CN112694097A - Control method for chemical waste-throwing phosphoric acid treatment and synthesis of aluminum phosphate molecular sieve - Google Patents
Control method for chemical waste-throwing phosphoric acid treatment and synthesis of aluminum phosphate molecular sieve Download PDFInfo
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- CN112694097A CN112694097A CN202110179489.3A CN202110179489A CN112694097A CN 112694097 A CN112694097 A CN 112694097A CN 202110179489 A CN202110179489 A CN 202110179489A CN 112694097 A CN112694097 A CN 112694097A
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- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/04—Aluminophosphates (APO compounds)
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
Abstract
The invention relates to a control method for chemical waste phosphoric acid treatment and synthesis of an aluminum phosphate molecular sieve. The method comprises the following steps: starting a system; the rinsing device detects whether the total phosphorus concentration of the selected area reaches a set value, if so, a signal is sent to the PLC, and the PLC controls to open the waste liquid discharge valve; if not, closing the waste liquid discharge valve; the liquid level sensor detects whether the liquid level of the transfer adjusting barrel reaches a set liquid level, if so, the vacuumizing evaporation cycle is started, and if not, the liquid inlet valve is closed; the PLC controls the evaporation concentrated solution to be discharged into the nuclear reactor, controls a feed valve and a feed pump to add liquid caustic soda, alumina monohydrate, a template agent and a mold aid according to a set proportion, and starts a stirrer; is the determination time reached to the set value If yes, the PLC controls the nucleated mother liquor to be discharged into a crystallization dryer, and if not, the nucleated mother liquor is returned; the PLC controls the crystal dryer to be turned on, and determines whether the time reaches a set value Closing the crystallization dryer, taking out the product, repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a control method for chemical waste phosphoric acid treatment and synthesis of an aluminum phosphate molecular sieve.
Background
The main pollutants in the waste water in the anodic oxidation industry come from various chemical auxiliary materials, acid and alkali and aluminum ions generated by the dissolution of the surface of an aluminum material. The main acids are phosphoric acid, sulfuric acid and nitric acid, which are produced in the chemical polishing process and the anodic oxidation process. The chemical polishing solution is usually mixed with phosphoric acid, sulfuric acid and nitric acid according to the proportion of 6:3: 1-7: 2:1 for use, aluminum ions are accumulated after long-term use, the concentration reaches a certain value and is repeatedly used, the product performance is influenced, and waste acid is formed immediately. The waste acid flows into a waste water system, so that most of TP and TN in the system are polluted, and a large amount of sludge is generated.
At present, the following three modes are generally adopted in the anodic oxidation wastewater treatment industry to treat the waste acid:
the method comprises the following steps: and completely mixing waste acid into the wastewater to form phosphorus-containing wastewater, and adding lime to react with phosphate radicals and sulfate radicals in the wastewater to form precipitates.
The method comprises the following steps of impurity removal, purification, evaporation and concentration regeneration: the waste phosphoric acid is collected, impurities are removed in modes of adsorption of aluminum ion barrel ion exchange resin in waste liquid and the like, then the waste acid liquid after the impurities are removed is recovered through evaporation and concentration, and evaporated water is mixed with other waste water for treatment.
The method for preparing the potassium hydrogen phosphate comprises the following steps: collecting waste phosphoric acid, precipitating by secondary reaction, filtering, reacting with lime milk under the condition of no pH value, grading and separating different products, and finally recovering potassium hydrogen phosphate.
However, the three common wastewater treatment methods have certain disadvantages. The first method produces a large amount of phosphorus-containing sludge. Meanwhile, nitrate radicals in the waste liquid are not removed in the reaction, so that the total nitrogen of the waste water system does not reach the standard. The second method has the defects that the optimal impurity removal rate of aluminum ions is only 30 percent, the recovery efficiency of waste acid is 60 percent, the recovery cost is high, the economic benefit is poor, and nearly 40 percent of phosphoric acid is converted into sludge. The third method has higher requirements on process control and equipment, and the recovery efficiency of waste acid can reach 90 percent, and is generally adopted by hazardous waste disposal units. For anode plants, the disposal cost is high by directly outsourcing the waste liquid to dangerous waste companies.
