CN107266500B - A kind of crystal evolution reaction system of tenofovir production line - Google Patents

A kind of crystal evolution reaction system of tenofovir production line Download PDF

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Publication number
CN107266500B
CN107266500B CN201710681340.9A CN201710681340A CN107266500B CN 107266500 B CN107266500 B CN 107266500B CN 201710681340 A CN201710681340 A CN 201710681340A CN 107266500 B CN107266500 B CN 107266500B
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reaction kettle
low
autoclave body
distillation
pair
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CN201710681340.9A
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CN107266500A (en
Inventor
林培鹏
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Xining Kejin Industrial Design Co ltd
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Huang Zhemin
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02Phosphorus compounds
    • C07F9/547Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
    • C07F9/6561Heterocyclic 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
    • C07F9/65616Heterocyclic 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/805Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis wherein the stirrers or the receptacles are moved in order to bring them into operative position; Means for fixing the receptacle
    • B01F27/806Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis wherein the stirrers or the receptacles are moved in order to bring them into operative position; Means for fixing the receptacle with vertical displacement of the stirrer, e.g. in combination with means for pivoting the stirrer about a vertical axis in order to co-operate with different receptacles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside

Abstract

A kind of crystal evolution reaction system of tenofovir production line, it includes low-temp reaction kettle and distillation type reaction kettle, low-temp reaction kettle includes low-temp reaction kettle autoclave body, low-temperature control device, agitating device and centrifugal equipment for separating liquid from solid, feed inlet is equipped at the top of low-temp reaction kettle autoclave body, bottom is equipped with discharge port, low-temperature control device includes alcohol cabinet, electrically-controlled valve and rotary-atomizing spray head, and alcohol cabinet is fixedly mounted on the top of low-temp reaction kettle autoclave body;Rationally, low-temp reaction kettle uses electronic slide unit driving fan formula stirring blade, during stirring blade is up and down for structure of the invention design, due to fluid principles, automatic rotation, to achieve the purpose that stirring, not only reduces power of motor, also reduce calorific value, evolution reaction is high-efficient, and distillation type reaction kettle can be efficiently completed the distillation reaction of tenofovir semi-finished product diethyl tenofovir, and distillation efficiency is high, product purity is high, has good practical value.

