CN114195665A - Neutralization and acidification process and equipment for high-purity NCAA - Google Patents
Neutralization and acidification process and equipment for high-purity NCAA Download PDFInfo
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- CN114195665A CN114195665A CN202111525297.XA CN202111525297A CN114195665A CN 114195665 A CN114195665 A CN 114195665A CN 202111525297 A CN202111525297 A CN 202111525297A CN 114195665 A CN114195665 A CN 114195665A
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- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000020477 pH reduction Effects 0.000 title claims abstract description 25
- 230000008569 process Effects 0.000 title claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 123
- 238000003756 stirring Methods 0.000 claims abstract description 78
- 239000002253 acid Substances 0.000 claims abstract description 49
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 33
- 239000003513 alkali Substances 0.000 claims description 55
- 238000005406 washing Methods 0.000 claims description 45
- 239000002904 solvent Substances 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 28
- 238000012544 monitoring process Methods 0.000 claims description 22
- 230000008859 change Effects 0.000 claims description 13
- 230000007246 mechanism Effects 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 4
- 230000008676 import Effects 0.000 claims 3
- 238000000746 purification Methods 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 106
- 150000003613 toluenes Chemical class 0.000 description 14
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- HMVPMZFEYCGSTC-UHFFFAOYSA-N 2-(2-amino-4-chloroanilino)benzoic acid Chemical compound NC1=CC(Cl)=CC=C1NC1=CC=CC=C1C(O)=O HMVPMZFEYCGSTC-UHFFFAOYSA-N 0.000 description 1
- -1 N-substituted phenylanthranilic acid Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1881—Stationary reactors having moving elements inside resulting in a loop-type movement externally, i.e. the mixture leaving the vessel and subsequently re-entering it
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
Abstract
The application relates to a neutralization acidification process and equipment for high-purity NCAA, in particular to the field of NCAA purification, wherein the neutralization acidification process comprises the steps of adding an organic solvent capable of forming an organic solvent layer above an NCAA solution layer into an NCAA solution; and stirring the NCAA solution layer, continuously dropwise adding the neutralizing acid solution while stirring until the pH value of the NCAA solution layer is adjusted to 4-5, and separating the organic solvent layer from the NCAA solution layer to obtain the high-purity NCAA solution. The method has the effect of improving the purification purity of the NCAA while maintaining the yield of the NCAA.
Description
Technical Field
The application relates to the field of NCAA purification, in particular to a neutralization and acidification process and equipment for high-purity NCAA.
Background
NCAA, N- (4-chloro-2-aminophenyl) anthranilic acid, is a special N-substituted phenylanthranilic acid derivative, and is an important intermediate for synthesizing some medicinal compounds. The NCAA synthesized by the prior art contains more toluene derivative impurities, so that the purity of the obtained NCAA is lower.
In order to increase the purity of NCAA, neutralization and acidification treatments are usually performed on a synthesized NCAA solution, that is, a neutralization acid solution is injected into the NCAA solution to neutralize an alkaline NCAA solution, so that a toluene derivative in the NCAA solution is crystallized, but a part of NCAA is crystallized together with the crystallization of the toluene derivative, so that in order to reduce the influence of the neutralization and acidification process on the yield of NCAA, the requirement on the purity of NCAA is usually only selected to be reduced.
In view of the related art in the above, the inventors considered that it was difficult to improve the NCAA purity while maintaining the NCAA yield.
Disclosure of Invention
In order to improve the purity of NCAA while maintaining the yield of NCAA, the application provides a neutralization and acidification process and equipment for high-purity NCAA.
In a first aspect, the present application provides a neutralization acidification process for high purity NCAA, which adopts the following technical scheme:
a neutralization acidification process for high-purity NCAA comprises the following steps:
the method comprises the following steps: adding an organic solvent capable of forming an organic solvent layer above the NCAA solution layer to the NCAA solution;
step two: and stirring the NCAA solution layer, continuously dropwise adding a neutralization acid solution from the upper part of the organic solvent layer while stirring until the pH value of the NCAA solution layer is adjusted to 4-5, and separating the organic solvent layer from the NCAA solution layer to obtain the high-purity NCAA solution.
