CN213416718U - 4, 6-dichloropyrimidine synthesis system - Google Patents
4, 6-dichloropyrimidine synthesis system Download PDFInfo
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- CN213416718U CN213416718U CN202021263738.4U CN202021263738U CN213416718U CN 213416718 U CN213416718 U CN 213416718U CN 202021263738 U CN202021263738 U CN 202021263738U CN 213416718 U CN213416718 U CN 213416718U
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Abstract
The utility model relates to the field of 4, 6-dichloropyrimidine production systems, and discloses a 4, 6-dichloropyrimidine synthesis system, which comprises a finished product synthesis assembly, wherein the finished product synthesis assembly comprises a substitution kettle, a hydrolysis kettle, an alkali washing kettle, a first sewage discharge pipe and a first distillation kettle, the device comprises a first exhaust pipe, a crystallization kettle and a centrifugal separator, wherein a feed inlet of the hydrolysis kettle is connected with a discharge outlet of a substitution kettle, a feed inlet of an alkali washing kettle is connected with a discharge outlet of the hydrolysis kettle, a liquid inlet end of a first sewage discharge pipe and a feed inlet of a first distillation kettle are selectively connected with a discharge outlet of the alkali washing kettle, a first steam outlet of the first distillation kettle is connected with the substitution kettle, a first exhaust pipe is communicated with a second steam outlet of the first distillation kettle, a feed inlet of the crystallization kettle is communicated with a liquid outlet of the first distillation kettle, a feed inlet of the centrifugal separator is connected with a discharge outlet of the crystallization kettle, and a liquid phase outlet of the centrifugal separator is communicated with a feed inlet of the. The utility model discloses can effectively carry out recycle to the tetrachloroethylene.
Description
Technical Field
The utility model relates to a 4, 6-dichloro pyrimidine production system field, concretely relates to 4, 6-dichloro pyrimidine synthesis system.
Background
4, 6-dichloropyrimidine is an important medical intermediate. Can be used for synthesizing medicines for treating bacterial infection such as hemolytic streptococcus, pneumococcus, meningococcus, etc., such as sulfonamides, sulfanilamide-6-methoxypyrimidine; sulfamonomethoxine (sulfametoxin); also can be used for synthesizing anticancer drug fluorouracil. Synthesizing the strobilurin fungicide azoxystrobin.
4, 6-dichloropyrimidine is produced in the production process and needs to be distilled through a distillation still, the steam product obtained by distillation at present contains tetrachloroethylene serving as an extracting agent, and the products are regarded as waste to be treated and cannot be recycled.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome above-mentioned technique not enough, provide a 4, 6-dichloro pyrimidine synthesis system, solve among the prior art 4, 6-dichloro pyrimidine and do not carry out recycle's technical problem to tetrachloroethylene in the in-process of production.
In order to achieve the technical purpose, the technical scheme of the utility model provides a 4, 6-dichloropyrimidine synthesis system, which is characterized in that the system comprises a finished product synthesis assembly, the finished product synthesis assembly comprises a substitution kettle, a hydrolysis kettle, an alkaline washing kettle, a first sewage discharge pipe, a first distillation kettle, a first exhaust pipe, a crystallization kettle, a centrifugal separator and a dryer, a feed inlet of the hydrolysis kettle is connected with a discharge port of the substitution kettle, a feed inlet of the alkaline washing kettle is connected with a discharge port of the hydrolysis kettle, a liquid inlet end of the first sewage discharge pipe and a feed inlet of the first distillation kettle are selectively connected with a discharge port of the alkaline washing kettle, a first steam outlet of the first distillation kettle is connected with the substitution kettle, the first exhaust pipe is communicated with a second steam outlet of the first distillation kettle, a feed inlet of the crystallization kettle is communicated with a liquid outlet of the first distillation kettle, the feed inlet of the centrifugal separator is connected with the discharge hole of the crystallization kettle, the liquid phase outlet of the centrifugal separator is communicated with the feed inlet of the crystallization kettle, and the feed inlet of the dryer is connected with the solid phase outlet of the centrifugal separator.
