CN212167381U - Benzamide production test system - Google Patents

Abstract

The utility model discloses a benzamide production test system, which comprises a common working section unit, a reaction working section unit, a recrystallization working section unit and a rectification working section unit, wherein the common working section unit is respectively communicated with a vacuum system main pipe, a compressed air main pipe, a circulating water return main pipe, a circulating water upper water main pipe, a softened water upper water main pipe and a sewage discharge main pipe; the reaction section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization workshop section unit is respectively communicated with the vacuum system main pipe, the compressed air main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the rectification workshop section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization working section unit and the rectification working section unit are respectively communicated with a material pipe.

Description

Benzamide production test system

Technical Field

The utility model relates to a benzamide production test system.

Background

Benzamide is a class of chemical raw materials or products used in the process of drug synthesis. The chemical products can be produced in a common chemical plant without the production license of the medicine, and can be used for synthesizing the medicine as long as the chemical products reach a certain level. The method is characterized in that ammonia water and benzoyl chloride are used as raw materials, acyl chloride is added under certain conditions to react to produce benzamide, the reaction belongs to an amination reaction, a target product is a white flaky crystal, and the benzamide can be used as an organic synthesis intermediate for synthesizing medicines, dyes and the like. However, the conventional technology lacks a systematic and modular production test system for benzamide.

Disclosure of Invention

An object of the utility model is to provide a benzamide production test system:

the system comprises a common working section unit, a reaction working section unit, a recrystallization working section unit and a rectification working section unit, and also comprises a vacuum system main pipe, a compressed air main pipe, a circulating water return main pipe, a circulating water upper water main pipe, a softened water upper water main pipe and a sewage discharge main pipe which run through all the units; the public working section unit is respectively communicated with the vacuum system main pipe, the compressed air main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the reaction section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization workshop section unit is respectively communicated with the vacuum system main pipe, the compressed air main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the rectification workshop section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization working section unit and the rectification working section unit are respectively communicated with a material pipe.

Further, the public workshop section unit comprises a softened water tank, a circulating water tank, an air buffer tank and a vacuum buffer tank, wherein the vacuum buffer tank is communicated with a vacuum system main pipe and a sewage discharge main pipe, the air buffer tank is communicated with a compressed air main pipe and a sewage discharge main pipe, the circulating water tank is communicated with a circulating water return main pipe, a circulating water upper water main pipe, a softened water upper water main pipe and a sewage discharge main pipe, and the softened water tank is communicated with the softened water upper water main pipe and the sewage discharge main pipe.

Furthermore, the public workshop section unit also comprises a refrigeration circulating pump, a softened water column, a circulating water pump, an air compressor and a vacuum pump; the circulating water tank is responsible for through circulating water pump intercommunication circulating water, the softened water tank be responsible for through softening water pump intercommunication softened water, air buffer tank intercommunication air compressor machine, vacuum buffer tank intercommunication vacuum pump, softened water column intercommunication softened water tank, circulating water tank, refrigeration circulating pump and blowdown be responsible for.

Further, the reaction section unit comprises an ammonia water storage tank, an acyl chloride storage tank, a mother liquor tank, an absorption liquor tank, an acyl chloride pump, an ammonia water pump, a condenser, an absorption tower, a condenser, a circulating water bath container, a reaction kettle, a bag filter and a neutralization kettle, the mother liquid tank is communicated with the vacuum system main pipe and the sewage discharge main pipe, the absorption liquid tank is communicated with the softened water upper main pipe and the sewage discharge main pipe, the reaction kettle is directly communicated with the softened water upper water main pipe and is communicated with the circulating water return main pipe and the circulating water upper water main pipe through the condenser, the reaction kettle is circularly communicated with the circulating water bath container, the reaction kettle is also communicated with the centrifuge, the ammonia water storage tank is communicated with the mother liquor tank and the sewage discharge main pipe, the ammonia water storage tank is also communicated with the reaction kettle through the ammonia water pump, the acyl chloride storage tank is communicated with the reaction kettle through the acyl chloride pump, the neutralization kettle is communicated with the circulating water return main pipe and the circulating water upper water main pipe and the sewage discharge main pipe, and the neutralization kettle is also communicated with the bag filter.

Furthermore, the reaction section unit comprises a mother liquor pump and an absorption liquid pump, the mother liquor tank is also communicated with the centrifuge and the condenser, the mother liquor tank is also respectively communicated with the reaction kettle and the neutralization kettle through the mother liquor pump, the absorption liquid tank is also communicated with the neutralization kettle and the condenser, and the absorption liquid tank is also circularly communicated with the absorption tower through the absorption liquid pump.

