CN112174849A

CN112174849A - Preparation method and equipment of L-asparagine

Info

Publication number: CN112174849A
Application number: CN202011152368.1A
Authority: CN
Inventors: 张胜
Original assignee: Zhejiang Tianrui Chemical Co ltd
Current assignee: Zhejiang Tianrui Chemical Co ltd
Priority date: 2020-10-26
Filing date: 2020-10-26
Publication date: 2021-01-05

Abstract

The invention relates to a preparation method of L-asparagine and equipment thereof, which optimizes and improves the traditional synthesis process of the L-asparagine, greatly improves the yield of the L-asparagine and reduces the generation of side reactions; the method for producing the L-asparagine can improve the purity of the L-asparagine to 99.6 percent, improve the transmittance to 99.9 percent and control the specific rotation degree between +31 degrees and +35 degrees, and compared with the prior art, the method reduces the occurrence of side reactions, has good stirring effect and improves the quality of finished products and the working efficiency.

Description

Preparation method and equipment of L-asparagine

Technical Field

The invention relates to the technical field of chemistry, in particular to a preparation method of L-asparagine and equipment thereof.

Background

L-asparagine, also known as asparagine, asparagine and alpha-amino succinic acid monoamide, is first separated from asparagus juice by French chemist LOUIS and the like in 1806, and then is sequentially found and separated in various animals and plants, L-asparagine is necessary for brain development and functions, under the action of oligosaccharide transferase, L-asparagine can be combined with N-acetylglucosamine in endoplasmic reticulum, is vital for the stability and the function of protein structure and is an important form of protein glycosylation, therefore, L-asparagine is very important for human body, L-asparagine and sugar can carry out amino-carbonyl reaction to form a special flavor substance, can be used as a food additive for cold drinks, and is also an important additive for microbial culture and animal cell culture, l-asparagine is commonly used in amino acid transfusion and has effects of lowering blood pressure, relieving asthma, resisting peptic ulcer and gastric dysfunction, and can be used for treating myocardial infarction, myocardial metabolic disturbance, heart failure, heart conduction block and fatigue, in addition, L-asparagine can relieve cell apoptosis induced by homoglutaminyl inhibition, further realizes the treatment of tumor, therefore, the L-asparagine is widely applied to the fields of food, medicine, chemical synthesis, microorganism culture and the like, at present, the preparation of the L-asparagine mainly adopts an extraction method and a chemical synthesis method, wherein the extraction method comprises separating L-asparagine from natural materials rich in L-asparagine, such as Lupinus albus and sweet clover, the method is greatly influenced by the quality factor of raw materials, the process is complex and is not easy to control, and the pollution is serious; the chemical synthesis method is mainly prepared by amidating L-aspartic acid and ammonia water, but the method also has the defects of large pollution, more side reactions and the like, reduces the quality of finished products, is easy to generate stirring and insufficient reaction, and has low working efficiency, so the improvement is needed.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a preparation method of L-asparagine with good finished product quality and high working efficiency and equipment thereof.

The technical scheme of the invention is realized as follows: a method for preparing L-asparagine, which is characterized in that: cooling methanol to-9-13 ℃ for the first time, then dropwise adding thionyl chloride into the methanol at a speed of 32-38mL/h under the condition that the temperature is not more than 2 ℃, continuously stirring for 12-18 min after the dropwise adding is finished, then adding aspartic acid into the methanol to perform a first heat preservation reaction at the temperature of 32-38 ℃ to obtain an esterified material, firstly performing first concentration on the esterified material, supplementing the methanol, and then performing second concentration to obtain an acid-driving material; cooling the acid-removing material for the second time to be not more than 18 ℃, dropwise adding ammonia water into the acid-removing material for the first time at a speed of 52-98 mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12-18 min after the addition is finished, and finally carrying out a second heat preservation reaction at 32-38 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to below 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 88-92 ℃ for dissolution, and adjusting the pH value for the second time to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12-18 min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 55 ℃ to obtain a filtrate; cooling the filtrate for crystallization, stopping crystallization when the filtrate is cooled to below 2 ℃, and performing suction filtration to obtain the finished product of the L-asparagine.

