CN115253982A - Purification equipment and method for moxidectin - Google Patents
Purification equipment and method for moxidectin Download PDFInfo
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- CN115253982A CN115253982A CN202211023406.2A CN202211023406A CN115253982A CN 115253982 A CN115253982 A CN 115253982A CN 202211023406 A CN202211023406 A CN 202211023406A CN 115253982 A CN115253982 A CN 115253982A
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- driving
- moxidectin
- reaction barrel
- piece
- rotating
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- YZBLFMPOMVTDJY-CBYMMZEQSA-N moxidectin Chemical compound O1[C@H](C(\C)=C\C(C)C)[C@@H](C)C(=N/OC)\C[C@@]11O[C@H](C\C=C(C)\C[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 YZBLFMPOMVTDJY-CBYMMZEQSA-N 0.000 title claims abstract description 75
- 229960004816 moxidectin Drugs 0.000 title claims abstract description 75
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 91
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 38
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 34
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 238000002347 injection Methods 0.000 claims abstract description 23
- 239000007924 injection Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims description 21
- 239000013078 crystal Substances 0.000 claims description 18
- 238000010828 elution Methods 0.000 claims description 13
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 230000003028 elevating effect Effects 0.000 claims 2
- 238000002156 mixing Methods 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 5
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 235000006708 antioxidants Nutrition 0.000 description 23
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- AZSNMRSAGSSBNP-UHFFFAOYSA-N 22,23-dihydroavermectin B1a Natural products C1CC(C)C(C(C)CC)OC21OC(CC=C(C)C(OC1OC(C)C(OC3OC(C)C(O)C(OC)C3)C(OC)C1)C(C)C=CC=C1C3(C(C(=O)O4)C=C(C)C(O)C3OC1)O)CC4C2 AZSNMRSAGSSBNP-UHFFFAOYSA-N 0.000 description 2
- SPBDXSGPUHCETR-JFUDTMANSA-N 8883yp2r6d Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O[C@@H]([C@@H](C)CC4)C(C)C)O3)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1C[C@H](C)[C@@H]([C@@H](C)CC)O[C@@]21O[C@H](C\C=C(C)\[C@@H](O[C@@H]1O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C1)[C@@H](C)\C=C\C=C/1[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\1)O)C[C@H]4C2 SPBDXSGPUHCETR-JFUDTMANSA-N 0.000 description 2
- 239000005660 Abamectin Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 230000000507 anthelmentic effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 229960002418 ivermectin Drugs 0.000 description 2
- 239000003120 macrolide antibiotic agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- UIAGMCDKSXEBJQ-IBGZPJMESA-N 3-o-(2-methoxyethyl) 5-o-propan-2-yl (4s)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate Chemical class COCCOC(=O)C1=C(C)NC(C)=C(C(=O)OC(C)C)[C@H]1C1=CC=CC([N+]([O-])=O)=C1 UIAGMCDKSXEBJQ-IBGZPJMESA-N 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000244206 Nematoda Species 0.000 description 1
- 241000187747 Streptomyces Species 0.000 description 1
- 230000002141 anti-parasite Effects 0.000 description 1
- 239000003096 antiparasitic agent Substances 0.000 description 1
- 229940125687 antiparasitic agent Drugs 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013058 crude material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 244000078703 ectoparasite Species 0.000 description 1
- 239000012156 elution solvent Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229940041033 macrolides Drugs 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- FXWHFKOXMBTCMP-WMEDONTMSA-N milbemycin Natural products COC1C2OCC3=C/C=C/C(C)CC(=CCC4CC(CC5(O4)OC(C)C(C)C(OC(=O)C(C)CC(C)C)C5O)OC(=O)C(C=C1C)C23O)C FXWHFKOXMBTCMP-WMEDONTMSA-N 0.000 description 1
- ZLBGSRMUSVULIE-GSMJGMFJSA-N milbemycin A3 Chemical class O1[C@H](C)[C@@H](C)CC[C@@]11O[C@H](C\C=C(C)\C[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 ZLBGSRMUSVULIE-GSMJGMFJSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/22—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains four or more hetero rings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to the technical field of medicine processing, and particularly discloses equipment and a method for purifying moxidectin. The technical scheme of the invention is that a controller controls a solvent to enter the interior of a reaction barrel through a solvent injection port according to a preset amount; the rotary driving piece searches a preset feeding proportion-reverse driving quantity information table according to a preset feeding proportion to obtain reverse driving quantity; the reverse driving quantity of the rotary driving piece is consistent with that of the reverse driving; the rotary driving piece positively drives the rotary shaft to rotate, and the driving disc rotates to complete feeding of the Moxidectin crude product and the antioxidant through the first driven piece and the second driven piece; stirring and adding a dissolving agent, and then cooling and precipitating. And finally, forming negative pressure inside the reaction barrel for drying. The invention can complete automatic feeding, mixing, cooling and drying, realizes automatic purification, has simple device structure and improves processing efficiency.