Furthermore, the reaction section unit comprises a sulfuric acid storage tank and a sulfuric acid pump, the neutralization kettle is communicated with the vacuum system main pipe, the circulating water return main pipe and the circulating water upper water main pipe through a condenser, and the neutralization kettle is communicated with the sulfuric acid storage tank through the sulfuric acid pump.

Further, the recrystallization working section unit comprises a recrystallization kettle, an ethanol raw material tank, an ethanol pump, a circulating water bath container, a condenser, a centrifugal machine and a mother liquor tank; ethanol head tank intercommunication vacuum system be responsible for and the material pipe, recrystallization cauldron intercommunication softened water on water be responsible for, recrystallization cauldron still be responsible for through condenser intercommunication circulating water return and the circulating water is responsible for, mother liquor jar intercommunication vacuum system be responsible for, the blowdown is responsible for and the material pipe, centrifuge communicates mother liquor jar, recrystallization cauldron and vacuum system respectively and is responsible for, recrystallization cauldron circulation intercommunication circulation water bath container, recrystallization cauldron still communicates the ethanol head tank through the ethanol pump.

Further, the rectification workshop section unit comprises a raw material tank, a tower kettle, a distillation device, a tower top product tank, a tower kettle liquid tank, a raw material pump, a reflux pump, a tower kettle heat exchange tank, a condenser and a sieve plate rectification tower, wherein the raw material tank is communicated with a softened water upper water main pipe, a vacuum system main pipe and a sewage discharge main pipe, the tower kettle is communicated with the condenser through the sieve plate rectification tower, the sewage discharge main pipe, the tower top product tank is communicated with the vacuum system main pipe, the condenser, a material pipe and the sewage discharge main pipe, the tower kettle liquid tank is communicated with the vacuum system main pipe, the condenser and the sewage discharge main pipe, the tower kettle heat exchange tank is communicated with the sieve plate rectification tower kettle and the tower kettle, the tower kettle heat exchange tank is also communicated with the tower kettle liquid tank and the material pipe, the tower kettle heat exchange tank is also communicated with the raw material tank through the raw material pump, the condenser is communicated with a, the condenser is communicated with a vacuum system main pipe and a fraction device, and the fraction device is communicated with a tower top product tank and a sieve plate rectifying tower through a reflux pump.

Has the advantages that:

specifically, the utility model discloses divide into 4 workshop sections with benzamide production test, be four workshop sections of public work, reaction, recrystallization, sieve rectification respectively, during raw materials aqueous ammonia was squeezed into reation kettle from aqueous ammonia head tank through the ammonia pump ration, squeezed into reation kettle with benzoyl chloride from the acyl chloride storage tank through the pump, opened stirring and circulation water bath and carried out the dropwise add reaction. Ammonia volatilized in the reaction process enters an ammonia spraying absorption tower and is sprayed and absorbed by absorption liquid from an absorption storage tank. Benzoyl chloride finishes with the aqueous ammonia reaction, opens reation kettle bottom baiting valve, and the reaction feed liquid gets into bag filter carries out the solid-liquid separation operation, and the mother liquor of separating puts into the mother liquor jar, because in this reaction sequence, the aqueous ammonia is excessive, still contains the ammonia of higher concentration in the mother liquor, so but mother liquor cyclic utilization accessible pump squeezes into reation kettle, gets into the neutralization kettle after the active ingredient finishes using, adds sulphuric acid and comes from the sulphuric acid storage tank and carries out neutralization treatment, discharges after reaching the index.

Quantitatively putting the benzamide crude product obtained by solid-liquid separation into a recrystallization kettle, quantitatively pumping ethanol in an ethanol raw material tank into the recrystallization kettle by an ethanol pump, pumping a certain amount of softened water into the recrystallization kettle by opening a softened water inlet valve, quantitatively putting the crude product into the recrystallization kettle, dissolving the crude product under the heating and stirring conditions, cooling for recrystallization, opening a discharge valve to enter a centrifuge, and performing centrifugal filtration to obtain the refined benzamide. And the centrifuged filtrate ethanol and aqueous solution enter a mother liquor tank through a vacuum system.

And (3) the filtrate generated by centrifugation enters a mother liquor tank, is conveyed to a raw material tank of a rectification working section through a vacuum system, is conveyed to a tower kettle of a rectification tower through heat exchange of the tower kettle by a mother liquor pump, is heated to start rectification, purification and separation, the steam at the tower top enters a condenser to be cooled and then enters a fraction device, the fraction passes through a reflux pump, one part of the fraction flows back to the top of the rectification tower, and the other part of the fraction enters a product tank at the tower top to be stored as a product and.