By adopting the technical scheme, the organic solvent is added into the NCAA solution, and the organic solvent can dissolve and absorb toluene derivative impurities in the NCAA solution, so the toluene derivative impurities in the organic solvent tend to migrate to an organic solvent layer under the action of poor solubility, the toluene derivative tends to be polymerized and crystallized by dropwise adding the neutralizing acid liquid, and then the toluene derivative continuously passes through a region close to the organic solvent layer along with the flowing of the NCAA solution under the stirring action, and is absorbed by the organic solvent, so that the effect of full purification is achieved.
In addition, the existence of the organic solvent layer enables the neutralizing acid solution to firstly pass through the organic solvent layer and enter the NCAA solution layer after being buffered by the organic solvent layer when the neutralizing acid solution is dripped into the NCAA solution layer, so that the neutralizing acid solution is relatively dispersed when entering the NCAA solution layer, the possibility of advanced crystallization near a neutralizing acid solution dripping area above the NCAA layer is reduced, the neutralizing acid solution can be rapidly dispersed after entering the NCAA solution layer by matching with stirring, the possibility of local crystallization in the NCAA solution layer is further reduced, the yield of the NCAA is favorably maintained, and the purity of the NCAA is improved.
Optionally, in the step two, during the neutralization by adding acid, the organic solvent layer is pumped and injected with the organic solvent, and the organic solvent in the organic solvent layer is extracted at the same time, so as to replace the organic solvent in the organic solvent layer.
By adopting the technical scheme, the organic solvent is dynamically replaced, so that the dissolving amount of the toluene derivatives in the organic solvent layer is always at a lower level, the absorption strength of the toluene derivatives in the organic solvent layer is ensured, the purification quality of the NCAA is further improved, and the purity of the NCAA is improved.
Optionally, the organic solvent extracted in the second step is subjected to alkali washing by introducing alkali liquor, impurities dissolved in the organic solvent are washed away, and the organic solvent obtained by alkali washing is pumped into the organic solvent layer again for circulation.
By adopting the technical scheme, the organic solvent is recycled by alkaline washing, the use amount of the organic solvent is reduced, energy is saved, the environment is protected, and the purification cost is reduced.
In a second aspect, the present application provides a neutralization and acidification device, which adopts the following technical scheme:
a neutralization acidification device is based on the neutralization acidification process of the high-purity NCAA, and comprises a stirring kettle and an alkali washing circulating device; an acid adding pipe is arranged at the top of the stirring kettle body, the inner cavity of the stirring kettle is divided into a solution area for containing NCAA solution and an organic solvent area for containing organic solvent, the organic solvent area is arranged above the solution area, a solvent inlet and a solvent outlet are arranged on the side wall of the stirring kettle corresponding to the organic solvent area, and the solvent inlet and the solvent outlet are arranged at two opposite sides of the stirring kettle;
the alkali washing circulating device comprises an alkali washing tank, a circulating pipe and a circulating pump, wherein the solvent inlet and the solvent outlet are communicated with the inner cavity of the alkali washing tank through the circulating pipe, and the circulating pump is arranged on the circulating pipe.
By adopting the technical scheme, when the device is used, firstly, prepared alkali liquor is injected into an alkali washing tank, NCAA solution and organic solvent are injected into a stirring kettle, after the NCAA solution and the organic solvent are layered, a stirring mechanism of the stirring kettle is started, then neutralizing acid liquor is added into the stirring kettle through an acid adding pipe, the neutralizing acid liquor is buffered through an organic solvent layer after being dripped in, and then is dispersed into an NCAA solution layer, a circulating pump is started after the neutralizing acid liquor is dripped in for a period of time, so that the organic solvent starts to circulate, the organic solvent in the stirring kettle is conveyed into the alkali washing tank for alkali washing, toluene derivatives in the organic solvent are pumped into the stirring kettle again after being absorbed, and after the purification is finished by adding acid, a liquid discharge pipe of the stirring kettle is opened, the NCAA solution and the organic solvent are discharged, and the high-purity NCAA solution can be obtained after separation. The neutralization and acidification device is simple, can be used only by simple transformation on the basis of the existing stirring kettle, and is convenient and practical.
