CN107383100B - A kind of tenofovir process units - Google Patents
A kind of tenofovir process units Download PDFInfo
- Publication number
- CN107383100B CN107383100B CN201710681339.6A CN201710681339A CN107383100B CN 107383100 B CN107383100 B CN 107383100B CN 201710681339 A CN201710681339 A CN 201710681339A CN 107383100 B CN107383100 B CN 107383100B
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- Prior art keywords
- reaction kettle
- autoclave body
- tank
- kettle
- lid
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- 229960004556 tenofovir Drugs 0.000 title claims abstract description 22
- VCMJCVGFSROFHV-WZGZYPNHSA-N tenofovir disoproxil fumarate Chemical compound OC(=O)\C=C\C(O)=O.N1=CN=C2N(C[C@@H](C)OCP(=O)(OCOC(=O)OC(C)C)OCOC(=O)OC(C)C)C=NC2=C1N VCMJCVGFSROFHV-WZGZYPNHSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 155
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 238000004821 distillation Methods 0.000 claims abstract description 50
- 238000007670 refining Methods 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 238000004064 recycling Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 57
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 55
- 239000007787 solid Substances 0.000 claims description 20
- 239000007921 spray Substances 0.000 claims description 19
- 239000012153 distilled water Substances 0.000 claims description 14
- 230000005540 biological transmission Effects 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000001376 precipitating effect Effects 0.000 claims description 12
- 239000002985 plastic film Substances 0.000 claims description 11
- 229920006255 plastic film Polymers 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 8
- 239000003651 drinking water Substances 0.000 claims description 7
- 235000020188 drinking water Nutrition 0.000 claims description 7
- 229920003023 plastic Polymers 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 4
- 238000013019 agitation Methods 0.000 abstract description 2
- 229960002050 hydrofluoric acid Drugs 0.000 description 21
- 238000010586 diagram Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- GCOFRXOOFANVPB-SNVBAGLBSA-N 9-[(2r)-2-(diethoxyphosphorylmethoxy)propyl]purin-6-amine Chemical compound N1=CN=C2N(C[C@@H](C)OCP(=O)(OCC)OCC)C=NC2=C1N GCOFRXOOFANVPB-SNVBAGLBSA-N 0.000 description 2
- 208000030507 AIDS Diseases 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- 239000003443 antiviral agent Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229940072651 tylenol Drugs 0.000 description 2
- NIDNOXCRFUCAKQ-UMRXKNAASA-N (1s,2r,3s,4r)-bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1[C@H]2C=C[C@@H]1[C@H](C(=O)O)[C@@H]2C(O)=O NIDNOXCRFUCAKQ-UMRXKNAASA-N 0.000 description 1
- HUPNQNOWXCVQSW-UHFFFAOYSA-N 2h-pyran-4-carboxamide Chemical compound NC(=O)C1=CCOC=C1 HUPNQNOWXCVQSW-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- -1 diethyl Tylenol Chemical compound 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6561—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing systems of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring or ring system, with or without other non-condensed hetero rings
- C07F9/65616—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing systems of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring or ring system, with or without other non-condensed hetero rings containing the ring system having three or more than three double bonds between ring members or between ring members and non-ring members, e.g. purine or analogs
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A kind of tenofovir process units, it includes primary first-order equation kettle, low-temp reaction kettle, distillation type reaction kettle, secondary response kettle and recycling settling tank, primary first-order equation kettle includes reaction kettle ontology and at least two refining plates, refining board ends are respectively equipped with shaft, refining plate mounting bracket is equipped in reaction kettle, the shaft of refining plate one end is equipped with gear；Structure of the invention design is reasonable, primary first-order equation kettle stops the liquid rotated in reaction kettle by refining plate, improve stirring efficiency, it simultaneously can be according to the process of liquid agitation in reaction kettle, the angle of refining plate is adjusted to change the flowing velocity of liquid in reaction kettle, low-temp reaction kettle uses electronic slide unit driving fan formula stirring blade, during stirring blade is up and down, due to fluid principles, automatic rotation, to achieve the purpose that stirring, not only reduce power of motor, also reduce calorific value, evolution reaction is high-efficient, distillation type reaction kettle distillation efficiency is high, product purity is high, with good practical value.
Description
Technical field
The present invention relates to tenofovir production technical fields, and in particular to a kind of tenofovir process units.
Background technique
Tenofovir (compound I) also known as tenofovir, Chinese name: (R is secondary for tenofovir process units
Evolution reaction kettle) the fast secondary precipitation reaction kettle purine for tenofovir process units of -9- (2- phosphate methoxy propyl)-gland,
It is a kind of AIDS antiviral drugs, tenofovir is also that the better AIDS antiviral drugs fumaric acid Tylenol good fortune of effect is used for
The secondary precipitation reaction kettle Wei ester (the secondary precipitation reaction kettle II for tenofovir process units) of tenofovir process units
Key intermediate.In tenofovir process units, after needing to add salt water to be stirred primary first-order equation solution, HPA is precipitated and produces
Product crystal, existing low-temp reaction kettle are stirred using heavy-duty motor, so not only waste of energy, and will increase additional
Heat hinders evolution reaction.Diethyl tenofovir, existing distillation reactor distillation efficiency are generated by the way of distillation
Low, product purity is low.