Description
Technical Field
The invention relates to the technical field of medicine processing, in particular to equipment and a method for purifying moxidectin.
Background
Moxidectin is a semi-synthetic single-component macrolide antibiotic generated by streptomyces fermentation, and is a derivative of nimodipine. Macrolides antiparasitics consist of two major classes, namely avermectins and milbemycins. Compared with ivermectin and avermectin, moxidectin has the characteristics of wider insect expelling activity, long-acting property, safety and the like. In the middle of the 80's of the 20 th century, moxidectin began to be used as an anthelmintic for animals. As a new generation of anthelmintic, moxidectin can efficiently kill nematodes and ectoparasites, and has good safety to animals. It is superior to ivermectin in medicine dosage, form development, medicine resistance, medicine distribution in body, etc.
The currently known moxidectin purification method comprises the steps of adding water into a solution of moxidectin and methylcyclohexane, and stirring vigorously for a plurality of days to obtain a white moxidectin precipitate. The method has long time consumption and low yield, and each operation needs a plurality of devices to be matched, so the devices are complex and the operation is complicated.
Disclosure of Invention
In order to solve the technical problem, the invention provides a moxidectin purification device, which comprises:
a reaction barrel; a rotating shaft is rotatably arranged in the reaction barrel, the top of the rotating shaft extends out of the reaction barrel, the rotating shaft is of a hollow structure, a temperature regulating agent injection connecting valve is arranged at the end part of the rotating shaft, and the temperature regulating agent injection connecting valve is used for being communicated with a circulating heating and refrigerating device; the rotating shaft is fixedly connected with a plurality of fan blades, the fan blades are positioned in the reaction barrel, flow channels are formed in the fan blades, and the flow channels are communicated with the temperature regulating agent injection connecting valve;
the rotary driving piece is used for driving the rotating shaft to rotate; the reaction barrel is communicated with a solvent injection port, and a valve is arranged on the solvent injection port; the reaction barrel is also communicated with a vacuumizing tube, and the vacuumizing tube is provided with a valve; a dissolving agent box is fixedly arranged on the outer wall of the reaction barrel, the dissolving agent box is communicated with the reaction barrel and is provided with a valve, and a dissolving agent is contained in the dissolving agent box;
the raw material box is fixedly arranged on the reaction barrel, the interior of the raw material box is used for containing a Moxidectin crude product, the bottom of the raw material box is provided with a valve and a first driven part, and a driving disc is arranged on a rotating shaft; an antioxidant box is fixedly arranged on the reaction barrel and is used for containing an antioxidant; the bottom of the antioxidant box is provided with a valve and a second driven part, the first driven part and the second driven part are provided with spiral blades, and the two spiral blades are respectively positioned in the raw material box and the antioxidant box; the driving disc is driven by the rotating shaft to rotate so that the first driven part and the second driven part rotate, and the spiral blades rotate in the raw material box and the antioxidant box, so that the raw moxidectin product and the antioxidant are fed; the bottom of the reaction barrel is provided with a discharge port, and a control valve is arranged on the discharge port;
a pressure sensing member for sensing a pressure inside the reaction tub;
the controller is electrically connected or wirelessly connected with the rotary driving piece and each valve of the pressure sensing piece; the controller controls the solvent to enter the reaction barrel through the solvent injection port according to a preset amount; the rotary driving piece searches a preset feeding proportion-reverse driving quantity information table according to a preset feeding proportion to obtain reverse driving quantity; the reverse driving amount of the rotary driving piece is consistent with the reverse driving amount; the rotary driving piece positively drives the rotary shaft to rotate, and the driving disc rotates to complete feeding of the Moxidectin crude product and the antioxidant through the first driven piece and the second driven piece; controlling the temperature to be 60-80 ℃ to dissolve the moxidectin; the dissolving agent in the dissolving agent box enters the reaction barrel, and the driving piece is continuously rotated to positively rotate for a preset stirring time period; rotating a driving piece to positively drive a rotating shaft to stir and controlling the temperature to be 0-20 ℃ to obtain moxidectin crystals; the control valve opens a preset opening to discharge the solution, and the moxidectin crystal is remained in the reaction barrel; negative pressure is formed inside the reaction barrel, and when the pressure sensing piece senses that the pressure inside the reaction barrel is smaller than a preset pressure, the controller enables the pressure inside the reaction barrel to be maintained for a preset drying time period; the control valve is opened to discharge the moxidectin crystals.
