A centrifuge tube and its application in pyrolysis liquid quality improvement and succinic acid or hexanoic acid extraction

By using an on-off assembly and a timed locking assembly in a centrifuge tube, the problems of easy clogging of the porous diaphragm and easy backmixing of materials are solved, miniaturization of the centrifuge tube and efficient separation effect are achieved, and processing costs and energy consumption are reduced.

CN119386949BActive Publication Date: 2025-09-30ENERGY RES INST OF SHANDONG ACAD OF SCI
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Patent Information

Application Number
CN202411531832.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-30
Publication Date
2025-09-30
Estimated Expiration
2044-10-30

AI Technical Summary

Technical Problem

The porous diaphragm of the existing centrifuge tube is easily clogged when reused, the anti-backflow effect is not ideal, and it is difficult to achieve a miniaturized design after the device is enlarged.

Method used

The on-off assembly is used to connect and disconnect the upper and lower parts of the centrifuge tube according to the size of the centrifugal force. The on-off state is controlled by the timing locking assembly to avoid diaphragm blockage and material backmixing.

Benefits of technology

The miniaturized design of the centrifuge tube is realized, diaphragm blockage and material backmixing are avoided, the concentration of the solution after centrifugation is increased, and the subsequent processing cost and energy consumption are reduced.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of separation and purification of fine chemical products, and specifically relates to a centrifuge tube and its application in the quality improvement of pyrolysis liquid and the extraction of succinic acid or hexanoic acid. The present invention enables a limiting piece in an on-off component to move up and down along the length direction of the tube body in a discharge hole, so that the dynamic contact and the static contact are sealedly connected or disconnected, thereby realizing the isolation and connection of the upper and lower parts of the tube body; or the connection and isolation of the upper and lower parts of the tube body are realized through the cooperation between the on-off component and the timing locking component, thereby solving the problems of easy blockage of the diaphragm of the centrifuge tube and easy backmixing of materials. The centrifuge tube has good application value in the quality improvement of pyrolysis liquid and the extraction of succinic acid and hexanoic acid.
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Description

Technical Field

[0001] The invention belongs to the technical field of separation and purification of fine chemical products, and particularly relates to a centrifuge tube and application thereof in improving the quality of pyrolysis liquid and extracting succinic acid or caproic acid. Background Art

[0002] Centrifugation utilizes a high-speed motor to generate a centrifugal field, placing mixed particles in a suspension or immiscible liquids of varying densities in an emulsion into a centrifuge tube for separation and extraction. Conventional centrifuge tubes are simple in structure and limited in function, making them difficult to meet user needs.

[0003] A large number of studies have been conducted in the prior art to improve centrifuge tubes. For example, ZL202021300317.4 discloses an ultrafiltration centrifuge tube device, comprising: a tube cover, a filter cavity, an ultrafiltration membrane, a support sleeve, and a collection tube. ZL201610042368.3 provides a density gradient centrifuge tube with a position-adjustable porous diaphragm, comprising a centrifuge tube body, a centrifuge tube cover provided on the upper part of the centrifuge tube body, a diaphragm layer provided in the centrifuge tube body, an internal thread provided on the inner wall of the centrifuge tube body, an external thread provided on the outer wall of the diaphragm layer, the internal thread of the centrifuge tube body cooperates with the external thread of the diaphragm layer, and the diaphragm layer is provided with multiple small holes. ZL201610527560.1 discloses an integrated ultrafiltration centrifuge tube. ZL202022277914.6 discloses an ultrafiltration centrifuge tube, comprising a main body, a placement protection mechanism provided on the lower outer surface of the main body, an outer tube provided on the upper outer surface of the placement protection mechanism, an anti-backflow mechanism provided on the inner surface of the outer tube, and an ultrafiltration tube provided on the upper outer surface of the anti-backflow mechanism. Although the centrifuge tube using the above scheme can effectively achieve the purpose of centrifugal separation and can play a role in anti-backflow to a certain extent, the porous diaphragm in the centrifuge tube is easily clogged when reused, especially for more complex samples such as fermentation broth; the anti-backflow effect is still not ideal, especially after the device is scaled up, and a new technology needs to be sought to solve this problem.