Summary of the invention
The object of the invention is in order to solve the above-mentioned technical problem, and provide a kind of tenofovir process units.
The present invention includes primary first-order equation kettle, low-temp reaction kettle, distillation type reaction kettle, secondary response kettle and recycles settling tank,
Primary first-order equation kettle includes reaction kettle ontology and at least two refining plates, and refining board ends are respectively equipped with shaft, are equipped in reaction kettle
Refining plate mounting bracket, the shaft of refining plate one end are equipped with gear, are driven between the gear of multiple refining plates by gear ring；It
Also rack gear driver, gear ring driver are equipped with transmission gear group and rocking handle, and gear ring driver is mounted on reaction kettle ontology top
Portion, and driven gear ring rotates；Strainer is equipped in the discharge nozzle of the reaction kettle ontology；Low-temp reaction kettle includes low-temp reaction kettle kettle
Body, low-temperature control device, agitating device and centrifugal equipment for separating liquid from solid, low-temp reaction kettle autoclave body top are equipped with feed inlet, bottom
Portion is equipped with discharge port, and feed inlet passes through the outlet of pipeline and reaction kettle ontology, and low-temperature control device includes alcohol cabinet, electricity
Control valve and rotary-atomizing spray head, alcohol cabinet are fixedly mounted on the top of low-temp reaction kettle autoclave body, and rotary-atomizing spray head is mounted on
On the bottom surface of low-temp reaction kettle autoclave body lid, and the outlet of alcohol cabinet entering by pipeline and electrically-controlled valve and rotary-atomizing spray head
Mouth connection, agitating device include a pair of electronic slide unit, a pair of of stirring blade frame and a pair of fan-type stirring blade, a pair of of electric sliding
The track of platform is respectively and fixedly installed on the inner wall of low-temp reaction kettle autoclave body, and a pair of of stirring blade frame is separately mounted to a pair of electronic
On the sliding block of slide unit, a pair of of fan-type stirring blade passes through shaft respectively and is movably arranged on a pair of of stirring blade frame, centrifugal
Equipment for separating liquid from solid includes centrifugal type solid/liquid separator, crystal hopper and solution hopper, the feed inlet of centrifugal type solid/liquid separator
It is connected to the outlet at bottom of low-temp reaction kettle autoclave body, the entrance of crystal hopper and the solid-phase outlet of centrifugal type solid/liquid separator connect
Logical, the entrance of solution hopper is connected to the liquid-phase outlet of centrifugal type solid/liquid separator；Distillation type reaction kettle includes that distillation type is anti-
Kettle autoclave body, kettle cover, distilling apparatus, hydrofluoric acid adding device and clear liquid draw-out device are answered, is spacious at the top of distillation type reaction kettle autoclave body
Mouthful, kettle cover is hinged on distillation type reaction kettle autoclave body, and kettle cover is equipped with feed inlet, and feed inlet passes through the outlet of pipeline and solution hopper
Connection, kettle cover are inverted cone-shaped, and one group of condensate tank(trap) of the lower surface annular array of taper bevel edge, and the bottom for being equipped with kettle cover is equipped with point
The collecting channel not being connected to one group of condensate tank(trap), distilling apparatus include electric boiling plate, cold plate, collector pipe and distilled water tank, electricity
Heating plate is fixedly mounted on distillation type reaction kettle inner wall of kettle, and cold plate is mounted on the upper surface of kettle cover, and distilled water tank is fixed
It is mounted on the outer wall of distillation type reaction kettle autoclave body, the both ends of collector pipe are separately connected the water inlet of collecting channel and distilled water tank
Mouthful, hydrofluoric acid adding device includes hydrofluoric acid hopper, hydrofluoric acid feeder pipe and metering valve, and hydrofluoric acid hopper is fixedly mounted on distillation
On the outer wall of formula reaction kettle autoclave body, one end of hydrofluoric acid feeder pipe and the outlet of hydrofluoric acid hopper, metering valve are mounted on hydrogen
The other end of fluoric acid feeder pipe, and be located in distillation type reaction kettle autoclave body, clear liquid draw-out device includes web plate, pump and drinking-water pipe,
Web plate is fixedly mounted on the inner wall of distillation type reaction kettle autoclave body, and pump is fixedly mounted on web plate, and the both ends of drinking-water pipe connect respectively
Connect the entrance of pump and distilled water tank；Secondary response kettle includes evolution reaction kettle autoclave body, Moveable lid body device, spray equipment, a pair
Agitating device and discharging device, evolution reaction kettle autoclave body are that top is open bulk containers, and sealing is equipped at open top