Optionally, the solvent outlet is arranged at the top of the organic solvent area, the opening of the alkaline washing tank directly communicated with the solvent outlet is used as an organic solvent inlet, the opening of the alkaline washing tank directly communicated with the solvent inlet is used as an organic solvent outlet, the organic solvent inlet is arranged at the bottom of the alkaline washing tank, the organic solvent outlet is arranged at the top of the alkaline washing tank, and the organic solvent inlet and the organic solvent outlet are arranged at two sides of the alkaline washing tank.
By adopting the technical scheme, the solvent outlet is arranged at the top of the organic solvent area, which is beneficial to the automatic overflow discharge of the organic solvent and is convenient for the circulation of the organic solvent; the organic solvent inlet and the organic solvent outlet are arranged in a relative staggered manner, so that the contact time of the organic solvent and the alkali liquor is prolonged, the toluene derivatives in the organic solvent are fully absorbed, and the alkali washing quality is improved.
Optionally, the stirring blade in the stirring kettle is a pushing stirring blade.
Through adopting above-mentioned technical scheme, adopt the characteristics that impulse type stirring vane can promote liquid to specific direction flow, help NCAA solution directional flow when stirring, form the circulation of flowing, and then make whole NCAA solution fully contact with organic solvent, further promote the purification quality.
Optionally, the system further comprises an automatic control device, wherein the automatic control device comprises:
the first pH monitoring meter is arranged in the inner cavity of the stirring kettle and is used for monitoring the pH of the NCAA solution in the solution area;
the second pH monitoring meter is arranged in the inner cavity of the alkaline washing tank and is used for monitoring the pH of the alkaline liquor in the inner cavity of the alkaline washing tank;
and the input end of the controller is used for being electrically connected with the first pH monitoring meter and the second pH monitoring meter, and the output end of the controller is used for being electrically connected with the circulating pump and the stirring mechanism of the stirring kettle.
Through adopting above-mentioned technical scheme, adopt first pH monitor meter and second pH monitor meter to monitor NCAA solution and alkali lye pH respectively, the controller of being convenient for judges whether the purification process is accomplished according to NCAA solution and alkali lye pH value, and then automatic control rabbling mechanism and circulating pump shut down, realize accurate control to the purification in-process.
Optionally, an automatic control system is provided in the controller, and the automatic control system includes:
the pH information acquisition module is used for receiving the pH value information of the NCAA solution detected by the first pH monitoring meter and the pH value information of the alkali liquor detected by the second pH monitoring meter in real time;
the NCAA solution analysis and processing module is used for setting the pH value to be 4-5 as the pH threshold of the NCAA solution, comparing the pH value information of the NCAA solution acquired by the pH information acquisition module with the pH set threshold of the NCAA solution and judging whether the pH value of the received NCAA solution is within the set pH threshold range of the NCAA solution or not;
the alkali liquor analysis processing module is used for converting the pH value of the alkali liquor received by the pH information acquisition module into the pH change rate of the alkali liquor within the set time;
and the driving execution module is used for sending a shutdown signal to the stirring mechanism and the circulating pump when the pH value of the NCAA solution falls into the pH threshold interval of the NCAA solution and the change rate of the pH of the alkali liquor in the set time is less than 5%, or the pH value of the NCAA solution is lower than the lower limit of the pH threshold interval of the NCAA solution.
By adopting the technical scheme, the pH value of the NCAA solution and the pH change rate of the alkali liquor are jointly used as the judgment basis for finishing the purification, the defect that the purification purity is unstable when the pH value of the NCAA solution is used as the judgment basis independently is avoided, the defect that the purification is finished by misjudgment in the early stage of the purification when the pH change rate of the alkali liquor is used as the judgment basis independently is also avoided, the judgment accuracy is improved, the injection of the neutralizing acid liquor can be timely reduced after the purification is finished, and the use of the neutralizing acid liquor is saved.