Description

A kind of crystal evolution reaction system of tenofovir production line
Technical field
The present invention relates to chemical equipment technical fields, and in particular to a kind of crystal evolution reaction system of tenofovir production line System.
Background technique
Tenofovir (compound I) also known as tenofovir, Chinese name: (R is used for the secondary analysis of tenofovir production line Reaction kettle out) the fast secondary precipitation reaction kettle purine for tenofovir production line of -9- (2- phosphate methoxy propyl)-gland is one Kind AIDS antiviral drugs, tenofovir are also the better AIDS antiviral drugs fumaric acid Tylenol good fortune of effect for Tylenol (the secondary precipitation reaction kettle II for tenofovir production line is used for Tylenol good fortune to the secondary precipitation reaction kettle Wei ester of good fortune Wei production line The secondary precipitation reaction kettle of Wei production line) key intermediate.In tenofovir production line, need to add salt to primary first-order equation solution After water is stirred, HPA product crystal is precipitated, existing low-temp reaction kettle is stirred using heavy-duty motor, so not only Waste of energy, and will increase additional heat, hinder evolution reaction.
Summary of the invention
The object of the invention is in order to solve the above-mentioned technical problem, and provide a kind of crystal analysis of tenofovir production line Reaction system out.
The present invention includes low-temp reaction kettle and distillation type reaction kettle, and low-temp reaction kettle includes low-temp reaction kettle autoclave 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, and bottom is equipped with Material mouth, low-temperature control device include alcohol cabinet, electrically-controlled valve and rotary-atomizing spray head, and alcohol cabinet is fixedly mounted on low-temp reaction The top of kettle autoclave body, rotary-atomizing spray head are mounted on the bottom surface of low-temp reaction kettle autoclave body lid, and the outlet of alcohol cabinet is logical Piping and electrically-controlled valve are connected to the entrance of rotary-atomizing spray head, and agitating device includes a pair of electronic slide unit, a pair of of stirring blade The track of frame and a pair of of fan-type stirring blade, a pair of electronic slide unit is respectively and fixedly installed to the inner wall of low-temp reaction kettle autoclave body On, a pair of of stirring blade frame is separately mounted on the sliding block of a pair of electronic slide unit, and fan-type stirring blade is living by shaft respectively Dynamic to be mounted on stirring blade frame, centrifugal equipment for separating liquid from solid includes centrifugal type solid/liquid separator, crystal hopper and solution material The feed inlet of case, centrifugal type solid/liquid separator is connected to the outlet at bottom of low-temp reaction kettle autoclave body, the entrance of crystal hopper with from The solid-phase outlet of core type solid-liquid separator is connected to, and the entrance of solution hopper is connected to the liquid-phase outlet of centrifugal type solid/liquid separator, Distillation type reaction kettle includes distillation type reaction kettle autoclave body, kettle cover, distilling apparatus, hydrofluoric acid adding device and clear liquid draw-out device, It is opening at the top of distillation type reaction kettle autoclave body, kettle cover is hinged on distillation type reaction kettle autoclave body, and kettle cover is equipped with feed inlet, feed inlet By the outlet of pipeline and solution hopper, kettle cover is inverted cone-shaped, and the one group of condensation of the lower surface annular array of taper bevel edge Slot-, and the bottom for being equipped with kettle cover is equipped with the collecting channel-being connected to respectively with one group of condensate tank(trap)-, distilling apparatus includes electric heating Plate, cold plate, collector pipe and distilled water tank, electric boiling plate are fixedly mounted on distillation type reaction kettle inner wall of kettle, cold plate patch Mounted in the upper surface of kettle cover, distilled water tank is fixedly mounted on the outer wall of distillation type reaction kettle autoclave body, the both ends difference of collector pipe The water inlet of collecting channel-and distilled water tank is connected, hydrofluoric acid adding device includes hydrofluoric acid hopper, hydrofluoric acid feeder pipe and meter Valve is measured, hydrofluoric acid hopper is fixedly mounted on the outer wall of distillation type reaction kettle autoclave body, one end of hydrofluoric acid feeder pipe and hydrofluoric acid The outlet of hopper, metering valve is mounted on the other end of hydrofluoric acid feeder pipe, and is located in distillation type reaction kettle autoclave body, clear liquid Draw-out device includes web plate, pump and drinking-water pipe, and web plate is fixedly mounted on the inner wall of distillation type reaction kettle autoclave body, and pump is fixedly mounted On web plate, the both ends of drinking-water pipe are separately connected the entrance of pump and distilled water tank.
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 invention has the advantages that: the present invention provides a kind of crystal evolution reaction system of tenofovir production line, structure design Rationally, low-temp reaction kettle uses electronic slide unit driving fan formula stirring blade, during stirring blade is up and down, due to fluid Principle, it is automatic to rotate, to achieve the purpose that stirring, power of motor is not only reduced, also reduces calorific value, evolution reaction effect Rate is high, and distillation type reaction kettle can be efficiently completed the distillation reaction of tenofovir semi-finished product diethyl tenofovir, distillation efficiency Height, product purity is high, has good practical 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.
Coding is respectively as follows: 60 for low-temp reaction kettle autoclave body in figure, and 61 be alcohol cabinet, and 62 be electrically-controlled valve, and 64 be rotation mist Change spray head, 65 be electronic slide unit, and 66 be stirring blade frame, and 67 be fan-type stirring blade, and 68 be centrifugal type solid/liquid separator, 69 It is solution hopper for crystal hopper, 70,80 be distillation type reaction kettle autoclave body, and 81 be kettle cover, and 81-1 is condensate tank(trap), and 81-2 is to catchment Channel, 82 be electric boiling plate, and 83 be cold plate, and 84 be collector pipe, and 85 be distilled water tank, and 86 be hydrofluoric acid hopper, and 87 be hydrogen fluorine Sour feeder pipe, 88 be metering valve, and 89 be web plate, and 90 be pump, and 91 be drinking-water pipe.
