Centrifugal tube and application thereof in pyrolysis liquid upgrading and succinic acid or hexanoic acid extraction

Abstract

The invention belongs to the technical field of separation and refining of fine chemical products, and particularly relates to a centrifugal tube and application of the centrifugal tube in pyrolysis liquid upgrading and succinic acid or hexanoic acid extraction.A limiting piece in an on-off assembly moves up and down in a discharging hole in the length direction of a tube body, so that a movable contact piece and a static contact piece are connected or disconnected in a sealed mode, and therefore the centrifugal tube can be used for improving the quality of pyrolysis liquid or extracting succinic acid or hexanoic acid; the upper part and the lower part in the pipe body are separated and communicated; or communication and separation of the upper part and the lower part of the tube body are achieved through cooperation of the on-off assembly and the timing locking assembly, so that the problems that a diaphragm of the centrifugal tube is prone to blockage, materials are prone to backmixing and the like are solved, and the centrifugal tube has good application value in the aspects of pyrolysis liquid upgrading, succinic acid and hexanoic acid extraction and the like.

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 quality improvement of pyrolysis liquid and extraction of succinic acid or caproic acid. Background Art

[0002] Centrifugal separation is a method of separating and extracting different particles mixed in a suspension or immiscible liquids of different densities in an emulsion by using a high-speed rotating motor to generate a centrifugal field. Conventional centrifuge tubes have a simple structure and a single function, which makes it difficult to meet people's usage needs.

[0003] There have been a lot of studies in the prior art to improve centrifuge tubes. For example, ZL202021300317.4 discloses an ultrafiltration centrifuge tube device, including: a tube cover, a filter chamber, an ultrafiltration membrane, a support sleeve and a collection tube. ZL201610042368.3 provides a density gradient centrifuge tube with a position-adjustable porous diaphragm, including a centrifuge tube body, a centrifuge tube cover is provided on the upper part of the centrifuge tube body, a diaphragm layer is provided in the centrifuge tube body, an internal thread is provided on the inner wall of the centrifuge tube body, an external thread is provided on the outer wall of the diaphragm layer, the internal thread of the centrifuge tube body matches the external thread of the diaphragm layer, and a plurality of small holes are provided on the diaphragm layer. ZL201610527560.1 discloses an integrated ultrafiltration centrifuge tube. ZL202022277914.6 discloses an ultrafiltration centrifuge tube, comprising a main body, a placement protection mechanism disposed on the lower outer surface of the main body, an outer tube disposed on the upper outer surface of the placement protection mechanism, an anti-backflow mechanism disposed on the inner surface of the outer tube, and an ultrafiltration tube disposed 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 prone to clogging when reused, especially for more complex samples such as fermentation broth; the anti-backflow effect is still not ideal, especially after the device is enlarged, 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 feed tube located inside the tube body, the bottom of the feed tube is closed, the top is open, a piston and a spring are arranged in sequence from top to bottom inside the feed tube, and a discharge hole is arranged in the middle and upper part of the tube wall of the feed tube. The centrifuge tube can realize the connection and separation of the upper and lower parts of the centrifuge tube according to the magnitude of the centrifugal force generated by the piston when rotating at high speed, which can solve the problems of easy blockage of the diaphragm of the centrifuge tube and easy backflow of materials. However, because the movement of the piston is limited due to the incompressibility of the liquid material when the upper and lower parts of the centrifuge tube are separated; because the realization of the connection and separation 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 whole assembly larger, which is not conducive to realizing 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 pyrolysis liquid quality improvement and succinic acid or caproic acid extraction. The upper and lower parts of the centrifuge tube are connected and disconnected according to 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 disconnected through the cooperation between the on-off component and the timing locking component, thereby effectively realizing the miniaturized design of the centrifuge tube and solving the problems of easy blockage of the diaphragm of the centrifuge tube and easy remixing 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 an upper and lower part;

[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 in the discharge hole along the length direction of the tube body, so that the moving contact and the static contact are sealedly connected or disconnected, so as to realize the separation and connection of the upper and lower parts inside 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 outside 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 taken out from the inside of the tube body.

[0013] In some embodiments, a trigger pin is provided at the bottom of the moving contact; 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 into the centrifuge tube of the first aspect for centrifugation: during the centrifugation, the limiting piece moves downward in the feeding hole along the length direction of the centrifuge tube, so that the moving contact piece is disconnected from the static contact piece, so as to achieve communication between the upper and lower parts of the tube body, and obtain a centrifuge liquid;

[0015] After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body;

[0016] The upper centrifugal liquid is poured out from the top of the tube body; the moving contact is pressed to disconnect the moving 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.