[0004] In addition, ZL202210258849.3 discloses a centrifuge tube, which includes a tube body and a discharge tube located inside the tube body, wherein the bottom of the discharge tube is closed and the top is open, and a piston and a spring are sequentially arranged inside the discharge tube from top to bottom, and a discharge hole is provided in the upper and middle part of the tube wall of the discharge tube. The centrifuge tube can achieve communication and isolation between the upper and lower parts of the centrifuge tube according to the magnitude of the centrifugal force generated by the piston during high-speed rotation, which can solve the problems of easy blockage of the diaphragm of the centrifuge tube and easy backflow of materials. However, when the upper and lower parts of the centrifuge tube are isolated, the movement of the piston is restricted due to the incompressibility of the liquid material; since the connection and isolation between the piston and the discharge hole requires the piston to move a certain distance, the spring also occupies a certain space, which makes the entire assembly larger, which is not conducive to the miniaturization design of the centrifuge tube. Summary of the Invention

[0005] In order to overcome the above technical problems, the present invention provides a centrifuge tube and its application in the quality improvement of pyrolysis liquid and the extraction of succinic acid or hexanoic acid. The upper and lower parts of the centrifuge tube are connected and isolated according to the magnitude of the centrifugal force generated by the on-off component during high-speed rotation, or the upper and lower parts of the centrifuge tube are connected and isolated through the cooperation between the on-off component and the timing locking component, thereby effectively realizing the miniaturization design of the centrifuge tube and solving the problems of easy blockage of the diaphragm of the centrifuge tube and easy backmixing of materials.

[0006] In order to achieve the above object, the technical solution of the present invention is:

[0007] In a first aspect, the present invention provides a centrifuge tube, comprising a tube body and an on-off assembly located inside the tube body and separating the tube body into upper and lower parts;

[0008] The switch assembly includes a static contact, an elastic band, a gasket, a bottom plate, and a dynamic contact; wherein the bottom plate is connected to the gasket, and a flow hole is provided on the bottom plate; the gasket is provided with an elastic band, and the elastic band is connected to the dynamic contact; the dynamic contact is provided with a limit plate, the limit plate is provided with a static contact, and the static contact is provided with a feed hole;

[0009] The limiting piece can move up and down along the length direction of the tube body in the discharge hole, so that the dynamic contact and the static contact are sealed and connected or disconnected, so as to realize the separation and connection between the upper and lower parts of the tube body.

[0010] In some embodiments, the top of the tube body is open, the bottom of the tube body is closed, the top outer wall of the tube body is provided with a top external thread, a top cover is provided on the top outside of the tube body, and a top cover internal thread is provided at the bottom position inside the top cover, and the top cover internal thread is used in conjunction with the top external thread provided on the top outer wall of the tube body.

[0011] In some embodiments, the bottom of the tube body is open, and the outer wall of the bottom is provided with a bottom external thread; a bottom cover is provided on the outside of the bottom of the tube body, and a bottom cover internal thread is provided at the bottom position inside the bottom cover, and the bottom cover internal thread is used in conjunction with the bottom external thread provided on the bottom outer wall of the tube body.

[0012] In some embodiments, a sleeve is provided above the static contact, and the switch assembly and the sleeve can be removed from the interior of the tube body.

[0013] In some embodiments, a trigger pin is provided at the bottom of the dynamic contact member; the elastic band is provided with an elastic hole; the bottom plate is provided with a pin hole, and the bottom of the bottom plate is connected to the gasket and the timing locking assembly in sequence; the timing locking assembly is provided with a limiting hole; the trigger pin passes through the elastic hole, the pin hole, the gasket and the limiting hole in sequence.

[0014] In a second aspect, the present invention provides a method for using a centrifuge tube, comprising the following steps: adding a sample to the centrifuge tube of the first aspect and centrifuging the sample; during the centrifugation, the limiting plate moves downward in the discharge hole along the length direction of the centrifuge tube, disconnecting the movable contact member from the static contact member, thereby achieving communication between the upper and lower parts of the tube body, and obtaining a centrifuge liquid;

[0015] After centrifugation is completed, the limiting piece moves upward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact member and the static contact member are sealed and connected, thereby separating the upper and lower parts of the tube body;

[0016] Pour the upper centrifuge liquid out from the top of the tube body; press the movable contact to disconnect the movable contact from the static contact, so that the upper and lower parts of the tube body are connected, and pour the lower centrifuge liquid out from the top of the tube body.

[0017] In some embodiments, the method comprises the following steps: adding a sample to the centrifuge tube of the first aspect and centrifuging the sample; during the centrifugation, the limiting piece moves downward in the discharge hole along the length direction of the centrifuge tube, disconnecting the movable contact member from the static contact member, thereby achieving communication between the upper and lower parts of the tube body, and obtaining a centrifuge liquid;

[0018] After centrifugation is completed, the limiting piece moves upward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact member and the static contact member are sealed and connected, thereby separating the upper and lower parts of the tube body;

[0019] Pour the upper centrifuge liquid out from the top of the tube body; remove the bottom cover at the bottom of the tube body and pour the lower centrifuge liquid out from the bottom of the tube body.