Preferably: the bottom of reaction bucket fixedly be provided with the base, the base supports the reaction bucket, the bottom of base is provided with universal wheel and/or the wheel that rolls, is provided with the cardboard that is used for the braking on universal wheel and/or the wheel that rolls.
Preferably, the following components: the side wall of the elution agent box is provided with an observation window, scale marks can be marked on the observation window, and the amount of elution agent in the elution agent box can be observed through the scale marks.
Preferably: the driving disc is of a disc structure with conical upper and lower surfaces, a rotating lifting driving piece is arranged between the driving disc and the rotating shaft, the rotating lifting driving piece completes the rotating driving of the driving disc through forward rotation, and the reverse rotation completes the lifting adjustment of the driving disc.
Preferably: first follower and second follower all include the rotating tube, the elastic expansion link, the rotating tube rotates the bottom of connecting at raw materials case or anti-oxidant case, and with spiral leaf fixed connection, all radial fixedly connected with a plurality of protrusions on the upper and lower conical surface of driving-disc, the radial fixedly connected with of lateral wall of rotating tube is a plurality of elastic expansion links, first follower and second follower are in the last downside of driving-disc respectively and contact with the upper and lower face of driving-disc, the driving-disc goes up and down to adjust the contact point radial position of elastic expansion link and driving-disc, with this rotational speed proportion of adjusting first follower and second follower, further regulation moxidectin crude and the feeding proportion of anti-oxidant.
Preferably, the following components: elasticity telescopic link including fixed outer tube, movable rod and spring, fixed outer tube radial fixed connection is at the outer wall of rotating-tube, the slip chamber has been seted up to the inside of rotating-tube, the one end of movable rod slides and imbeds the inside in slip chamber, the inside in slip chamber is provided with the spring, the spring makes the movable rod outwards slide.
Preferably, the following components: the rotation lift driving piece include the outer tube, unidirectional rotation cover and circulation groove, unidirectional rotation cover unidirectional rotation nestification is in the axis of rotation, outer tube fixed connection is in the axis position of driving-disc, the one-way bearing of tip fixedly connected with of outer tube, the slip nestification of one-way bearing liftable is in the axis of rotation, the outer tube nestification is in the periphery of unidirectional rotation cover, the transmission opposite direction of one-way bearing and unidirectional rotation cover, the inner wall rotation of outer tube is provided with the ball, the circulation groove has been seted up to the outer wall of unidirectional rotation cover, the ball rotates the inside of nestification in the circulation groove, rotate the rotation of drive unidirectional rotation cover through the axis of rotation, the inside lift of unidirectional rotation cover rotation drive ball relative circulation inslot.
Preferably: the circulating groove comprises a spiral groove and a connecting groove, the spiral groove forms axial displacement, and the end parts of the spiral groove are communicated in a smooth transition mode through the connecting groove.