Disclosure of Invention
The invention aims to provide a control method for chemical waste-disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis, which can comprehensively solve the problem of overproof total phosphorus in an anodic oxidation plant, greatly reduce the addition of lime, phosphorus removing agent and other agents in wastewater treatment, reduce the wastewater treatment cost by half, improve the treatment efficiency by one time, recycle and intelligentize chemical waste-disposal phosphoric acid in the treatment process and thoroughly solve the problem of high cost outside the commission of dangerous waste.
The technical scheme of the invention is that the control method for chemical waste-throwing phosphoric acid treatment and synthesis of the aluminum phosphate molecular sieve is characterized by comprising the following steps:
firstly, electrifying and starting a system;
the novel three-level rinsing device detects the total phosphorus concentration in the selected area;
thirdly, judging whether the concentration reaches a set value, if so, sending a signal to a PLC (programmable logic controller), and controlling to open a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the second step;
fourthly, starting a vacuumizing evaporation cycle;
fifthly, discharging the evaporation concentrated solution into the nuclear reactor, controlling a feed valve and a feed pump by the PLC to add liquid alkali, alumina monohydrate, a template agent and a mold aid according to a set proportion, and starting a stirrer;
judging whether the set time is reached, and if not, returning to the step of the first step; if yes, entering the next step;
turn-on nuclear reactor discharge valves, slurry pumps;
judging whether the set time is reached, if not, returning to step-quietness; if yes, entering the next step;
the self-lifting closes a discharge valve and a slurry discharge pump of the nuclear reactor;
simultaneously starting a crystallization dryer;
judging whether the set time is reached or not, and if not, returning to the step to obtain the advantages; if yes, entering the next step;
closing the crystallization dryer, taking out the product, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
Preferably, the method comprises the following steps: step four the evacuation evaporation cycle includes:
(4.1.1) detecting the liquid level of the transfer adjusting barrel through a liquid level sensor;
(4.1.2) detecting whether the liquid level reaches a set liquid level, if so, starting a circulating water pump communicated with a circulating water tank by PLC control, opening a liquid inlet valve, and continuously pumping out air in the evaporator by the circulating water pump to change the interior of the evaporator into negative pressure;
(4.1.3) if not, the liquid level sensor transmits a signal to the PLC, the PLC controls to close the circulating water pump and open the emptying valve, and the step (4.1.1) is returned;
(4.1.4) detecting the vacuum degree in the evaporator by a vacuum gauge;
(4.1.5) judging whether the vacuum degree is greater than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling the starting of an evaporator by the PLC to heat, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), sucking waste liquid into the evaporator through a liquid inlet valve by negative pressure, and detecting the liquid level of the evaporator by a liquid level sensor in the evaporator;
(4.1.7) judging whether the liquid level in the evaporator is higher than a high liquid level, if so, transmitting a signal to a PLC by a liquid level sensor in the evaporator, and controlling to close a liquid inlet valve by the PLC; if not, returning to the step (6.1.6);
(4.1.8) judging whether the liquid level in the evaporator is lower than a low liquid level, if so, transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the evaporator, controlling to close a circulating water pump communicated with a circulating water tank, open an emptying valve and a discharge valve and open a liquid discharge pump communicated with the discharge valve by the PLC;
(4.1.9) judging whether the time reaches a set value, if so, after waiting for the set time, discharging the concentrated solution, closing an emptying valve, a discharge valve and a liquid discharge pump, and returning to the step (4.1.2); if not, the step (4.1.8) is returned.
