CN115025728A - Preparation device and method of hydroxypyrazine sodium salt - Google Patents
Preparation device and method of hydroxypyrazine sodium salt Download PDFInfo
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- CN115025728A CN115025728A CN202210463193.9A CN202210463193A CN115025728A CN 115025728 A CN115025728 A CN 115025728A CN 202210463193 A CN202210463193 A CN 202210463193A CN 115025728 A CN115025728 A CN 115025728A
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Abstract
The invention discloses a preparation device and a preparation method of hydroxypyrazine sodium salt, wherein the preparation device comprises a first raw material supply system, a first microchannel reactor, a second raw material supply system, a second microchannel reactor and a distillation crystallization tank which are sequentially connected through pipelines along the moving direction of materials, the first raw material supply system comprises a plurality of first raw material tanks and a plurality of first temperature control modules connected with the first raw material tanks, the first temperature control modules are connected with the first microchannel reactor through pipelines, the second raw material supply system comprises a second raw material tank and a plurality of third raw material tanks, the inlet end of the second raw material tank is connected with the outlet end of the first microchannel reactor through a pipeline, the outlet end of the second raw material tank and the outlet end of the third raw material tank are respectively connected with the second temperature control module through pipelines, and the second temperature control module is connected with the second microchannel reactor through a pipeline. The invention can obviously improve the reaction efficiency, has high yield, reduces side reaction and has simple operation.
Description
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a device and a method for preparing hydroxypyrazine sodium salt.
Background
The hydroxypyrazine sodium salt is an important chemical raw material for preparing bulk drugs and human medicines, is also an important organic intermediate, and has various problems of laggard production process, harsh conditions of high-temperature distillation, more side reactions, further improved product quality, severe market competition and the like in the industrial production of the hydroxypyrazine sodium salt. At present, the main industrial production process of the hydroxypyrazine sodium salt adopts a kettle type reaction mode, but because the difficulty of the synthesis process is high, generally conventional preparation processes all need high temperature and high vacuum equipment, the operation is complicated, and the yield is low, so that a microchannel reactor and a method for preparing the hydroxypyrazine sodium salt by using the microchannel reactor are needed to be researched.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a device and a method for preparing a hydroxypyrazine sodium salt, which are capable of remarkably improving reaction efficiency, high in yield, capable of reducing side reactions and simple in operation.
In order to achieve the above object, the present invention adopts the following technical solutions:
the utility model provides a preparation facilities of hydroxypyrazine sodium salt, include the first raw materials feed system who connects gradually through the pipeline along the material moving direction, first microchannel reactor, second raw materials feed system, second microchannel reactor and distillation crystallizer, first raw materials feed system includes a plurality of first head tanks and a plurality of first accuse temperature module of being connected with first head tank, first accuse temperature module passes through the first microchannel reactor of tube coupling, second raw materials feed system includes second head tank and a plurality of third head tank, the exit end of the first microchannel reactor of tube coupling is passed through to the entrance point of second head tank, the exit end of second head tank and the exit end of third head tank are passed through tube coupling second accuse temperature module respectively, second accuse temperature module passes through tube coupling second microchannel reactor.
Preferably, a metering pump and a pressure gauge are arranged on connecting pipelines between the first raw material tank and the first temperature control module, between the second raw material tank and the second temperature control module and between the third raw material tank and the second temperature control module.
The method for preparing the hydroxypyrazine sodium salt by using the preparation device comprises the following specific steps:
s1, respectively placing methyl chloroacetate and ammonia water in two first material tanks, and respectively introducing the two first material tanks into corresponding first temperature control modules according to a certain proportion to control the temperature;
s2, introducing the temperature-controlled methyl chloroacetate and ammonia water into a first microchannel reactor for reaction to obtain a glycinamide reaction solution, and sending the glycinamide reaction solution into a second raw material tank;
s3, respectively placing the sodium hydroxide aqueous solution and the glyoxal aqueous solution into two third material tanks, and respectively introducing the glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into corresponding second temperature control modules according to a certain proportion to control the temperature;
s4, introducing the temperature-controlled glycinamide reaction liquid, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor for reaction to obtain a hydroxypyrazine sodium salt reaction liquid;
and S5, introducing the reaction liquid of the hydroxypyrazine sodium salt into a distillation crystallization tank, cooling and crystallizing after distilling water, and drying to obtain the hydroxypyrazine sodium salt.
Preferably, in step S1, the concentration of the ammonia water is 20 to 30%, and the molar ratio of methyl chloroacetate to ammonia water (calculated as ammonia) is 1: (2.1-2.3).