Preferably: the inside of circulation groove be provided with presses the inductor, press the inductor and be used for responding to the pressure of ball, when pressing the inductor and sensing the pressure of ball, the height of driving-disc is in initial condition.
The invention also provides a purification method of moxidectin, which is applied to the purification equipment of moxidectin, and the purification method of moxidectin comprises the following steps:
s1, allowing a solvent to enter a reaction barrel through a solvent injection port according to a preset amount;
s2, the rotary driving piece searches a preset feeding proportion-reverse driving quantity information table according to a preset feeding proportion to obtain reverse driving quantity;
s3, the reverse driving amount of the rotary driving piece is consistent with the reverse driving amount;
s4, the rotating driving piece positively drives the rotating shaft to rotate, and the driving disc rotates to complete feeding of the Moxidectin crude product and the antioxidant through the first driven piece and the second driven piece;
s5, controlling the temperature to dissolve the moxidectin at 60-80 ℃;
s6, enabling the dissolving agent in the dissolving agent box to enter the reaction barrel, and continuously rotating the driving piece to rotate forwards for a preset stirring time period;
s7, rotating the driving piece to positively drive the rotating shaft to stir and controlling the temperature to be 0-20 ℃ to obtain Moxidectin crystals;
s8, opening a preset opening by the control valve to discharge the solution, and leaving the moxidectin crystal in the reaction barrel;
s9, forming negative pressure inside the reaction barrel, and when the pressure sensing piece senses that the pressure inside the reaction barrel is smaller than a preset pressure, enabling the pressure inside the reaction barrel to be maintained for a preset drying time period by the controller;
and S10, opening a control valve to discharge the moxidectin crystals.
The invention has the technical effects and advantages that: the invention can complete automatic feeding, mixing, cooling and drying, realizes automatic purification, has simple device structure and improves the processing efficiency. The rotation of the driving disc is changed through the forward and reverse driving of the rotary driving piece to complete feeding and reverse adjustment of the feeding proportion, the control is convenient and fast, the structure is simple, and energy is saved.
Drawings
FIG. 1 is a schematic perspective view of a purification apparatus for moxidectin provided in the present invention.
FIG. 2 is a schematic top view of a purification apparatus for moxidectin according to the present invention.
Fig. 3 isbase:Sub>A partial sectional structural view ofbase:Sub>A sectionbase:Sub>A-base:Sub>A in fig. 2.
Fig. 4 is a schematic view of a combination structure of a driving disc, a first driven member and a second driven member in the purification apparatus of moxidectin provided in the present invention.
FIG. 5 is a schematic structural diagram of a rotary lifting driving member in the purification equipment of moxidectin provided by the present invention.
Fig. 6 is a partially enlarged structural diagram of a in fig. 3.
FIG. 7 is a flow chart of a purification method of moxidectin provided in the present invention.
Description of reference numerals: the device comprises a base 1, a mixing barrel body 2, a solvent dissolving agent box 3, a solvent injection port 4, a cover plate 5, a raw material box 6, a temperature adjusting agent injection connecting valve 7, a rotary driving piece 8, an antioxidant box 9, a vacuumizing pipe 10, a discharge port 11, a control valve 12, a rotary shaft 13, fan blades 14, spiral blades 15, a first driven piece 16, a driving disc 17, a second driven piece 18, a protrusion 19, a rotary pipe 20, a fixed outer pipe 21, a movable rod 22, an outer sleeve 23, a one-way bearing 24, a ball 25, a spiral groove 26, a pressing inductor 27, a connecting groove 28, a one-way rotating sleeve 29 and a spring 30.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Example 1
Referring to fig. 1 to fig. 3, in this embodiment, a moxidectin purifying apparatus is provided for processing and purifying crude moxidectin, the moxidectin purifying apparatus includes:
the reaction barrel can be of a cylindrical structure and can be made of stainless steel materials, so that certain rigidity is guaranteed, a sealed space is formed inside the reaction barrel, and the moxidectin crude product is purified inside the sealed space. The reaction barrel can comprise a mixing barrel body 2 and a cover plate 5, wherein the mixing barrel body 2 is of a cylinder structure, the cover plate 5 is of a disc structure, and the cover plate 5 can be fixed on the top of the mixing barrel body 2 through bolts or buckles, so that the reaction barrel is formed. The cover plate 5 may be formed by splicing and combining two semicircular plate-shaped structures, so as to facilitate the disassembly and assembly of the cover plate 5, which is not described herein. The fixed base 1 that is provided with in bottom of reaction barrel, base 1 can be square font structure, and base 1 supports the reaction barrel, and the bottom of base 1 can also be provided with universal wheel and/or the wheel that rolls, and the wheel that rolls here is the wheel that can not change direction, is provided with the cardboard that is used for the braking on universal wheel and/or the wheel that rolls to be convenient for be used for moxidectin's purification equipment's removal and fixed.