In summary, the present application includes at least one of the following beneficial technical effects:
according to the neutralization acidification process, the organic solvent is added into the NCAA solution, toluene derivative impurities in the organic solvent tend to migrate to an organic solvent layer under the action of poor solubility and are absorbed by the organic solvent, so that a sufficient purification effect is achieved, the dropwise added neutralization acid liquid can be buffered by the organic solvent layer, the neutralization acid liquid is sufficiently dispersed, the possibility of local crystallization in the NCAA solution layer is reduced, the NCAA yield is favorably maintained, and the NCAA purity is further improved;
the neutralization acidification equipment is simple in structure, can be used only by simple modification on the basis of the existing stirring kettle, and is convenient and practical;
the utility model provides a neutralization acidification equipment is through monitoring NCAA solution pH value and alkali lye pH value to NCAA solution pH value and alkali lye pH change rate are as the judgement foundation that the purification was accomplished jointly, help promoting and judge the accuracy, and can in time reduce the notes of neutralization acid liquid and add after the purification is accomplished, save the use of neutralization acid liquid.
Drawings
Fig. 1 is a schematic diagram of the overall structure of a neutralization and acidification device in embodiment 2 of the application.
FIG. 2 is a schematic cross-sectional view of the stirred tank of FIG. 1.
Fig. 3 is a schematic sectional view of the alkaline washing cycle apparatus of fig. 1.
Reference numerals: 1. stirring the mixture in a kettle; 11. a kettle body; 111. a liquid feeding pipe; 1111. a first flow meter; 112. adding an acid pipe; 1121. a second flow meter; 113. a liquid discharge pipe; 114. a solution zone; 115. an organic solvent zone; 116. a solvent inlet; 117. a solvent outlet; 12. a stirring mechanism; 121. a stirring motor; 1211. a motor base; 122. a stirring shaft; 123. a stirring blade; 2. an alkaline washing circulating device; 21. an alkaline washing tank; 211. an alkali liquor tube; 212. an organic solvent inlet; 213. an organic solvent outlet; 22. a circulation pipe; 23. a circulation pump; 3. an automated control device; 31. a first pH monitor; 32. a second pH monitor; 33. and a controller.
Detailed Description
The present application is described in further detail below with reference to figures 1-3.
Example 1:
the embodiment of the application discloses a high-purity NCAA neutralizing acid and a process.
Referring to fig. 1, the neutralization acid and process of high purity NCAA comprises the steps of:
the method comprises the following steps: adding the NCAA solution into a stirring kettle 1, and then adding an organic solvent into the stirring kettle 1, so that the organic solvent forms an organic solvent layer above the NCAA solution layer, wherein the organic solvent is preferably toluene in the embodiment;
step two: starting a stirring plate device of the stirring kettle 1 to stir the NCAA solution layer, continuously dropwise adding a neutralization acid solution from the upper part of the organic solvent layer while stirring, introducing the organic solvent in the organic solvent layer into an alkali liquor to carry out alkali washing after the total volume of the dropwise added neutralization acid solution reaches 20% of the total volume of the expected neutralization acid solution to remove toluene derivative impurities in the organic solvent by absorption, and then pumping the organic solvent subjected to alkali washing into the stirring kettle 1 again to circulate the organic solvent; and when the purification is finished, discharging the NCAA solution and the organic solvent in the stirring kettle 1 and separating the organic solvent from the NCAA solution to obtain the high-purity NCAA solution, wherein the pH value of the NCAA solution layer is adjusted to 4-5 and the change rate of the pH value of the alkali solution within 3 minutes continuously is lower than 5%.