Preferably, in the step S1, the temperature is controlled to be 15 to 25 ℃.
Preferably, in the step S2, the reaction time is 30 to 90S, and the reaction pressure is 0 to 5 bar.
Preferably, in the step S3, the concentration of the glyoxal aqueous solution is 30-40%, and the concentration of the sodium hydroxide aqueous solution is 50-60%.
Preferably, in the step S3, the molar ratio of the glycinamide reaction liquid (calculated as methyl chloroacetate), the aqueous glyoxal solution (calculated as glyoxal) and the aqueous sodium hydroxide solution (calculated as sodium hydroxide) is 1: (0.95-1.05): (2.0-2.2).
Preferably, in the step S3, the temperature is controlled to be-5 to 5 ℃.
Preferably, in the step S4, the reaction time is 30 to 90S, and the reaction pressure is 0 to 5 bar.
The invention has the advantages that:
(1) the method adopts a continuous flow microchannel reactor, greatly shortens the reaction time, has the total yield of two-step reaction of 95-97.5 percent, obviously improves the reaction efficiency, reduces the unit consumption of raw materials, and has the advantages of simple operation, safe use, low production cost, environment-friendly process and avoidance of high-temperature risk;
(2) the mixing effect of all raw materials in the microchannel is excellent, the amplification effect is avoided, the reaction temperature is accurately controlled, the reaction conversion rate is improved, the side reaction is reduced, and the method is suitable for industrial production of the hydroxypyrazine sodium salt;
(3) the microchannel reactor used in the invention is made of special glass, has excellent corrosion resistance, and is a continuous flow reaction in the processes of feeding, mixing, reacting and the like in the microchannel reactor, thereby effectively avoiding the serious problem of ammonia gas overflow, and being safe and environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
The meaning of the reference symbols in the figures: 1. the system comprises a first microchannel reactor, a second microchannel reactor, a distillation crystallizer, a first raw material tank, a first temperature control module, a second raw material tank, a third raw material tank, a first raw material tank, a second temperature control module, a metering pump, a pressure gauge and a control module, wherein the first microchannel reactor, the second microchannel reactor, the 3 distillation crystallizer, the first raw material tank, the 5 first temperature control module, the 6 second raw material tank, the 7 third raw material tank, the 8 second temperature control module, the 9 metering pump, the 10 metering pump and the pressure gauge are arranged in the distillation crystallizer.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments.
Referring to fig. 1, the device for preparing hydroxypyrazine sodium salt of the present invention comprises a first raw material supply system and a first microchannel reactor 1 connected in sequence by a pipeline along the material moving direction, the second raw material supply system, second microchannel reactor 2 and distillation crystallizer 3, first raw material supply system includes a plurality of first head tanks 4 and a plurality of first accuse temperature module 5 of being connected with first head tank 4, first accuse temperature module 5 passes through first microchannel reactor 1 of tube coupling, second raw material supply system includes second head tank 6 and a plurality of third head tank 7, the exit end of the entrance point of second head tank 6 passes through the exit end of tube coupling first microchannel reactor 1, the exit end of second head tank 6 and the exit end of third head tank 7 pass through tube coupling second accuse temperature module 8 respectively, second accuse temperature module 8 passes through tube coupling second microchannel reactor 2.
And a metering pump 9 and a pressure gauge 10 are arranged on connecting pipelines between the first raw material tank 4 and the first temperature control module 5, between the second raw material tank 6 and the second temperature control module 8 and between the third raw material tank 7 and the second temperature control module 8.
Each module in the microchannel reactor is made of monocrystalline silicon, special glass, ceramics, corrosion-resistant alloy, Teflon and the like, and has excellent corrosion resistance.
The method for preparing the hydroxyl pyrazine sodium salt by using the preparation device comprises the following specific steps of:
s1, respectively placing methyl chloroacetate and ammonia water in two first material tanks 4, and respectively introducing the methyl chloroacetate and the ammonia water into corresponding first temperature control modules 5 according to a certain ratio to control the temperature, wherein the temperature is 15-25 ℃; wherein the concentration of the ammonia water is 20-30%, and the molar ratio of methyl chloroacetate to ammonia water calculated by ammonia is 1: 2.1 to 2.3.