By adopting the technical scheme, the traditional synthesis process of the L-asparagine is optimized and improved, the yield of the L-asparagine is greatly improved, and the generation of side reactions is reduced; the method for producing the L-asparagine can improve the purity of the L-asparagine to 99.6 percent, improve the transmittance to 99.9 percent and control the specific rotation degree to be between +31 degrees and +35 degrees.

The invention is further configured to: cooling methanol to-11 ℃ for the first time, dripping thionyl chloride into the methanol at the speed of 34mL/h at the temperature of 2 ℃, continuously stirring for 12min after the dripping is finished, adding aspartic acid into the methanol, carrying out a first heat preservation reaction at the temperature of 34 ℃ to obtain an esterified material, firstly carrying out first concentration on the esterified material, supplementing the methanol, and then carrying out second concentration to obtain an acid-dispelling material; cooling the acid-removing material for the second time to 18 ℃, then dropwise adding ammonia water into the acid-removing material for the first time at a speed of 98mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12min after the addition is finished, and finally carrying out a second heat preservation reaction at 34 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 90 ℃ for dissolution, and carrying out second pH adjustment to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 75 ℃ to obtain a filtrate; and cooling and crystallizing the filtrate, stopping crystallization when the filtrate is cooled to 2 ℃, and performing suction filtration to obtain a finished product of the L-asparagine.

By adopting the technical scheme, the traditional synthesis process of the L-asparagine is further optimized and improved, the yield of the L-asparagine is greatly improved, and the generation of side reactions is reduced; the method for producing the L-asparagine can improve the purity of the L-asparagine to 99.6 percent, improve the transmittance to 99.9 percent and control the specific rotation degree to be between +31 degrees and +35 degrees.

The invention also discloses equipment suitable for the preparation method of the L-asparagine, which is characterized by comprising the following steps: the automatic stirring device comprises a kettle body, be provided with the feed inlet on the lateral wall of the cauldron body, the bottom of the cauldron body is provided with the discharge gate, the upper surface of the cauldron body is provided with driving motor, the vertical puddler that is provided with in the cauldron body, the upper end of puddler and driving motor's output fixed connection, the lower extreme of puddler is provided with stirring portion, be provided with the stirring subassembly that meets an emergency that is used for reducing the motor load on the puddler, be provided with the dropwise add subassembly that is used for reducing the side reaction in the cauldron body, be provided with the heat preservation chamber on the lateral wall of the cauldron body, the heat preservation chamber wraps up cauldron external lateral wall completely, be provided with medium export and medium import on the outer wall.

By adopting the technical scheme, in the process of preparing the L-asparagine, the cold medium is firstly introduced into the heat preservation cavity from the medium inlet, the cold medium exchanges heat with the kettle body in the process of passing through the heat preservation cavity and reduces the temperature in the kettle body, the cold medium flows out from the medium outlet after absorbing the heat, then the main raw material is added into the kettle body from the feed inlet, the secondary raw material to be dripped is added into the kettle body through the dripping component, the dripping component can uniformly add the secondary raw material into the main raw material, the phenomenon of overhigh local concentration is reduced, the occurrence of side reaction is reduced, the driving motor is started, the driving motor drives the stirring rod and the stirring part to rotate, the strain stirring component can reduce the load of the motor when the motor rotates at high speed, the overload phenomenon of the motor is reduced, and the raw material is uniformly stirred under the combined action of the stirring part and the strain stirring component, and finally, the raw materials are discharged from the discharge hole, compared with the prior art, the invention reduces the occurrence of side reactions, has good stirring effect and improves the quality of finished products and the working efficiency.

The present invention is preferably: the strain stirring component comprises two annular chutes and a plurality of stirring sheets which are coaxially arranged with the stirring rod, the two annular chutes are symmetrically arranged on the stirring rod from top to bottom, a fixing part is arranged between the two annular chutes, a plurality of sliding blocks are sleeved in the annular sliding groove, springs are arranged among the sliding blocks and between the fixing part and the sliding blocks, the spring is sleeved in the annular chute, the stirring pieces are in a willow leaf shape, one ends of the stirring pieces are respectively hinged with one side wall of the sliding blocks, one ends of the stirring pieces, far away from the sliding blocks, are hinged with each other through hinged shafts, the stirring pieces are sequentially arranged along the front-back direction, the fixed part is improved level and is provided with the telescopic link, the one end and the fixed part fixed connection of telescopic link, the other end passes through the articulated shaft and is articulated with the stirring piece, and a plurality of stirring pieces use the puddler to set up as symmetry axis bilateral symmetry.

