CN113582919A - Method and device for synthesizing 3-aminopyridine by tubular reactor - Google Patents
Method and device for synthesizing 3-aminopyridine by tubular reactor Download PDFInfo
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- CUYKNJBYIJFRCU-UHFFFAOYSA-N 3-aminopyridine Chemical compound NC1=CC=CN=C1 CUYKNJBYIJFRCU-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 33
- DFPAKSUCGFBDDF-UHFFFAOYSA-N Nicotinamide Chemical compound NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005086 pumping Methods 0.000 claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 22
- 239000010409 thin film Substances 0.000 claims abstract description 20
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 15
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- 229960003966 nicotinamide Drugs 0.000 claims abstract description 14
- 235000005152 nicotinamide Nutrition 0.000 claims abstract description 14
- 239000011570 nicotinamide Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 230000008020 evaporation Effects 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 239000000155 melt Substances 0.000 claims description 19
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001308 synthesis method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 3
- 239000000543 intermediate Substances 0.000 description 24
- 238000006731 degradation reaction Methods 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- 150000003927 aminopyridines Chemical class 0.000 description 4
- FFNVQNRYTPFDDP-UHFFFAOYSA-N 2-cyanopyridine Chemical compound N#CC1=CC=CC=N1 FFNVQNRYTPFDDP-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000003222 pyridines Chemical class 0.000 description 3
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- -1 aminopyridine compounds Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- RUPDGJAVWKTTJW-UHFFFAOYSA-N 2,3-dinitropyridine Chemical compound [O-][N+](=O)C1=CC=CN=C1[N+]([O-])=O RUPDGJAVWKTTJW-UHFFFAOYSA-N 0.000 description 1
- HLTDBMHJSBSAOM-UHFFFAOYSA-N 2-nitropyridine Chemical compound [O-][N+](=O)C1=CC=CC=N1 HLTDBMHJSBSAOM-UHFFFAOYSA-N 0.000 description 1
- GZPHSAQLYPIAIN-UHFFFAOYSA-N 3-pyridinecarbonitrile Chemical compound N#CC1=CC=CN=C1 GZPHSAQLYPIAIN-UHFFFAOYSA-N 0.000 description 1
- DFPAKSUCGFBDDF-ZQBYOMGUSA-N [14c]-nicotinamide Chemical compound N[14C](=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-ZQBYOMGUSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- CRWJEUDFKNYSBX-UHFFFAOYSA-N sodium;hypobromite Chemical compound [Na+].Br[O-] CRWJEUDFKNYSBX-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/73—Unsubstituted amino or imino radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses a method and a device for synthesizing 3-aminopyridine by using a tubular reactor, which comprises the following steps: step 1: pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor for reaction by adopting a first centrifugal pump and a second centrifugal pump, then pumping a reaction solution into a second tubular reactor, and pumping a sodium hydroxide solution into the second tubular reactor by adopting a third centrifugal pump; step 2: and then the reaction liquid enters a third tubular reactor for reaction, part of the reaction liquid circulates back to the third tubular reactor through a fourth centrifugal pump, part of the reaction liquid enters a centrifugal extractor for continuous extraction, the organic phase enters an intermediate tank, the organic phase in the intermediate tank enters a thin film evaporator for evaporation through a fifth centrifugal pump, and then the organic phase enters a melting crystallizer for crystallization to obtain a 3-aminopyridine product. The process can improve the content and yield of the 3-aminopyridine, greatly improve the production efficiency and greatly improve the safety.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a method and a device for synthesizing 3-aminopyridine by using a tubular reactor.
Background
Aminopyridine is an important derivative of pyridine and has wide application in the field of chemistry and chemical engineering. With the continuous development of scientific technology, the application range of aminopyridine compounds is on the rising trend year by year. Wherein, the 3-aminopyridine is one of the main aminopyridine compounds and is mainly used for synthesizing pesticides and medical intermediates. The current method for preparing 3-aminopyridine mainly comprises the following process routes: firstly, halogenated pyridine compounds are catalyzed and synthesized; secondly, the catalyst is synthesized by catalytic reduction of nitropyridine; thirdly, cyanopyridine is hydrolyzed and then synthesized by Hofmann degradation; fourthly, the pyridine is synthesized by acid amine of picoline and then Hofmann degradation; fifthly, formamide is directly synthesized by Hofmann degradation.