Example 2:
the embodiment of the application discloses neutralization and acidification equipment based on the neutralization acid and process of high-purity NCAA in embodiment 1, and referring to FIGS. 1 and 2, the neutralization and acidification equipment comprises a stirring kettle 1, an alkaline washing circulating device 2 and an automatic control device 3;
the stirring kettle 1 comprises a kettle body 11 and a stirring mechanism 12 arranged on the kettle body 11, wherein a liquid adding pipe 111 and an acid adding pipe 112 are welded at the top of the kettle body 11, a liquid discharging pipe 113 is welded at the bottom of the kettle body 11, a first flowmeter 1111 is in threaded connection with the liquid adding pipe 111, a second flowmeter 1121 is in threaded connection with the acid adding pipe 112, the first flowmeter 1111 is used for quantitatively adding an NCAA solution and an organic solvent, the acid adding pipe 112 is used for adding a neutralizing acid liquid, and the second flowmeter 1121 is used for measuring the acid adding amount; the inner cavity of the stirring kettle 1 is divided into a solution area 114 for containing NCAA solution and an organic solvent area 115 for containing organic solvent, the organic solvent area 115 is positioned above the solution area 114, a solvent inlet 116 and a solvent outlet 117 are arranged on the side wall of the kettle body 11 corresponding to the organic solvent area 115, the solvent inlet 116 and the solvent outlet 117 are arranged at two opposite sides of the kettle body 11, the solvent inlet 116 is arranged near the bottom of the organic solvent area 115, and the solvent outlet 117 is arranged near the top of the organic solvent area 115; the stirring mechanism 12 comprises a stirring motor 121, a stirring shaft 122 and a stirring blade 123, the top of the kettle body 11 is welded with a motor base 1211, the stirring motor 121 is fixed on the motor base 1211 through a bolt, the stirring shaft 122 is coaxially welded on an output shaft of the stirring motor 121 and is inserted into an inner cavity of the kettle body 11, and the stirring blade 123 is welded on a part of the stirring shaft 122 located in the solution area 114.
Referring to fig. 1 and 3, the caustic washing circulation device 2 includes a caustic washing tank 21, a circulation pipe 22, and a circulation pump 23; the bottom of one side wall of the alkaline washing tank 21 is welded with an alkaline liquid pipe 211 for injecting and discharging alkaline liquid, two opposite side walls of the alkaline washing tank 21 are respectively provided with an opening, the two openings are respectively used as an organic solvent inlet 212 and an organic solvent outlet 213, the organic solvent inlet 212 is arranged at the bottom of the alkaline washing tank 21, and the organic solvent outlet 213 is arranged at the top of the alkaline washing tank 21; the circulation pipe 22 is divided into two parts, one part of the circulation pipe 22 is in threaded connection between the solvent outlet 117 and the organic solvent inlet 212, the other part of the circulation pipe 22 is in threaded connection between the organic solvent outlet 213 and the solvent inlet 116, and the circulation pump 23 is in threaded connection with the circulation pipe 22 communicating the organic solvent outlet 213 and the solvent inlet 116.
Referring to fig. 1-3, the automatic control device 3 includes a first pH monitor 31 fixed in the inner cavity of the kettle 11 by bolts, a second pH monitor 32 fixed in the inner cavity of the alkaline washing tank 21 by bolts, and a controller 33 fixed outside the kettle 11 by bolts, in this embodiment, the controller 33 is configured as an LED display screen controller 33, which facilitates the fact display of the pH value of the NCAA solution and the pH value of the alkaline solution received by the controller 33. The first pH monitor 31 is installed on the top of the solution zone 114 so as to monitor the pH value of the NCAA solution in the solution zone 114 and verify the liquid level of the NCAA solution according to the detected change of the pH value when the NCAA solution is added into the kettle body 11; the second pH monitoring meter 32 is arranged on the side wall of the alkaline washing tank 21 close to the top, and is used for monitoring the pH of the alkaline liquor in the inner cavity of the alkaline washing tank 21 and verifying the liquid level of the alkaline liquor by detecting the change of the pH value; the input end of the controller 33 is electrically connected to the first pH monitor 31, the second pH monitor 32 and the second flow meter 1121, the output end is electrically connected to the stirring mechanism 12 and the circulation pump 23, and an automatic control system is disposed in the controller 33.