By adopting the technical scheme, in the process of preparing the L-asparagine, the driving motor is started, the driving motor drives the stirring rod and the stirring part to rotate, when the driving motor rotates at low speed, the centrifugal force applied to the stirring sheet on the strain stirring component is small, a plurality of stirring sheets are driven by the telescopic rod driven by the stirring rod to rotate and stir raw materials in the kettle body in an unfolded rotating state, the stirring rod can fully stir the raw materials in low-speed rotation by increasing the stirring area, when the driving motor rotates at high speed, the plurality of stirring sheets are under the action of the centrifugal force, one ends of the plurality of stirring sheets, which are far away from the sliding blocks, move in the direction far away from the stirring rod under the action of the centrifugal force, the other ends of the plurality of stirring sheets drive the plurality of sliding blocks to move to the fixed part, the springs are compressed at the same time, the telescopic rod is driven by the stirring sheets to extend, and the, compared with the prior art, the invention can automatically adjust the stirring area according to the rotating speed of the driving motor, reduce the load of the motor and improve the stirring efficiency at the same time of reducing the load, thereby improving the quality of finished products and the working efficiency.

The present invention is preferably: the dropwise add subassembly is including the fixed three toroidal tube that sets up on cauldron body upper portion, the upper surface of the cauldron body is provided with three inlet pipes, three inlet pipes respectively with three toroidal tube intercommunication, all establish ties on three inlet pipes and be provided with the flowmeter, the lower surface of toroidal tube is provided with a plurality of shower nozzles, shower nozzle and toroidal tube intercommunication, a plurality of shower nozzles are along the even interval distribution of toroidal tube circumference.

Through adopting above-mentioned technical scheme, in the in-process of preparation L-asparagine, after adding the main ingredient, the secondary ingredient that will need the dropwise add is imported by the inlet pipe, the secondary ingredient passes through the inlet pipe and gets into in the ring pipe and by the shower nozzle blowout with the ring pipe intercommunication, the secondary ingredient evenly sprays on the main ingredient through the shower nozzle, the addition of secondary ingredient can the person of facilitating the use observation and control by the flowmeter on the inlet pipe, can adjust respectively through three inlet pipes and ring pipe when adjusting a plurality of secondary ingredients simultaneously, and the work efficiency is improved, the phenomenon that the side reaction appears has been reduced.

The present invention is preferably: one side of the cauldron body is provided with the heat preservation subassembly, the heat preservation subassembly includes heating pipe, transmission pipe and inert gas system, the one end setting of transmission pipe is in the bottom of the cauldron body, and the other end is vertical upwards to extend and wear out the outside that the cauldron body set up at the cauldron body, the one end and the heating pipe intercommunication of cauldron body bottom are kept away from to the transmission pipe, the one end and the inert gas system intercommunication of transmission pipe are kept away from to the heating pipe, the fixed heat preservation medium coil pipe that is provided with in the heating pipe, the import and the export of heat preservation medium coil pipe all set up outside the heating pipe, the upper surface of the cauldron body is provided with gas outlet, gas outlet and inert gas system intercommunication.

By adopting the technical scheme, in the process of preparing the L-asparagine, a heat medium is conveyed into the heat preservation medium coil pipe from an inlet of the heat preservation medium coil pipe, the temperature of the heat medium in the heating pipe is raised in the process of passing through the heat preservation medium coil pipe, the inert gas system conveys inert gas into the heating pipe, the inert gas absorbs heat in the heating pipe when passing through the heating pipe, then the inert gas enters the bottom of the kettle body from a conveying pipe, the inert gas is gradually raised towards the upper part of the kettle body after being discharged from the bottom of the kettle body, and exchanges heat with the raw material in the raising process to raise the temperature of the raw material and maintain the reaction temperature of the raw material, meanwhile, the inert gas can turn over the raw material in the raising process so as to enable the raw material to react more fully, and finally the inert gas is discharged from a gas outlet on the upper surface of the kettle body and returns to, the invention further improves the stirring and mixing efficiency of the raw materials and improves the quality of finished products.