The inside of reaction barrel rotates and is provided with axis of rotation 13, and the reaction barrel is stretched out at the top of axis of rotation 13, and axis of rotation 13 is hollow structure and tip are provided with tempering agent and pour into connecting valve 7, and axis of rotation 13 can pour into connecting valve 7 through the tempering agent and communicate circulation heating refrigerating plant, and circulation heating refrigerating plant is additional equipment, and circulation heating refrigerating plant can circulate the mobile condensate and the heating fluid of drive, heats or cools off through the inside that drives condensate or heating fluid inflow rotation axis 13. The circulation heating and cooling device is the prior art, and is not described herein. The rotating shaft 13 is fixedly connected with a plurality of fan blades 14, the fan blades 14 are located inside the reaction barrel, a flow channel is formed in the fan blades 14 and is communicated with the temperature adjusting agent injection connecting valve 7, condensate and heating liquid can enter the flow channel, so that the fan blades 14 have a heat exchange function, and under the stirring of the fan blades 14, a solvent in the reaction barrel can flow relative to the fan blades 14, the heat exchange efficiency is improved, and the reaction temperature control sensitivity is improved. Of course, heating wires or condensing pipes may be disposed inside the reaction barrel, which is not described herein.
The rotary driving member 8 can be installed on the reaction barrel for driving the rotation shaft 13 to rotate, and the rotary driving member 8 can be a motor or a combination structure of the motor and the belt pulley, which is not described herein. The reaction barrel can be communicated and provided with a solvent injection port 4, the solvent injection port 4 is provided with a valve which can be communicated with a solvent source and a driving pump, the solvent can be quantitatively added into the reaction barrel through the driving pump, and the solvent can be methanol, ethanol, normal propyl alcohol or isopropyl alcohol and the like, and is not specifically described herein. The reaction barrel is further communicated with a vacuum-pumping tube 10, the vacuum-pumping tube 10 is provided with a valve and communicated with a vacuum pump or a negative pressure source, and the vacuum state inside the reaction barrel can be controlled through the vacuum-pumping tube 10, which is not described herein in detail. The outer wall of reaction barrel is fixed with elution agent case 3, and elution agent case 3 communicates and is provided with the valve with the reaction barrel to can communicate with external pneumatic pump or high-pressure air supply, the inside of elution agent case 3 is used for holding the elution agent. The gas pressure is driven by the gas pressure pump to feed the elution reagent in the elution reagent tank 3 into the reaction tank. The observation window can be seted up to the lateral wall of the solvent case 3, can observe the condition of the inside solvent of solvent case 3 through the observation window, can be impressed scale mark on the observation window, can observe the volume of the inside solvent of solvent case 3 through the scale mark. The elution reagent tank 3 is provided with an injection port through which the elution reagent can be injected into the elution reagent tank 3. The elution solvent may be n-heptane or n-hexane, and is not described herein in detail. By sealing the elutant tank 3, the elutant is prevented from volatilizing. The bottom of reaction barrel has seted up bin outlet 11, is provided with control valve 12 on the bin outlet 11, and bin outlet 11 is used for the row material, and control valve 12 is used for controlling the switch of bin outlet 11.
The forced induction spare can be installed in the inside of reaction barrel for the inside pressure of response reaction barrel, and forced induction spare is prior art, specifically does not describe here any more.