Slot, bottom are equipped with outlet, and Moveable lid body device includes lid, shaft, uncap speed reducer and clip, lid be equipped with feed inlet and
One group of spray tube installing port, feed inlet are connected to by pipeline with the discharge port of distillation type reaction kettle autoclave body, and the side of lid passes through
Shaft and evolution reaction kettle autoclave body are hinged, and the other side of lid passes through locked clip device on evolution reaction kettle autoclave body, deceleration of uncapping
The shell of machine is fixedly mounted on the outer wall of evolution reaction kettle autoclave body, and line shaft is connected by transmission belt with rotating shaft transmission, is sprayed
Shower device includes water tank, force (forcing) pump and one group of atomizer, and water tank and force (forcing) pump are respectively and fixedly installed to evolution reaction kettle autoclave body
Side wall on, the water outlet of water tank is connected to by pipeline with the water inlet of force (forcing) pump, and atomizer is separately mounted on lid
It at spray tube installing port, and is connected to respectively by pipeline with the high-pressure water outlet of force (forcing) pump, agitating device includes power head, stirring
Axis and one group of agitating paddle, power head are fixedly mounted on evolution reaction kettle autoclave body outer wall, the power output of agitating shaft and power head
End transmission is connected, and one group of agitating paddle is respectively and fixedly installed on agitating shaft, and discharging device includes annular slide carriage, discharge nozzle and solid-liquid
Separator, annular slide carriage are fixedly mounted on the inner wall of evolution reaction kettle autoclave body, the connection of one end of discharge nozzle evolution reaction
Kettle autoclave body exit, and it is located at the underface of annular slide carriage, the feed inlet of solid-liquid separator is communicated with the other end of discharge nozzle；It returns
Receiving settling tank includes recycling precipitating tank, water collecting tank, plastic film and transparent orthopyramid shape lid, recycles settling tank tank
The entrance of body is connected to the liquid-phase outlet of secondary response kettle solid-liquid separator, and the outer wall of recycling precipitating tank is provided with for adding
Recuperation of heat precipitates the electric heating cover or steam jacket of tank, and plastic film is layered on bottom in recycling precipitating tank, and water is received
Collect tank to place on a plastic film, transparent orthopyramid shape lid is inverted in recycling settling tank top of the tank, and water collecting tank position
It may pass through transparent orthopyramid in being provided on the underface at transparent plastic cover pyramid tip, transparent orthopyramid shape lid
Shape lid is to the light source heated in recycling settling tank tank body.
The track of a pair of electronic slide unit is fixedly mounted on the inner wall of low-temp reaction kettle autoclave body in parallel vertically respectively.
The refining plate is mesh plate, and the aperture of the mesh plate is 10-30mm.
The strainer is equipped with axis, and is movably arranged in the discharge nozzle of reaction kettle ontology by axis.
The reaction kettle bodies top is equipped with multiple limited blocks, and limited block is located at gear ring and gear engagement place, on limited block
Equipped with a pair of of roller, gear ring rotates between a pair of of roller.
The orthopyramid shape lid is transparent high-temperature resistance plastice or transparent glass.
The invention has the advantages that: the present invention provides a kind of tenofovir process units, reasonable in design, primary first-order equation kettle mistake
Refining plate stops the liquid rotated in reaction kettle, improves stirring efficiency, while can be according to liquid agitation in reaction kettle
Process, adjust the angle of refining plate to change the flowing velocity of liquid in reaction kettle, low-temp reaction kettle is using the drive of electronic slide unit
Dynamic fan-type stirring blade, it is automatic to rotate due to fluid principles during stirring blade is up and down, to reach stirring
Purpose not only reduces power of motor, also reduces calorific value, and evolution reaction is high-efficient, and distillation type reaction kettle can be efficient complete
At the distillation reaction of tenofovir semi-finished product diethyl tenofovir, distillation efficiency is high, and product purity is high, has practical well
Value.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
Fig. 2 is low-temp reaction kettle structural schematic diagram of the present invention；
Fig. 3 is distillation type reaction kettle structural schematic diagram of the present invention；
Fig. 4 is primary first-order equation kettle structural schematic diagram of the present invention；
Fig. 5 is primary first-order equation kettle overlooking structure diagram of the present invention；
Fig. 6 is secondary response kettle structural schematic diagram of the present invention；
Fig. 7 is present invention recycling settling tank structural schematic diagram；
Fig. 8 is present invention recycling settling tank side structure schematic view.