The present invention is preferably: if the stirring piece is provided with the interference flow hole, a plurality of vortex holes are arranged along the length direction of the stirring piece at even intervals.

By adopting the technical scheme, in the process of preparing the L-asparagine, if the interference flow holes on the stirring sheet can further improve the stirring effect of the stirring sheet on the raw materials, the raw materials are more fully mixed, and the quality of finished products is improved.

The present invention is preferably: and a temperature sensor is arranged in the kettle body.

Through adopting above-mentioned technical scheme, temperature sensor can the temperature condition in the real-time supervision cauldron body, and the temperature in the user of being convenient for in time adjusts the cauldron body to guaranteed that the raw materials can normal reaction, improved finished product quality.

The invention also discloses an operation method suitable for the equipment, which is characterized by comprising the following steps: the method comprises the following steps:

firstly, precooling: and the cold medium is introduced into the heat preservation cavity from the medium inlet, exchanges heat with the kettle body in the process of passing through the heat preservation cavity and reduces the temperature in the kettle body, and the cold medium flows out from the medium outlet after absorbing heat.

II, feeding materials: the main raw materials are added into the kettle body through a feeding hole, the secondary raw materials needing to be dripped are input through a feeding pipe, the secondary raw materials enter the annular pipe through the feeding pipe and are sprayed out through a spray head communicated with the annular pipe, and the secondary raw materials are uniformly sprayed on the main raw materials through the spray head. Thirdly, stirring: starting a driving motor, wherein the driving motor drives a stirring rod and a stirring part to rotate, when the driving motor rotates at a low speed, centrifugal force applied to stirring blades on a strain stirring assembly is small, a plurality of stirring blades are driven by a telescopic rod driven by the stirring rod to rotate and stir raw materials in a kettle body in an unfolded rotating state, the stirring rod can fully stir the raw materials in the low-speed rotation by increasing stirring area, when the driving motor rotates at a high speed, the stirring blades are under the action of centrifugal force, one ends of the stirring blades, far away from a sliding block, move towards the direction far away from the stirring rod under the action of the centrifugal force, the other ends of the stirring blades drive the sliding blocks to move towards a fixed part, meanwhile, a spring is compressed, the telescopic rod is driven by the stirring blades to extend, the stirring blades are gradually overlapped together, so that the stirring area is reduced, and the load applied to the driving motor in the high, and the phenomenon of overload of the driving motor is reduced.

Fourthly, heat preservation reaction: the method comprises the steps that a heat medium is conveyed into a heat preservation medium coil pipe from an inlet of the heat preservation medium coil pipe, the temperature of the heat medium in a heating pipe is raised in the process of passing through the heat preservation medium coil pipe, an inert gas system conveys inert gas into the heating pipe, the inert gas absorbs heat in the heating pipe when passing through the heating pipe, then the inert gas enters the bottom of a kettle body from a conveying pipe, the inert gas is gradually raised towards the upper part of the kettle body after being discharged from the bottom of the kettle body, the heat is exchanged with raw materials in the raising process to enable the temperature of the raw materials to be raised and the reaction temperature of the raw materials to be kept, meanwhile, the inert gas can turn the raw materials in the raising process to enable the raw materials to react more fully, and finally the inert gas is discharged from a gas.

Fifthly, discharging: discharging the stirred raw materials from a discharge port, collecting and placing.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

FIG. 1 is a schematic structural diagram of an embodiment of the present invention.

Fig. 2 is a schematic view of a slider structure.

Fig. 3 is a schematic view of the structure of the annular tube.