Compared with the preparation method, the method has the advantages that the initial raw material halogenated pyridine used in the first method is difficult to synthesize and expensive, the cost is increased due to the use of a metal catalyst in the reaction process, and the method is difficult to treat waste water and is not advisable. The method has harsh synthesis conditions of the dinitropyridine, lower yield, higher cost and non-mild conditions during the synthesis of the aminopyridine, and is not advisable. In the method, cyanopyridine serving as a raw material is low in price, reaction conditions are mild, the method is common, and the hydrolysis of cyanopyridine is followed by further Hofmann degradation reaction, so that the total yield of the reaction is not too high. In the fourth method, the picoline is firstly synthesized into acid amine and then subjected to Hofmann degradation to obtain the aminopyridine, the synthesis steps are more, and the final yield is lower, so that the method is not advisable. In the method five, formamide is directly used as a raw material, and aminopyridine is synthesized in a sodium hypobromite solution through Hofmann degradation.
As 3-aminopyridine is an important chemical raw material and has large market demand, the research and development of the environment-friendly, efficient and economic 3-aminopyridine preparation method suitable for industrial production has great significance.
Patent CN201810066600.6 discloses a one-step method for preparing 3-aminopyridine, which takes 3-cyanopyridine, sodium hydroxide and sodium hypochlorite as raw materials, and the raw materials are hydrolyzed, subjected to Hofmann degradation, and then extracted to obtain the 3-aminopyridine with the content of 98.2 percent and the yield of 93.8 percent; the early-stage reaction of the process requires 0 ℃, and sodium hypochlorite is supplemented for many times in the later stage, so that the process conditions are strict, the reaction is an intermittent reaction, the efficiency is low, and the yield is low.
CN202010017180.X discloses a preparation method of 3-aminopyridine, which takes nicotinamide, sodium hypochlorite and sodium hydroxide as raw materials, the reaction temperature is 0-20 ℃, and the reaction yield is 90%; the process is a batch reaction, the production efficiency is low, and the reaction yield is low.
The existing 3-aminopyridine production process has the following defects:
the 3-aminopyridine reaction is carried out under the condition of low temperature, the temperature requirement is higher, the energy consumption is high, the reaction yield is not high, most of the reaction is intermittent reaction, and the production efficiency is low.
Disclosure of Invention
The invention aims to provide a method and a device for synthesizing 3-aminopyridine by using a tubular reactor with high efficiency, high selectivity and high safety, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for synthesizing 3-aminopyridine by using a tubular reactor comprises the following steps:
step 1: pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor for reaction by adopting a first centrifugal pump and a second centrifugal pump, then pumping a reaction solution into a second tubular reactor, and pumping a sodium hydroxide solution into the second tubular reactor by adopting a third centrifugal pump;
step 2: and then the reaction liquid enters a third tubular reactor for reaction, part of the reaction liquid circulates back to the third tubular reactor through a fourth centrifugal pump, part of the reaction liquid enters a centrifugal extractor for continuous extraction, the organic phase enters an intermediate tank, the organic phase in the intermediate tank enters a thin film evaporator for evaporation through a fifth centrifugal pump, and then the organic phase enters a melting crystallizer for crystallization to obtain a 3-aminopyridine product.
Further, the concentration of the nicotinamide aqueous solution is 5% -20%.
Further, the concentration of the sodium hydroxide solution is 5% -30%.
Further, the reaction temperature of the first tubular reactor and the second tubular reactor is 0-50 ℃, preferably 10-30 ℃.
Further, the temperature of the third tubular reactor is 70-95 ℃.
Further, the feeding speed of the nicotinamide aqueous solution is 7-10 kg/min; the feeding speed of the sodium hypochlorite is 10-20 kg/min; the feeding speed of the sodium hydroxide solution is 2-5 kg/min.
Further, the temperature of the melt crystallization is 60-63 ℃.
The invention provides another technical scheme that: a device for utilizing a method for synthesizing 3-aminopyridine by using a tubular reactor comprises a first centrifugal pump, a second centrifugal pump, a first tubular reactor, a second tubular reactor, a third centrifugal pump, a third tubular reactor, a fourth centrifugal pump, a centrifugal extractor, an intermediate tank, a fifth centrifugal pump, a thin film evaporator and a melt crystallizer, wherein the first centrifugal pump and the second centrifugal pump are connected with the first tubular reactor, the first tubular reactor and the third centrifugal pump are connected with the second tubular reactor, the second tubular reactor is connected with the third tubular reactor, the third tubular reactor is connected with the centrifugal extractor through the fourth centrifugal pump, the centrifugal extractor is connected with the intermediate tank, the intermediate tank is connected with the thin film evaporator through the fifth centrifugal pump, and the thin film evaporator is connected with the melt crystallizer.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts a melt crystallizer and a melt crystallization mode, and the content of the 3-aminopyridine can reach more than 99.5 percent.