S2, introducing the methyl chloroacetate and ammonia water subjected to temperature control into the first microchannel reactor 1 for reaction, wherein the reaction time is 30-90S, and the reaction pressure is 0-5 bar, so as to obtain a glycinamide reaction solution, and sending the glycinamide reaction solution into the second raw material tank 6;
s3, respectively placing a sodium hydroxide aqueous solution and a glyoxal aqueous solution in two third material tanks 7, wherein the concentration of the glyoxal aqueous solution is 30-40% and the concentration of the sodium hydroxide aqueous solution is 50-60%, and then respectively introducing the glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into corresponding second temperature control modules 8 according to a certain ratio to control the temperature, wherein the temperature is-5 ℃; wherein the molar ratio of the glycinamide reaction liquid calculated by methyl chloroacetate, the glyoxal aqueous solution calculated by glyoxal and the sodium hydroxide aqueous solution calculated by sodium hydroxide is 1: 0.95-1.05: 2.0 to 2.2;
s4, introducing the temperature-controlled glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor 2 for reaction, wherein the reaction time is 30-90S, and the reaction pressure is 0-5 bar, so as to obtain a hydroxypyrazine sodium salt reaction solution;
and S5, introducing the reaction liquid of the hydroxypyrazine sodium salt into a distillation crystallization tank 3, cooling and crystallizing after distilling water, and drying to obtain the hydroxypyrazine sodium salt.
Example 1
The preparation method of the hydroxypyrazine sodium salt comprises the following specific steps:
s1, respectively placing methyl chloroacetate and ammonia water with the mass concentration of 20% into two first raw material tanks 4, setting the flow rate ratio of the ammonia water solution to the methyl chloroacetate corresponding to a metering pump 9 to 178.5g2.1mol, and setting the flow rate ratio to be 2.1 eq: 108g of 1.00mol and 1.0eq are respectively introduced into the corresponding first temperature control modules 5 for temperature control, and the temperature is 15-25 ℃;
s2, introducing the methyl chloroacetate and ammonia water subjected to temperature control into the first microchannel reactor 1 for reaction, wherein the reaction time is 90S, and the reaction pressure is 0-5 bar, so as to obtain a glycinamide reaction solution, and sending the glycinamide reaction solution into the second raw material tank 6;
s3, placing the 50% sodium hydroxide aqueous solution and the 40% glyoxal aqueous solution into two third raw material tanks 7, respectively, and setting the flow rate ratio of the metering pump 9 corresponding to the sodium hydroxide solution, the glyoxal solution, and the glycinamide solution to 160g2.0mol, 2.0 eq: 138g0.95mol, 0.95 eq: 278g, and respectively introducing into corresponding second temperature control modules 8 for temperature control, wherein the temperature is-5 ℃;
s4, introducing the temperature-controlled glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor 2 for reaction, wherein the reaction time is 90S, and the reaction pressure is 0-5 bar, so as to obtain a hydroxypyrazine sodium salt reaction solution;
and S5, introducing the hydroxyl pyrazine sodium salt reaction liquid into a distillation crystallization tank 3, cooling and crystallizing after distilling water, and drying to obtain the hydroxyl pyrazine sodium salt.
Example 2
The preparation method of the hydroxypyrazine sodium salt comprises the following specific steps:
s1, respectively placing methyl chloroacetate and ammonia water with the mass concentration of 25% into two first raw material tanks 4, and setting the flow rate ratio of the ammonia water solution to the methyl chloroacetate corresponding to a metering pump 9 to be 150g2.2mol, 2.2 eq: 108g of 1.00mol and 1.0eq are respectively introduced into the corresponding first temperature control modules 5 for temperature control, and the temperature is 15-25 ℃;
s2, introducing the methyl chloroacetate and ammonia water subjected to temperature control into the first microchannel reactor 1 for reaction, wherein the reaction time is 60S, and the reaction pressure is 0-5 bar, so as to obtain a glycinamide reaction solution, and sending the glycinamide reaction solution into the second raw material tank 6;
s3, placing the 55% sodium hydroxide aqueous solution and the 30% glyoxal aqueous solution into two third material tanks 7, respectively, and setting the flow rate ratio of the metering pump 9 corresponding to the sodium hydroxide solution, the glyoxal solution, and the glycinamide solution to 168g2.1mol, 2.1 eq: 193g1.0mol, 1.0 eq: 258g, respectively introducing the temperature control materials into corresponding second temperature control modules 8 for temperature control, wherein the temperature is-5 ℃;
s4, introducing the temperature-controlled glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor 2 for reaction, wherein the reaction time is 60S, and the reaction pressure is 0-5 bar, so as to obtain a hydroxypyrazine sodium salt reaction solution;
and S5, introducing the reaction liquid of the hydroxypyrazine sodium salt into a distillation crystallization tank 3, cooling and crystallizing after distilling water, and drying to obtain the hydroxypyrazine sodium salt.