[0020] In some embodiments, the method comprises the following steps: adding a sample to the centrifuge tube of the first aspect and centrifuging the sample; during the centrifugation, the limiting piece moves downward in the discharge hole along the length direction of the centrifuge tube, disconnecting the movable contact member from the static contact member, thereby achieving communication between the upper and lower parts of the tube body, and obtaining a centrifuge liquid;

[0021] After centrifugation is completed, the limiting piece moves upward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact member and the static contact member are sealed and connected, thereby separating the upper and lower parts of the tube body;

[0022] Remove the on-off assembly and the sleeve from the inside of the tube body to obtain the upper layer of centrifugal liquid; pour out the lower layer of centrifugal liquid from the top of the tube body.

[0023] In some embodiments, the centrifuge tube of the first aspect is used, comprising the following steps: pressing the movable contact member to open the feed hole, and simultaneously causing the trigger pin to be confined within the limiting hole of the timing locking assembly; adding the sample to the centrifuge tube of the first aspect, and centrifuging the timing locking assembly at the start of the timing locking time;

[0024] During the centrifugation process, the limiting piece moves downward in the discharge hole along the length direction of the centrifuge tube, disconnecting the dynamic contact member from the static contact member, thereby achieving communication between the upper and lower parts of the tube body and obtaining centrifuge liquid;

[0025] When the timed locking time of the timing locking assembly ends, the limit of the trigger pin ends, and the limit piece moves upward along the length direction of the centrifuge tube in the discharge hole, so that the dynamic contact member and the static contact member are sealed and connected, thereby realizing the separation of the upper and lower parts of the tube body;

[0026] When the bottom of the tube is closed and the top is open, the upper layer of centrifugal liquid is poured out from the top of the tube; the movable contact is pressed to disconnect the movable contact from the static contact, so that the upper and lower parts of the tube are connected, and the lower layer of centrifugal liquid is poured out from the top of the tube;

[0027] Or, when the bottom of the tube body is open and used in conjunction with a bottom cover, the bottom cover at the bottom of the tube body is removed to pour the lower layer of centrifuge liquid out from the bottom of the tube body;

[0028] Alternatively, when a sleeve tightly connected to the static contact is provided above the on-off assembly, the on-off assembly and the sleeve are removed from the tube body to obtain the upper centrifuge liquid; the lower centrifuge liquid is poured out from the top of the tube body.

[0029] In a third aspect, the present invention provides applications of the centrifuge tube described in the first aspect, including but not limited to applications in upgrading pyrolysis liquid and extracting succinic acid or hexanoic acid.

[0030] Beneficial effects of the present invention:

[0031] (1) The centrifuge tube proposed by the present invention is easy to operate and does not have the problems of pollution and clogging;

[0032] (2) The centrifuge tube proposed by the present invention realizes the connection and separation of the upper and lower parts of the centrifuge tube according to the on-off component under the action of centrifugal force. The product structure is simple and compact, and it is easy to realize miniaturization design and mass production;

[0033] (3) The centrifuge tube provided by the present invention can increase the concentration of the solution after centrifugation and significantly reduce subsequent processing costs and energy consumption.

[0034] (4) The on-off state of the on-off assembly is controlled by a timing locking assembly, or the on-off state of the on-off assembly in a centrifugal state is controlled by adjusting the specification parameters of the elastic band to solve the problem of easy remixing of materials in the centrifuge tube. It has good application potential in scientific research and industrial production in technical fields such as oil quality improvement, biomedicine, isotope separation, isomer separation, gas separation, liquid propellant, and supergravity separation. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 Schematic diagram of the structure of the centrifuge tube of the present invention;

[0036] Figure 2 This is a schematic structural diagram of a centrifuge tube with an open bottom according to the present invention;

[0037] Figure 3 This is a schematic structural diagram of the switch assembly of the present invention;

[0038] Figure 4 This is a schematic structural diagram of the switch assembly of the present invention in a centrifugal state;

[0039] Figure 5 This is a structural schematic diagram of an on-off assembly provided with a timing locking assembly according to the present invention;

[0040] Figure 6 Schematic diagram of the structure of the static contact of the present invention;

[0041] Figure 7 AA sectional view of the static contact of the present invention;

[0042] Figure 8 Schematic diagram of the structure of the gasket of the present invention;