[0017] In some embodiments, the method comprises the following steps: adding a sample into the centrifuge tube of the first aspect and centrifuging the sample; during the centrifugation, the limiting piece moves downward in the feeding hole along the length direction of the centrifuge tube, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body, and obtain the centrifuge liquid;

[0018] After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body;

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

[0020] In some embodiments, the method comprises the following steps: adding a sample into the centrifuge tube of the first aspect and centrifuging the sample; during the centrifugation, the limiting piece moves downward in the feeding hole along the length direction of the centrifuge tube, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body, and obtain the centrifuge liquid;

[0021] After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body;

[0022] The on-off assembly and the sleeve are taken out from the inside of the tube body to obtain the upper layer of centrifugal liquid; and the lower layer of centrifugal liquid is poured out from the top of the tube body.

[0023] In some embodiments, the centrifuge tube described in the first aspect is used, comprising the following steps: pressing the movable contact member to open the feed hole, and at the same time limiting the trigger pin in the limiting hole of the timing locking component; adding the sample to the centrifuge tube described in the first aspect, and centrifuging the timing locking component at the beginning 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, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body and obtain the centrifuge liquid;

[0025] When the timing locking time of the timing locking assembly ends, the limit of the trigger pin ends, and the limit piece moves upward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact piece is sealed and connected with the static contact piece, so as to realize 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 centrifugal liquid is poured out from the top of the tube; the moving contact is pressed to disconnect the moving contact from the static contact, so that the upper and lower parts of the tube are connected, and the lower 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 the 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] Or, when a sleeve tightly connected to the static contact is provided above the on-off assembly, the on-off assembly and the sleeve are taken out from the tube body to obtain the upper centrifugal liquid; and the lower centrifugal 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 pyrolysis liquid quality improvement and succinic acid or caproic acid extraction.

[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 assembly under the action of centrifugal force. The product structure is simple and compact, and it is easy to realize miniaturized design and mass production;

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

[0034] (4) The on-off state of the on-off component is controlled by a timing locking component, or the on-off state of the on-off component 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 It is a structural schematic diagram of a centrifuge tube of the present invention;

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

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

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

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

[0040] Figure 6 It is a structural schematic diagram of the static contact of the present invention;

[0041] Figure 7 It is a cross-sectional view of the stationary contact of the present invention along the AA direction;

[0042] Figure 8 It is a structural schematic diagram of the gasket of the present invention;

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

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

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

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

[0047] Fig.13 It is a cross-sectional view of the movable contact DD of the present invention;

[0048] Fig.14 It is a cross-sectional view of the movable contact member of the present invention along the EE direction;

[0049] Fig.15 It is a schematic diagram of the structure of the elastic band of the present invention;

[0050] Fig.16 It is a structural schematic diagram of the elastic band of the present invention when it is in working state;

[0051] Fig.17 is a top view of the elastic band of the present invention;

[0052] Fig.18 It is a structural schematic 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; gasket 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 removal 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 a switch assembly 2 located inside the tube body 1 and separating the tube body into two parts, the upper and lower 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 of the tube body 1 is provided with a top cover ( Figure 1 The top cover is provided with an internal top cover thread at the inner bottom position, and the internal top cover thread cooperates with the top external thread provided on the top outer wall of the tube body.

[0056] like Figure 3 As shown, the switch assembly 2 is composed of a static contact 5, an elastic band 10, a gasket 6, a bottom plate 7 and a dynamic contact 9; wherein the bottom plate 7 is connected to the gasket 6, and a flow hole 17 is provided on the bottom plate 7; the gasket 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 in the discharge hole 11 along the length direction of the tube body 1 to seal or disconnect the moving contact 9 and the static contact 5 to separate and connect 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, 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 feeding hole 11 is provided at the center of the stationary contact 5. Figure 7 As shown, the diameter of the static contact 5 is larger than the feed hole 11; the static contact 5 is used to keep the on-off assembly 2 tightly connected to the tube body 1; the feed hole 11 is used to cooperate with the limit plate 8 and the limit plate 8 can move up and down in the feed hole 11 along the length direction of the tube body 1, so that the dynamic contact 9 is sealedly connected or disconnected with the static contact 5, so as to realize the separation and connection between the upper and lower parts inside the tube body 1.