Wholly, the utility model provides a production test system of systematization modular benzamide, the production of systematization is convenient for to the whole supervision of production of benzamide, and the production of the clear benzamide of being convenient for of level logic is intervened and is adjusted to the more transparent and level logic of modular production technology.

Drawings

Fig. 1 is a schematic view of the overall structure of the system of the present invention;

FIG. 2 is a schematic diagram showing the detailed connection of the common section units in the overall structure of the present invention;

FIG. 3 is a schematic diagram showing the detailed connection of reaction section units in the overall structure of the present invention;

FIG. 4 is a schematic diagram showing the detailed connection of the recrystallization working section units in the overall structure of the present invention;

FIG. 5 is a schematic diagram showing the detailed connection of the rectification section units in the overall structure of the present invention;

in the figure:

a refrigeration circulating pump P101, a softened water column X101, a softened water tank V101, a softened water pump P102, a circulating water tank V102, a circulating water pump P103, an air compressor C101, an air buffer tank V103, a vacuum buffer tank V104 and a vacuum pump P104;

an ammonia water storage tank V201, a circulating water bath container P201, a reaction kettle R201, a bag filter X201, a mother liquor tank V203, a mother liquor pump P204, an absorption liquid pump P205, an absorption liquid tank V204, a neutralization kettle R202, a sulfuric acid pump P206, a sulfuric acid storage tank V205, an acyl chloride storage tank V202, an acyl chloride pump P203, an ammonia water pump P202, a condenser E201, an absorption tower T201 and a condenser E202;

an ethanol raw material tank V301, an ethanol pump P301, a circulating water bath P302, a condenser E301, a recrystallization kettle R301, a centrifuge X301 and a mother liquor tank V302;

a raw material tank V401, a tower bottom V402, a fractionator V403, a tower top product tank V404, a tower bottom liquid tank V405, a raw material pump P401, a reflux pump P402, a tower bottom heat exchange tank E401, a condenser E402 and a sieve plate rectifying tower T401.

The vacuum system comprises a main pipe L1 of the vacuum system, a main pipe L2 of compressed air, a main pipe L3 of circulating water return, a main pipe L4 of circulating water upper water, a main pipe L5 of softened water upper water, a main pipe L6 of sewage disposal and a material pipe L7.

Detailed Description

The present invention will be further described with reference to the following specific embodiments. The following examples are intended to illustrate the invention and are not intended to limit the scope of the invention.

In specific implementation, as shown in fig. 1-5, especially fig. 1, the system of the present invention includes a common process unit, a reaction process unit, a recrystallization process unit, a rectification process unit, and further includes a vacuum system main pipe L1, a compressed air main pipe L2, a circulating water return main pipe L3, a circulating water upper water main pipe L4, a softened water upper water main pipe L5, and a sewage main pipe L6, which run through the units; the common working section unit is respectively communicated with a vacuum system main pipe L1, a compressed air main pipe L2, a circulating water return main pipe L3, a circulating water upper water main pipe L4, a softened water upper water main pipe L5 and a sewage discharge main pipe L6; the reaction working section unit is respectively communicated with a vacuum system main pipe L1, a circulating water return main pipe L3, a circulating water upper water main pipe L4, a softened water upper water main pipe L5 and a sewage discharge main pipe L6; the recrystallization working section unit is respectively communicated with a vacuum system main pipe L1, a compressed air main pipe L2, a circulating water return main pipe L3, a circulating water upper water main pipe L4, a softened water upper water main pipe L5 and a sewage discharge main pipe L6; the rectification workshop section unit is respectively communicated with a vacuum system main pipe L1, a circulating water return main pipe L3, a circulating water upper water main pipe L4, a softened water upper water main pipe L5 and a sewage discharge main pipe L6; the recrystallization section unit and the rectification section unit are respectively communicated with a material pipe L7.

As shown in fig. 2, the common process unit includes a softened water tank V101, a circulation water tank V102, an air buffer tank V103, and a vacuum buffer tank V104, the vacuum buffer tank V104 is communicated with a vacuum system main pipe L1 and a sewage main pipe L6, the air buffer tank V103 is communicated with a compressed air main pipe L2 and a sewage main pipe L6, the circulation water tank V102 is communicated with a circulation water return main pipe L3, a circulation water upper main pipe L4, a softened water upper main pipe L5 and a sewage main pipe L6, and the softened water tank V101 is communicated with a softened water upper main pipe L5 and a sewage main pipe L6.