[0043] Figure 9 A BB-section view of the gasket of the present invention;

[0044] Figure 10 It is a structural schematic diagram of the bottom plate of the present invention;

[0045] Figure 11 It is a CC sectional view of the bottom plate of the present invention;

[0046] Figure 12 It is a structural schematic diagram of the movable contact of the present invention;

[0047] Figure 13 2 is a cross-sectional view of the movable contact DD of the present invention;

[0048] Figure 14 EE-direction cross-sectional view of the movable contact of the present invention;

[0049] Figure 15 Schematic diagram of the structure of the elastic band of the present invention;

[0050] Figure 16 This is a schematic structural diagram of the elastic band of the present invention in a working state;

[0051] Figure 17 A top view of the elastic band of the present invention;

[0052] Figure 18 This is a schematic structural diagram of a switch assembly provided with a sleeve according to the present invention;

[0053] In the figure: tube body 1; on-off assembly 2; top external thread 3; bottom external thread 4; static contact 5; washer 6; bottom plate 7; limit plate 8; dynamic contact 9; elastic band 10; feed hole 11; pin removal hole 12; gasket 13; limit hole 14; trigger pin 15; timing locking assembly 16; flow hole 17; sleeve 18. DETAILED DESCRIPTION

[0054] Example 1

[0055] A centrifuge tube, such as Figure 1 As shown, it includes a tube body 1 and an on-off assembly 2 located inside the tube body 1 to separate the tube body into two parts, the top of the tube body 1 is open and the bottom is closed. The top outer wall of the tube body is provided with a top external thread 3, and the top outer surface of the tube body 1 is provided with a top cover ( Figure 1 The top cover is provided with an internal thread at the bottom of the top cover, and the internal thread of the top cover is used in conjunction with the top external thread provided on the outer wall of the top of the tube body.

[0056] like Figure 3 As shown, the switch assembly 2 consists of a static contact 5, an elastic band 10, a washer 6, a base plate 7, and a dynamic contact 9; wherein the base plate 7 is connected to the washer 6, and a flow hole 17 is provided on the base plate 7; the washer 6 is provided with an elastic band 10, and the elastic band 10 is connected to the dynamic contact 9; the dynamic contact 9 is provided with a limit plate 8, and the limit plate 8 is provided with a static contact 5; the static contact 5 is provided with a feed hole 11;

[0057] The limiting piece 8 can move up and down along the length direction of the tube body 1 in the discharge hole 11 to seal or disconnect the dynamic contact 9 from the static contact 5, thereby realizing the separation and connection between the upper and lower parts of the tube body 1.

[0058] like Figure 4 As shown, during the centrifugal process, the on-off assembly 2 moves downward, and under the action of the centrifugal force, the elastic band 10, when the centrifugal force is greater than the restoring force of the elastic band 10, the limit plate 8 can move downward in the discharge hole 11 along the length direction of the tube body 1, so that the dynamic contact 9 is disconnected from the static contact 5, so as to realize the connection between the upper and lower parts of the tube body 1.

[0059] like Figure 6 As shown, a feed hole 11 is provided at the center of the static contact 5. Figure 7 As shown, the diameter of the static contact 5 is larger than the discharge hole 11; the static contact 5 is used to keep the on-off assembly 2 tightly connected to the tube body 1; the discharge hole 11 is used to cooperate with the limit plate 8 and the limit plate 8 can move up and down along the length direction of the tube body 1 in the discharge hole 11, so that the dynamic contact 9 is sealed and connected or disconnected with the static contact 5, so as to realize the separation and connection of the upper and lower parts inside the tube body 1.

[0060] like Figure 8 As shown, the washer 6 is provided with an elastic band 10, as shown in FIG. Figure 9 The washer shown is annular; the washer is used to support and fix the elastic band 10.

[0061] like Figure 10 As shown, the bottom plate 7 is a circular thin plate. Figure 11 As shown, a plurality of flow holes 17 are provided on the bottom plate 7 ; the bottom plate 7 is used to keep the on-off assembly 2 tightly connected to the tube body 1 ; the flow holes 17 are used for the sample to flow up and down in the tube body 1 .

[0062] like Figure 12 As shown, a limit piece 8 is provided on the movable contact 9; Figure 13 As shown, the limiting piece 8 is located at the center of the moving contact 9; Figure 14 As shown, the dynamic contact 9 is a circular plate; the dynamic contact 9 is used to move up and down when subjected to force, driving the limit plate 8 to move up and down along the length direction of the tube body 1 in the discharge hole 11, so that the dynamic contact 9 and the static contact 5 are sealed and connected or disconnected, controlling the connection and disconnection of the upper and lower parts of the tube body 1.

