year, and is obtained in summer and autumn. When the bear bile is mixed, the volume ratio of the first bear bile raw material to the second bear bile raw material is preferably controlled to be 1:1.8-2.3.

The bile of black bear has low and thick yield in winter (about 11 to 3 months of the next year), high and thin yield in summer and autumn (about 4 to 10 months); when the bear bile in different seasons is subjected to freeze-drying treatment independently, the obtained bear bile powder has large mass difference, and the problem of certain energy waste exists when the universal freeze-drying technology is adopted to carry out the freeze-drying treatment of the bear bile in summer and autumn. The method comprises the steps of mixing winter and summer and autumn bear bile according to a proportion, wherein the concentration of the obtained mixed bear bile raw material is proper, and the freezing point/co-melting point of the mixed bear bile raw material is higher than that of the winter bear bile (thick), so that the temperature in the freeze-drying process can be regulated to be relatively high (-10 ℃ to-15 ℃) for freeze-drying and maintaining, the freeze-drying effect is achieved, the energy consumption is reduced, and the quality stability of the obtained bear bile powder product is good.

The water content of the bear gall powder prepared by the method is lower than 2%, and the content of tauroursodeoxycholic acid is 40.5% -43.5%.

Based on the same purpose, the invention also provides a freeze-drying device for producing bear gall powder.

As shown in fig. 4-11, the freeze-drying device for producing bear gall powder comprises a freeze-drying bin 1, wherein a plurality of freeze-drying laminates 2 are arranged in the freeze-drying bin 1 at intervals up and down, and the intervals between the adjacent freeze-drying laminates 2 are equal.

The freeze-dried laminate 2 has an internal heat transfer medium flowing through it for heat transfer between the heat transfer medium and the freeze-dried material. The freeze-dried laminate 2 comprises an upper panel 3 and a lower panel 4, and is formed by welding the upper panel 3 and the lower panel 4.

Specifically, as shown in fig. 5, 6, 8 and 9, one surface of the upper panel 3 is a smooth heat conduction surface 31 for contacting with a material tray or material; the other side of the upper panel 3 is provided with an inward concave groove 32, the groove wall of the groove 32 is at the edge of the upper panel 3, a plurality of division bars 33 are arranged in the groove 32 at intervals in parallel, the division bars 33 are connected with two opposite sides of the groove 32 in a staggered manner, the division bars 33 divide the groove 32 into continuous serpentine flow channels, one end of each serpentine flow channel is provided with an inlet, the other end of each serpentine flow channel is provided with an outlet, and heat supply and conduction media circulate.

As shown in fig. 7, 9, 10 and 11, the lower panel 4 is sized to fit over the upper panel 3 to fit over the recess 32 side of the upper panel 3, covering the opening of the recess 32. The lower panel 4 is provided with a plurality of notches 41 corresponding to the parting strips 33 in the upper panel 3, one end of each notch 41 is open, the other end is a blind end, the notches 41 are parallel to each other, and the openings are arranged towards two opposite sides of the lower panel 4 in a staggered manner.

Wherein, the upper panel 3 and the parting bead 33 are integrated into one piece structure, and the heat conduction is even. The lower panel 4 is welded to the spacer bar 33 by extending the electrode/rod through the slot 41, preferably with the weld surface being level with the side of the lower panel 4 remote from the recess 32. The edges of the lower panel 4 are welded with the edges of the grooves 32, i.e. the edges of the lower panel 4 are welded with the edges of the other side of the upper panel 3.

In a preferred embodiment, as shown in fig. 6, 7, 9, 10 and 11, the top of the parting bead 33 is provided with a large V-shaped groove 331 along the length direction, and the bottom of the large V-shaped groove 331 is an included angle α; the width of the notch 41 is consistent with the width of the large V-shaped groove 331, when the upper panel 3 and the lower panel 4 are correspondingly covered, the notch 41 is correspondingly matched with the large V-shaped groove 331, and the side wall of the notch 41 is butted with the opening of the side wall of the large V-shaped groove 331 to form an included angle beta. The angle alpha of the bottom of the large V-shaped groove 331 and the angle beta of the side wall of the large V-shaped groove 331 and the side wall of the notch 41 are 110-140 degrees, and the angles of the angle alpha and the angle beta are preferably 120 degrees.

Correspondingly, a circle of first grooves 34 are arranged on the outer side of the edges of the grooves 32 of the upper panel 3. The edge of the lower panel 4 is provided with a second bevel 42 corresponding to the first bevel 34, and when the upper panel 3 and the lower panel 4 are covered, the first bevel 34 and the second bevel 42 are butted to form a large V-shaped welding slot. Preferably, the included angle of the large V-shaped welding slot is 110-140 degrees.