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

[0061] like Fig.10 As shown, the bottom plate 7 is a circular thin plate. Fig.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 Fig.12 As shown, a limit plate 8 is provided on the movable contact 9; Fig.13 As shown, the limiting piece 8 is located at the center of the moving contact 9; Fig.14 As shown, the moving contact 9 is a circular plate; the moving contact 9 is used to move up and down when subjected to force, driving the limit plate 8 to move up and down in the discharge hole 11 along the length direction of the tube body 1, so that the moving contact 9 is sealedly connected or disconnected with the static contact 5, controlling the connection and disconnection of the upper and lower parts of the tube body 1.

[0063] like Fig.15 As shown, the elastic band 10 is a rectangular elastic band; Fig.16 As shown, when the elastic band 10 is subjected to the 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 portion bends downward. Fig.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 bottom plate 7 are fixed together in sequence by 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 diameter of the feed hole 11 is 10mm. The static contact 5, washer 6 and bottom plate 7 are made of polypropylene, and the material of the elastic band 10 is made of rubber band. The thickness of the static contact 5, washer 6 and bottom plate 7 are 4mm, 10mm and 4mm respectively. The dynamic contact 9 is made of stainless steel 316L material, with a bottom diameter of 15mm, and the width of the limit plate 8 is 10mm.

[0065] The specification of the elastic band 10 is selected and determined by the centrifugal force used in the experiment. When the elastic band 10 is under the action of the centrifugal force and the centrifugal force is greater than the restoring force of the elastic band 10, the stopper 8 can move downward along the length direction of the tube body 1 in the discharge hole 11 to achieve the connection between the upper and lower parts of the tube body 1. The magnitude of the centrifugal force can be set according to the rotation speed, such as the moving contact 9 moves to open the on-off assembly 2 under the centrifugal state of more than 30000rpm (revolutions / minute), and close the on-off assembly 2 under the centrifugal state of less than 30000rpm.

[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 a metal spring sheet; the static contact 5, the elastic band 10, the gasket 6 and the bottom plate 7 are glued together in sequence using an 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 Fig.18 As shown, a hollow sleeve 18 tightly connected to the static contact 5 is provided above the on-off assembly 2, and 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 centrifugal 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 difference lies in that:

[0075] like Figure 5 As shown, a trigger pin 15 is connected to the bottom of the moving 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 at the bottom of 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 and mechanical timer, such as CN201620351704.8 a fan timer and fan, CN201920507464.X a timer that is noiseless after an alarm, CN200520014060.5 a washing machine washing timer or CN97206802.3 a full plastic timer for a fan, etc., without any other special structural requirements.

[0077] The centrifuge tube provided by the present invention has good application potential in scientific research and industrial production in the technical fields of oil quality improvement, biomedicine, isotope separation, isomer separation, gas separation, liquid propellant, supergravity separation, etc. The application of the centrifuge tube provided by the present invention in the quality improvement of pyrolysis liquid and the extraction of succinic acid or caproic acid is taken as an example to explain in detail the application effect of the centrifuge tube provided by the present invention. This application is only for example and is not limited to the application in the quality improvement of pyrolysis liquid and the extraction of succinic acid or caproic acid.

[0078] Example 5

[0079] The gas generated by the thermal decomposition of biomass is cooled and the obtained liquid is left to stand, and the 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 flocculent substances, and are brown to black in color. They have high phase stability and need 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. In order to compare the improvement effect of the pyrolysis solution, the transmittance of the pyrolysis solution was measured using an ultraviolet-visible spectrophotometer (model SP-752PC, Shanghai Spectrum Instrument Co., Ltd.), the working wavelength of the measurement was 550nm, a 1.0cm quartz cuvette was used, and air was used as a reference. The pyrolysis solution improvement process includes the following steps:

[0081] The process of preparing pyrolysis liquid by using a spiral propulsion pyrolysis furnace is as follows: using a spiral propulsion pyrolysis furnace with an inner diameter of 80 mm and a length of 3000 mm, heating by a resistance wire (rated power of 3.5 kW), temperature control by a thermostat, and an outer layer provided with a heat preservation layer; using corn stalks (water content of 10 wt%) with a length of less than 1 to 5 mm as a raw material, entering the spiral propulsion pyrolysis furnace at a speed of 3.0 kg / h, and a pyrolysis temperature of 550° C. After the liquid obtained by cooling the gas generated by the pyrolysis is allowed to stand, the upper clear liquid obtained 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 30000 rpm for 30 min at 5°C, the upper centrifuge liquid was poured out, the transmittance was measured to be 91.30%, the moving contact 9 was pressed and the lower centrifuge liquid was poured out through the on-off assembly 2 and used for the next centrifugation quality improvement.