Preferably, the method comprises the following steps: step four the evacuation evaporation cycle includes:
(4.2.1) detecting the water level in the circulating water tank by a liquid level sensor in the circulating water tank;
(4.2.2) judging whether the water level is higher than the set high water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.3) transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the circulating water tank, controlling by the PLC to open a drain valve, draining water outwards, and returning to the step (4.2.1);
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.5) the liquid level sensor in the circulating water tank transmits a signal to the PLC, the PLC controls the closing of the drain valve, and the step (4.2.1) is returned.
Compared with the prior art, the invention has the beneficial effects that:
the waste phosphoric acid produced in the chemical polishing process of the anodic oxidation plant is the largest source of total phosphorus pollution in wastewater, and has the characteristics of dispersive distribution, small amount, high concentration, high sludge production and the like. Compared with other chemical waste liquid treatment methods, the method provided by the invention can realize 100% harmless and resource treatment of waste phosphoric acid. The invention adopts a novel three-stage water washing device to control and select the chemical polishing waste phosphoric acid, thereby ensuring that the waste phosphoric acid system TP stably reaches the standard, and simultaneously, the waste phosphoric acid is treated to the utmost extent through the method of the invention in a harmless and resource way. The intelligent and efficient control of the dephosphorization efficiency is realized, and the TP standard of the wastewater is ensured. The generated waste phosphoric acid is rich in phosphorus and aluminum and finally serves as a main material for synthesizing the aluminum phosphate molecular sieve. In the process, all the chemical phosphorus-containing waste liquid does not generate sludge any more, and secondary economic benefit is obtained.
And in the process, 100% of phosphorus-containing waste liquid is chemically thrown, so that no sludge is generated, the sludge generation amount of an anodic oxidation plant can be integrally reduced by 2/3, the large sludge treatment and disposal cost of enterprises can be saved, and the environmental protection benefit can be created for the society.
The waste phosphoric acid generated by the method is rich in phosphorus and aluminum and is used as a main material, and the aluminum phosphate molecular sieve is produced in situ by a synthesis method in the invention, so that secondary recovery economic benefits are generated.
The synthetic raw materials only need to be added with a small amount of liquid alkali, alumina monohydrate, a template agent and a mold aid. The dosage is less, thereby reducing the synthesis cost.
The wastewater generated in the synthesis process of the invention has extremely low phosphorus concentration, and has no influence on a wastewater system.
Sixthly, separating sulfuric acid in the synthesis process, wherein the quality of an aluminum phosphate molecular sieve product is not affected.
Drawings
FIG. 1 is a schematic diagram of the structure of a chemical waste-disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system of an anodic oxidation plant according to the present invention;
FIG. 2 is a schematic diagram of the drainage of the chemical waste phosphoric acid disposal and aluminum phosphate molecular sieve synthesis system of the anodic oxidation plant according to the present invention;
FIG. 3 is a schematic structural diagram of a novel three-stage rinsing device of the chemical waste phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system of the anodic oxidation plant according to the present invention;
FIG. 4 is a flow diagram of the process for chemical polishing of waste phosphoric acid and controlling synthesis of aluminum phosphate molecular sieves in an anodic oxidation plant according to the present invention;
FIG. 5 is a process diagram of the process of the present invention for chemical waste phosphoric acid treatment and aluminum phosphate molecular sieve synthesis in an anodic oxidation plant.
