CN112694097B - Control method for chemical waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis - Google Patents
Control method for chemical waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis Download PDFInfo
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Abstract
The invention relates to a control method for chemical waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis. Comprising the following steps: starting a system; the rinsing device detects whether the total phosphorus concentration in the selection area reaches a set value, if so, a signal is sent to the PLC, and the PLC controls the waste liquid discharge valve to be opened; if not, closing the waste liquid discharge valve; the liquid level sensor detects whether the liquid level of the transfer regulating 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 concentrate to be discharged into a nucleation reactor, controls a feed valve and a feed pump to add liquid alkali, alumina monohydrate, a template agent and a mold aid according to a set proportion, and starts a stirrer; judging that the time reaches the set value If yes, the PLC controls the nucleation mother liquor to be discharged into a crystallization dryer, if not, the nucleation mother liquor is returned; the PLC controls the crystallization dryer to be turned on, and determines whether the time reaches the set value And closing the crystallization dryer, taking out the product, and 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 disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis.
Background
The main pollutants in the wastewater in the anodic oxidation industry come from various chemical auxiliary materials, acid and alkali and aluminum ions generated by the surface dissolution of aluminum materials. The main acids are phosphoric acid, sulfuric acid, nitric acid, and are produced from chemical polishing and anodic oxidation processes. 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, aluminum ions are accumulated after long-term use, the concentration reaches a certain value, the product performance is influenced by repeated use, and the chemical polishing solution becomes waste acid. Such waste acid flows into the wastewater system to cause pollution of most of TP and TN of the system, and a large amount of sludge is generated.
At present, the waste acid is treated in three ways in the anodic oxidation waste water treatment industry:
chemical method: the waste acid is fully mixed into the waste water to form phosphorus-containing waste water, and reacts with phosphate radical and sulfate radical in the waste water to form precipitate by adding lime for reaction.
Impurity removal purification-evaporation concentration regeneration method: and collecting waste phosphoric acid, removing impurities in the waste liquid by means of adsorption of an aluminum ion barrel ion exchange resin and the like, recovering the waste acid liquid after removing the impurities through evaporation concentration, and mixing the evaporated water with other waste water for treatment.
The method for preparing the potassium hydrogen phosphate comprises the following steps: and collecting waste phosphoric acid, performing secondary reaction precipitation, 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 in the waste liquid is not removed in the reaction, so that the total nitrogen in the waste water system does not reach the standard. The second method has the defects that the impurity removal rate of aluminum ions is only 30% optimally, the recovery efficiency of waste acid is 60%, the recovery cost is high, the economic benefit is poor, and nearly 40% of phosphoric acid is still converted into sludge. The third method has higher requirements on process control and equipment, the recovery efficiency of waste acid can reach 90%, and the waste acid is generally adopted by hazardous waste disposal units. For the anode factories, the cost of directly outsourcing waste liquid to hazardous waste companies is high.
Disclosure of Invention
The invention aims to provide a control method for treating waste disposal phosphoric acid and synthesizing an aluminum phosphate molecular sieve, which comprehensively solves the problem of exceeding total phosphorus in an anodic oxidation factory, greatly reduces the addition amount of lime, phosphorus removing agent and other agents in wastewater treatment, reduces the wastewater treatment cost by half, improves the treatment efficiency by one time, recycles and intellectuzes waste disposal phosphoric acid in the treatment process, and thoroughly solves the problem of high cost outside hazardous waste commission.