The automatic control system includes:
the pH information acquisition module is used for receiving the pH value information of the NCAA solution detected by the first pH monitoring meter 31 and the pH value information of the alkali liquor detected by the second pH monitoring meter 32 in real time;
the neutralizing acid liquid adding amount obtaining module is used for presetting predicted adding total volume information of the neutralizing acid liquid and receiving the adding amount information of the neutralizing acid liquid detected by the second flowmeter 1121 in real time;
the NCAA solution analysis and processing module is used for setting the pH value to be 4-5 as the pH threshold of the NCAA solution, comparing the pH value information of the NCAA solution acquired by the pH information acquisition module with the pH set threshold of the NCAA solution and judging whether the pH value of the received NCAA solution is within the set pH threshold range of the NCAA solution or not;
the alkali liquor analysis processing module is used for converting the pH value of the alkali liquor received by the pH information acquisition module into the pH change rate of the alkali liquor within the set time;
the driving execution module is used for sending an operation signal to the circulating pump 23 when the addition amount of the neutralizing acid liquid received by the neutralizing acid liquid addition amount acquisition module reaches 20% of the preset total addition volume of the neutralizing acid liquid;
when the pH value of the NCAA solution falls into the pH threshold interval of the NCAA solution and the change rate of the pH value of the alkali liquor in a set time is less than 5 percent, or when the pH value of the NCAA solution is lower than the lower limit of the pH threshold interval of the NCAA solution, a stop signal is sent to the stirring mechanism 12 and the circulating pump 23;
and the display module is used for converting the pH value information of the NCAA solution and the pH value information of the alkali liquor received by the pH information acquisition module into visual signals and displaying the visual signals.
The implementation principle of the embodiment 2 is as follows: when the device is used, prepared alkali liquor is injected into the alkali washing tank 21 through the alkali liquor pipe 211, a quantitative NCAA solution is injected into the kettle body 11 through the liquid adding pipe 111, after the NCAA solution is injected, whether the pH value of the NCAA solution monitored by the first pH monitoring meter 31 displayed on the controller 33 is the normal pH value of the NCAA solution is checked, an organic solvent is quantitatively added into the kettle body 11 through the liquid adding pipe 111 after the NCAA solution is confirmed to be correct, and after the NCAA solution and the organic solvent are layered, the preparation work is completed.
Then, a stirring motor 121 of the stirring kettle 1 is started, the stirring motor 121 drives a stirring blade 123 to rotate through a stirring shaft 122, and further drives the NCAA solution to be stirred up and down in the solution area 114; when stirring is started, adding neutralizing acid liquor into the kettle body 11, after the neutralizing acid liquor is dripped, buffering the neutralizing acid liquor through an organic solvent layer, and then dispersing the neutralizing acid liquor into an NCAA solution layer, when the volume of the dripped neutralizing acid liquor reaches 20% of the total volume of the expected neutralizing acid liquor, controlling a circulating pump 23 to be started by a controller 33, so that the organic solvent starts to circulate, sending the organic solvent in the kettle body 11 into an alkaline washing tank 21 for alkaline washing, and pumping a toluene derivative in the organic solvent into the kettle body 11 again after being absorbed;
and when the pH value of the NCAA solution falls into the pH threshold interval of the NCAA solution and the change rate of the pH of the alkali liquor in a set time is less than 5 percent, or when the pH value of the NCAA solution is lower than the lower limit of the pH threshold interval of the NCAA solution, the controller 33 controls the stirring motor 121 and the circulating pump 23 to stop, the purification is finished, the liquid discharge pipe 113 of the kettle body 11 is opened, the NCAA solution and the organic solvent are discharged and separated, and the high-purity NCAA solution can be obtained.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. A neutralization acidification process of high-purity NCAA is characterized in that: the method comprises the following steps:
the method comprises the following steps: adding an organic solvent capable of forming an organic solvent layer above the NCAA solution layer to the NCAA solution;
step two: and stirring the NCAA solution layer, continuously dropwise adding a neutralization acid solution from the upper part of the organic solvent layer while stirring until the pH value of the NCAA solution layer is adjusted to 4-5, and separating the organic solvent layer from the NCAA solution layer to obtain the high-purity NCAA solution.
2. The process for neutralizing and acidifying high-purity NCAA of claim 1, wherein: and in the step two, in the process of adding acid and neutralizing, pumping the organic solvent into the organic solvent layer, and simultaneously extracting the organic solvent in the organic solvent layer so as to replace the organic solvent in the organic solvent layer.