Description of the main component symbols:
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Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings:
referring to fig. 4, the method for controlling the chemical waste disposal of phosphoric acid and the synthesis of aluminum phosphate molecular sieve includes the following steps:
firstly, electrifying and starting a system;
the novel three-level rinsing device detects the total phosphorus concentration in the selected area;
thirdly, judging whether the concentration reaches a set value, if so, sending a signal to a PLC (programmable logic controller), and controlling to open a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the second step;
fourthly, starting a vacuumizing evaporation cycle;
(4.1.1) detecting the liquid level of the transfer adjusting barrel through a liquid level sensor;
(4.1.2) detecting whether the liquid level reaches a set liquid level, if so, starting a circulating water pump communicated with a circulating water tank by PLC control, opening a liquid inlet valve, and continuously pumping out air in the evaporator by the circulating water pump to change the interior of the evaporator into negative pressure;
(4.1.3) if not, the liquid level sensor transmits a signal to the PLC, the PLC controls to close the circulating water pump and open the emptying valve, and the step (4.1.1) is returned;
(4.1.4) detecting the vacuum degree in the evaporator by a vacuum gauge;
(4.1.5) judging whether the vacuum degree is greater than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling the starting of an evaporator by the PLC to heat, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), sucking waste liquid into the evaporator through a liquid inlet valve by negative pressure, and detecting the liquid level of the evaporator by a liquid level sensor in the evaporator;
(4.1.7) judging whether the liquid level in the evaporator is higher than a high liquid level, if so, transmitting a signal to a PLC by a liquid level sensor in the evaporator, and controlling to close a liquid inlet valve by the PLC; if not, returning to the step (6.1.6);
(4.1.8) judging whether the liquid level in the evaporator is lower than a low liquid level, if so, transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the evaporator, controlling to close a circulating water pump communicated with a circulating water tank, open an emptying valve and a discharge valve and open a liquid discharge pump communicated with the discharge valve by the PLC;
(4.1.9) judging whether the time reaches a set value, if so, after waiting for the set time, discharging the concentrated solution, closing an emptying valve, a discharge valve and a liquid discharge pump, and returning to the step (4.1.2); if not, the step (4.1.8) is returned.
(4.2.1) detecting the water level in the circulating water tank by a liquid level sensor in the circulating water tank;
(4.2.2) judging whether the water level is higher than the set high water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.3) transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the circulating water tank, controlling by the PLC to open a drain valve, draining water outwards, and returning to the step (4.2.1);
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.5) transmitting a signal to a PLC by a liquid level sensor in the circulating water tank, controlling by the PLC to close the drain valve, and returning to the step (4.2.1);
fifthly, discharging the evaporation concentrated solution into the nuclear reactor, controlling a feed valve and a feed pump by the PLC to add liquid alkali, alumina monohydrate, a template agent and a mold aid according to a set proportion, and starting a stirrer;
judging whether the set time is reached, and if not, returning to the step of the first step; if yes, entering the next step;
turn-on nuclear reactor discharge valves, slurry pumps;
judging whether the set time is reached, if not, returning to step-quietness; if yes, entering the next step;
the self-lifting closes a discharge valve and a slurry discharge pump of the nuclear reactor;
simultaneously starting a crystallization dryer;
judging whether the set time is reached or not, and if not, returning to the step to obtain the advantages; if yes, entering the next step;
closing the crystallization dryer, taking out the product, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
Fig. 1 to 3 show the structure of the system for treating waste phosphoric acid from the anodic oxidation plant and synthesizing aluminum phosphate molecular sieves according to the present invention.