The technical scheme of the invention is that the method for controlling the chemical waste disposal phosphoric acid treatment and the synthesis of the aluminum phosphate molecular sieve is characterized by comprising the following steps:
the method comprises the steps of powering up and starting a system;
detecting the total phosphorus concentration of a selection area by a novel three-level rinsing device;
judging whether the concentration reaches a set value, if so, sending a signal to a PLC, and controlling the opening of a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the step (II);
starting vacuumizing and evaporating circulation;
fifthly, discharging the evaporated concentrated solution into a nucleation reactor, controlling a feed valve and a feed pump by a PLC (programmable logic controller) to add liquid alkali, alumina monohydrate, a template agent and a mold aid agent according to a set proportion, and starting a stirrer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
starting a nucleation reactor discharge valve and a slurry discharge pump;
judging whether the set time is reached, if not, returning to the step I; if yes, entering the next step;
closing a nucleation reactor discharge valve and a slurry discharge pump;
simultaneously starting a crystallization dryer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
and (3) closing the crystallization dryer, taking out the product, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
As preferable: the step four, the vacuumizing evaporation cycle comprises the following steps:
(4.1.1) detecting the liquid level of the transfer regulating 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 operating the circulating water pump to continuously pump out air in the evaporator so as to change the interior of the evaporator into negative pressure;
if not, the liquid level sensor transmits a signal to the PLC, and the PLC controls the circulating water pump to be closed and the vent valve to be opened, 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 larger than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling and starting the evaporator to heat by the PLC, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), wherein the negative pressure sucks the waste liquid into the evaporator through the liquid inlet valve, and a liquid level sensor in the evaporator detects the liquid level of 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 (programmable logic controller) by a liquid level sensor in the evaporator, and controlling the PLC to close a liquid inlet valve; 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 by a liquid level sensor in the evaporator, and controlling to close a circulating water pump communicated with a circulating water tank, open a vent valve and a discharge valve by the PLC, and open a liquid discharge pump communicated with the discharge valve;
(4.1.9) judging whether the time reaches a set value, if so, waiting for the set time, discharging the concentrated solution, closing a discharge valve and a discharge valve, discharging the liquid pump, and returning to the step (4.1.2); if not, returning to the step (4.1.8).
As preferable: the step four, the vacuumizing evaporation cycle comprises the following steps:
(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, entering the following steps:
(4.2.3) a liquid level sensor in the circulating water tank transmits a signal to a PLC, the PLC controls the opening of a drain valve, water is discharged outwards, and the step (4.2.1) is returned;
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, and if not, returning to the step (4.2.1); if yes, entering the following steps:
and (4.2.5) transmitting a signal to a PLC by a liquid level sensor in the circulating water tank, closing the drain valve by the PLC, and returning to the step (4.2.1).
Compared with the prior art, the invention has the beneficial effects that:
the waste phosphoric acid generated in the chemical polishing process of an anodic oxidation factory is the largest total phosphorus pollution source in wastewater, and has the characteristics of dispersed distribution, small quantity, large concentration, large mud yield and the like. Compared with other chemical waste liquid disposal methods, the method provided by the invention can realize 100% innocuous and resource disposal of waste phosphoric acid. The invention adopts the novel three-stage washing device to control and select the chemical polishing waste phosphoric acid, thereby ensuring that the waste phosphoric acid is harmless and recycled by the method of the invention to the maximum extent while ensuring that the TP of the waste water system meets the standard. The intelligent and efficient control of the dephosphorization efficiency is realized, and the wastewater TP is ensured to reach the standard. The generated waste phosphoric acid is rich in phosphorus and aluminum and is finally used as a main material for synthesizing the aluminum phosphate molecular sieve. In the process, all the chemical throwing phosphorus-containing waste liquid does not generate sludge any more, and secondary economic benefit is obtained.
In the process, all chemical throwing phosphorus-containing waste liquid is 100% free of sludge, so that the sludge generation amount of an anodic oxidation factory can be reduced by 2/3 as a whole, the large sludge treatment and disposal cost is saved for enterprises, and environmental protection benefits are created for 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 the secondary recovery economic benefit is generated.
Only a small amount of liquid alkali, alumina monohydrate, a template agent and a mold aid are needed to be added into the synthetic raw materials. The dosage is small, thereby reducing the synthesis cost.
The phosphorus concentration of the wastewater generated in the synthesis process is extremely low, and the wastewater system is not influenced.
The sulfuric acid is separated in the synthesis process, and the quality of the aluminum phosphate molecular sieve product is not affected.