2. The invention is characterized in that the reaction is carried out by the first tubular reactor, the second tubular reactor and the third tubular reactor, and then the procedures of centrifugal extraction, evaporation, melting crystallization and the like are carried out in sequence, the process is continuous production, the production efficiency is greatly improved, the safety is greatly improved, the yield of the 3-aminopyridine can reach more than 98 percent, the process energy consumption is low, the reaction condition range is wide, and the operability is strong.
Drawings
FIG. 1 is a system configuration diagram of the apparatus of the present invention.
In the figure: 1. a first centrifugal pump; 2. a second centrifugal pump; 3. a first tubular reactor; 4. a second tubular reactor; 5. a third centrifugal pump; 6. a third tubular reactor; 7. a fourth centrifugal pump; 8. a centrifugal extractor; 9. an intermediate tank; 10. a fifth centrifugal pump; 11. a thin film evaporator; 12. a melt crystallizer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for synthesizing 3-aminopyridine by using a tubular reactor comprises the following steps:
step 1: pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by adopting a first centrifugal pump 1 and a second centrifugal pump 2, then pumping a reaction solution into a second tubular reactor 4, and pumping a sodium hydroxide solution into the second tubular reactor 4 by adopting a third centrifugal pump 5;
step 2: and then the reaction liquid enters a third tubular reactor 6 for reaction, a part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, a part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product.
A device used by a method for synthesizing 3-aminopyridine by using a tubular reactor comprises a first centrifugal pump 1, a second centrifugal pump 2, a first tubular reactor 3, a second tubular reactor 4, a third centrifugal pump 5, a third tubular reactor 6, a fourth centrifugal pump 7, a centrifugal extractor 8, an intermediate tank 9, a fifth centrifugal pump 10, a thin film evaporator 11 and a melt crystallizer 12, the first centrifugal pump 1 and the second centrifugal pump 2 are both connected with a first tubular reactor 3, the first tubular reactor 3 and the third centrifugal pump 5 are both connected with a second tubular reactor 4, the second tubular reactor 4 is connected with a third tubular reactor 6, the third tubular reactor 6 is connected with a centrifugal extractor 8 through a fourth centrifugal pump 7, the centrifugal extractor 8 is connected with an intermediate tank 9, the intermediate tank 9 is connected with a thin film evaporator 11 through a fifth centrifugal pump 10, and the thin film evaporator 11 is connected with a melt crystallizer 12.
Example 1:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 7kg/min, the feeding speed of the second centrifugal pump 2 is 20kg/min, and the reaction temperature is 20 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 2kg/min, and the reaction temperature is 20 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 85 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.6% and the yield is 98.3%.
Example 2:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 7kg/min, the feeding speed of the second centrifugal pump 2 is 20kg/min, and the reaction temperature is 10 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 2kg/min, and the reaction temperature is 10 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 95 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.7% and the yield is 98.5%.
Example 3:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 10kg/min, the feeding speed of the second centrifugal pump 2 is 10kg/min, and the reaction temperature is 30 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 5kg/min, and the reaction temperature is 30 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 70 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.5% and the yield is 98.5%.
Example 4:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 9kg/min, the feeding speed of the second centrifugal pump 2 is 15kg/min, and the reaction temperature is 40 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 4kg/min, and the reaction temperature is 40 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 80 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.5% and the yield is 98.2%.
Example 5:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 8kg/min, the feeding speed of the second centrifugal pump 2 is 20kg/min, and the reaction temperature is 50 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 4kg/min, and the reaction temperature is 50 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 90 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.5% and the yield is 98.1%.