Referring to fig. 1, the system for treating chemically-discarded waste phosphoric acid and synthesizing an aluminum phosphate molecular sieve comprises a novel three-stage rinsing device, an evaporation concentration unit, a heterogeneous nucleation reaction unit and a crystallization dryer which are sequentially communicated by pipelines,
referring to fig. 2 and 3, the novel three-stage rinsing device is composed of a selection area, an overflow area and a rinsing area; the bottom of the selection area is provided with a waste liquid discharge valve communicated with the transfer adjusting barrel, the detection linkage control is used for discharging and chemically throwing a waste liquid, an online specific gravity signal is set through a PLC program to be linked with the waste liquid discharge valve of the selection area, and the selection area is provided with an online specific gravity detector; the upper part of the overflow area is provided with an overflow pipe, and a pipeline is connected to a wastewater treatment station for phosphorus-containing wastewater treatment; the bottom of the rinsing area is communicated with the overflow area, and the upper part of the rinsing area is provided with a cleaning water inlet pipe;
referring to fig. 1, the evaporation concentration unit is composed of a transfer adjusting barrel, an evaporator with the transfer adjusting barrel communicated with a liquid inlet valve through a pipeline, a discharge valve and a liquid discharge pump with the output end of the evaporator communicated with each other sequentially through a pipeline, a condenser with the evaporator communicated with each other through a steam channel, a circulating water tank with the condenser communicated with the ejector through a pipeline, and drain valves respectively communicated with the ejector through a pipeline and connected to the circulating water pump; the circulating water pump is communicated with the circulating water tank; a liquid level sensor and a pH meter are arranged in the transfer adjusting barrel, waste liquid is discharged into the transfer adjusting barrel through selective chemical polishing, when the liquid level sensor in the transfer adjusting barrel reaches a set liquid level in the barrel, a signal is transmitted to the PLC, and a waste liquid discharge valve of the novel three-stage rinsing device is closed; the heterogeneous nucleation reaction unit consists of a nucleation reactor with an input port communicated with a liquid discharge pump, a stirrer arranged in the nucleation reactor, a second discharge valve connected with an output port of the nucleation reactor, a slurry discharge pump, a feeding valve connected with the other output port of the nucleation reactor, a feeding pump and a dosing tank communicated with the feeding pump; a feed valve and a feed pump connected with the nuclear reactor; the novel three-stage rinsing device, the evaporation concentration unit, the heterogeneous nucleation reaction unit and the crystallization dryer are controlled and linked by a PLC (programmable logic controller); the system further comprises a control circuit, wherein the control circuit comprises a PLC (programmable logic controller), and the PLC controls the novel three-level rinsing device, the evaporation concentration unit, the heterogeneous nucleation reaction unit and the crystallization dryer respectively in a control signal communication mode.
Referring to fig. 1 to 3, the method for treating chemically-discarded waste phosphoric acid and detecting an aluminum phosphate molecular sieve comprises the following steps:
the novel three-stage rinsing device comprises an online specific gravity detector, a waste liquid discharge valve, a control circuit and a control circuit, wherein the online specific gravity detector detects the total phosphorus concentration of a selection area of the novel three-stage rinsing device, and the waste liquid discharge valve is opened after the total phosphorus concentration of the selection area reaches a set value;
when the waste liquid discharge valve is opened, the PLC receives a total phosphorus concentration signal of a selected area, and transmits the total phosphorus concentration signal of the phosphorus-containing wastewater of the overflow area to a wastewater treatment station, so that the adding amount of a phosphorus removing agent is controlled, and total phosphorus in the wastewater is accurately and stably removed;
after the equipment is started, the liquid level sensor in the transfer adjusting barrel senses that the liquid level reaches a set value, and a circulating water pump communicated with the circulating water tank is started;
fourthly, the distilled water in the circulating water tank is pressurized by a circulating water pump and then returns to the circulating water tank through an ejector, high-speed jet flow is formed in the ejector through high-pressure water, air in the evaporator and a connecting pipeline is pumped out, and a low-pressure environment is formed in the evaporator;
fifthly, when the set vacuum degree in the evaporator is achieved, starting a liquid inlet valve; the negative pressure makes the waste liquid in the transit regulating barrel enter the evaporator through a liquid inlet valve arranged in the pipeline, when a liquid level sensor in the evaporator senses that the liquid level of the evaporator reaches a set value, the liquid inlet valve is closed, the evaporator starts a heating device, and the waste liquid is evaporated and concentrated;
sixthly, enabling the steam to reach a condenser through a steam pipeline, condensing the steam into water in the condenser, and pumping the water into an ejector so as to enter a circulating water tank; when the liquid level sensor in the circulating water tank automatically senses that the liquid level is higher than a set value, the drain valve is opened, and when the liquid level sensor in the circulating water tank automatically senses that the liquid level is lower than the set value, the drain valve is closed;
when the liquid level of the waste liquid in the evaporator is lower than the set value of a liquid level sensor in the evaporator, the circulating water pump stops working, an emptying valve of the evaporator is opened, after the pressure is emptied, a first emptying valve is opened, and a concentrated liquid is discharged to the nuclear reactor by a liquid discharge pump;
a feeding valve and a feeding pump which are connected in turn through a pipeline in the nuclear reactor, wherein the feeding pump is opened and then liquid alkali, alumina monohydrate, a template agent and a mold aid are added according to a set proportion, a reaction stirrer is started, and the reaction stirrer is stopped after a set time is reached; opening a slurry discharge valve, and discharging the nucleation mother liquor into a crystallization dryer through a slurry discharge pump connected with a pipeline;
the self-lifting starts a crystallization dryer and stops after a set time is reached;
the product in the crystallization dryer is backwashed, washed and dried to obtain the aluminum phosphate molecular sieve product.