One end of the large V-shaped groove 331 on the parting bead 33 is connected to the opening of the first groove 34 in an extending way, and the other end is a blind end; the notch 41 of the lower panel 41 is open at one side edge; the large V-shaped groove 331, the notch 41 and the large V-shaped welding slot are communicated when being welded, so that leakage points can be effectively avoided.

According to the freeze-drying device, the groove 32 and the parting bead 33 are designed on the upper panel 3 of the freeze-drying laminate 2, the parting bead 33 and the upper panel 3 are integrally formed, and a welding structure is not adopted (the parting bead, the upper panel and the lower panel of the traditional freeze-drying laminate are of split structures and are respectively connected through welding, namely, the parting bead is welded with the upper panel and the lower panel, so that heat conduction between a heat conduction medium and the heat conduction surface 31 is more uniform, temperature adjustment is more sensitive, and further, the temperature distribution of materials contacted with the heat conduction surface 31 is more uniform; when the method is used for controlling the freeze-drying process of the bear gall powder production method, the control requirement of cooling/heating can be effectively met, and the freeze-drying process is controlled more accurately; this freeze-drying plywood 2, its lower panel 4 set up the notch 41 that corresponds with parting bead 33, welds parting bead 33 and lower panel 3 through notch 41 to and the edge welds for the welding position of this freeze-drying plywood 2 reduces, and the welding degree of difficulty reduces, and the operation is simpler, can effectively reduce manufacturing cost, and the heat-conduction face 31 of upper panel 3 does not have the condition of welding deformation, and the quality is more easily controlled. The large V-shaped groove 331, the large V-shaped welding slot (the first groove 34 and the second groove 42) and the large V-shaped groove 331 and the large V-shaped welding slot are communicated, so that the welding quality of a welding line can be effectively ensured, the condition of unfused penetration welding is avoided, and the quality of the freeze-drying laminate 2 is further ensured.

Experimental example 1

A production method of bear gall powder comprises the following steps:

S01, collecting bear bile of healthy black bear with the age of 4-6 years in a culturing farm, packaging, rapidly freezing and preserving at about-20 ℃, transporting at-18 ℃ to-22 ℃ and sending to a freeze-drying workshop as bear bile freezing raw materials. Wherein, bear bile collected in the period of 11 months to 3 months of the next year is used as a first bear bile raw material, bear bile collected in the period of 4 months to 10 months is used as a second bear bile raw material, and the materials are respectively stored and marked.

S02, quickly thawing the frozen raw materials of the bear bile in a water bath at about 15 ℃ to obtain the required raw materials of the bear bile after thawing;

S1, mixing a first bear bile raw material and a second bear bile raw material according to a volume ratio of 1:2, sequentially filtering the mixed bear bile through a filter element with a pore diameter of 0.45 mu m for the first time, and filtering the mixed bear bile through a filter element with a pore diameter of 0.25 mu m for the second time to obtain a filtered bile solution;

S2, sub-packaging the filtered bile solution in a material tray, controlling the depth of the solution to be about 2.0cm, and controlling the area to be not less than 0.2 square meter; placing the mixture into a freeze-drying bin of a freeze-drying device, controlling the temperature to be about-42 ℃, controlling the cooling speed to be about 0.5 ℃/min by controlling the flow rate of a heat conduction medium, and performing pre-freezing treatment for 2.2-2.5 h; then maintaining the temperature at about-42 ℃ for 2.0h; then controlling the vacuum degree at 40-60 Pa, controlling the temperature to rise at a speed of about 0.5 ℃/min, raising the temperature to about-15 ℃, and maintaining the temperature for about 2.0h; then controlling the vacuum degree within 15-25 Pa, controlling the temperature to rise in stages at the speed of about 0.4 ℃/min, and controlling the temperature to be maintained in stages, wherein the specific stage is as follows:

The first stage, controlling the temperature to rise from-15 ℃ to-5 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 100min;

the second stage, controlling the temperature to rise from-5 ℃ to 5 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 100min;

The third stage, controlling the temperature to rise from 5 ℃ to 15 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 145min;

a fourth stage, controlling the temperature to rise from 15 ℃ to 25 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 145min;

A fifth stage, controlling the temperature to rise from 25 ℃ to 0 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 330 minutes;

a sixth step of controlling the temperature rise from 30 ℃ to 35 ℃, controlling the temperature rise speed, and controlling the total duration of the temperature rise process and the temperature control maintenance to be 330 minutes;

and seventh, controlling the temperature to rise from 35 ℃ to 40 ℃, and controlling the total duration of the temperature rising process and the temperature control maintenance to be 80 minutes.

And (3) obtaining fluffy dry materials after the freeze-drying process of the step S2.