Specific embodiment
As shown in the picture, the present invention includes low-temp reaction kettle and distillation type reaction kettle, and low-temp reaction kettle includes low-temp reaction Kettle autoclave body 60, low-temperature control device, agitating device and centrifugal equipment for separating liquid from solid, be equipped at the top of low-temp reaction kettle autoclave body 60 into Material mouth, bottom are equipped with discharge port, and low-temperature control device includes alcohol cabinet 61, electrically-controlled valve 62 and rotary-atomizing spray head 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 the lid of low-temp reaction kettle autoclave body 60 On the bottom surface of body, and the outlet of alcohol cabinet 61 is connected to by pipeline and electrically-controlled valve 62 with the entrance of rotary-atomizing spray head 64, is stirred Mixing 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, a pair of electronic slide unit 65 track is respectively and fixedly installed on the inner wall of low-temp reaction kettle autoclave body 60, and a pair of of stirring blade frame 66 is separately mounted to a pair On the sliding block of electronic slide unit 65, fan-type stirring blade 67 is movably arranged on stirring blade frame 66 by shaft respectively, centrifugation Formula equipment for separating liquid from solid includes centrifugal type solid/liquid separator 68, crystal hopper 69 and solution hopper 70, centrifugal type solid/liquid separator 68 feed inlet is connected to the outlet at bottom of low-temp reaction kettle autoclave body 60, the entrance and centrifugal type solid/liquid separator of crystal hopper 69 68 solid-phase outlet connection, the entrance of solution hopper 70 are connected to the liquid-phase outlet of centrifugal type solid/liquid separator 68, and distillation type is anti- Answering kettle includes distillation type reaction kettle autoclave body 80, kettle cover 81, distilling apparatus, hydrofluoric acid adding device and clear liquid draw-out device, distillation It is opening at the top of formula reaction kettle autoclave body 80, kettle cover 81 is hinged on distillation type reaction kettle autoclave body 80, and kettle cover 81 is equipped with feed inlet, into Material mouth is by the outlet of pipeline and solution hopper 70, and kettle cover 81 is inverted cone-shaped, and the lower surface annular array of taper bevel edge One group of condensate tank(trap) 81-1, and the bottom for being equipped with kettle cover 81 is equipped with the collecting channel 81-2 being connected to respectively with one group of condensate tank(trap) 81-1, Distilling apparatus includes electric boiling plate 82, cold plate 83, collector pipe 84 and distilled water tank 85, and electric boiling plate 82 is fixedly mounted on distillation On 80 inner wall of formula reaction kettle autoclave body, cold plate 83 is mounted on the upper surface of kettle cover 81, and distilled water tank 85 is fixedly mounted on distillation type On the outer wall of reaction kettle autoclave body 80, the both ends of collector pipe 84 are separately connected the water inlet of collecting channel 81-2 and distilled water tank 85, Hydrofluoric acid adding device includes hydrofluoric acid hopper 86, hydrofluoric acid feeder pipe 87 and metering valve 88, and hydrofluoric acid hopper 86 is fixedly mounted On the outer wall of distillation type reaction kettle autoclave body 80, one end of hydrofluoric acid feeder pipe 87 and the outlet of hydrofluoric acid hopper 86, meter Amount valve 88 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 packet It includes web plate 89, pump 90 and drinking-water pipe 91, web plate 89 to be fixedly mounted on the inner wall of distillation type reaction kettle autoclave body 80, the fixed peace of pump 90 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.
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.
Working method and principle: primary first-order equation solution is added by the feed inlet at 60 top of low-temp reaction kettle autoclave body, then plus Enter appropriate concentration salt water, a pair of electronic slide unit 65 of starting, a pair of electronic slide unit 65 respectively drives a pair of of fan-type stirring blade 67 It moves reciprocatingly up and down, due to fluid principles, liquid just drives fan-type stirring blade 67 to rotate, and has thus reached stirring Purpose opens electrically-controlled valve 62, and low temperature alcohol just passes through rotary-atomizing spray head 64 and is uniformly sprayed at reaction downwards in alcohol cabinet 61 On liquid, cool down to reaction liquid, the precipitation of HPA product is made to remain at higher reaction efficiency, after the reaction was completed, reaction is mixed It closes object and centrifugal type solid/liquid separator 68 is flowed by the outlet of 60 bottom of low-temp reaction kettle autoclave body, crystal, which is separated, to be entered Crystal hopper 69, liquid enter solution hopper 70, and the solution in solution hopper 70 is added to distillation type reaction by kettle cover 81 In kettle autoclave body 80, opens electric boiling plate 82 and cold plate 83, electric boiling plate 82 add the solution in distillation type reaction kettle autoclave body 80 Temperature, cold plate 83 cool down to kettle cover 81, on the moisture in solution in such distillation type reaction kettle autoclave body 80 will largely gasify It rises, encounters low temperature kettle cover 81 and condense rapidly, condensed water is imported into collecting channel 81-2 along one group of condensate tank(trap) 81-1, and finally leads to Collector pipe 84 is crossed to be flowed into distilled water tank 85, after setting time, solution in distillation type reaction kettle autoclave body 80 gradually it is sticky at The metering valve 88 of grease, hydrofluoric acid adding device is opened, and the hydrofluoric acid in hydrofluoric acid hopper 86 passes through hydrofluoric acid feeder pipe 87 It is quantitatively adding in distillation type reaction kettle autoclave body 80, hydrolysis occurs with grease, obtains diethyl Tylenol after distilling again Fu Wei.