Specifically, the common section unit further comprises a refrigeration circulating pump P101, a softened water pump P102, a softened water column X101, a circulating water pump P103, an air compressor C101 and a vacuum pump P104; circulating water tank V102 is responsible for L4 through circulating water pump P103 intercommunication circulating water, demineralized water tank V101 be responsible for L5 through demineralized water pump P102 intercommunication demineralized water, air buffer tank V103 intercommunication air compressor C101, vacuum buffer tank V104 intercommunication vacuum pump P104, demineralized water column X101 intercommunication demineralized water tank V101, circulating water tank V102, refrigeration circulating pump P101 and blowdown be responsible for L6.

As shown in fig. 3, the reaction section unit includes an ammonia water storage tank V201, an acid chloride storage tank V202, a mother liquor tank V203, an absorption liquor tank V204, an acid chloride pump P20, an ammonia water pump P202, a condenser E201, an absorption tower T201, a condenser E202, a circulating water bath container P201, a reaction vessel R201, a bag filter X201, and a neutralization vessel R202, the mother liquor tank V203 communicates with a vacuum system main pipe L1 and a blowdown main pipe L6, the absorption liquor tank V204 communicates with a softened water upper water main pipe L5 and a blowdown main pipe L6, the reaction vessel R201 communicates with a softened water upper water L5 directly and communicates with a circulating water upper water main pipe L3 and a circulating water upper water L main pipe 4 through the condenser E201, the reaction vessel R201 communicates with the circulating water bath container P201 circularly, the reaction vessel R201 communicates with the bag filter X201, the ammonia water storage tank V communicates with the mother liquor tank V203 and the blowdown main pipe L6, the ammonia water storage tank V201 communicates with the reaction vessel R201 through the ammonia water pump P202 and the acid, the neutralization kettle R202 is communicated with a circulating water return main pipe L3, a circulating water upper main pipe L4 and a sewage discharge main pipe L6, and the neutralization kettle R202 is also communicated with a bag filter X201.

Specifically, the reaction section unit comprises a mother liquor pump P204 and an absorption liquid pump P205, the mother liquor tank V203 is further communicated with the bag filter X201 and the condenser E201, the mother liquor tank V203 is further communicated with the reaction kettle R201 and the neutralization kettle R202 through the mother liquor pump P204, the absorption liquid tank V204 is further communicated with the neutralization kettle R202 and the condenser E201, and the absorption liquid tank V204 is further communicated with the absorption tower T201 through the absorption liquid pump P205 in a circulating manner.

Specifically, the reaction section unit comprises a sulfuric acid storage tank V205 and a sulfuric acid pump P206, the neutralization kettle R202 is also communicated with a vacuum system main pipe L1, a circulating water return main pipe L3 and a circulating water upper water main pipe L4 through a condenser E202, and the neutralization kettle R202 is also communicated with the sulfuric acid storage tank V205 through the sulfuric acid pump P206.

As shown in fig. 4, the recrystallization section unit comprises a recrystallization kettle R301, an ethanol raw material tank V301, an ethanol pump P301, a circulating water bath container P302, a condenser E301, a centrifuge X301, and a mother liquor tank V302; ethanol head tank V301 intercommunication vacuum system be responsible for L1 and material pipe L7, recrystallization cauldron R301 intercommunication demineralized water upper water be responsible for L5, recrystallization cauldron R301 still communicate circulating water return be responsible for L3 and circulating water upper water be responsible for L4 through condenser E301, mother liquor jar V302 communicate vacuum system be responsible for L1, blowdown be responsible for L6 and material pipe L7, centrifuge X301 communicates mother liquor jar V302, recrystallization cauldron R301 and vacuum system respectively and is responsible for L1, recrystallization cauldron R301 circulation intercommunication circulation water bath container P302, recrystallization cauldron R301 still communicates ethanol head tank V301 through ethanol pump P301.

As shown in fig. 5, the rectification section unit includes a raw material tank V401, a tower bottom V402, a fractionator V403, a tower top product tank V404, a tower bottom liquid tank V405, a raw material pump P401, a reflux pump P402, a tower bottom heat exchange tank E401, a condenser E402, a sieve plate rectification tower T401, the raw material tank V401 is communicated with a softened water main pipe L5, a vacuum system main pipe L1, and a blowdown main pipe L6, the tower bottom V402 is communicated with the condenser E402 through the sieve plate rectification tower T401, the tower bottom V402 is further communicated with a blowdown main pipe L6, the tower top product tank V404 is communicated with a vacuum system main pipe L1, a condenser E402, a material pipe L7, and a blowdown main pipe L6, the tower bottom liquid tank V405 is communicated with a vacuum system main pipe L1, a condenser E402, and a blowdown main pipe L6, the tower bottom heat exchange tank E401 is communicated with the sieve plate rectification tower T401 and the raw material tank V401 through the heat exchange tank V401, the condenser E402 is communicated with a circulating water return main pipe L3 and a circulating water upper main pipe L4, the condenser E402 is communicated with a vacuum system main pipe L1 and a fraction device V403, and the fraction device V403 is communicated with a tower top product tank V404 and a sieve plate rectifying tower T401 through a reflux pump P402.