3. The process for neutralizing acidification of high purity NCAA according to claim 2, characterized in that: and (2) introducing alkali liquor into the organic solvent extracted in the step two for alkali washing, washing off impurities dissolved in the organic solvent, and pumping the organic solvent obtained by alkali washing into the organic solvent layer again for circulation.
4. A neutralization acidification device based on the neutralization acidification process of high purity NCAA as claimed in claim 3, characterized in that: comprises a stirring kettle (1) and an alkaline washing circulating device (2); an acid adding pipe (112) is arranged at the top of a kettle body (11) of the stirring kettle (1), an inner cavity of the stirring kettle (1) is divided into a solution area (114) for containing NCAA solution and an organic solvent area (115) for containing organic solvent, the organic solvent area (115) is arranged above the solution area (114), a solvent inlet (116) and a solvent outlet (117) are arranged on the side wall of the stirring kettle (1) corresponding to the organic solvent area (115), and the solvent inlet (116) and the solvent outlet (117) are arranged at two opposite sides of the stirring kettle (1);
the alkali washing circulating device (2) comprises an alkali washing tank (21), a circulating pipe (22) and a circulating pump (23), wherein a solvent liquid inlet (116) and a solvent liquid outlet (117) are communicated with an inner cavity of the alkali washing tank (21) through the circulating pipe (22), and the circulating pump (23) is arranged on the circulating pipe (22).
5. The neutralizing acidifying device of claim 4, characterized in that: the solvent outlet (117) set up in organic solvent district (115) top, alkali wash jar (21) with the opening of solvent outlet (117) direct intercommunication is as organic solvent import (212), alkali wash jar (21) with the opening of solvent inlet (116) direct intercommunication is as organic solvent export (213), organic solvent import (212) set up in alkali wash jar (21) bottom, organic solvent export (213) set up in alkali wash jar (21) bottom top, just organic solvent import (212) and organic solvent export (213) set up in alkali wash jar (21) both sides.
6. The neutralizing acidifying device of claim 4, characterized in that: stirring blades (123) in the stirring kettle (1) are arranged to be pushing type stirring blades (123).
7. The neutralizing acidification device according to any one of claims 4 to 6, wherein: still include automated control device (3), automated control device (3) includes:
a first pH monitoring meter (31) arranged in the inner cavity of the stirring kettle (1) and used for monitoring the pH of the NCAA solution in the solution area (114);
the second pH monitoring meter (32) is arranged in the inner cavity of the alkaline washing tank (21) and is used for monitoring the pH of the alkaline liquor in the inner cavity of the alkaline washing tank (21);
and the input end of the controller (33) is electrically connected with the first pH monitoring meter (31) and the second pH monitoring meter (32), and the output end of the controller is electrically connected with the circulating pump (23) and the stirring mechanism (12) of the stirring kettle.
8. The neutralizing acidifying device of claim 7, wherein: be provided with automatic control system in controller (33), automatic control system includes:
the pH information acquisition module is used for receiving the pH value information of the NCAA solution detected by the first pH monitoring meter (31) and the pH value information of the alkali liquor detected by the second pH monitoring meter (32) in real time;
the NCAA solution analysis and processing module is used for setting the pH value to be 4-5 as the pH threshold of the NCAA solution, comparing the pH value information of the NCAA solution acquired by the pH information acquisition module with the pH set threshold of the NCAA solution and judging whether the pH value of the received NCAA solution is within the set pH threshold range of the NCAA solution or not;
the alkali liquor analysis processing module is used for converting the pH value of the alkali liquor received by the pH information acquisition module into the pH change rate of the alkali liquor within the set time;
and the driving execution module is used for sending a shutdown signal to the stirring mechanism (12) and the circulating pump (23) when the pH value of the NCAA solution falls into the pH threshold interval of the NCAA solution and the change rate of the pH of the alkali liquor in the set time is less than 5%, or the pH value of the NCAA solution is lower than the lower limit of the pH threshold interval of the NCAA solution.
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