Coding is respectively as follows: 2 for water collecting tank in figure, and 3 be plastic film, and 4 be lid, and 10 be reaction kettle ontology, and 11 be even
Flitch, 12 be mounting bracket, and 13 be gear, and 14 be gear ring, and 15 be gear ring driver, and 16 be strainer, and 17 be limited block, and 35 be one
Secondary response kettle, 36 be low-temp reaction kettle, and 37 be distillation type reaction kettle, and 38 be secondary response kettle, and 39 be recycling settling tank, and 46 be card
Hoop, 47 be power head, and 48 be discharge nozzle, and 49 be solid-liquid separator, and 50 be reaction kettle autoclave body, and 51 be lid, and 52 be shaft, and 53 are
It uncaps retarder, 54 be water tank, and 55 be force (forcing) pump, and 56 be atomizer, and 57 be agitating shaft, and 58 be agitating paddle, and 59 slip for annular
Plate, 60 be low-temp reaction kettle autoclave body, and 61 be alcohol cabinet, and 62 be electrically-controlled valve, and 64 be rotary-atomizing spray head, and 65 be electronic slide unit,
66 be stirring blade frame, and 67 be fan-type stirring blade, and 68 be centrifugal type solid/liquid separator, and 69 be crystal hopper, and 70 be solution
Hopper, 80 distillation type reaction kettle autoclave bodies, 81 be kettle cover, and 81-1 is condensate tank(trap), and 81-2 is collecting channel, and 82 be electric boiling plate, 83
For cold plate, 84 collector pipes, 85 be distilled water tank, and 86 be hydrofluoric acid hopper, and 87 be hydrofluoric acid feeder pipe, and 88 be metering valve, 89
It is pump for web plate, 90,91 be drinking-water pipe.
Specific embodiment
As shown in the picture, the present invention includes primary first-order equation kettle 35, low-temp reaction kettle 36, distillation type reaction kettle 37, secondary counter
Kettle 38 and recycling settling tank 39 are answered, primary first-order equation kettle 35 includes reaction kettle ontology 10 and at least two refining plates 11, refining plate 11
Both ends are respectively equipped with shaft, and 11 mounting bracket 12 of refining plate is equipped in reaction kettle, and the shaft of 11 one end of refining plate is equipped with gear
13, it is driven by gear ring 14 between the gear 13 of multiple refining plates 11；It goes back rack gear driver 15, sets on gear ring driver 15
There are transmission gear group and rocking handle, gear ring driver 15 is mounted on 10 top of reaction kettle ontology, and driven gear ring 14 rotates；It is described anti-
It answers and is equipped with strainer 16 in the discharge nozzle of kettle ontology 10；Low-temp reaction kettle 36 include low-temp reaction kettle autoclave body 60, low-temperature control device,
Agitating device and centrifugal equipment for separating liquid from solid are equipped with feed inlet at the top of low-temp reaction kettle autoclave body 60, and bottom is equipped with discharge port, into
Material mouth passes through the outlet of pipeline and reaction kettle ontology 10, and low-temperature control device includes alcohol cabinet 61, electrically-controlled valve 62 and rotation
Turn atomizer 64, alcohol cabinet 61 is fixedly mounted on the top of low-temp reaction kettle autoclave body 60, and rotary-atomizing spray head 64 is mounted on
On the bottom surface of 60 lid of low-temp reaction kettle autoclave body, and the outlet of alcohol cabinet 61 is sprayed by pipeline and electrically-controlled valve 62 and rotary-atomizing
First 64 entrance connection, agitating device include a pair of electronic slide unit 65, a pair of of stirring blade frame 66 and a pair of of fan-type paddle
The track of piece 67, a pair of electronic slide unit 65 is respectively and fixedly installed on the inner wall of low-temp reaction kettle autoclave body 60, a pair of of stirring blade
Frame 66 is separately mounted on the sliding block of a pair of electronic slide unit 65, and a pair of of fan-type stirring blade 67 is installed by shaft activity respectively
On a pair of of stirring blade frame 66, centrifugal equipment for separating liquid from solid includes centrifugal type solid/liquid separator 68, crystal hopper 69 and molten
The feed inlet of liquid tank 70, centrifugal type solid/liquid separator 68 is connected to the outlet at bottom of low-temp reaction kettle autoclave body 60, crystal hopper
69 entrance is connected to the solid-phase outlet of centrifugal type solid/liquid separator 68, the entrance of solution hopper 70 and centrifugal separation of solid and liquid
The liquid-phase outlet of device 68 is connected to；Distillation type reaction kettle 37 includes distillation type reaction kettle autoclave body 80, kettle cover 81, distilling apparatus, hydrogen fluorine
Sour adding set and clear liquid draw-out device, be at the top of distillation type reaction kettle autoclave body 80 it is open, kettle cover 81 is hinged on distillation type reaction
On kettle autoclave body 80, kettle cover 81 is equipped with feed inlet, and feed inlet passes through the outlet of pipeline and solution hopper 70, and kettle cover 81 is back taper
Type, and one group of condensate tank(trap) 81-1 of the lower surface annular array of taper bevel edge, and be equipped with kettle cover 81 bottom be equipped with respectively with one group
The collecting channel 81-2 of condensate tank(trap) 81-1 connection, distilling apparatus includes electric boiling plate 82, cold plate 83, collector pipe 84 and distilled water
Case 85, electric boiling plate 82 are fixedly mounted on 80 inner wall of distillation type reaction kettle autoclave body, and cold plate 83 is mounted on the upper table of kettle cover 81
Face, distilled water tank 85 are fixedly mounted on the outer wall of distillation type reaction kettle autoclave body 80, and the both ends of collector pipe 84, which are separately connected, catchments
The water inlet of channel 81-2 and distilled water tank 85, hydrofluoric acid adding device include hydrofluoric acid hopper 86,87 and of hydrofluoric acid feeder pipe
Metering valve 88, hydrofluoric acid hopper 86 are fixedly mounted on the outer wall of distillation type reaction kettle autoclave body 80, and the one of hydrofluoric acid feeder pipe 87
The outlet at end and hydrofluoric acid hopper 86, metering valve 88 is mounted on the other end of hydrofluoric acid feeder pipe 87, and is located at distillation type
In reaction kettle autoclave body 80, clear liquid draw-out device includes web plate 89, pump 90 and drinking-water pipe 91, and it is anti-that web plate 89 is fixedly mounted on distillation type
On the inner wall for answering kettle autoclave body 80, pump 90 is fixedly mounted on web plate 89, and the both ends of drinking-water pipe 91 are separately connected pump 90 and distilled water
The entrance of case 85.