The specific implementation principle is as follows:

the benzamide production test is divided into 4 working sections, namely four working sections of public engineering, reaction, recrystallization and sieve plate rectification, raw material ammonia water is quantitatively pumped into a reaction kettle R201 from an ammonia water raw material tank V201 through an ammonia water pump P202, benzoyl chloride is pumped into the reaction kettle from an acyl chloride storage tank V202 through a pump, and stirring and circulating water bath P201 are started for dropwise adding reaction. The ammonia volatilized during the reaction enters the ammonia spray absorption tower T201, and is sprayed and absorbed by the absorption liquid from the absorption storage tank V204. After the benzoyl chloride and the ammonia water are reacted, a discharge valve at the bottom of the reaction kettle R201 is opened, reaction liquid enters the bag filter X201 to be subjected to solid-liquid separation, separated mother liquid is placed into the mother liquid tank V203, and in the reaction process, the ammonia water is excessive and still contains ammonia with high concentration in the mother liquid, so that the mother liquid can be recycled and can be pumped into the reaction kettle through the pump P204, after the use of effective components is finished, the mother liquid enters the neutralization kettle, sulfuric acid is added to be neutralized from the sulfuric acid storage tank V205, and the reaction liquid is discharged after reaching indexes.

Quantitatively putting a benzamide crude product obtained by solid-liquid separation into a recrystallization kettle R301, quantitatively putting ethanol in an ethanol raw material tank V301 into the recrystallization kettle R301 by an ethanol pump P301, opening a softened water inlet valve to put a certain amount of softened water, quantitatively putting the crude product into the recrystallization kettle R301, dissolving under a heating and stirring condition, cooling for recrystallization, opening an R301 discharge valve to enter a centrifuge X301, and performing centrifugal filtration to obtain refined benzamide. The centrifuged ethanol and water solution of the filtrate enter a mother liquor tank V302 through a vacuum system.

The filtrate generated by centrifugation enters a mother liquor tank V302, is conveyed to a raw material tank V401 of a rectification working section through a vacuum system, is conveyed to a tower kettle V402 of a rectification tower T401 through tower kettle heat exchange E401 through a mother liquor pump P401, is heated to start rectification, purification and separation, tower top steam enters a condenser E402 to be cooled and then enters a fraction device V403, fraction passes through a reflux pump P402, a part of the fraction reflows to the top of the rectification tower, and a part of the fraction enters a tower top product tank V404 to be stored as a product and recycled as a recrystallization raw material. The utility model provides a systematization modular pharmaceutical intermediate benzamide's production system, the whole supervision of production of being convenient for to benzamide of systematization production, the production of the clear benzamide of being convenient for of level logic of more transparent and the modular production technology intervenes and adjusts.

The process operation of the system in the actual production test was as follows:

1. common section operation

(1) Powering on to turn on a main power supply, and turning on a main power supply and a control power supply of the public engineering unit module;

(2) checking whether the related measuring range, scale and valve state of the control system are displayed normally, wherein the valve check can refer to a valve initial state diagram 2 and correspondingly fill a related confirmation table 2;

(3) after the process parameters are set to check, manually setting a control system softening water tank, wherein the upper limit of the liquid level is 550mm, and the potential difference is 50 mm; setting a circulating water tank, wherein the upper limit of the liquid level is 550mm, the potential difference is 50mm, the upper limit of the temperature is 30 ℃, and the temperature difference is 5 ℃;

(4) the softened water control valve is opened when water is supplied, and the tap water main water valve is opened;

(5) when the water softening tank is operated, the liquid level of the V101 of the water softening tank is observed to rise to more than 350mm, the VA103 valve is opened, the P102 water softening pump is started for standby, and the valve VA107 is opened, so that water can be observed to enter the circulating water tank;

(6) when the liquid level of the circulating water tank rises to more than 350mm after the circulating water tank is operated, a valve VA106 is opened, a P103 circulating water pump is started, the running state of the equipment is maintained, and the equipment is standby (the circulating water outlet flow is displayed through a turbine flowmeter FI101, a VA117 valve can be adjusted as required, and the water outlet flow is controlled); opening a P101 refrigeration circulating pump, setting the circulating refrigeration temperature to be about 15 ℃, and opening valves VA118 and VA119 for later use;