Compared with the prior art, the beneficial effects of the utility model include: in the production process of the 4, 6-dichloropyrimidine, in a first distillation kettle, the substituted material is heated to start decompression distillation to remove the solvent tetrachloroethylene, and the product obtained by distillation is introduced into the substitution kettle, so that the solvent tetrachloroethylene is recycled.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The utility model provides a 4, 6-dichloropyrimidine synthesis system, as shown in figure 1, including finished product synthesis subassembly 1, byproduct recovery subassembly 2, waste gas absorption tower 3, finished product synthesis subassembly 1 is including replacing cauldron 1a, hydrolysis kettle 1b, alkali wash cauldron 1c, first blow-off pipe 1j, first stills 1d, first exhaust pipe 1e, crystallization kettle 1f, centrifugal separator 1g, desicator 1h, hydrolysis kettle 1 b's feed inlet links to each other with the discharge gate of replacing cauldron 1 a.
A valve is arranged at a feed inlet of the substituted kettle 1 a.
Specifically, a jacket is arranged outside the hydrolysis kettle 1b, the hydrolysis kettle 1b is cooled by injecting frozen brine into the jacket, and a valve is arranged at a feed inlet of the hydrolysis kettle 1 b.
The feed inlet of the alkaline washing kettle 1c is connected with the discharge outlet of the hydrolysis kettle 1b, the liquid inlet end of the first drain pipe 1j and the feed inlet of the first distillation kettle 1d are selectively connected with the discharge outlet of the alkaline washing kettle 1c, and the first steam outlet of the first distillation kettle 1d is connected with the substitution kettle 1 a.
The liquid inlet end of the first sewage discharge pipe 1j and the liquid inlet end of the first distillation still 1d can be selectively opened or closed by arranging a valve.
Specifically, a valve is arranged at a first steam outlet of the first distillation kettle 1d, the finished product synthesis assembly 1 further comprises a containing tank 1i, a liquid inlet end of the containing tank 1i is connected with the first steam outlet of the first distillation kettle 1d, a liquid outlet end of the containing tank 1i is connected with a feed inlet of the substituted kettle 1a, and a valve is arranged at a liquid outlet end of the containing tank 1 i.
The first exhaust pipe 1e communicates with the second vapor outlet of the first still 1 d.
Specifically, the first exhaust pipe 1e is provided with a valve.
The feed inlet of the crystallization kettle 1f is communicated with the liquid outlet of the first distillation kettle 1 d.
Specifically, a valve is arranged at a feed inlet of the crystallization kettle 1 f.
The feed inlet of the centrifugal separator 1g is connected with the discharge outlet of the crystallization kettle 1f, and the liquid phase outlet of the centrifugal separator 1g is communicated with the feed inlet of the crystallization kettle 1 f.
The centrifugal separator 1g may be any of various devices having a centrifugal separation function, and specifically, a centrifugal separator is used in the present application, but the type of the centrifugal separator 1g is not limited thereto.
Specifically, the feed port and the liquid phase outlet of the centrifugal separator 1g are provided with valves.
The feed inlet of the drier 1h was connected to the solid phase outlet of the centrifugal separator 1 g.
Specifically, a valve is arranged at a feed inlet of the dryer 1 h.
The dryer 1h may be various apparatuses having a drying function, and specifically, the dryer 1h is a double cone dryer, but the type of the dryer 1h is not limited thereto.
The byproduct recovery assembly 2 comprises a second distillation kettle 2a, a first recovery tank 2b, a neutralization kettle 2c, a first condenser 2d, a dehydration kettle 2e, a filter 2f, an evaporator 2g, a solvent intermediate tank 2h and a second recovery tank 2i, wherein feed inlets of the second distillation kettle 2a and the alkali washing kettle 1c can be selectively connected with a discharge outlet of the hydrolysis kettle 1 b.
The feed inlet of the second distillation still 2a is provided with a valve.
The feed inlets of the second distillation kettle 2a and the caustic washing kettle 1c are selectively opened as required by arranging valves.
The feed port of the first recovery tank 2b is connected to the vapor outlet of the second distillation still 2 a.
Specifically, a valve is arranged at the feed inlet of the first recovery tank 2 b.
The neutralization kettle 2c is connected with a liquid outlet of the second distillation kettle 2 a.
Specifically, a valve is arranged at a feed inlet of the neutralization kettle 2 c.
The feed inlets of the dehydration kettle 2e and the first condenser 2d are selectively connected with the discharge outlet of the neutralization kettle 2 c.
Specifically, a valve is arranged at the feed inlet of the dehydration kettle 2 e.