[0083] 60 ml of the wood vinegar (transmittance 15.40%) prepared in the above process was added to the centrifuge tube, centrifuged at 30000 rpm for 30 min at 5°C, the upper centrifuge liquid was poured out, the transmittance was measured to be 94.56%, the moving contact 9 was pressed and the lower centrifuge liquid was poured out through the on-off assembly 2 and used for the next centrifugation quality improvement.

[0084] Example 6

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

[0086] The succinic acid fermentation liquid was added to a common centrifuge tube and centrifuged at 6000rpm for 10 minutes at 5°C to remove the bacteria, and the supernatant was obtained. The succinic acid concentration was 33.15 g / L as determined by gas chromatography. 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; 60 mL of the succinic acid supernatant was added to the centrifuge tube, and centrifuged at 30000rpm for 30 minutes at 5°C, the upper centrifuge liquid was poured out and used for further fermentation, and the bottom cover was removed to obtain the lower centrifuge liquid. The succinic acid concentration in the lower centrifuge liquid was determined to be 48.65 g / L, and the lower centrifuge liquid was used for the next step of extracting succinic acid.

[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 take out and the operation is more convenient.

[0088] Example 7

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

[0090] The caproic acid fermentation liquid was added to a common centrifuge tube and centrifuged at 6000 rpm for 10 min at 5°C to remove the bacteria, and a supernatant was obtained. The caproic acid concentration was 17.24 g / L as determined by gas chromatography. 60 mL of the caproic acid supernatant was added to the centrifuge tube described in this embodiment, and centrifuged at 30000 rpm for 30 min at 5°C to obtain an upper centrifuge liquid. The caproic acid concentration was determined to be 21.15 g / L. The upper centrifuge liquid was used for the next step of extracting caproic acid; the on-off assembly 2 and the sleeve 18 can be removed from the tube body 1 to obtain a lower centrifuge liquid for continued fermentation.

[0091] Example 8

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

[0093] The process of preparing pyrolysis liquid by using a spiral propeller pyrolysis furnace is as follows: dry avermectin residue (water content is 2.1wt%) is used as raw material, enters the spiral propeller pyrolysis furnace at a speed 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, and the obtained 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 moving 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 is removed and a hollow rubber ball with an outer diameter of 6 mm is placed in it, and the bottom cover is installed; the moving contact 9 is pressed to open the feed hole 11, and at the same time, the trigger pin 15 is limited in the limiting hole 14 of the timing locking component 16; 60 ml of wood tar (transmittance 10.17%) is added to the centrifuge tube, centrifuged at 30000 rpm for 30 min at 5°C, the upper centrifuge liquid is poured out, and the transmittance is measured to be 90.05%; the on-off component 2 and the sleeve 18 can be taken out 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 is removed and a hollow rubber ball with an outer diameter of 6 mm is placed in it, and the bottom cover is installed; the moving contact 9 is pressed to open the feed hole 11, and at the same time, the trigger pin 15 is limited in the limiting hole 14 of the timing locking component 16; 60 ml of wood vinegar (transmittance 15.03%) is added to the centrifuge tube, centrifuged at 30000 rpm for 30 min at 5°C, the upper centrifuge liquid is poured out, and the transmittance is measured to be 92.24%; the on-off component 2 and the sleeve 18 can be taken out from the tube body 1 to obtain the lower centrifuge liquid and use it for the next centrifugation quality improvement.

[0098] Comparative Example 1

[0099] The similarities between this embodiment and embodiment 5 are not repeated here, and the difference lies in that:

[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 centrifuged at 30000 rpm for 30 min at 5°C. The upper centrifuge liquid was poured out and the transmittance was measured to be 65.20%.

[0102] By comparing Example 1 with Comparative Example 5, it can be seen that the use of the centrifuge tube provided in Example 1 of the present invention greatly increases the light 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 succinic acid supernatant (succinic acid concentration is 33.15 g / L) was added to an ordinary centrifuge tube, 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 with Comparative Example 6, it can be seen that the centrifuge tube provided by Example 1 of the present invention can greatly increase 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 difference lies in that:

[0109] 60 mL of caproic acid supernatant (caproic acid concentration is 17.24 g / L) was added to an ordinary centrifuge tube, centrifuged at 30000 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 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 is used to increase the concentration of caproic acid, which can reduce the energy consumption and cost of subsequent extraction of caproic acid.