(7) the air buffer tank is operated to check that the VA110 is in a closed state, the C101 air compressor is opened, the valve VA109 is closed, and the valve VA110 is opened for standby after the pressure in the air buffer tank is observed to be stable;

(8) and checking that the VA113 is in a closed state through the operation of the vacuum buffer tank, opening the vacuum pump P104, starting the valve VA114, closing the valve VA112, setting the upper limit of the pressure in the vacuum buffer tank to-0.06 MPa and the lower limit to-0.08 MPa, and opening the valve VA113 for later use after the pressure in the vacuum buffer tank is observed to be stable.

2. Operation of reaction section

(1) The main power supply and the control power supply of the reaction unit module are powered on and started;

(2) checking whether the related range, scale and valve state of the control system are displayed normally, referring to the initial state diagram 2 of the valve, and correspondingly filling a related confirmation table 3;

(3) opening a valve VA202, adding 30% ammonia water solution into an ammonia water storage tank V201, opening valves VA203 and VA206, opening an ammonia water pump P202, opening a reaction kettle R201, stirring at a set rotation speed of about 50rpm, and quantitatively adding 12.5L of 30% ammonia water solution; opening a rotor flow meter FG201 of a condenser E201 and introducing circulating water;

(4) opening valves VA225 and VA232, adding water and a small amount of sulfuric acid or only adding water (about 10L) into the absorption liquid tank to serve as absorption liquid, opening valves VA227 and VA228 at the bottom of the absorption liquid tank, opening an absorption liquid pump P205, opening electric regulating valves VA235 and VA234, regulating the opening degree of the electric regulating valves, and spraying the absorption liquid to an absorption tower T201 to absorb ammonia gas;

(5) starting a circulating water bath P201, setting the temperature to be about 20 ℃, and introducing cooling water into a jacket of the reaction kettle R201; adding 2.5L of benzoyl chloride into a benzoyl chloride storage tank V202, starting a peristaltic pump P203, setting the rotating speed of the peristaltic pump to enable the benzoyl chloride to be slowly dripped into a reaction kettle, observing the temperature in the reaction kettle, adjusting the dripping speed of acyl chloride according to the temperature in the kettle, keeping the temperature in the kettle below 40 ℃, and finishing dripping within 1 hour;

(6) after the benzoyl chloride is added dropwise, continuously stirring and reacting for 0.5h under the condition of heat preservation until no benzoyl chloride smell exists;

(7) opening a vacuum electromagnetic valve VA236, opening a valve VA216, opening a discharge valve VA214 at the bottom of a reaction kettle R201, adjusting the opening of the valve, discharging to a bag filter X201, retaining solids in the bag filter, and allowing mother liquor to enter a mother liquor tank V203; closing valves VA236 and VA216, opening valves VA243, VA217 and VA238, opening valve VA210, introducing softened water into the reaction kettle, washing the crude benzamide product in the bag filter with water for 2-3 times until no obvious pungent taste exists, and allowing the water washing liquid to enter a neutralization kettle;

(8) opening a bag filter X201 emptying valve VA207, and extracting a filter bag to take out crude benzamide;

(9) opening valves VA219 and VA221 at the bottom of the mother liquor tank V203, opening a mother liquor pump P204, opening valves VA224 and VA237, and pumping the mother liquor in the mother liquor tank to a neutralization kettle R202; opening a rotor flow meter FG202 of a condenser E202 and introducing circulating water;

(10) opening water inlet and outlet valves VA242 and VA244 of a jacket of a neutralization kettle R202, adding dilute sulfuric acid into a sulfuric acid storage tank, opening a valve VA241, opening a sulfuric acid pump P206, dropwise adding sulfuric acid into the neutralization kettle, observing that the temperature in the kettle does not exceed 60 ℃, adjusting the dropwise adding rate of the sulfuric acid in time, opening bottom discharge valves VA245 and VA246, sampling, detecting the neutralization effect, and performing environment-friendly discharge treatment;

(11) in the reaction process, the ammonia water is excessive, the mother liquor still contains ammonia with higher concentration, the sampling valve VA220 at the bottom of the mother liquor tank V203 can be taken for sampling and detecting the effective components of the mother liquor ammonia water, the mother liquor pump P204 can be opened, the valves VA219, VA221, VA223 and VA213 are opened, and the mother liquor is pumped into the reaction kettle R201 for mother liquor recycling.