Step two in this embodiment is 5 ~ 10:1 for novel tertiary rinsing device selective area total phosphorus concentration and overflow area total phosphorus concentration ratio, and when the waste liquid discharge valve was opened, PLC received selective area total phosphorus concentration signal, and the phosphorus wastewater concentration in equal proportion calculation overflow area simultaneously, with signal transmission to waste water treatment station, through control measuring pump intelligent regulation dephosphorization agent input volume, total phosphorus obtains accurate stability in the waste water and gets rid of.
Referring to fig. 5, the method for treating chemical waste phosphoric acid and synthesizing an aluminum phosphate molecular sieve comprises the following steps:
the novel three-stage rinsing device is adopted for selecting, collecting and cooling the concentration of waste liquid in one chemical polishing step;
evaporating and concentrating the waste liquid by adopting a negative pressure evaporation method to obtain an aluminum phosphate molecular sieve synthetic mother liquid;
thirdly, adding liquid caustic soda, alumina monohydrate, a template agent and a mold aid into the mother liquor; stirring and reacting at normal temperature, and performing natural nucleation;
and fourthly, allowing the nucleated mother liquor to enter a crystallization dryer, completing crystallization reaction at 800-910 ℃, taking out the crystal after the crystal is cooled to normal temperature, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
In the embodiment, the novel three-stage rinsing device is a three-stage countercurrent rinsing device and consists of a selection area, an overflow area and a rinsing area; the bottom of the selection area is provided with a waste liquid discharge valve communicated with the transfer adjusting barrel, the detection linkage control is used for discharging and chemically throwing a waste liquid, and an online specific gravity signal is set through a PLC program to be linked with the waste liquid discharge valve of the selection area; the selection area is provided with an online specific gravity detector, the measurement range of the online specific gravity detector is 1.05-2.0, and the total phosphorus concentration of the once-treated discharge waste liquid is controlled to be more than or equal to 10000 mg/L; the upper part of the overflow area is provided with an overflow pipe, a pipeline is connected to a wastewater treatment station for phosphorus-containing wastewater treatment, the bottom of the rinsing area is communicated with the overflow area, and the upper part of the rinsing area is provided with a cleaning water inlet pipe.
In the embodiment, the evaporation concentration unit in the second step consists of a transfer adjusting barrel, a liquid level sensor, a pH meter, an evaporator, a first discharge valve, a first discharge pump, a liquid level sensor, a vacuum meter, an emptying valve, a condenser, a circulating water tank, a drain valve, a jet device and a drain valve, wherein the liquid level sensor, the pH meter and the transfer adjusting barrel are arranged in the transfer adjusting barrel; the circulating water pump is communicated with the circulating water tank; the waste liquid from the selected chemical polishing step flows into a transfer adjusting barrel, and when a liquid level sensor in the transfer adjusting barrel reaches a set high liquid level in the barrel, a signal is transmitted to a PLC (programmable logic controller), and a waste liquid discharge valve of the novel three-stage rinsing device is closed; when the vacuum degree in the evaporator reaches 0.09Mpa, a liquid inlet valve is opened, and liquid is sucked through negative pressure; the single liquid inlet amount is more than or equal to 100L, and the concentration ratio is 10-80 percent.