Example 3
The preparation method of the hydroxypyrazine sodium salt comprises the following specific steps:
s1, respectively placing methyl chloroacetate and ammonia water with the mass concentration of 30% in two first material tanks 4, setting the flow rate ratio of the ammonia water solution to the methyl chloroacetate corresponding to a metering pump 9 to be 130g2.3mol, and setting the flow rate ratio to be 2.3 eq: 108g of 1.00mol and 1.0eq are respectively introduced into the corresponding first temperature control modules 5 for temperature control, and the temperature is 15-25 ℃;
s2, introducing the methyl chloroacetate and ammonia water subjected to temperature control into the first microchannel reactor 1 for reaction for 30S at a reaction pressure of 0-5 bar to obtain a glycinamide reaction solution, and feeding the glycinamide reaction solution into the second raw material tank 6;
s3, respectively placing a 60% sodium hydroxide aqueous solution and a 35% glyoxal aqueous solution into two third material tanks 7, and setting the flow rate ratio of a metering pump 9 corresponding to the sodium hydroxide solution, the glyoxal solution and the glycinamide solution to 176g2.2mol, 2.2 eq: 174g1.05mol, 1.05 eq: 238g, and respectively introducing the temperature control materials into corresponding second temperature control modules 8 for temperature control, wherein the temperature is-5 ℃;
s4, introducing the temperature-controlled glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor 2 for reaction, wherein the reaction time is 30S, and the reaction pressure is 0-5 bar, so as to obtain a hydroxypyrazine sodium salt reaction solution;
and S5, introducing the reaction liquid of the hydroxypyrazine sodium salt into a distillation crystallization tank 3, cooling and crystallizing after distilling water, and drying to obtain the hydroxypyrazine sodium salt.
Comparative example
The preparation method of the hydroxypyrazine sodium salt comprises the following specific steps:
s1, placing ammonia water with the mass concentration of 30% into a reaction kettle, introducing frozen fresh water into a jacket of the reaction kettle to control the temperature, wherein the temperature is 15-25 ℃, placing methyl chloroacetate into a dropwise adding kettle, and the feeding amounts of the 30% ammonia water and the 30% methyl chloroacetate are 189kg, 3.3kmol and 2.36eq respectively: 152kg, 1.40Kmol, 1.0 eq;
s2, dropwise adding methyl chloroacetate into temperature-controlled ammonia water for reaction, wherein the dropwise adding time is 1h, the reaction time is 3-4 h, the reaction pressure is 0-5 bar, and the reaction temperature is 12-25 ℃, so that a glycinamide reaction solution is obtained;
s3, respectively placing a 50% sodium hydroxide aqueous solution and a 35% glyoxal aqueous solution into two dropping tanks, setting the feeding amount of the sodium hydroxide aqueous solution and the glyoxal aqueous solution to 235kg, 2.94 Kmol: 220kg, 1.33 kmol;
s4, introducing glycol into a jacket of the reaction kettle of the glycinamide reaction liquid to control the temperature, wherein the temperature is-5 ℃, simultaneously dropwise adding 50% of sodium hydroxide aqueous solution and 35% of glyoxal aqueous solution for 3-4 hours, reacting for 1 hour, the reaction pressure is 0-5 bar, and the reaction temperature is-5 ℃ to obtain a sodium salt reaction liquid of the hydroxypyrazine;
and S5, cooling and crystallizing the reaction solution of the hydroxypyrazine sodium salt after distilled water is added, and drying to obtain the hydroxypyrazine sodium salt.
And (3) analyzing an experimental result:
1. the products obtained in examples 1 to 3 and comparative example were weighed and the yield was calculated, respectively, and the calculation results are shown in table 1.
TABLE 1 quality and yield of hydroxypyrazine sodium salts in examples 1-3 and comparative examples
As can be seen from table 1, the yield of the product obtained in examples 1 to 3 is significantly higher than that of the conventional preparation method in the comparative example, which indicates that the preparation method of the present invention can improve the yield of the hydroxypyrazine sodium salt.
2. 1000g of hydroxypyrazine sodium salt product was produced by the methods of example 3 and comparative example, respectively, and the consumption amounts of methyl chloroacetate, ammonia water, aqueous glyoxal solution, and aqueous sodium hydroxide solution were calculated, and the calculation results are shown in Table 2.