Claims (2)

1. a kind of crystal evolution reaction system of tenofovir production line, which is characterized in that it includes low-temp reaction kettle and distillation Formula reaction kettle, low-temp reaction kettle include low-temp reaction kettle autoclave body (60), low-temperature control device, agitating device and centrifugal solid-liquid point From device, feed inlet is equipped at the top of low-temp reaction kettle autoclave body (60), bottom is equipped with discharge port, and low-temperature control device includes alcohol tank Body (61), electrically-controlled valve (62) and rotary-atomizing spray head (64), alcohol cabinet (61) are fixedly mounted on low-temp reaction kettle autoclave body (60) Top, rotary-atomizing spray head (64) is mounted on the bottom surface of low-temp reaction kettle autoclave body (60) lid, and alcohol cabinet (61) Outlet is connected to by pipeline and electrically-controlled valve (62) with the entrance of rotary-atomizing spray head (64), and 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 solid respectively On the inner wall of low-temp reaction kettle autoclave body (60), a pair of of stirring blade frame (66) is separately mounted to a pair of electronic slide unit for Dingan County (65) on sliding block, a pair of of fan-type stirring blade (67) is movably arranged on a pair of of stirring blade frame (66) by shaft respectively On, centrifugal equipment for separating liquid from solid includes centrifugal type solid/liquid separator (68), crystal hopper (69) and solution hopper (70), centrifugation The feed inlet of formula solid-liquid separator (68) is connected to the outlet at bottom of low-temp reaction kettle autoclave body (60), the entrance of crystal hopper (69) It is connected to the solid-phase outlet of centrifugal type solid/liquid separator (68), the entrance of solution hopper (70) and centrifugal type solid/liquid separator (68) Liquid-phase outlet connection, distillation type reaction kettle includes distillation type reaction kettle autoclave body (80), kettle cover (81), distilling apparatus, hydrofluoric acid Adding set and clear liquid draw-out device, distillation type reaction kettle autoclave body (80) top is opening, and it is anti-that kettle cover (81) is hinged on distillation type It answers 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), kettle cover (81) it is inverted cone-shaped, and one group of condensate tank(trap) (81-1) of the lower surface annular array of taper bevel edge, and is equipped with the bottom of kettle cover (81) Equipped with the collecting channel (81-2) being connected to respectively with one group of condensate tank(trap) (81-1), distilling apparatus includes electric boiling plate (82), refrigeration Plate (83), collector pipe (84) and distilled water tank (85), electric boiling plate (82) are fixedly mounted in distillation type reaction kettle autoclave body (80) On wall, cold plate (83) is mounted on the upper surface of kettle cover (81), and distilled water tank (85) is fixedly mounted on distillation type reaction kettle autoclave body (80) on outer wall, the both ends of collector pipe (84) are separately connected the water inlet of collecting channel (81-2) and distilled water tank (85), hydrogen Fluoric acid adding set includes hydrofluoric acid hopper (86), hydrofluoric acid feeder pipe (87) and metering valve (88), and hydrofluoric acid hopper (86) is solid Dingan County is on the outer wall of distillation type reaction kettle autoclave body (80), one end and hydrofluoric acid hopper (86) of hydrofluoric acid feeder pipe (87) Outlet, metering valve (88) is mounted on the other end of hydrofluoric acid feeder pipe (87), and is located at distillation type reaction kettle autoclave body (80) Interior, clear liquid draw-out device includes that web plate (89), pump (90) and drinking-water pipe (91), web plate (89) are fixedly mounted on distillation type reaction kettle On the inner wall of autoclave body (80), pump (90) be fixedly mounted on web plate (89), the both ends of drinking-water pipe (91) be separately connected pump (90) and The entrance of distilled water tank (85).
2. a kind of crystal evolution reaction system of tenofovir production line according to claim 1, which is characterized in that a pair of The track of electronic slide unit (65) is fixedly mounted on the inner wall of low-temp reaction kettle autoclave body (60) in parallel vertically respectively.
CN201710681340.9A 2017-08-10 2017-08-10 A kind of crystal evolution reaction system of tenofovir production line Active CN107266500B (en)

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107262008A (en) * 2017-08-21 2017-10-20 荆门市帅邦化学科技有限公司 A kind of crystal evolution reaction system of tenofovir production line
CN114164343A (en) * 2021-12-07 2022-03-11 江西宏科特种合金有限公司 Method for producing small-particle titanium sponge and special device thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102228463A (en) * 2005-06-13 2011-11-02 博瑞生物医药技术(苏州)有限公司 Tenofovir crystals
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102228463A (en) * 2005-06-13 2011-11-02 博瑞生物医药技术(苏州)有限公司 Tenofovir crystals
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

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