Secondary response kettle 38 include evolution reaction kettle autoclave body 50, Moveable lid body device, spray equipment, a pair of of agitating device and
Discharging device, evolution reaction kettle autoclave body 50 are that top is open bulk containers, and seal groove is equipped at open top, and bottom is set
There is outlet, Moveable lid body device includes lid 51, shaft 52, uncap speed reducer 53 and clip 46, and lid 51 is equipped with feed inlet
With one group of spray tube installing port, feed inlet is connected to by pipeline with the discharge port of distillation type reaction kettle autoclave body 80, and the one of lid 51
Side is hinged by shaft 52 and evolution reaction kettle autoclave body 50, and the other side of lid 51 is locked at evolution reaction kettle kettle by clip 46
On body 50, the shell for speed reducer 53 of uncapping is fixedly mounted on the outer wall of evolution reaction kettle autoclave body 50, and line shaft passes through transmission
Band is connected with the transmission of shaft 52, and spray equipment includes water tank 54, force (forcing) pump 55 and one group of atomizer 56, water tank 54 and force (forcing) pump
55 are respectively and fixedly installed on the side wall of evolution reaction kettle autoclave body 50, the water outlet of water tank 54 by pipeline and force (forcing) pump 55 into
Mouth of a river connection, atomizer 56 are separately mounted at the spray tube installing port on lid 51, and pass through pipeline and force (forcing) pump respectively
55 high-pressure water outlet connection, agitating device include power head 47, agitating shaft 57 and one group of agitating paddle 58, the fixed peace of power head 47
On 50 outer wall of evolution reaction kettle autoclave body, agitating shaft 57 is connected with the transmission of the power output end of power head 47, one group of agitating paddle
58 are respectively and fixedly installed on agitating shaft 57, and discharging device includes annular slide carriage 59, discharge nozzle 48 and solid-liquid separator 49, annular
Slide carriage 59 is fixedly mounted on the inner wall of evolution reaction kettle autoclave body 50, the connection of one end of discharge nozzle 48 evolution reaction kettle autoclave body
50 exits, and it is located at the underface of annular slide carriage 59, the feed inlet of solid-liquid separator 49 is communicated with the other end of discharge nozzle 48.
Recycling settling tank 39 includes recycling precipitating tank, water collecting tank 2, plastic film 3 and transparent orthopyramid shape lid
The entrance of body 4, recycling precipitating tank is connected to the liquid-phase outlet of 38 solid-liquid separator 49 of secondary response kettle, recycles settling tank tank
The outer wall of body is provided with electric heating cover or steam jacket for heating recovery precipitating tank, and plastic film 3 is layered on recycling
Bottom in tank is precipitated, water collecting tank 2 is placed on plastic film 3, and transparent orthopyramid shape lid 4 is inverted in recycling precipitating
At the top of tank, and water collecting tank 2 is located at the underface at transparent 4 pyramid tip of plastic cover, transparent orthopyramid shape lid 4
On be provided with may pass through transparent orthopyramid shape lid 4 to recycling settling tank tank body in heat light source.
The track of a pair of electronic slide unit 65 is fixedly mounted on the inner wall of low-temp reaction kettle autoclave body 60 in parallel vertically respectively.
The refining plate 11 is mesh plate, and the aperture of the mesh plate 11 is 10-30mm.
The strainer 16 is equipped with axis, and is movably arranged in the discharge nozzle of reaction kettle ontology 10 by axis.
Multiple limited blocks 17 are equipped at the top of the reaction kettle ontology 10, limited block 17 is located at gear ring 14 and engages with gear 13
Place, limited block 17 are equipped with a pair of of roller, and gear ring 14 rotates between a pair of of roller.
The orthopyramid shape lid 4 is transparent high-temperature resistance plastice or transparent glass.