Fig. 4 is a schematic structural view of the heat-insulating assembly.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

As shown in fig. 1 to 4, the present invention discloses a method for preparing L-asparagine, in the embodiments of the present invention: cooling methanol to-9-13 ℃ for the first time, then dropwise adding thionyl chloride into the methanol at a speed of 32-38mL/h under the condition that the temperature is not more than 2 ℃, continuously stirring for 12-18 min after the dropwise adding is finished, then adding aspartic acid into the methanol to perform a first heat preservation reaction at the temperature of 32-38 ℃ to obtain an esterified material, firstly performing first concentration on the esterified material, supplementing the methanol, and then performing second concentration to obtain an acid-driving material; cooling the acid-removing material for the second time to be not more than 18 ℃, dropwise adding ammonia water into the acid-removing material for the first time at a speed of 52-98 mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12-18 min after the addition is finished, and finally carrying out a second heat preservation reaction at 32-38 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to below 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 88-92 ℃ for dissolution, and adjusting the pH value for the second time to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12-18 min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 55 ℃ to obtain a filtrate; cooling the filtrate for crystallization, stopping crystallization when the filtrate is cooled to below 2 ℃, and performing suction filtration to obtain the finished product of the L-asparagine.

In a specific embodiment of the invention: cooling methanol to-11 ℃ for the first time, dripping thionyl chloride into the methanol at the speed of 34mL/h at the temperature of 2 ℃, continuously stirring for 12min after the dripping is finished, adding aspartic acid into the methanol, carrying out a first heat preservation reaction at the temperature of 34 ℃ to obtain an esterified material, firstly carrying out first concentration on the esterified material, supplementing the methanol, and then carrying out second concentration to obtain an acid-dispelling material; cooling the acid-removing material for the second time to 18 ℃, then dropwise adding ammonia water into the acid-removing material for the first time at a speed of 98mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12min after the addition is finished, and finally carrying out a second heat preservation reaction at 34 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 90 ℃ for dissolution, and carrying out second pH adjustment to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 75 ℃ to obtain a filtrate; and cooling and crystallizing the filtrate, stopping crystallization when the filtrate is cooled to 2 ℃, and performing suction filtration to obtain a finished product of the L-asparagine.

The invention also discloses equipment suitable for the preparation method of the L-asparagine, and in the specific embodiment of the invention: including the cauldron body 1, be provided with feed inlet 2 on the lateral wall of the cauldron body 1, the bottom of the cauldron body 1 is provided with discharge gate 3, the upper surface of the cauldron body 1 is provided with driving motor 4, the vertical puddler 5 that is provided with in the cauldron body 1, the upper end of puddler 5 and driving motor 4's output fixed connection, the lower extreme of puddler 5 is provided with stirring portion 6, be provided with the stirring subassembly 7 that meets an emergency that is used for reducing motor load on the puddler 5, be provided with the dropwise add subassembly 8 that is used for reducing side reaction in the cauldron body 1, be provided with heat preservation chamber 9 on the lateral wall of the cauldron body 1, heat preservation chamber 9 wraps up the cauldron body 1 lateral wall completely, be provided with medium export and medium import on heat preservation chamber 9's the outer wall.

In a specific embodiment of the invention: the strain stirring assembly 7 comprises two annular sliding grooves 71 and a plurality of stirring blades 72 which are coaxially arranged with the stirring rod 5, the two annular sliding grooves 71 are symmetrically arranged on the stirring rod 5 from top to bottom, a fixing part 73 is arranged between the two annular sliding grooves 71, a plurality of sliding blocks 74 are sleeved in the annular sliding grooves 71, springs 75 are arranged between the sliding blocks 74 and between the fixing part 73 and the sliding blocks 74, the springs 75 are sleeved in the annular sliding grooves 71, the stirring blades 72 are in a willow-leaf shape, one ends of the stirring blades 72 are respectively hinged with one side wall of the sliding blocks 74, one ends of the stirring blades 72, which are far away from the sliding blocks 74, are hinged with each other through hinge shafts 76, the stirring blades 72 are sequentially arranged along the front-back direction, telescopic rods 77 are horizontally arranged on the fixing part 73, one ends of the telescopic rods 77 are fixedly connected with the fixing part 73, and the, the stirring pieces 72 are arranged symmetrically with the stirring rod 5 as a symmetry axis.