[0063] like Figure 15 As shown, the elastic band 10 is a rectangular elastic band; Figure 16 As shown, under the action of centrifugal force, when the centrifugal force is greater than the restoring force of the elastic band 10, the two ends of the elastic band 10 remain taut and the middle part bends downward. Figure 17As shown, there are at least two elastic bands 10 , both ends of the elastic bands 10 are connected to the washers 6 , and a dynamic contact piece 9 is provided on the elastic bands 10 .

[0064] The static contact 5, elastic band 10, washer 6, and base plate 7 are secured together using screws and nuts. The tube body 1 is made of polypropylene, with an inner diameter of 30mm and a height of 120mm. The distance between the top of the static contact 5 and the top of the tube body 1 is 70mm, and the feed hole 11 has a diameter of 10mm. The static contact 5, washer 6, and base plate 7 are also made of polypropylene, and the elastic band 10 is made of rubber. The thicknesses of the static contact 5, washer 6, and base plate 7 are 4mm, 10mm, and 4mm, respectively. The dynamic contact 9 is made of 316L stainless steel, with a bottom diameter of 15mm. The limiter 8 is 10mm wide.

[0065] The specifications of the elastic band 10 are selected and determined by the centrifugal force used in the experiment. When the centrifugal force exceeds the restoring force of the elastic band 10, the stopper 8 can move downward along the length of the tube 1 within the feed hole 11, thereby establishing communication between the upper and lower parts of the tube 1. The magnitude of the centrifugal force can be adjusted according to the rotational speed. For example, the movement of the movable contact 9 causes the switch assembly 2 to open at a centrifugal speed of 30,000 rpm or above, and to close at a centrifugal speed of less than 30,000 rpm.

[0066] Example 2

[0067] The similarities between this embodiment and embodiment 1 are not repeated here, but the differences are as follows:

[0068] like Figure 2 As shown, the bottom of the tube body 1 is open, and the outer wall of the bottom of the tube body 1 is provided with a bottom external thread 4, which is used in conjunction with the bottom cover; the elastic band 10 is made of metal spring; the static contact 5, the elastic band 10, the gasket 6 and the bottom plate 7 are glued together in sequence using adhesive.

[0069] Example 3

[0070] The similarities between this embodiment and embodiment 2 are not repeated here, and the differences are as follows:

[0071] like Figure 18 As shown, a hollow sleeve 18 tightly connected to the static contact 5 is provided above the on-off assembly 2. The on-off assembly 2 and the sleeve 18 can be removed from the tube body 1, thereby avoiding the influence of pressing the dynamic contact 9 on the centrifuge liquid.

[0072] The distance between the top of the static contact 5 and the top of the tube body 1 is 60 mm.

[0073] Example 4

[0074] The similarities between this embodiment and embodiment 3 are not repeated here, and the differences are as follows:

[0075] like Figure 5 As shown, a trigger pin 15 is connected to the bottom of the movable contact 9, a pin hole 12 is provided in the middle of the bottom plate 7, a gasket 13 and a timing locking assembly 16 are provided in sequence under the bottom plate 7, and a limiting hole 14 is provided in the middle of the timing locking assembly 16; the trigger pin 15 passes through the pin hole 12 and the gasket 13 to the limiting hole 14 in sequence; thereby accurately controlling the centrifugal time.

[0076] The timing locking component 16 is an existing commonly used timing locking component structure, and can adopt a timing locking component based on clock timing or mechanical timer, such as CN201620351704.8 a fan timer and fan, CN201920507464.X a timer that is silent after an alarm, CN200520014060.5 washing machine washing timer or CN97206802.3 fan full plastic timer, etc., without any other special structural requirements.

[0077] The centrifuge tubes provided by the present invention have great application potential in scientific research and industrial production in technical fields such as oil quality improvement, biomedicine, isotope separation, isomer separation, gas separation, liquid propellants, and high-gravity separation. The following uses the centrifuge tubes provided by the present invention in pyrolysis solution quality improvement and succinic acid or hexanoic acid extraction as examples to illustrate the application effects of the centrifuge tubes provided by the present invention. This application is for illustrative purposes only and is not limited to applications in pyrolysis solution quality improvement and succinic acid or hexanoic acid extraction.