3. Operation of recrystallization section

(1) The main power supply and the control power supply of the recrystallization unit module are powered on and started;

(2) checking whether the related measuring range, scale and valve state of the control system are displayed normally, wherein the valve check can refer to a valve initial state diagram 2 and correspondingly fill a related confirmation table 4;

(3) starting a raw material pump P301, quantitatively adding ethanol into a recrystallization kettle R301 through a turbine flowmeter FI301, starting valves VA309 and VA310, adding quantitative softened water into the recrystallization kettle R301 through the turbine flowmeter FI303, preparing an ethanol solution with the concentration of about 20 percent by the ethanol solution and stirring, starting, adding crude benzamide, starting a valve VA308, and introducing circulating water into a condenser;

(4) opening water inlet and outlet valves VA322 and VA323 of the jacket, setting the temperature of the circulating water bath between 45 ℃ and 55 ℃, heating to about 50 ℃ until the circulating water bath is completely dissolved, and stirring for about 1 h; setting the temperature of the circulating water bath between 5 and 10 ℃, cooling and crystallizing, and setting the stirring speed at 20 to 30 rpm;

(5) after the crystals are completely separated out, starting a vacuum system, keeping the pressure of a vacuum buffer tank at-0.05 MPa, starting a valve VA312, starting a centrifuge X301, opening blanking valves VA313 and VA316, starting centrifugal filtration, and introducing a small amount of softened water to wash the benzamide crystals;

4. operation of sieve plate rectification section

(1) The main power supply and the control power supply of the recrystallization unit module are powered on and started;

(2) checking whether the related measuring range, scale and valve state of the control system are displayed normally, wherein the valve check can refer to a valve initial state diagram 2 and correspondingly fill a related confirmation table 4;

(3) and opening a bottom discharge valve and a raw material pump for feeding, adjusting the feeding amount to be 30mL/min, and closing when the liquid level of the tower kettle is level with the discharge hole of the tower kettle.

(4) And opening the tower kettle for heating and condensing water.

(5) And (4) switching the reflux ratio operation to a manual state, closing the extraction electromagnetic valve, and opening the reflux electromagnetic valve to enable the tower to be in a full reflux state.

(6) After reflux at the top of the column, the pressure in the column bottom is maintained at about 1 to 1.5 kPa. After the total reflux operation is stable for a certain time, the raw material pump is started, and the feeding flow is adjusted to 3 mL/min. The operation is stable only after the temperature at the top of the column is maintained.

(7) The reflux ratio operation is switched to an automatic state, and the opening time of the extraction solenoid valve and the reflux solenoid valve is set, and the reflux ratio control is generally in a range of R = L/D =2-4 (which can be determined according to the situation).

(8) And respectively reading the temperatures of the tower top, the tower kettle and the feeding material, sampling and detecting the concentration, and recording related data.

(9) When the temperature at the tower top rises obviously, the production is finished, the reflux ratio operation is switched to a manual state, the feeding pump and the electromagnetic valve are closed, the electric heating is closed, and the cooling water at the tower top is closed when no gas liquid exists on the plates.

(10) And after production is finished, introducing quantitative tap water into each kettle, stirring and cleaning equipment and pipelines, discharging, and closing a power supply and a water inlet valve.

Claims (8)

1. The benzamide production test system is characterized by comprising a common working section unit, a reaction working section unit, a recrystallization working section unit and a rectification working section unit, and further comprising a vacuum system main pipe, a compressed air main pipe, a circulating water return main pipe, a circulating water upper water main pipe, a softened water upper water main pipe and a sewage discharge main pipe which penetrate through all the units; the public working section unit is respectively communicated with the vacuum system main pipe, the compressed air main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the reaction section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization workshop section unit is respectively communicated with the vacuum system main pipe, the compressed air main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the rectification workshop section unit is respectively communicated with the vacuum system main pipe, the circulating water return main pipe, the circulating water upper water main pipe, the softened water upper water main pipe and the sewage discharge main pipe; the recrystallization working section unit and the rectification working section unit are respectively communicated with a material pipe.

2. The benzamide production test system according to claim 1, wherein the common working section unit comprises a water softening tank, a circulating water tank, an air buffer tank and a vacuum buffer tank, the vacuum buffer tank is communicated with a vacuum system main pipe and a sewage discharge main pipe, the air buffer tank is communicated with a compressed air main pipe and a sewage discharge main pipe, the circulating water tank is communicated with a circulating water return main pipe, a circulating water upper water main pipe, a softened water upper water main pipe and a sewage discharge main pipe, and the water softening tank is communicated with a softened water upper water main pipe and a sewage discharge main pipe.