In a specific embodiment of the invention: dropwise add subassembly 8 is including the fixed three toroidal tube 81 that sets up on cauldron body 1 upper portion, the upper surface of cauldron body 1 is provided with three inlet pipes 82, and three inlet pipes 82 communicate with three toroidal tube 81 respectively, all establish ties on three inlet pipes 82 and be provided with flowmeter 83, the lower surface of toroidal tube 81 is provided with a plurality of shower nozzles 84, shower nozzle 84 and toroidal tube 81 intercommunication, a plurality of shower nozzles 84 are along the even interval distribution of toroidal tube 81 circumference.

In a specific embodiment of the invention: one side of the cauldron body 1 is provided with the heat preservation subassembly, the heat preservation subassembly includes heating pipe 10, transmission pipe 11 and inert gas system 12, the one end setting of transmission pipe 11 is in the bottom of the cauldron body 1, and the vertical upwards extension of the other end wears out the outside that cauldron body 1 set up at the cauldron body 1, the one end and the heating pipe 10 intercommunication of cauldron body 1 bottom are kept away from to transmission pipe 11, the one end and the inert gas system 12 intercommunication of transmission pipe 11 are kept away from to heating pipe 10, the fixed heat preservation medium coil pipe 13 that is provided with in the heating pipe 10, the import and the export of heat preservation medium coil pipe 13 all set up outside heating pipe 10, the upper surface of the cauldron body 1 is provided with gas outlet 14, gas outlet 14 and inert gas system 12 intercommunication.

In a specific embodiment of the invention: the stirring piece 72 is provided with a plurality of turbulence holes 78 which are uniformly arranged along the length direction of the stirring piece 72 at intervals if the turbulence holes 78 are formed.

In a specific embodiment of the invention: and a temperature sensor 15 is arranged in the kettle body 1.

The invention also discloses an operation method suitable for the equipment, and in the specific embodiment of the invention: the method comprises the following steps:

firstly, precooling: the cold medium is introduced into the heat preservation cavity 9 from the medium inlet, the cold medium exchanges heat with the kettle body 1 in the process of passing through the heat preservation cavity 9 and reduces the temperature in the kettle body 1,

the cold medium flows out from the medium outlet after absorbing heat.

II, feeding materials: the main raw materials are added into the kettle body 1 through the feed inlet 2, the secondary raw materials to be dripped are input through the feed pipe 82, the secondary raw materials enter the annular pipe 81 through the feed pipe 82 and are sprayed out through the spray head 84 communicated with the annular pipe 81, and the secondary raw materials are uniformly sprayed on the main raw materials through the spray head 84.

Thirdly, stirring: starting the driving motor 4, the driving motor 4 drives the stirring rod 5 and the stirring part 6 to rotate, when the driving motor 4 rotates at a low speed, the centrifugal force applied to the stirring blades 72 on the strain stirring component 7 is small, the stirring blades 72 are driven by the telescopic rod 77 driven by the stirring rod 5 in an unfolded rotating state to rotate and stir the raw materials in the kettle body 1, the stirring rod 5 can fully stir the raw materials in the low-speed rotation by increasing the stirring area, when the driving motor 4 rotates at a high speed, the stirring blades 72 are under the action of the centrifugal force, one end of each stirring blade 2 far away from the sliding block 74 moves in a direction far away from the stirring rod 5 under the action of the centrifugal force, the other end of each stirring blade 72 drives the sliding blocks 74 to move towards the fixing part 73, meanwhile, the spring 75 is compressed, the telescopic rod 77 is driven by the stirring blades 72 and extends, the stirring blades 72 are gradually overlapped together, so that the stirring area is reduced, the load on the driving motor 4 during high-speed rotation is reduced, and the phenomenon of overload of the driving motor 4 is reduced.