Through setting up the valve for the feed inlet of dehydration cauldron 2e, first condenser 2d is optional to be opened.
The first condenser 2d may be any of various devices having a condensing function, and the first condenser 2d used in the present application is a shell and tube condenser, but the type of the first condenser 2d is not limited thereto.
The inlet of the filter 2f is connected to the outlet of the first condenser 2 d.
The filter 2f may be various filters 2f such as a plate and frame filter, and the filter 2f used in the present application is a frame filter, but the type of the filter 2f is not limited thereto.
Specifically, the inlet port of the filter 2f is provided with a valve.
The feed inlet of the evaporator 2g is connected to the liquid phase outlet of the filter 2f, and the liquid phase outlet of the evaporator 2g is connected to the feed inlet of the first condenser 2 d.
Specifically, the feed inlet and the liquid phase port of the evaporator 2g are provided with valves.
The feed inlet of the solvent intermediate tank 2h is communicated with the steam outlet of the dehydration kettle 2e, and the second recovery tank 2i is communicated with the liquid outlet of the dehydration kettle 2 e.
The inlet end of the waste gas absorption tower 3 is communicated with the outlet end of the first exhaust pipe 1 e.
The utility model discloses a concrete work flow: adding phosphorus oxychloride and 4, 6-dihydroxypyrimidine serving as raw materials into a substitution kettle 1a according to a certain ratio, stirring while slowly heating, controlling the temperature in the substitution kettle 1a to be 40 ℃, starting to dropwise add N, N-dimethylaniline, slowly increasing the temperature during dropwise adding, controlling the temperature to be not more than 58 ℃ through the dropwise adding speed and circulating water, after dropwise adding is completed, slowly heating to 70-85 ℃, maintaining for 2-4 hours, after sampling and analyzing that substitution reaction is qualified, cooling to below 35 ℃, adding tetrachloroethylene serving as a solvent, and stirring for half an hour.
Adding clear water into the hydrolysis kettle 1b, starting the jacket of the hydrolysis kettle 1b to freeze brine for cooling, then starting a ball valve at the bottom of the substitution kettle 1a, putting the material in the substitution kettle 1a into the hydrolysis kettle 1b, keeping the temperature not more than 30 ℃, completing the first standing and layering within 20-30 minutes, sending the lower material after hydrolysis to an alkaline washing kettle 1c, and sending the upper material to a second distillation kettle 2 a.
Adding clear water into the alkaline washing kettle 1c, adding the lower material for replacing the detergent, adjusting the pH value to 7 by using soda ash, stirring, standing for 20-30 minutes, feeding the lower material into the first distillation kettle 1d, and feeding the upper washing water into a decontamination water treatment system through the first drain pipe 1 j.
In the first distillation kettle 1d, the substituted material is heated to 40-45 ℃ to begin to distill the solvent tetrachloroethylene under reduced pressure, the product obtained by distillation is introduced into the substitution kettle 1a, the solvent tetrachloroethylene is recycled, the first distillation kettle 1d is heated to 100 ℃ to carry out negative pressure distillation, the steam generated by distillation is discharged into the waste gas absorption tower 3 through the first exhaust pipe 1e, and the harmful substances in the steam are recovered through the alkali liquor in the waste gas absorption tower 3.
Introducing a product obtained by bending and distilling the substituted substance in the first distillation kettle 1d into a crystallization kettle 1f, cooling and crystallizing the distillation product at 5-10 ℃ in the crystallization kettle 1f, introducing the crystallized product into a centrifugal separator 1g, separating crystals from liquid under the action of the centrifugal separator 1g, introducing crystallized particles into a dryer 1h for drying to obtain a finished product, introducing the liquid separated by the centrifugal separator 1g into the crystallization kettle 1f, and mixing the liquid with subsequent liquid to be crystallized to continuously separate out the product in the liquid.