3. The benzamide production test system according to claim 2, wherein the utility section unit further comprises a refrigeration circulating pump, a softened water column, a circulating water pump, an air compressor, and a vacuum pump; the circulating water tank is responsible for through circulating water pump intercommunication circulating water, the softened water tank be responsible for through softening water pump intercommunication softened water, air buffer tank intercommunication air compressor machine, vacuum buffer tank intercommunication vacuum pump, softened water column intercommunication softened water tank, circulating water tank, refrigeration circulating pump and blowdown be responsible for.

4. The benzamide production test system according to claim 1, wherein the reaction section unit comprises an ammonia water storage tank, an acyl chloride storage tank, a mother liquid tank, an absorption liquid tank, an acyl chloride pump, an ammonia water pump, a condenser, an absorption tower, a circulating water bath container, a reaction kettle, a bag filter and a neutralization kettle, the mother liquid tank is communicated with a vacuum system main pipe and a sewage discharge main pipe, the absorption liquid tank is communicated with a softened water upper main pipe and a sewage discharge main pipe, the reaction kettle is directly communicated with the softened water upper main pipe and is communicated with a circulating water return main pipe and the circulating water upper main pipe through the condenser, a reaction kettle jacket is circularly communicated with the circulating water bath container, the reaction kettle is also communicated with the bag filter, the ammonia water storage tank is communicated with the mother liquid tank and the sewage discharge main pipe, the ammonia water storage tank is also communicated with the reaction kettle through the ammonia water pump, the acyl chloride storage tank is communicated with the reaction kettle, the neutralization kettle is also communicated with a bag filter.

5. The benzamide production test system according to claim 4, wherein the reaction section unit comprises a mother liquor pump and an absorption liquid pump, the mother liquor tank is further communicated with a bag filter and a condenser, the mother liquor tank is further communicated with the reaction kettle and the neutralization kettle respectively through the mother liquor pump, the absorption liquid tank is further communicated with the neutralization kettle and the condenser, and the absorption liquid tank is further communicated with the absorption tower through the absorption liquid pump in a circulating manner.

6. The benzamide production test system according to claim 4 or 5, wherein the reaction section unit comprises a sulfuric acid storage tank and a sulfuric acid pump, the neutralization kettle is further communicated with the vacuum system main pipe, the circulating water return main pipe and the circulating water upper main pipe through a condenser, and the neutralization kettle is further communicated with the sulfuric acid storage tank through the sulfuric acid pump.

7. The benzamide production test system according to claim 1, wherein the recrystallization section unit comprises a recrystallization kettle, an ethanol raw material tank, an ethanol pump, a circulating water bath container, a condenser, a centrifuge, a mother liquor tank; ethanol head tank intercommunication vacuum system be responsible for and the material pipe, recrystallization cauldron intercommunication softened water on water be responsible for, recrystallization cauldron still be responsible for through condenser intercommunication circulating water return and the circulating water is responsible for, mother liquor jar intercommunication vacuum system be responsible for, the blowdown is responsible for and the material pipe, centrifuge communicates mother liquor jar, recrystallization cauldron and vacuum system respectively and is responsible for, recrystallization cauldron circulation intercommunication circulation water bath container, recrystallization cauldron still communicates the ethanol head tank through the ethanol pump.

8. The benzamide production test system according to claim 1, wherein the distillation section unit comprises a raw material tank, a tower kettle, a fraction device, a tower top product tank, a tower kettle liquid tank, a raw material pump, a reflux pump, a tower kettle heat exchange tank, a condenser and a sieve plate distillation tower, the raw material tank is communicated with a softened water main pipe, a vacuum system main pipe and a sewage discharge main pipe, the tower kettle is communicated with the condenser through the sieve plate distillation tower, the tower kettle is also communicated with a sewage discharge main pipe, the tower top product tank is communicated with the vacuum system main pipe, the condenser, a material pipe and the sewage discharge main pipe, the tower kettle liquid tank is communicated with the vacuum system main pipe, the condenser and the sewage discharge main pipe, the tower kettle heat exchange tank is circularly communicated with the sieve plate distillation tower and the tower kettle, the tower kettle heat exchange tank is also communicated with the tower kettle liquid tank and the material pipe, the tower kettle heat exchange tank is also communicated with the raw material tank through the raw material, the condenser is communicated with a circulating water return main pipe and a circulating water upper main pipe, the condenser is communicated with a vacuum system main pipe and a fraction device, and the fraction device is communicated with a tower top product tank and a sieve plate rectifying tower through a reflux pump.

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