[0078] Example 5

[0079] The gas generated by the thermal decomposition of biomass is cooled and the resulting liquid is left to stand. The resulting upper clear liquid is called wood vinegar, and the lower oily substance is called wood tar. Both wood vinegar and wood tar contain more or less oily solid particles, waxy substances and micellar substances, and are brown to black in color. They have high phase stability and require dozens of days or even longer to settle before becoming clear and transparent. The poor quality of wood vinegar and wood tar has seriously hindered their application and promotion.

[0080] The centrifuge tube described in Example 1 was used to improve the quality of the pyrolysis solution. To compare the improvement effect of the pyrolysis solution, the transmittance of the pyrolysis solution was measured using a UV-visible spectrophotometer (model SP-752PC, Shanghai Spectrum Instrument Co., Ltd.) at a wavelength of 550 nm, using a 1.0 cm quartz cuvette and air as a reference. The pyrolysis solution improvement process included the following steps:

[0081] The process of preparing pyrolysis liquid using a screw-propelled pyrolysis furnace is as follows: using a screw-propelled pyrolysis furnace with an inner diameter of 80 mm and a length of 3000 mm, heating with a resistance wire (rated power of 3.5 kW), temperature control with a thermostat, and an outer layer provided with a heat-insulating layer; using corn stalks (with a moisture content of 10 wt%) having a length of less than 1 to 5 mm as a raw material, feeding the screw-propelled pyrolysis furnace at a rate of 3.0 kg / h, and a pyrolysis temperature of 550° C. The gas generated by the pyrolysis is cooled and the obtained liquid is allowed to stand, and the obtained upper clear liquid is called wood vinegar, and the lower oily substance is called wood tar.

[0082] 60 ml of wood tar (transmittance 10.25%) prepared by the above process was added to the centrifuge tube, centrifuged at 30,000 rpm for 30 min at 5°C, the upper centrifuge liquid was poured out, and the transmittance was measured to be 91.30%. The movable contact 9 was pressed and the lower centrifuge liquid was poured out through the on-off component 2 and used for the next centrifugal quality improvement.

[0083] 60 ml of the wood vinegar (transmittance 15.40%) prepared by the above process was added to the centrifuge tube and centrifuged at 30,000 rpm for 30 min at 5° C. The upper centrifuge liquid was poured out and the transmittance was measured to be 94.56%. The movable contact 9 was pressed and the lower centrifuge liquid was poured out through the on-off assembly 2 and used for the next centrifugal quality improvement.

[0084] Example 6

[0085] The centrifuge tube described in Example 2 was used for succinic acid extraction, comprising the following steps:

[0086] The succinate fermentation broth was added to a conventional centrifuge tube and centrifuged at 6000 rpm for 10 minutes at 5°C to remove the bacterial cells, obtaining a supernatant. The succinate concentration was determined to be 33.15 g / L by gas chromatography. The bottom cap of the centrifuge tube described in this example was removed, and a hollow rubber ball with an outer diameter of 6 mm was placed in it. The bottom cap was then replaced. 60 mL of the succinate supernatant was added to the centrifuge tube and centrifuged at 30000 rpm for 30 minutes at 5°C. The upper centrifuge liquid was poured out and used for further fermentation. The bottom cap was removed and the lower centrifuge liquid was obtained. The succinate concentration in the lower centrifuge liquid was determined to be 48.65 g / L. The lower centrifuge liquid was used for the next step of extracting succinate.

[0087] Compared with Example 1, the bottom of the tube body 1 of this embodiment is open and is used in conjunction with the bottom cover, so that the lower layer of liquid after centrifugation is easier to remove and the operation is more convenient.

[0088] Example 7

[0089] The centrifuge tube described in Example 3 was used for hexanoic acid extraction, comprising the following steps:

[0090] The caproate fermentation broth was added to a conventional centrifuge tube and centrifuged at 6000 rpm for 10 minutes at 5°C to remove the bacterial cells. The supernatant was obtained. The caproate concentration was determined by gas chromatography to be 17.24 g / L. 60 mL of the caproate supernatant was added to the centrifuge tube described in this example and centrifuged at 30000 rpm for 30 minutes at 5°C to obtain the upper centrifuge liquid. The caproate concentration was determined to be 21.15 g / L. The upper centrifuge liquid was used for the next step of caproate extraction. The on-off assembly 2 and sleeve 18 were removed from the tube body 1 to obtain the lower centrifuge liquid, which was used for further fermentation.