Fourthly, heat preservation reaction: a heat medium is conveyed into the heat preservation medium coil 13 from an inlet of the heat preservation medium coil 13, the temperature of the heating pipe 10 rises in the process that the heat medium passes through the heat preservation medium coil 13, the inert gas system 12 conveys inert gas into the heating pipe 10, the inert gas absorbs heat in the heating pipe 10 when passing through the heating pipe 10, then the inert gas enters the bottom of the kettle body 1 from the conveying pipe 11, the inert gas is discharged from the bottom of the kettle body 1 and gradually rises towards the upper part of the kettle body 1, the heat is exchanged with the raw material in the rising process to enable the temperature of the raw material to rise and maintain the reaction temperature of the raw material, meanwhile, the inert gas turns over the raw material in the rising process to enable the raw material to react more fully, and finally the inert gas is discharged from a gas outlet 14 on the upper surface of the kettle body 1 and returns to the inert.

Fifthly, discharging: discharging the stirred raw materials from a discharge port 3, collecting and placing.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims

1. A method for preparing L-asparagine, which is characterized in that: cooling methanol to-9-13 ℃ for the first time, then dropwise adding thionyl chloride into the methanol at a speed of 32-38mL/h under the condition that the temperature is not more than 2 ℃, continuously stirring for 12-18 min after the dropwise adding is finished, then adding aspartic acid into the methanol to perform a first heat preservation reaction at the temperature of 32-38 ℃ to obtain an esterified material, firstly performing first concentration on the esterified material, supplementing the methanol, and then performing second concentration to obtain an acid-driving material; cooling the acid-removing material for the second time to be not more than 18 ℃, dropwise adding ammonia water into the acid-removing material for the first time at a speed of 52-98 mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12-18 min after the addition is finished, and finally carrying out a second heat preservation reaction at 32-38 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to below 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 88-92 ℃ for dissolution, and adjusting the pH value for the second time to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12-18 min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 55 ℃ to obtain a filtrate; cooling the filtrate for crystallization, stopping crystallization when the filtrate is cooled to below 2 ℃, and performing suction filtration to obtain the finished product of the L-asparagine.

2. The method of claim 1, wherein the L-asparagine moiety is selected from the group consisting of: cooling methanol to-11 ℃ for the first time, dripping thionyl chloride into the methanol at the speed of 34mL/h at the temperature of 2 ℃, continuously stirring for 12min after the dripping is finished, adding aspartic acid into the methanol, carrying out a first heat preservation reaction at the temperature of 34 ℃ to obtain an esterified material, firstly carrying out first concentration on the esterified material, supplementing the methanol, and then carrying out second concentration to obtain an acid-dispelling material; cooling the acid-removing material for the second time to 18 ℃, then dropwise adding ammonia water into the acid-removing material for the first time at a speed of 98mL/h, continuously releasing heat and raising the temperature in the process, then adding ammonia water into the acid-removing material for the second time after the temperature rise is stopped, continuously stirring for 12min after the addition is finished, and finally carrying out a second heat preservation reaction at 34 ℃ to obtain an ammonolysis material; carrying out third concentration, first pH adjustment, cooling crystallization on the ammonolysis material, stopping crystallization when the ammonolysis material is cooled to 2 ℃, carrying out suction filtration to obtain a crude L-asparagine product, adding the crude L-asparagine product into water, heating to 90 ℃ for dissolution, and carrying out second pH adjustment to obtain an aqueous solution of L-asparagine; adding activated carbon into the L-asparagine aqueous solution for decoloring for 12min, and filtering before the temperature of the L-asparagine aqueous solution is not lower than 75 ℃ to obtain a filtrate; and cooling and crystallizing the filtrate, stopping crystallization when the filtrate is cooled to 2 ℃, and performing suction filtration to obtain a finished product of the L-asparagine.

3. An apparatus suitable for use in the process for preparing L-asparagine according to claim 2, characterized in that: the automatic stirring device comprises a kettle body, be provided with the feed inlet on the lateral wall of the cauldron body, the bottom of the cauldron body is provided with the discharge gate, the upper surface of the cauldron body is provided with driving motor, the vertical puddler that is provided with in the cauldron body, the upper end of puddler and driving motor's output fixed connection, the lower extreme of puddler is provided with stirring portion, be provided with the stirring subassembly that meets an emergency that is used for reducing the motor load on the puddler, be provided with the dropwise add subassembly that is used for reducing the side reaction in the cauldron body, be provided with the heat preservation chamber on the lateral wall of the cauldron body, the heat preservation chamber wraps up cauldron external lateral wall completely, be provided with medium export and medium import on the outer wall.