And the controller can be electrically connected with the rotary driving piece 8 and each valve of the pressure sensing piece or wirelessly connected with the rotary driving piece and each valve of the pressure sensing piece. The controller controls the solvent to enter the reaction barrel through the solvent injection port 4 according to a preset amount, and the rotary driving member 8 searches a preset feeding proportion-reverse driving amount information table according to a preset feeding proportion, so as to obtain the reverse driving amount. The controller controls the rotary drive member 8 to be back-driven by the same amount as the back-driving amount. The controller controls the rotary driving piece 8 to positively drive the rotary shaft 13 to rotate, the driving disc 17 rotates to complete feeding of the moxidectin crude product and the antioxidant through the first driven piece 16 and the second driven piece 18, and the controller controls the temperature to be 60-80 ℃ so that the moxidectin is dissolved. The eluent in the eluent box 3 enters the reaction barrel and continues to rotate the driving member 8 forward for a preset stirring period. The rotating shaft 13 is driven by the rotating driving piece 8 in the positive direction to stir and control the temperature to be 0-20 ℃ to obtain the moxidectin crystals. The controller control valve 12 opens a predetermined trompil and makes the solution discharge, and the moxidectin crystal is stayed in the inside of reaction vessel, and the inside negative pressure that forms of reaction vessel is controlled to the controller, and when the pressure response piece sensed that the inside pressure of reaction vessel is less than a predetermined pressure, the controller made the inside pressure of reaction vessel maintain a predetermined dry time period, and controller control valve 12 is opened and is discharged the moxidectin crystal. The invention can complete automatic feeding, mixing, cooling and drying, realizes automatic purification, has simple device structure and improves processing efficiency. The rotation of the driving disc 17 is changed through the forward and reverse driving of the rotary driving piece 8 to complete the feeding and the adjustment of the feeding proportion reversely, the control is convenient and fast, the structure is simple, and the energy is saved.
Example 2
Referring to fig. 7, a purification method of moxidectin includes the following steps:
s1, a solvent enters the reaction barrel through a solvent injection port 4 according to a preset amount.
S2, the rotary driving piece 8 searches a preset feeding proportion-reverse driving quantity information table according to a preset feeding proportion to obtain reverse driving quantity.
And S3, the reverse driving amount of the rotary driving piece 8 is consistent with the reverse driving amount.
S4, the rotating driving piece 8 positively drives the rotating shaft 13 to rotate, and the driving disc 17 rotates to complete feeding of the moxidectin crude product and the antioxidant through the first driven piece 16 and the second driven piece 18.
S5, controlling the temperature to dissolve the moxidectin at the temperature of 60-80 ℃.
S6, the dissolving agent in the dissolving agent box 3 enters the reaction barrel, and the driving piece 8 is continuously rotated to rotate forwards for a preset stirring time period.
S7, positively driving the rotating shaft 13 to stir by the rotating driving piece 8, and controlling the temperature to be 0-20 ℃ to obtain the moxidectin crystals.
S8, opening a preset opening by the control valve 12 to discharge the solution, and leaving the moxidectin crystals in the reaction barrel.
S9, negative pressure is formed inside the reaction barrel, and when the pressure sensing piece senses that the pressure inside the reaction barrel is smaller than a preset pressure, the controller enables the pressure inside the reaction barrel to be maintained for a preset drying time period.
S10, opening the control valve 12 to discharge the Moxidectin crystals.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by one of ordinary skill in the art and related arts based on the embodiments of the present invention without any creative effort, shall fall within the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are not specifically illustrated or described, but are instead contemplated to be practiced in the art by those skilled in the art.