Working method and principle: the mounting bracket 12 of primary first-order equation kettle is provided with shaft mounting groove, 10 top of reaction kettle ontology
It is provided with shaft through hole, 11 both ends of refining plate are flexibly connected with mounting bracket 12 and reaction kettle ontology 10 respectively, and gear ring 14 is distinguished
Cooperate with the gear 13 of multiple refining plates 11,15 driven gear ring 14 of gear ring driver rotates to adjust the angle of refining plate 11, even
The angle difference of flitch 11 is also different to the resistance and refining degree of working fluid；Refining plate 11 is mesh plate, is stopping to react
Refining is carried out while liquid rotates in kettle, improves stirring efficiency；The discharge valve of reaction kettle ontology 10 is opened after the reaction was completed,
Strainer 16 in 10 discharge nozzle of reaction kettle ontology is filtered liquid, when needing to clean autoclave body, rotates strainer 16, makes to filter
Net 16 is vertical, carries out sewage discharge.Primary first-order equation solution is added by the feed inlet at 60 top of low-temp reaction kettle autoclave body, is added
Appropriate concentration salt water, a pair of electronic slide unit 65 of starting, a pair of electronic slide unit 65 respectively drive on a pair of of fan-type stirring blade 67
Under move reciprocatingly, due to fluid principles, liquid just drive fan-type stirring blade 67 rotate, thus reached stirring mesh
, electrically-controlled valve 62 is opened, low temperature alcohol just passes through rotary-atomizing spray head 64 and is uniformly sprayed at reaction solution downwards in alcohol cabinet 61
On body, cools down to reaction liquid, the precipitation of HPA product is made to remain at higher reaction efficiency, after the reaction was completed, reaction mixing
Object is flowed into centrifugal type solid/liquid separator 68 by the outlet of 60 bottom of low-temp reaction kettle autoclave body, and crystal, which is separated, enters crystalline substance
Body hopper 69, liquid enter solution hopper 70, and the solution in solution hopper 70 is added to distillation type reaction kettle by kettle cover 81
In autoclave body 80, electric boiling plate 82 and cold plate 83 are opened, electric boiling plate 82 heats the solution in distillation type reaction kettle autoclave body 80,
Cold plate 83 cools down to kettle cover 81, and the moisture in solution in such distillation type reaction kettle autoclave body 80 will largely gasify rising,
Low temperature kettle cover 81 is encountered to condense rapidly, condensed water is imported into collecting channel 81-2 along one group of condensate tank(trap) 81-1, and eventually by
Collector pipe 84 is flowed into distilled water tank 85, and after setting time, the solution in distillation type reaction kettle autoclave body 80 is gradually sticky at oil
The metering valve 88 of shape object, hydrofluoric acid adding device is opened, and the hydrofluoric acid in hydrofluoric acid hopper 86 is fixed by hydrofluoric acid feeder pipe 87
Amount is added in distillation type reaction kettle autoclave body 80, and hydrolysis occurs with grease, obtains diethyl Tylenol good fortune after distilling again
Wei, the solution after distillation type reaction kettle autoclave body 80 is reacted are added in evolution reaction kettle autoclave body 50 from the feed inlet of lid 51,
Force (forcing) pump 55 starts, and the water in water tank 54 is passed through one group of atomizer 56 in evolution reaction kettle autoclave body 50 after being overpressurized
Solution carries out uniformly adding water, while power head 47 starts, and drives agitating shaft 57 and one group of agitating paddle 58 to rotate, increases Solution H PA
The speed of separating out of product crystal after the crystal of precipitation drops into annular slide carriage 59, drops into solid-liquid separator by discharge nozzle 48
In 49, after solid-liquid separator 49 separates crystal and liquid, crystal is finished product, and the solution of solid-liquid separator 49 is imported recycling
It precipitates in tank, covers plastic cover 4, under the heat effect of electric heating cover or light source, the water in solution starts to evaporate, and steams
Vapour, which is gathered on transparent plastic cover 4, forms water droplet, and water droplet is attached to transparent 4 bottom of plastic cover, due to the work of gravity
Pyramid tip is slipped down to along rib with water droplet and instills the discharge of water collecting tank 2, and the crystalline material left after water evaporation is dry is attached to
On plastic film 3, takes plastic film 3 off and complete recycling.