[0111] The above description is only a preferred embodiment of the present invention. The embodiments are all intermittent centrifugal operations, and the on-off assembly arranged in the centrifuge tube is only one, which is not used to limit the present invention. For those skilled in the art, the present invention can have various changes and variations. For example, the centrifuge tube of the present invention can be used for continuous centrifugal operation, or multiple on-off assemblies can be arranged in the centrifuge tube. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope 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 dividing the pipe body into two parts, an upper part and a 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 in the discharge hole along the length direction of the tube body, so that the moving contact and the static contact are sealedly connected or disconnected, so as to realize the separation and connection of the upper and lower parts inside the tube body.

2. The centrifuge tube according to claim 1, characterized in that: 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, characterized in that: 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 outside 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, characterized in that: A sleeve is arranged above the static contact, and the switch assembly and the sleeve can be taken out from the inside of the tube body.

5. The centrifuge tube according to any one of claims 2 to 4, characterized in that: A trigger pin is provided at the bottom of the moving contact; an elastic hole is provided at the elastic belt; a pin hole is provided at the bottom plate, and the bottom of the bottom plate is connected with the gasket and the timing locking assembly in sequence; a limiting hole is provided at the timing locking assembly; the trigger pin passes through the elastic hole, the pin hole, the gasket and the limiting hole in sequence.

6. A method for using a centrifuge tube, characterized in that: The following steps are involved: Add the sample into the centrifuge tube of claim 2 and centrifuge it: during the centrifugation, the limiting piece moves downward in the feeding hole along the length direction of the centrifuge tube, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body, and obtain the centrifuge liquid; After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body; The upper centrifugal liquid is poured out from the top of the tube body; the moving contact is pressed to disconnect the moving 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. A method for using a centrifuge tube, characterized in that: The following steps are involved: Add the sample into the centrifuge tube of claim 3 and centrifuge it: during the centrifugation, the limit plate moves downward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body, and obtain the centrifuge liquid; After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body; Pour the upper centrifugal liquid out from the top of the tube body; remove the bottom cover at the bottom of the tube body to pour the lower centrifugal liquid out from the bottom of the tube body.

8. A method for using a centrifuge tube, characterized in that: The following steps are involved: Add the sample into the centrifuge tube of claim 4 and centrifuge it: during the centrifugation, the limit plate moves downward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact member is disconnected from the static contact member, so as to achieve the connection between the upper and lower parts of the tube body, and obtain the centrifuge liquid; After the 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 piece is sealed and connected with the static contact piece, so as to separate the upper and lower parts of the tube body; The on-off assembly and the sleeve are taken out from the inside of the tube body to obtain the upper layer of centrifugal liquid; and the lower layer of centrifugal liquid is poured out from the top of the tube body.

9. A method for using a centrifuge tube, characterized in that: The centrifuge tube of claim 5 is used, comprising the following steps: pressing the moving contact to open the feed hole, and at the same time limiting the trigger pin in the limiting hole of the timing locking component; adding the sample into the centrifuge tube of claim 5, and centrifuging the timing locking component at the beginning 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, so that the moving contact piece is disconnected from the static contact piece, so as to achieve the connection between the upper and lower parts of the tube body and obtain the centrifuge liquid; When the timing locking time of the timing locking assembly ends, the limit of the trigger pin ends, and the limit piece moves upward in the discharge hole along the length direction of the centrifuge tube, so that the moving contact piece is sealed and connected with the static contact piece, so as to realize the separation of the upper and lower parts of the tube body; When the bottom of the tube is closed and the top is open, the upper centrifugal liquid is poured out from the top of the tube; the moving contact is pressed to disconnect the moving contact from the static contact, so that the upper and lower parts of the tube are connected, and the lower centrifugal liquid is poured out from the top of the tube; Or, when the bottom of the tube body is open and used in conjunction with the 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; Or, when a sleeve tightly connected to the static contact is provided above the on-off assembly, the on-off assembly and the sleeve are taken out from the tube body to obtain the upper centrifugal liquid; and the lower centrifugal liquid is poured out from the top of the tube body.

10. Use of the centrifuge tube according to any one of claims 1 to 5, characterized in that: The applications include but are not limited to applications in pyrolysis liquid upgrading and succinic acid or caproic acid extraction.

Images