4. The apparatus according to claim 3, wherein the apparatus comprises: the strain stirring component comprises two annular chutes and a plurality of stirring sheets which are coaxially arranged with the stirring rod, the two annular chutes are symmetrically arranged on the stirring rod from top to bottom, a fixing part is arranged between the two annular chutes, a plurality of sliding blocks are sleeved in the annular sliding groove, springs are arranged among the sliding blocks and between the fixing part and the sliding blocks, the spring is sleeved in the annular chute, the stirring pieces are in a willow leaf shape, one ends of the stirring pieces are respectively hinged with one side wall of the sliding blocks, one ends of the stirring pieces, far away from the sliding blocks, are hinged with each other through hinged shafts, the stirring pieces are sequentially arranged along the front-back direction, the fixed part is improved level and is provided with the telescopic link, the one end and the fixed part fixed connection of telescopic link, the other end passes through the articulated shaft and is articulated with the stirring piece, and a plurality of stirring pieces use the puddler to set up as symmetry axis bilateral symmetry.

5. The apparatus according to claim 4, wherein the apparatus comprises: the dropwise add subassembly is including the fixed three toroidal tube that sets up on cauldron body upper portion, the upper surface of the cauldron body is provided with three inlet pipes, three inlet pipes respectively with three toroidal tube intercommunication, all establish ties on three inlet pipes and be provided with the flowmeter, the lower surface of toroidal tube is provided with a plurality of shower nozzles, shower nozzle and toroidal tube intercommunication, a plurality of shower nozzles are along the even interval distribution of toroidal tube circumference.

6. The apparatus according to claim 5, wherein the apparatus comprises: one side of the cauldron body is provided with the heat preservation subassembly, the heat preservation subassembly includes heating pipe, transmission pipe and inert gas system, the one end setting of transmission pipe is in the bottom of the cauldron body, and the other end is vertical upwards to extend and wear out the outside that the cauldron body set up at the cauldron body, the one end and the heating pipe intercommunication of cauldron body bottom are kept away from to the transmission pipe, the one end and the inert gas system intercommunication of transmission pipe are kept away from to the heating pipe, the fixed heat preservation medium coil pipe that is provided with in the heating pipe, the import and the export of heat preservation medium coil pipe all set up outside the heating pipe, the upper surface of the cauldron body is provided with gas outlet, gas outlet and inert gas system intercommunication.

7. The apparatus according to claim 6, wherein the apparatus comprises: if the stirring piece is provided with the interference flow hole, a plurality of vortex holes are arranged along the length direction of the stirring piece at even intervals.

8. The apparatus according to claim 7, wherein the apparatus comprises: and a temperature sensor is arranged in the kettle body.

9. A method of operation adapted for use with the apparatus of claim 8, wherein: the method comprises the following steps:

II, feeding materials: the main raw materials are added into the kettle body through a feeding hole, the secondary raw materials needing to be dripped are input through a feeding pipe, the secondary raw materials enter the annular pipe through the feeding pipe and are sprayed out through a spray head communicated with the annular pipe, and the secondary raw materials are uniformly sprayed on the main raw materials through the spray head.

Thirdly, stirring: starting a driving motor, wherein the driving motor drives a stirring rod and a stirring part to rotate, when the driving motor rotates at a low speed, centrifugal force applied to stirring blades on a strain stirring assembly is small, a plurality of stirring blades are driven by a telescopic rod driven by the stirring rod to rotate and stir raw materials in a kettle body in an unfolded rotating state, the stirring rod can fully stir the raw materials in the low-speed rotation by increasing stirring area, when the driving motor rotates at a high speed, the stirring blades are under the action of centrifugal force, one ends of the stirring blades, far away from a sliding block, move towards the direction far away from the stirring rod under the action of the centrifugal force, the other ends of the stirring blades drive the sliding blocks to move towards a fixed part, meanwhile, a spring is compressed, the telescopic rod is driven by the stirring blades to extend, the stirring blades are gradually overlapped together, so that the stirring area is reduced, and the load applied to the driving motor in the high, the overload phenomenon of the motor is reduced.