Claims (6)
1. a kind of tenofovir process units, which is characterized in that it includes primary first-order equation kettle (35), low-temp reaction kettle (36), steams
Formula reaction kettle (37), secondary response kettle (38) and recycling settling tank (39) are evaporated, primary first-order equation kettle (35) includes reaction kettle ontology
(10) it is respectively equipped with shaft, refining plate (11) is equipped in reaction kettle and pacifies at least two refining plates (11), refining plate (11) both ends
It fills bracket (12), the shaft of refining plate (11) one end is equipped with gear (13), leads between the gear (13) of multiple refining plates (11)
Cross gear ring (14) transmission；It goes back rack gear driver (15), and gear ring driver (15) is equipped with transmission gear group and rocking handle, gear ring
Driver (15) is mounted at the top of reaction kettle ontology (10), and driven gear ring (14) rotates；The reaction kettle ontology (10) goes out
Strainer (16) are equipped in expects pipe；Low-temp reaction kettle (36) includes low-temp reaction kettle autoclave body (60), low-temperature control device, agitating device
With centrifugal equipment for separating liquid from solid, low-temp reaction kettle autoclave body (60) top is equipped with feed inlet, and bottom is equipped with discharge port, and feed inlet is logical
The outlet of piping and reaction kettle ontology (10), low-temperature control device include alcohol cabinet (61), electrically-controlled valve (62) and rotation
Turn atomizer (64), alcohol cabinet (61) is fixedly mounted on the top of low-temp reaction kettle autoclave body (60), rotary-atomizing spray head
(64) it is mounted on the bottom surface of low-temp reaction kettle autoclave body (60) lid, and the outlet of alcohol cabinet (61) passes through pipeline and electrically-controlled valve
(62) it is connected to the entrance of rotary-atomizing spray head (64), agitating device includes a pair of electronic slide unit (65), a pair of of stirring blade frame
(66) and a pair of of fan-type stirring blade (67), the track of a pair of electronic slide unit (65) are respectively and fixedly installed to low-temp reaction kettle kettle
On the inner wall of body (60), a pair of of stirring blade frame (66) is separately mounted on the sliding block of a pair of electronic slide unit (65), a pair of of fan
Formula stirring blade (67) is movably arranged on a pair of of stirring blade frame (66) by shaft respectively, centrifugal equipment for separating liquid from solid packet
Include centrifugal type solid/liquid separator (68), crystal hopper (69) and solution hopper (70), the charging of centrifugal type solid/liquid separator (68)
Mouth is connected to the outlet at bottom of low-temp reaction kettle autoclave body (60), the entrance of crystal hopper (69) and centrifugal type solid/liquid separator (68)
Solid-phase outlet connection, the entrance of solution hopper (70) is connected to the liquid-phase outlet of centrifugal type solid/liquid separator (68)；Distillation
Formula reaction kettle (37) includes that distillation type reaction kettle autoclave body (80), kettle cover (81), distilling apparatus, hydrofluoric acid adding device and clear liquid are taken out
Device is taken, is opening at the top of distillation type reaction kettle autoclave body (80), kettle cover (81) is hinged on distillation type reaction kettle autoclave body (80), kettle
It covers (81) and is equipped with feed inlet, feed inlet passes through the outlet of pipeline and solution hopper (70), and kettle cover (81) is inverted cone-shaped, and is bored
One group of condensate tank(trap) (81-1) of lower surface annular array of shape bevel edge, and be equipped with kettle cover (81) bottom be equipped with respectively with one group of condensation
Slot (81-1) connection collecting channel (81-2), distilling apparatus include electric boiling plate (82), cold plate (83), collector pipe (84) and
Distilled water tank (85), electric boiling plate (82) are fixedly mounted on distillation type reaction kettle autoclave body (80) inner wall, cold plate (83) attachment
In the upper surface of kettle cover (81), distilled water tank (85) is fixedly mounted on the outer wall of distillation type reaction kettle autoclave body (80), collector pipe
(84) both ends are separately connected the water inlet of collecting channel (81-2) and distilled water tank (85), and hydrofluoric acid adding device includes hydrogen fluorine
Sour hopper (86), hydrofluoric acid feeder pipe (87) and metering valve (88), hydrofluoric acid hopper (86) are fixedly mounted on distillation type reaction kettle
On the outer wall of autoclave body (80), one end of hydrofluoric acid feeder pipe (87) and the outlet of hydrofluoric acid hopper (86), metering valve (88)
It is mounted on the other end of hydrofluoric acid feeder pipe (87), and is located in distillation type reaction kettle autoclave body (80), clear liquid draw-out device includes
Web plate (89), pump (90) and drinking-water pipe (91), web plate (89) are fixedly mounted on the inner wall of distillation type reaction kettle autoclave body (80), are pumped
(90) it is fixedly mounted on web plate (89), the both ends of drinking-water pipe (91) are separately connected the entrance of pump (90) and distilled water tank (85)；
Secondary response kettle (38) includes evolution reaction kettle autoclave body (50), Moveable lid body device, spray equipment, a pair of of agitating device and discharging
Device, evolution reaction kettle autoclave body (50) are that top is open bulk containers, and seal groove is equipped at open top, and bottom is equipped with
Outlet, Moveable lid body device includes lid (51), shaft (52), speed reducer of uncapping (53) and clip (46), and lid is set on (51)