S3, performing ozone sterilization treatment for 60min in a screening operation room, removing the freeze-dried dry materials, and performing vibration screening by using a sterilized 60-mesh screen to obtain a bear gall powder product with Jin Huangjing bright color and uniform particles/grains, as shown in fig. 2 and 3; the moisture content of the bear gall powder is 1.28 percent and the content of the tauroursodeoxycholic acid is 42.2 percent through detection.

As can be seen from fig. 3, the bear gall powder prepared by the experimental example is more Jin Huangjing bright in color, higher in crystal grain cleanliness and better in quality and appearance; the bear gall powder produced by a drying process on the market contains black impurities and is brown in color.

Experimental example 2

The experimental example differs from experimental example 1 in that the quick freezing and preservation in step S01 and the thawing treatment in S02 are not performed, and the fresh bear bile directly used in step S1 in summer and autumn is subjected to the filtration treatment. The rest of the operations of this experimental example are identical to those of experimental example 1, and will not be described again.

The bear gall powder product obtained by the experimental example has the advantages of Jin Huangjing bright color and uniform particles/grains; the moisture content of the bear gall powder is 1.17 percent and the content of the tauroursodeoxycholic acid is 40.9 percent through detection.

Experimental example 3

The experimental example is different from the experimental example 1 in that in the step S1, bear bile is obtained by mixing a first bear bile raw material and a second bear bile raw material according to a volume ratio of 1:1.8. The rest of the operations of this experimental example are identical to those of experimental example 1, and will not be described again.

The bear gall powder product obtained by the experimental example has the advantages of Jin Huangjing bright color and uniform particles/grains; the moisture content of the bear gall powder is 1.83 percent and the content of the tauroursodeoxycholic acid is 43.4 percent through detection.

Experimental example 4

The experimental example is different from the experimental example 1 in that in the step S1, bear bile is obtained by mixing a first bear bile raw material and a second bear bile raw material according to a volume ratio of 1:2.3. The rest of the operations of this experimental example are identical to those of experimental example 1, and will not be described again.

The bear gall powder product obtained by the experimental example has the advantages of Jin Huangjing bright color and uniform particles/grains; the moisture content of the bear gall powder is 1.18 percent and the content of the tauroursodeoxycholic acid is 41.2 percent through detection.

Comparative example 1

The comparative example is different from experimental example 1 in that the bear bile taken in step S1 is the first bear bile raw material; both the two filters were filtered using a filter element with a pore size of 0.45 μm. The rest of the operations are the same as those of experimental example 1, and will not be described again.

The obtained bear gall powder product is shown in figure 2, has orange color and uniform particles/grains; the moisture content of the bear gall powder is detected to be 4.69 percent, and the content of the tauroursodeoxycholic acid is detected to be 39.6 percent.

As can be seen from FIG. 2, the bear gall powder prepared in Experimental example 1 has a more Jin Huangjing bright color and a higher crystal grain cleanliness.

Comparative example 2

The comparative example is different from experimental example 1 in that the first filtration and the second filtration in step S1 are both filtration using a filter element having a pore size of 0.25 μm. The rest of the operations are the same as those of experimental example 1, and will not be described again.

The obtained bear gall powder product has orange color and uniform particles/grains; the moisture content of the bear gall powder is detected to be 1.43%, and the content of the tauroursodeoxycholic acid is detected to be 36.3%.

Comparative example 3

The comparative example is different from experimental example 1 in that in step S2, the filtered bile solution is packaged in a material tray and then is put into a freeze-drying bin of a freeze-drying device, the temperature is controlled to be about-42 ℃, and the pre-freezing treatment is carried out for 5-6 hours; and then heating and vacuumizing, controlling the temperature to be 40-50 ℃, controlling the vacuum degree to be 20-30Pa, and drying for 18-19h. The rest of the procedure was identical to that of experimental example 1.

The obtained bear gall powder product has a bright color Jin Huangjing and uniform particles/grains; the moisture content of the bear gall powder is detected to be 7.82 percent, and the content of the tauroursodeoxycholic acid is detected to be 38.4 percent.

Claims (10)

1. The production method of the bear gall powder is characterized by comprising the following steps:

S1, filtering bear bile to obtain a filtered bile solution;

s2, pre-freezing the filtered bile solution at the temperature of minus 40 ℃ to minus 45 ℃ for 1.5 to 2.5 hours, and keeping the pre-frozen solution for 1.5 to 2.0 hours; heating to-10 to-15 ℃ and keeping for 1.5-2.5 h; then controlling the temperature rise in stages, controlling the temperature to be kept in stages, and after the temperature is raised to 37-40 ℃ and kept, obtaining a dry material;

And S3, sieving the dried material to obtain bear gall powder.

2. The method of producing bear gall powder according to claim 1, wherein in the step S1, the filtration comprises two times of filtration, wherein the first filtration uses a filter element with a pore size of 0.45 μm and the second filtration uses a filter element with a pore size of 0.25 μm.