[0091] Example 8

[0092] The centrifuge tube described in Example 4 was used to improve the quality of the pyrolysis solution, and the process included the following steps:

[0093] The process of preparing pyrolysis liquid using a screw-propelled pyrolysis furnace is as follows: dried avermectin residue (water content of 2.1wt%) is used as raw material, entering the screw-propelled pyrolysis furnace at a rate of 3.0kg / h, and the pyrolysis temperature is 550°C. The gas generated by pyrolysis is cooled and the obtained liquid is allowed to stand. The upper clear liquid is called wood vinegar, and the lower oily substance is called wood tar.

[0094] The timing locking time RT of the timing locking assembly 16 is set to 30 minutes. When the trigger pin 15 is limited in the limiting hole 14 of the timing locking assembly 16, the timing locking time RT of the timing locking assembly 16 starts to run, and when the timing locking time RT ends, the limiting of the trigger pin 15 ends, and the dynamic contact 9 moves up to close the discharge hole 11.

[0095] A hollow rubber ball with an outer diameter of 5 mm was added to the centrifuge tube described in this embodiment.

[0096] The bottom cover of the centrifuge tube described in this embodiment was removed and a hollow rubber ball with an outer diameter of 6 mm was placed in it, and the bottom cover was installed; the dynamic contact member 9 was pressed to open the discharge hole 11, and at the same time, the trigger pull pin 15 was confined in the limiting hole 14 of the timing locking assembly 16; 60 ml of wood tar (transmittance 10.17%) was added to the centrifuge tube, and the tube was centrifuged at 30,000 rpm for 30 minutes at 5°C. The upper centrifuge liquid was poured out, and the transmittance was measured to be 90.05%; the on-off assembly 2 and the sleeve 18 could be removed from the tube body 1 to obtain the lower centrifuge liquid and use it for the next centrifugation quality improvement.

[0097] The bottom cover of the centrifuge tube described in this embodiment was removed and a hollow rubber ball with an outer diameter of 6 mm was placed therein. The bottom cover was then replaced. The movable contact 9 was pressed to open the feed hole 11, and the trigger pin 15 was simultaneously restrained within the limiting hole 14 of the timing locking assembly 16. 60 ml of wood vinegar (transmittance 15.03%) was added to the centrifuge tube. The tube was centrifuged at 30,000 rpm for 30 minutes at 5°C. The upper centrifuge liquid was poured out, and the transmittance was measured to be 92.24%. The on-off assembly 2 and the sleeve 18 were removed from the tube body 1 to obtain the lower centrifuge liquid, which was used for the next centrifugal quality improvement.

[0098] Comparative Example 1

[0099] The similarities between this embodiment and embodiment 5 are not repeated here, and the differences are as follows:

[0100] 60 ml of wood tar (transmittance 10.25%) was added to a common centrifuge tube, and the tube was centrifuged at 30,000 rpm for 30 min at 5°C. The upper centrifuge liquid was poured out and the transmittance was measured to be 62.18%.

[0101] 60 ml of wood vinegar (transmittance 15.40%) was added to a common centrifuge tube, and the mixture was centrifuged at 30,000 rpm for 30 min at 5° C. The upper centrifuge liquid was poured out, and the transmittance was measured to be 65.20%.

[0102] Comparative Example 1 and Comparative Example 5 show that the use of the centrifuge tube provided in Example 1 of the present invention greatly increases the transmittance of wood tar and wood vinegar, thereby improving their quality.

[0103] Comparative Example 2

[0104] The similarities between this embodiment and embodiment 6 are not repeated here, and the differences are as follows:

[0105] 60 mL of the succinic acid supernatant (succinic acid concentration of 33.15 g / L) was added to a common centrifuge tube, and centrifuged at 30,000 rpm for 30 min at 5°C. The centrifuge liquid was poured out, and the succinic acid concentration in the centrifuge liquid was measured to be 33.14 g / L.

[0106] By comparing Example 2 and Comparative Example 6, it can be seen that the centrifuge tube provided in Example 1 of the present invention greatly increases the concentration of succinic acid, and can greatly reduce the energy consumption and cost of subsequent succinic acid extraction.

[0107] Comparative Example 3

[0108] The similarities between this embodiment and embodiment 7 are not repeated here, and the differences are as follows:

[0109] 60 mL of the caproic acid supernatant (caproic acid concentration of 17.24 g / L) was added to a common centrifuge tube, centrifuged at 30,000 rpm for 30 min at 5°C, and the centrifuge liquid was poured out. The succinic acid concentration in the centrifuge liquid was measured to be 17.24 g / L.

[0110] By comparing Example 3 and Example 7, it can be seen that the centrifuge tube provided by Example 7 of the present invention increases the concentration of caproic acid and reduces the energy consumption and cost of subsequent caproic acid extraction.