There are feed inlet and one group of spray tube installing port, feed inlet is connected to by pipeline with the discharge port of distillation type reaction kettle autoclave body (80),
The side of lid (51) passes through shaft (52) and evolution reaction kettle autoclave body (50) hingedly, and the other side of lid (51) passes through clip
(46) it is locked on evolution reaction kettle autoclave body (50), the shell of speed reducer of uncapping (53) is fixedly mounted on evolution reaction kettle autoclave body
(50) on outer wall, and line shaft is connected by transmission belt with shaft (52) transmission, and spray equipment includes water tank (54), force (forcing) pump
(55) and one group of atomizer (56), water tank (54) and force (forcing) pump (55) are respectively and fixedly installed to evolution reaction kettle autoclave body (50)
On side wall, the water outlet of water tank (54) is connected to by pipeline with the water inlet of force (forcing) pump (55), and one group of atomizer (56) is respectively
It is mounted at one group of spray tube installing port on lid (51), and is connected respectively by pipeline and the high-pressure water outlet of force (forcing) pump (55)
Logical, agitating device includes that power head (47), agitating shaft (57) and one group of agitating paddle (58), power head (47) are fixedly mounted on precipitation
On reaction kettle autoclave body (50) outer wall, agitating shaft (57) is connected with the transmission of the power output end of power head (47), one group of agitating paddle
(58) it is respectively and fixedly installed on agitating shaft (57), discharging device includes annular slide carriage (59), discharge nozzle (48) and is separated by solid-liquid separation
Device (49), annular slide carriage (59) are fixedly mounted on the inner wall of evolution reaction kettle autoclave body (50), one end connection of discharge nozzle (48)
Evolution reaction kettle autoclave body (50) exit, and be located at the underface of annular slide carriage (59), the charging of solid-liquid separator (49)
Mouth is communicated with the other end of discharge nozzle (48)；Recycling settling tank (39) includes recycling precipitating tank, water collecting tank (2), plastics
Film (3) and transparent orthopyramid shape lid (4), the entrance and secondary response kettle (38) solid-liquid separator of recycling precipitating tank
(49) liquid-phase outlet connection, the outer wall of recycling precipitating tank are provided with the electric heating cover for heating recovery precipitating tank
Or steam jacket, plastic film (3) are layered on bottom in recycling precipitating tank, water collecting tank (2) is placed on plastic film (3)
On, transparent orthopyramid shape lid (4) is inverted in recycling settling tank top of the tank, and water collecting tank (2) is located at transparent plastics
The underface at lid (4) pyramid tip, being provided on transparent orthopyramid shape lid (4) may pass through transparent orthopyramid shape lid
(4) to the light source heated in recycling settling tank tank body.
2. a kind of tenofovir process units according to claim 1, which is characterized in that the rail of a pair of electronic slide unit (65)
Road is fixedly mounted on the inner wall of low-temp reaction kettle autoclave body (60) in parallel vertically respectively.
3. a kind of tenofovir process units according to claim 1, which is characterized in that the refining plate (11) is mesh
Plate, the aperture of the mesh plate (11) are 10-30mm.
4. a kind of tenofovir process units according to claim 1, which is characterized in that the strainer (16) is equipped with
Axis, and be movably arranged in the discharge nozzle of reaction kettle ontology (10) by axis.
5. a kind of tenofovir process units according to claim 1, which is characterized in that reaction kettle ontology (10) top
Portion is equipped with multiple limited blocks (17), and limited block (17) is located at gear ring (14) and gear (13) engagement place, and limited block (17) is equipped with
A pair of of roller, gear ring (14) rotate between a pair of of roller.
6. a kind of tenofovir process units according to claim 1, which is characterized in that the orthopyramid shape lid
It (4) is transparent high-temperature resistance plastice or transparent glass.
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| CN201710681339.6A CN107383100B (en) | 2017-08-10 | 2017-08-10 | A kind of tenofovir process units |
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| CN107383100B true CN107383100B (en) | 2019-04-12 |
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| CN107321287A (en) * | 2017-08-21 | 2017-11-07 | 荆门市帅邦化学科技有限公司 | A kind of tenofovir production line |
| CN112191196B (en) * | 2020-09-16 | 2022-07-26 | 湖州卓瑞化工科技有限公司 | Hydrolysis device for preparing paratoluensulfonyl chloride and processing technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203184010U (en) * | 2013-02-26 | 2013-09-11 | 常州市华人化工有限公司 | Tenofovir recrystallization reaction kettle |
| CN204034708U (en) * | 2014-08-26 | 2014-12-24 | 荆门市帅邦化学科技有限公司 | A kind of reaction unit for tenofovir production line |
| CN105859781A (en) * | 2016-05-03 | 2016-08-17 | 荆门市帅邦化学科技有限公司 | Industrialization production technology for tenofovir disoproxil fumarate |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203184010U (en) * | 2013-02-26 | 2013-09-11 | 常州市华人化工有限公司 | Tenofovir recrystallization reaction kettle |
| CN204034708U (en) * | 2014-08-26 | 2014-12-24 | 荆门市帅邦化学科技有限公司 | A kind of reaction unit for tenofovir production line |
| CN105859781A (en) * | 2016-05-03 | 2016-08-17 | 荆门市帅邦化学科技有限公司 | Industrialization production technology for tenofovir disoproxil fumarate |
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