TABLE 2 consumption of methyl chloroacetate, aqueous ammonia, aqueous glyoxal solution, and aqueous sodium hydroxide solution
As can be seen from Table 2, the consumption amounts of methyl chloroacetate, ammonia water, aqueous glyoxal solution, and aqueous sodium hydroxide solution in example 3 were much smaller than those in the comparative examples. This is because in example 3, methyl chloroacetate reacted with ammonia to form glycinamide and then immediately reacted with glyoxal and sodium hydroxide in the second step, which reduced the side reactions in the tank reaction process, in the comparative example, the tank reaction apparatus caused hydrolysis of glycinamide hydrochloride during a long reaction time and caused disproportionation of sodium hydroxide and glyoxal during the second reaction process, so that continuous production was possible by the microchannel reactor, and the generation of side reactions was reduced.
The foregoing shows and describes the general principles, principal features and advantages of the invention. It should be understood by those skilled in the art that the above embodiments do not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent variations fall within the scope of the present invention.
Claims (10)
1. The preparation device of the hydroxypyrazine sodium salt is characterized by comprising a first raw material supply system, a first microchannel reactor (1), a second raw material supply system, a second microchannel reactor (2) and a distillation crystallizer (3) which are sequentially connected through pipelines along the material moving direction, wherein the first raw material supply system comprises a plurality of first raw material tanks (4) and a plurality of first temperature control modules (5) connected with the first raw material tanks (4), the first temperature control modules (5) are connected with the first microchannel reactor (1) through pipelines, the second raw material supply system comprises a second raw material tank (6) and a plurality of third raw material tanks (7), the inlet end of the second raw material tank (6) is connected with the outlet end of the first microchannel reactor (1) through a pipeline, the outlet end of the second raw material tank (6) and the outlet end of the third raw material tanks (7) are respectively connected with the second temperature control modules (8) through pipelines, and the second temperature control module (8) is connected with the second microchannel reactor (2) through a pipeline.
2. The preparation device of hydroxypyrazine sodium salt according to claim 1, wherein a metering pump (9) and a pressure gauge (10) are disposed on the connection pipeline between the first raw material tank (4) and the first temperature control module (5), between the second raw material tank (6) and the second temperature control module (8), and between the third raw material tank (7) and the second temperature control module (8).
3. The method for preparing a hydroxypyrazine sodium salt by using the preparation apparatus according to claim 1, comprising the following specific steps:
s1, respectively placing methyl chloroacetate and ammonia water in two first material tanks (4), and respectively introducing the methyl chloroacetate and the ammonia water into corresponding first temperature control modules (5) according to a certain proportion to control the temperature;
s2, introducing the temperature-controlled methyl chloroacetate and ammonia water into the first microchannel reactor (1) for reaction to obtain a glycinamide reaction solution, and feeding the glycinamide reaction solution into a second raw material tank (6);
s3, respectively placing a sodium hydroxide aqueous solution and a glyoxal aqueous solution into two third material tanks (7), and then respectively introducing the glycinamide reaction liquid, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into corresponding second temperature control modules (8) according to a certain ratio for temperature control;
s4, introducing the temperature-controlled glycinamide reaction solution, the sodium hydroxide aqueous solution and the glyoxal aqueous solution into a second microchannel reactor (2) for reaction to obtain a hydroxypyrazine sodium salt reaction solution;
and S5, introducing the reaction liquid of the hydroxypyrazine sodium salt into a distillation crystallization tank (3), cooling and crystallizing after distilled water, and drying to obtain the hydroxypyrazine sodium salt.
4. A method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S1, the concentration of ammonia water is 20-30%, and the molar ratio of methyl chloroacetate to ammonia water (calculated as ammonia) is 1: (2.1-2.3).
5. The method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S1, the temperature is controlled to 15-25 ℃.
6. The method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S2, the reaction time is 30-90S, and the reaction pressure is 0-5 bar.
7. The method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S3, the concentration of the glyoxal water solution is 30-40%, and the concentration of the sodium hydroxide water solution is 50-60%.
8. The method for preparing a sodium salt of hydroxypyrazine according to claim 3, wherein in step S3, the molar ratio of the glycinamide reaction solution (calculated as methyl chloroacetate), the aqueous glyoxal solution (calculated as glyoxal) and the aqueous sodium hydroxide solution (calculated as sodium hydroxide) is 1: (0.95-1.05): (2.0-2.2).
9. The method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S3, the temperature is controlled to be-5 ℃.
10. The method for preparing a hydroxypyrazine sodium salt according to claim 3, wherein in step S4, the reaction time is 30-90S, and the reaction pressure is 0-5 bar.
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