[0111] The above descriptions are merely preferred embodiments of the present invention. These embodiments all depict intermittent centrifugation, with a single on / off assembly disposed within the centrifuge tube. These embodiments are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations are possible. For example, the centrifuge tube of the present invention may be used for continuous centrifugation, or multiple on / off assemblies may be disposed within the centrifuge tube. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A centrifuge tube, characterized in that: It includes a pipe body and a switch assembly located inside the pipe body and separating the pipe body into two parts, an upper part and an lower part; The switch assembly includes a static contact, an elastic band, a gasket, a bottom plate, and a dynamic contact; wherein the bottom plate is connected to the gasket, and a flow hole is provided on the bottom plate; the gasket is provided with an elastic band, and the elastic band is connected to the dynamic contact; the dynamic contact is provided with a limit plate, the limit plate is provided with a static contact, and the static contact is provided with a feed hole; The limiting piece can move up and down along the length direction of the tube body in the discharge hole, so that the dynamic contact and the static contact are sealed and connected or disconnected, thereby realizing the separation and connection between the upper and lower parts of the tube body; The moving contact controls the on-off assembly to open when the centrifugal state is above a certain speed, and controls the on-off assembly to close when the centrifugal state is below a certain speed; The bottom of the movable contact is provided with a trigger pin; the elastic band is provided with an elastic hole; the bottom plate is provided with a pin hole, and the bottom of the bottom plate is connected to the gasket and the timing locking assembly in sequence; the timing locking assembly is provided with a limiting hole; the trigger pin passes through the elastic hole, the pin hole, the gasket and the limiting hole in sequence; When the timing locking time of the timing locking component ends, the moving contact closes the on-off component.

2. The centrifuge tube according to claim 1, wherein The top of the tube body is open, the bottom of the tube body is closed, the top outer wall of the tube body is provided with a top external thread, a top cover is provided on the outside of the top of the tube body, and a top cover internal thread is provided at the bottom position inside the top cover, and the top cover internal thread is used in conjunction with the top external thread provided on the top outer wall of the tube body.

3. The centrifuge tube according to claim 1, wherein The bottom of the tube body is open, and the outer wall of the bottom is provided with a bottom external thread; a bottom cover is provided on the outside of the bottom of the tube body, and a bottom cover internal thread is provided at the bottom position inside the bottom cover, and the bottom cover internal thread is used in conjunction with the bottom external thread provided on the bottom outer wall of the tube body.

4. The centrifuge tube according to claim 2, wherein A sleeve is provided above the static contact, and the switch assembly and the sleeve can be taken out from the inside of the tube body.

5. A method for using a centrifuge tube, characterized in that: The centrifuge tube according to any one of claims 1 to 4 comprises the following steps: pressing the movable contact member to open the feed hole, and simultaneously limiting the trigger pin in the limiting hole of the timing locking assembly; adding the sample into the centrifuge tube, and centrifuging the timing locking assembly at the start of the timing locking time; During the centrifugation process, the limiting piece moves downward in the discharge hole along the length direction of the centrifuge tube, disconnecting the dynamic contact member from the static contact member, thereby achieving communication between the upper and lower parts of the tube body and obtaining centrifuge liquid; When the timing locking time of the timing locking assembly ends, the limit of the trigger pin ends, and the limit plate moves upward along the length direction of the centrifuge tube in the discharge hole, so that the dynamic contact and the static contact are sealed and connected to achieve the separation of the upper and lower parts of the tube body.

6. The method for using a centrifuge tube according to claim 5, wherein: When the bottom of the tube body is closed and the top is open, the upper centrifugal liquid is poured out from the top of the tube body; the movable contact is pressed to disconnect the movable contact from the static contact, so that the upper and lower parts of the tube body are connected, and the lower centrifugal liquid is poured out from the top of the tube body.

7. The method for using a centrifuge tube according to claim 5, wherein: When the bottom of the tube body is opened and used in conjunction with the bottom cover, the bottom cover at the bottom of the tube body is removed to pour out the lower layer of centrifuge liquid from the bottom of the tube body.

8. The method for using a centrifuge tube according to claim 5, wherein: When a sleeve tightly connected to the static contact is provided above the on-off assembly, the on-off assembly and the sleeve are removed from the tube body to obtain the upper centrifugal liquid; the lower centrifugal liquid is poured out from the top of the tube body.

9. Use of the centrifuge tube according to any one of claims 1 to 4, characterized in that: Application in pyrolysis liquid quality improvement and succinic acid or hexanoic acid extraction.

Citation Information

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