3. The production method of bear gall powder according to claim 1, wherein in the step S2, the filtered gall solution is split-packed into material trays for pre-freezing treatment, and the depth of the filtered gall solution in the material trays is controlled to be 1.8-2.2 cm.

4. The production method of bear gall powder according to claim 1 or 3, wherein in the step S2, the vacuum degree is controlled to be 40-60 Pa when the temperature is raised to-10 ℃ to-15 ℃ and maintained; controlling the vacuum degree to be 15-25 Pa when controlling the staged temperature rise and the staged temperature control and keeping;

and/or in the step S2, controlling the cooling speed to be 0.45-0.6 ℃/min when the pre-freezing treatment is carried out; in the process of heating to the temperature ranging from minus 10 ℃ to minus 15 ℃, the heating speed is controlled to be 0.45 ℃ to 0.6 ℃/min; and controlling the temperature rising speed to be 0.4-0.5 ℃/min during the staged temperature rising.

5. The production method of bear gall powder according to claim 4, wherein in step S2, the stepwise temperature rise is controlled, and the stepwise temperature is controlled and maintained, so that the temperature is raised to 37 ℃ to 40 ℃ and maintained, specifically comprising:

The first stage, controlling the temperature to be raised to-8 to-5 ℃ and the temperature raising and maintaining time to be 90-120 min;

In the second stage, heating to 2-5 ℃ and keeping the temperature for 90-120 min;

in the third stage, the temperature is controlled to be raised to 12-15 ℃ and the temperature is raised and the holding time is 120-150 min;

A fourth stage, controlling the temperature to be raised to 22-25 ℃ and the temperature raising and maintaining time to be 120-150 min;

in the fifth stage, the temperature is controlled to be raised to 27-30 ℃ and the temperature is raised and the holding time is 300-360 min

A sixth step of controlling the temperature to be raised to 32-35 ℃ and the temperature raising and maintaining time to be 300-360 min;

and seventh, controlling the temperature to be raised to 37-40 ℃ and the temperature raising and maintaining time to be 60-90 min.

6. The production method of bear gall powder according to claim 1, further comprising the steps of, before step S1:

s01, collecting fresh bear bile, quick-freezing at-18 ℃ to-22 ℃ for preservation and transportation, and taking the fresh bear bile as a raw material for freezing bear bile;

S02, thawing the bear bile frozen raw material in a water bath at the temperature of 10-15 ℃ to obtain the bear bile raw material.

7. The production method of bear gall powder according to claim 6, wherein in the step S1, the bear gall is a mixture of a first bear gall raw material and a second bear gall raw material, the first bear gall raw material is bear gall collected from 11 months to 3 months in the next year, the second bear gall raw material is bear gall collected from 4 months to 10 months, and the volume ratio of the first bear gall raw material to the second bear gall raw material is 1:1.8-2.3.

8. The production method of bear gall powder according to claim 1 or 7, wherein the moisture content of the bear gall powder is lower than 2%, and the content of tauroursodeoxycholic acid is 40.5% -43.5%.

9. Bear courage powder production freeze-drying device, its characterized in that includes freeze-drying storehouse (1), a plurality of freeze-drying plywood (2) of interval installation about in the freeze-drying storehouse, freeze-drying plywood (2) include:

The upper panel (3) is provided with a smooth heat conduction surface (31) on one side and a groove (32) on the other side, a plurality of division bars (33) are arranged in the groove (32) at intervals in parallel, and the division bars (33) divide the groove (32) into continuous serpentine flow channels;

a lower panel (4) which is adapted to cover the groove (32) of the upper panel (3), wherein the lower panel (4) is provided with a notch (41) corresponding to the parting bead (33);

Wherein the upper panel (3) and the parting bead (33) are integrally formed; the lower panel (4) is welded with the parting bead (33) through the notch (41), and the edge of the lower panel (4) is welded with the edge of the groove (32).

10. The bear gall powder production freeze-drying device according to claim 9, wherein:

the top of the parting bead (33) is provided with a large V-shaped groove (331) along the length direction, the width of the notch (41) is consistent with the width of the large V-shaped groove (331), and the angles of an included angle alpha at the bottom of the large V-shaped groove (331) and an included angle beta between the side wall of the large V-shaped groove (331) and the side wall of the notch (41) are 110-140 degrees;

A first groove (34) is formed in the outer side of the edge of the groove (32) of the upper panel (3), a second groove (42) corresponding to the first groove (34) is formed in the edge of the lower panel (4), and the first groove (34) and the second groove (42) form a large V-shaped welding slot;

The notch (41) is opened at one end of the edge of the lower panel (4), and the large V-shaped groove (331) is communicated with the large V-shaped welding slot.