Claims (10)
1. The equipment for purifying moxidectin is characterized by comprising the following steps:
a reaction barrel; a rotating shaft is rotatably arranged in the reaction barrel, the top of the rotating shaft extends out of the reaction barrel, the rotating shaft is of a hollow structure, a temperature regulating agent injection connecting valve is arranged at the end part of the rotating shaft, and the temperature regulating agent injection connecting valve is used for communicating the circulating heating and refrigerating device; a plurality of fan blades are fixedly connected to the rotating shaft, the fan blades are positioned in the reaction barrel, flow channels are formed in the fan blades, and the flow channels are communicated with a temperature regulating agent injection connecting valve;
the rotary driving piece is used for driving the rotating shaft to rotate; the reaction barrel is communicated with a solvent injection port, and a valve is arranged on the solvent injection port; the reaction barrel is also communicated with a vacuumizing tube, and the vacuumizing tube is provided with a valve; the outer wall of the reaction barrel is fixedly provided with a solventing-out agent box, the solventing-out agent box is communicated with the reaction barrel and is provided with a valve, and the interior of the solventing-out agent box is used for containing a solventing-out agent;
the raw material box is fixedly arranged on the reaction barrel, the interior of the raw material box is used for containing a crude moxidectin product, the bottom of the raw material box is provided with a valve and a first driven part, and a driving disc is arranged on a rotating shaft; an antioxidant box is fixedly arranged on the reaction barrel and is used for containing an antioxidant; the bottom of the antioxidant box is provided with a valve and a second driven part, the first driven part and the second driven part are provided with spiral blades, and the two spiral blades are respectively positioned in the raw material box and the antioxidant box; the driving disc is driven by the rotating shaft to rotate so that the first driven part and the second driven part rotate, and the spiral blades rotate in the raw material box and the antioxidant box, so that the raw moxidectin product and the antioxidant are fed; the bottom of the reaction barrel is provided with a discharge outlet, and a control valve is arranged on the discharge outlet;
a pressure sensing member for sensing a pressure inside the reaction tub;
the controller is electrically connected with the valves of the rotary driving piece and the pressure sensing piece or wirelessly connected with the valves of the rotary driving piece and the pressure sensing piece; the controller controls the solvent to enter the reaction barrel through the solvent injection port according to a preset amount; the rotary driving piece searches a preset feeding proportion-reverse driving quantity information table according to a preset feeding proportion to obtain reverse driving quantity; the reverse driving amount of the rotary driving piece is consistent with the reverse driving amount; the rotary driving piece positively drives the rotary shaft to rotate, and the driving disc rotates to complete feeding of the Moxidectin crude product and the antioxidant through the first driven piece and the second driven piece; controlling the temperature to be 60-80 ℃ to dissolve the moxidectin; the dissolving agent in the dissolving agent box enters the reaction barrel, and the driving piece is continuously rotated to positively rotate for a preset stirring time period; rotating the driving piece to positively drive the rotating shaft to stir and controlling the temperature to be 0-20 ℃ to obtain moxidectin crystals; the control valve opens a preset opening to discharge the solution, and the moxidectin crystal is left in the reaction barrel; negative pressure is formed inside the reaction barrel, and when the pressure sensing piece senses that the pressure inside the reaction barrel is smaller than a preset pressure, the controller enables the pressure inside the reaction barrel to be maintained for a preset drying time period; the control valve is opened to discharge the moxidectin crystals.
2. The apparatus for purifying moxidectin according to claim 1, wherein a base is fixedly arranged at the bottom of the reaction barrel and supports the reaction barrel, universal wheels and/or rolling wheels are arranged at the bottom of the base, and clamping plates for braking are arranged on the universal wheels and/or the rolling wheels.
3. The apparatus for purifying moxidectin according to claim 1, wherein an observation window is formed on the side wall of the elution agent box, and scale lines are marked on the observation window.
4. The apparatus for purifying moxidectin according to claim 1, wherein the driving disk is a disk structure with conical upper and lower surfaces, a rotary lifting driving member is arranged between the driving disk and the rotating shaft, the rotary lifting driving member completes the rotary driving of the driving disk through forward rotation, and the reverse rotation completes the lifting adjustment of the driving disk.