In the embodiment, the evaporation concentration unit is used for evaporating the selected chemical polishing waste liquid under negative pressure and controlling the specific gravity to be 1.2-2.0, the evaporation condensate TP is less than 50mg/L, when the evaporation concentrate reaches a low liquid level set by a liquid level sensor, a first discharge valve is opened, and the concentrate is discharged to the out-of-phase nucleation reaction unit through a liquid discharge pump; the evaporation temperature is 30-90 ℃, the negative pressure is 0.09-0.1 Mpa, and the evaporation concentration unit, the waste acid contact heating part and the container are both made of strong acid resistant materials; the evaporator is in butt joint with the condenser, the condenser is communicated with the circulating water tank through the ejector, the circulating water tank is provided with a liquid level sensor, steam enters the condenser through a steam pipeline, is condensed into water in the condenser and is sucked into the ejector to enter the circulating water tank, when the liquid level sensor automatically senses that the liquid level is higher than a set value, the drain valve is opened, and when the liquid level in the circulating water tank is lower than the set value, the drain valve is closed.
In this embodiment, an out-of-phase nucleation reaction unit is provided in step three, and the out-of-phase nucleation reaction unit is composed of a stirrer, a nucleation reactor with an input port communicated with a liquid discharge pump, a second discharge valve connected to an output port of the nucleation reactor, a slurry discharge pump, a feed valve, a feed pump, and a dosing tank, which are sequentially communicated with another output port of the nucleation reactor.
In this embodiment, the gel-state nucleation mother liquor in step three is synthesized by reaction in the nucleation reactor; the evaporation concentrated solution from the evaporation concentration unit enters the nucleation reactor from a pipeline, and is sequentially connected with a feed valve and a feed pump through the pipeline, the feed pump is opened, and the nucleation reaction zone is stirred through a stirrer and is provided with a liquid level sensor and a pH meter; adding liquid caustic soda, alumina monohydrate, template agent and auxiliary mold agent in proportion, and stopping after reaching set time; opening a second discharge valve, and discharging the slurry into a crystallization dryer through a slurry discharge pump connected with a pipeline; al: p: template agent: the proportion of H2O is 1 (1-0.6): (0.75-1.35): 25-75), the reaction time is not less than 2H; the pH value is 1.5-8.5.
In this embodiment, the material of the crystal dryer in the step four is hastelloy and is resistant to strong acid; step four, the crystallization dryer is a box dryer or a drum dryer, and the reaction temperature is 800-910 ℃; crystallizing the nucleation mother liquor in the crystallization dryer, wherein the volume of the nucleation mother liquor is more than or equal to 60%, the operating pressure is 0.1Mpa, the reaction temperature is 800-910 ℃, the reaction time is more than or equal to 48 hours, separating sulfuric acid during reaction, absorbing the separated sulfuric acid by using a drying absorption tower, and recycling the sulfuric acid in a workshop after saturation; and after the reaction is completed, washing, drying and drying the product for 24 hours to obtain the aluminum phosphate molecular sieve product.
The above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the claims of the present invention.