Example 6:
pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor 3 for reaction by using a first centrifugal pump 1 and a second centrifugal pump 2, wherein the feeding speed of the first centrifugal pump 1 is 8kg/min, the feeding speed of the second centrifugal pump 2 is 20kg/min, and the reaction temperature is 25 ℃; then the reaction liquid enters a second tubular reactor 4, and simultaneously a third centrifugal pump 5 is used for pumping the sodium hydroxide solution into the second tubular reactor 4, wherein the feeding speed of the third centrifugal pump 5 is 3kg/min, and the reaction temperature is 25 ℃; and then the reaction liquid enters a third tubular reactor 6 for reaction, the reaction temperature is 78 ℃, part of the reaction liquid circulates back to the third tubular reactor 6 through a fourth centrifugal pump 7, part of the reaction liquid enters a centrifugal extractor 8 for continuous extraction, an organic phase enters an intermediate tank 9, then the organic phase in the intermediate tank 9 enters a thin film evaporator 11 through a fifth centrifugal pump 10 for evaporation, and then enters a melt crystallizer 12 for crystallization to obtain a 3-aminopyridine product, and the detection shows that the content is 99.6% and the yield is 98.4%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. A method for synthesizing 3-aminopyridine by using a tubular reactor is characterized by comprising the following steps:
step 1: pumping a nicotinamide aqueous solution and a sodium hypochlorite solution into a first tubular reactor (3) for reaction by adopting a first centrifugal pump (1) and a second centrifugal pump (2), then pumping a reaction solution into a second tubular reactor (4), and simultaneously pumping a sodium hydroxide solution into the second tubular reactor (4) by adopting a third centrifugal pump (5);
step 2: and then the reaction liquid enters a third tubular reactor (6) for reaction, a part of the reaction liquid circulates back to the third tubular reactor (6) through a fourth centrifugal pump (7), a part of the reaction liquid enters a centrifugal extractor (8) for continuous extraction, an organic phase enters an intermediate tank (9), the organic phase in the intermediate tank (9) enters a thin film evaporator (11) for evaporation through a fifth centrifugal pump (10), and then enters a melt crystallizer (12) for crystallization to obtain a 3-aminopyridine product.
2. The process of claim 1, wherein the concentration of the aqueous nicotinamide solution is 5% to 20%.
3. The tubular reactor process of claim 1, wherein the sodium hydroxide solution is present in a concentration of 5% to 30%.
4. The tubular reactor process for the synthesis of 3-aminopyridine according to claim 1, characterized in that the reaction temperature of the first tubular reactor (3) and the second tubular reactor (4) is between 0 ℃ and 50 ℃, preferably between 10 ℃ and 30 ℃.
5. The tubular reactor process for the synthesis of 3-aminopyridine according to claim 1, characterized in that the temperature of the third tubular reactor (6) is comprised between 70 and 95 ℃.
6. The tubular reactor process for the synthesis of 3-aminopyridine of claim 1, wherein the aqueous nicotinamide solution is fed at a rate of 7-10 kg/min; the feeding speed of the sodium hypochlorite is 10-20 kg/min; the feeding speed of the sodium hydroxide solution is 2-5 kg/min.
7. The tubular reactor process of claim 1, wherein the melt crystallization temperature is from 60 ℃ to 63 ℃.
8. A device utilized by the tubular reactor synthesis method of 3-aminopyridine according to claim 1, characterized by comprising a first centrifugal pump (1), a second centrifugal pump (2), a first tubular reactor (3), a second tubular reactor (4), a third centrifugal pump (5), a third tubular reactor (6), a fourth centrifugal pump (7), a centrifugal extractor (8), an intermediate tank (9), a fifth centrifugal pump (10), a thin film evaporator (11) and a melt crystallizer (12), wherein the first centrifugal pump (1) and the second centrifugal pump (2) are connected with the first tubular reactor (3), the first tubular reactor (3) and the third centrifugal pump (5) are connected with the second tubular reactor (4), the second tubular reactor (4) is connected with the third tubular reactor (6), the third tubular reactor (6) is connected with the centrifugal extractor (8) through the fourth centrifugal pump (7), the centrifugal extractor (8) is connected with the intermediate tank (9), the intermediate tank (9) is connected with the thin film evaporator (11) through the fifth centrifugal pump (10), and the thin film evaporator (11) is connected with the melt crystallizer (12).
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| CN115282879A (en) * | 2022-08-08 | 2022-11-04 | 单县欣润化工有限公司 | Raw material supply system and process for synthesizing 2-chloro-5-trifluoromethylpyridine |
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| CN111943884A (en) * | 2019-05-14 | 2020-11-17 | 上海玲骰生物科技有限公司 | Preparation method of medical intermediate 2-chloro-3-aminopyridine |
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| CN115282879A (en) * | 2022-08-08 | 2022-11-04 | 单县欣润化工有限公司 | Raw material supply system and process for synthesizing 2-chloro-5-trifluoromethylpyridine |
| CN115282879B (en) * | 2022-08-08 | 2024-04-05 | 单县欣润化工有限公司 | Raw material supply system and process for synthesizing 2-chloro-5-trifluoromethyl pyridine |
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