Heating in a second distillation kettle 2a to volatilize hydrochloric acid in the upper material, feeding the volatilized hydrochloric acid into a first recovery tank 2b, introducing the remaining solution into a neutralization kettle 2c after a certain time, injecting ammonia water into the neutralization kettle 2c to neutralize the pH value to 9.0, standing for layering for the second time, decoloring the lower water phase material subjected to layering by standing for the second time by active carbon, feeding the lower water phase material subjected to layering by active carbon into a first condenser 2d, condensing in the first condenser 2d to crystallize diammonium hydrogen phosphate, introducing the condensed solid-liquid mixture into a filter 2f, separating disodium hydrogen phosphate from the solid-liquid mixture by the filter 2f, introducing the separated liquid into an evaporator 2g to evaporate, removing water in the liquid to realize concentration of the liquid, introducing the concentrated liquid into the condenser to mix with the subsequent lower water phase material subjected to layering by standing for the second time, and continuously concentrating and crystallizing to ensure that the disodium hydrogen phosphate in the liquid is completely separated out.
And (3) feeding the N, N-dimethylaniline into a dehydration kettle 2e, heating to 70-100 ℃ after water washing layering, dehydrating and removing the solvent, introducing the removed N, N-dimethylaniline and water into an intermediate tank, recycling the solvent, and allowing the removed water and the layered alkaline water to enter a sewage treatment system.
The above description of the present invention does not limit the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the scope of the claims of the present invention.
Claims (5)
1. A4, 6-dichloropyrimidine synthesis system is characterized by comprising a finished product synthesis assembly, wherein the finished product synthesis assembly comprises a substitution kettle, a hydrolysis kettle, an alkaline washing kettle, a first sewage discharge pipe, a first distillation kettle, a first exhaust pipe, a crystallization kettle, a centrifugal separator and a dryer, a feed inlet of the hydrolysis kettle is connected with a discharge outlet of the substitution kettle, a feed inlet of the alkaline washing kettle is connected with a discharge outlet of the hydrolysis kettle, a liquid inlet end of the first sewage discharge pipe and a feed inlet of the first distillation kettle are selectively connected with a discharge outlet of the alkaline washing kettle, a first steam outlet of the first distillation kettle is connected with the substitution kettle, a first exhaust pipe is communicated with a second steam outlet of the first distillation kettle, a feed inlet of the crystallization kettle is communicated with a liquid outlet of the first distillation kettle, a feed inlet of the centrifugal separator is connected with a discharge outlet of the crystallization kettle, and a liquid phase outlet of the centrifugal separator is communicated with a feeding hole of the crystallization kettle, and a feeding hole of the dryer is connected with a solid phase outlet of the centrifugal separator.
2. The 4, 6-dichloropyrimidine synthesis system according to claim 1, wherein the 4, 6-dichloropyrimidine synthesis system further comprises a byproduct recovery component, the byproduct recovery component comprises a second distillation kettle, a first recovery tank, a neutralization kettle, a first condenser and a dehydration kettle, feed inlets of the second distillation kettle and the alkali washing kettle are selectively connected with a discharge outlet of the hydrolysis kettle, a feed inlet of the first recovery tank is connected with a steam outlet of the second distillation kettle, and the neutralization kettle is connected with a liquid outlet of the second distillation kettle; the feed inlets of the dehydration kettle and the first condenser are selectively connected with the discharge outlet of the neutralization kettle.
3. The 4, 6-dichloropyrimidine synthesis system according to claim 2 wherein said byproduct recovery package further comprises a filter, the inlet of said filter being connected to the outlet of said first condenser.
4. The 4, 6-dichloropyrimidine synthesis system according to claim 3 wherein said byproduct recovery package further comprises an evaporator, the feed inlet of said evaporator being connected to the liquid phase outlet of said filter, the liquid phase outlet of said evaporator being connected to the feed inlet of said first condenser.
5. The system of claim 4, 6-dichloropyrimidine as synthesis system according to claim 4 wherein the byproduct recovery assembly further comprises a solvent intermediate tank and a second recovery tank, the feed inlet of the solvent intermediate tank being in communication with the vapor outlet of the dehydration kettle, the second recovery tank being in communication with the liquid outlet of the dehydration kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021263738.4U CN213416718U (en) | 2020-06-30 | 2020-06-30 | 4, 6-dichloropyrimidine synthesis system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021263738.4U CN213416718U (en) | 2020-06-30 | 2020-06-30 | 4, 6-dichloropyrimidine synthesis system |
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| Publication Number | Publication Date |
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| CN213416718U true CN213416718U (en) | 2021-06-11 |
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| CN202021263738.4U Active CN213416718U (en) | 2020-06-30 | 2020-06-30 | 4, 6-dichloropyrimidine synthesis system |
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