Claims (3)
1. A control method for chemical waste phosphoric acid disposal and synthesis of an aluminum phosphate molecular sieve is characterized by comprising the following steps:
firstly, electrifying and starting a system;
the novel three-level rinsing device detects the total phosphorus concentration in the selected area;
thirdly, judging whether the concentration reaches a set value, if so, sending a signal to a PLC (programmable logic controller), and controlling to open a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the second step;
fourthly, starting a vacuumizing evaporation cycle;
fifthly, discharging the evaporation concentrated solution into the nuclear reactor, controlling a feed valve and a feed pump by the PLC to add liquid alkali, alumina monohydrate, a template agent and a mold aid according to a set proportion, and starting a stirrer;
judging whether the set time is reached, and if not, returning to the step of the first step; if yes, entering the next step;
turn-on nuclear reactor discharge valves, slurry pumps;
judging whether the set time is reached, if not, returning to step-quietness; if yes, entering the next step; the self-lifting closes a discharge valve and a slurry discharge pump of the nuclear reactor;
simultaneously starting a crystallization dryer;
judging whether the set time is reached or not, and if not, returning to the step to obtain the advantages; if yes, entering the next step;
closing the crystallization dryer, taking out the product, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
2. The method for controlling chemical polishing waste phosphoric acid treatment and synthesis of an aluminum phosphate molecular sieve according to claim 1, wherein the vacuum evaporation cycle comprises:
(4.1.1) detecting the liquid level of the transfer adjusting barrel through a liquid level sensor;
(4.1.2) detecting whether the liquid level reaches a set liquid level, if so, starting a circulating water pump communicated with a circulating water tank by PLC control, opening a liquid inlet valve, and continuously pumping out air in the evaporator by the circulating water pump to change the interior of the evaporator into negative pressure;
(4.1.3) if not, the liquid level sensor transmits a signal to the PLC, the PLC controls to close the circulating water pump and open the emptying valve, and the step (4.1.1) is returned;
(4.1.4) detecting the vacuum degree in the evaporator by a vacuum gauge;
(4.1.5) judging whether the vacuum degree is greater than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling the starting of an evaporator by the PLC to heat, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), sucking waste liquid into the evaporator through a liquid inlet valve by negative pressure, and detecting the liquid level of the evaporator by a liquid level sensor in the evaporator;
(4.1.7) judging whether the liquid level in the evaporator is higher than a high liquid level, if so, transmitting a signal to a PLC by a liquid level sensor in the evaporator, and controlling to close a liquid inlet valve by the PLC; if not, returning to the step (6.1.6);
(4.1.8) judging whether the liquid level in the evaporator is lower than a low liquid level, if so, transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the evaporator, controlling to close a circulating water pump communicated with a circulating water tank, open an emptying valve and a discharge valve and open a liquid discharge pump communicated with the discharge valve by the PLC;
(4.1.9) judging whether the time reaches a set value, if so, after waiting for the set time, discharging the concentrated solution, closing an emptying valve, a discharge valve and a liquid discharge pump, and returning to the step (4.1.2); if not, the step (4.1.8) is returned.
3. The method for controlling the chemical polishing waste phosphoric acid treatment and the synthesis of the aluminum phosphate molecular sieve according to claim 1, wherein the vacuumizing evaporation cycle comprises:
(4.2.1) detecting the water level in the circulating water tank by a liquid level sensor in the circulating water tank;
(4.2.2) judging whether the water level is higher than the set high water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.3) transmitting a signal to a PLC (programmable logic controller) by a liquid level sensor in the circulating water tank, controlling by the PLC to open a drain valve, draining water outwards, and returning to the step (4.2.1);
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, if not, returning to the step (4.2.1); if yes, the next step is carried out:
(4.2.5) the liquid level sensor in the circulating water tank transmits a signal to the PLC, the PLC controls the closing of the drain valve, and the step (4.2.1) is returned.
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| JP2013071868A (en) * | 2011-09-28 | 2013-04-22 | Jgc Catalysts & Chemicals Ltd | Core-shell type crystalline silico-aluminophosphate particle, and molded catalyst including the particle |
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| JP2013071868A (en) * | 2011-09-28 | 2013-04-22 | Jgc Catalysts & Chemicals Ltd | Core-shell type crystalline silico-aluminophosphate particle, and molded catalyst including the particle |
| CN103553072A (en) * | 2013-08-26 | 2014-02-05 | 吉林大学 | Method for synthesizing aluminum phosphate molecular sieve and open framework material by using alkali metal as template |
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