5. The apparatus of claim 4, wherein the first and second driven members comprise a rotating tube and an elastic telescopic rod; the rotating pipe is rotatably connected to the bottom of the raw material box or the antioxidant box and is fixedly connected with the spiral blade; the upper conical surface and the lower conical surface of the driving disc are respectively fixedly connected with a plurality of bulges in the radial direction, the outer side wall of the rotating tube is fixedly connected with a plurality of elastic telescopic rods in the radial direction, the first driven piece and the second driven piece are respectively positioned on the upper side and the lower side of the driving disc and are in contact with the upper surface and the lower surface of the driving disc, the driving disc is lifted to adjust the radial position of a contact point of each elastic telescopic rod and the driving disc, so that the rotating speed ratio of the first driven piece and the second driven piece is adjusted, and the feeding ratio of the Moxidectin crude product and the antioxidant is adjusted.
6. The apparatus for purifying moxidectin according to claim 5, wherein the elastic telescopic rod comprises a fixed outer tube, a movable rod and a spring, the fixed outer tube is radially and fixedly connected to the outer wall of the rotating tube, a sliding cavity is formed inside the rotating tube, one end of the movable rod is slidably embedded into the sliding cavity, the spring is arranged inside the sliding cavity, and the movable rod slides outwards due to the spring.
7. The apparatus for purifying moxidectin according to claim 4, wherein the rotary elevating driving member comprises an outer sleeve, a unidirectional rotating sleeve and a circulating slot, the unidirectional rotating sleeve is nested on the rotating shaft in a unidirectional rotating manner, the outer sleeve is fixedly connected to the axial position of the driving disk, a unidirectional bearing is fixedly connected to the end of the outer sleeve, the unidirectional bearing is nested on the rotating shaft in a sliding manner and capable of elevating, the outer sleeve is nested on the periphery of the unidirectional rotating sleeve, the transmission directions of the unidirectional bearing and the unidirectional rotating sleeve are opposite, balls are arranged on the inner wall of the outer sleeve in a rotating manner, the circulating slot is formed in the outer wall of the unidirectional rotating sleeve, the balls are nested inside the circulating slot in a rotating manner, the unidirectional rotating sleeve is driven to rotate by the rotation of the rotating shaft, and the balls are driven to ascend and descend relative to the inside of the circulating slot by the rotation of the unidirectional rotating sleeve.
8. The apparatus of claim 7, wherein the circulation groove comprises a spiral groove and a connecting groove; the spiral groove forms axial displacement, and the end parts are communicated in a smooth transition mode through the connecting groove.
9. The apparatus of claim 7, wherein the circulation tank is provided therein with a pressing sensor for sensing the pressure of the balls, and the height of the driving plate is in an initial state when the pressing sensor senses the pressure of the balls.
10. A moxidectin purification method applied to the moxidectin purification equipment as claimed in any one of claims 1 to 9, wherein the moxidectin purification method comprises the following steps of:
s1, a solvent enters the interior of a reaction barrel through a solvent injection port according to a preset amount;
s2, the rotary driving piece searches a preset feeding proportion-reverse driving amount information table according to a preset feeding proportion to obtain reverse driving amount;
s3, the reverse driving amount of the rotary driving piece is consistent with the reverse driving amount;
s4, the rotating driving piece positively drives the rotating shaft to rotate, and the driving disc rotates to complete feeding of the Moxidectin crude product and the antioxidant through the first driven piece and the second driven piece;
s5, controlling the temperature to be 60-80 ℃ to dissolve the moxidectin;
s6, enabling the dissolving agent in the dissolving agent box to enter the reaction barrel, and continuously rotating the driving piece to rotate forwards for a preset stirring time period;
s7, rotating the driving piece to positively drive the rotating shaft to stir and controlling the temperature to be 0-20 ℃ to obtain moxidectin crystals;
s8, opening a preset opening by the control valve to discharge the solution, and leaving the moxidectin crystals in the reaction barrel;
s9, forming negative pressure inside the reaction barrel, and when the pressure sensing piece senses that the pressure inside the reaction barrel is smaller than a preset pressure, enabling the pressure inside the reaction barrel to be maintained for a preset drying time period by the controller;
and S10, opening a control valve to discharge the moxidectin crystals.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211023406.2A CN115253982B (en) | 2022-08-24 | 2022-08-24 | Equipment and method for purifying moxidectin |
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| CN202211023406.2A CN115253982B (en) | 2022-08-24 | 2022-08-24 | Equipment and method for purifying moxidectin |
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