Drawings
FIG. 1 is a schematic diagram of the anodic oxidation factory waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system of the invention;
FIG. 2 is a schematic diagram of the drainage mode of the anodic oxidation factory-like waste-disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system of the invention;
FIG. 3 is a schematic diagram of the structure of a novel three-stage rinsing device of the anodic oxidation factory-like waste polishing phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system;
FIG. 4 is a flow chart of the anodic oxidation factory-like waste-disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis control method of the invention;
FIG. 5 is a process diagram of the anodic oxidation factory waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis method of the invention.
Description of main reference numerals:
| novel three-level rinsing device 1 | Select area 11 | Waste liquid discharge valve 111 |
| Specific gravity detector 112 | Overflow area 12 | Overflow pipe 121 |
| Rinsing zone 13 | Cleaning water inlet pipe 131 | Evaporation concentration unit 2 |
| Transfer adjusting barrel 21 | Liquid inlet valve 211 | Liquid level sensor 212 |
| PH meter 213 | Evaporator 22 | Discharge valve 221 |
| Drain pump 222 | Vacuum gauge 223 | Blow-off valve 224 |
| Condenser 23 | Jet device 24 | Circulation tank 25 |
| Liquid level sensor 251 | Drain valve 26 | Liquid level sensor 27 |
| Circulating water pump 28 | Nucleation unit 3 | Stirrer 31 |
| Nucleation reactor 32 | Discharge valve 33 | Pulp discharge pump 34 |
| Feed valve 35 | Feed pump 36 | Dosing box 37 |
| Crystallization dryer 4 | PLC controller 5 |
Detailed Description
The invention will be further described in detail below with reference to the accompanying drawings:
referring to fig. 4, the method for controlling the chemical waste disposal phosphoric acid treatment and the synthesis of the aluminum phosphate molecular sieve comprises the following steps:
the method comprises the steps of powering up and starting a system;
detecting the total phosphorus concentration of a selection area by a novel three-level rinsing device;
judging whether the concentration reaches a set value, if so, sending a signal to a PLC, and controlling the opening of a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the step (II);
starting vacuumizing and evaporating circulation;
(4.1.1) detecting the liquid level of the transfer regulating 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 operating the circulating water pump to continuously pump out air in the evaporator so as to change the interior of the evaporator into negative pressure;
if not, the liquid level sensor transmits a signal to the PLC, and the PLC controls the circulating water pump to be closed and the vent valve to be opened, 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 larger than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling and starting the evaporator to heat by the PLC, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), wherein the negative pressure sucks the waste liquid into the evaporator through the liquid inlet valve, and a liquid level sensor in the evaporator detects the liquid level of 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 (programmable logic controller) by a liquid level sensor in the evaporator, and controlling the PLC to close a liquid inlet valve; 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 by a liquid level sensor in the evaporator, and controlling to close a circulating water pump communicated with a circulating water tank, open a vent valve and a discharge valve by the PLC, and open a liquid discharge pump communicated with the discharge valve;
(4.1.9) judging whether the time reaches a set value, if so, waiting for the set time, discharging the concentrated solution, closing a discharge valve and a discharge valve, discharging the liquid pump, and returning to the step (4.1.2); if not, returning to the step (4.1.8).
(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, entering the following steps:
(4.2.3) a liquid level sensor in the circulating water tank transmits a signal to a PLC, the PLC controls the opening of a drain valve, water is discharged outwards, and the step (4.2.1) is returned;
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, and if not, returning to the step (4.2.1); if yes, entering the following steps:
(4.2.5) a liquid level sensor in the circulating water tank transmits a signal to a PLC, the PLC controls the closing of the drain valve, and the step (4.2.1) is returned;
fifthly, discharging the evaporated concentrated solution into a nucleation reactor, controlling a feed valve and a feed pump by a PLC (programmable logic controller) to add liquid alkali, alumina monohydrate, a template agent and a mold aid agent according to a set proportion, and starting a stirrer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
starting a nucleation reactor discharge valve and a slurry discharge pump;
judging whether the set time is reached, if not, returning to the step I; if yes, entering the next step;
closing a nucleation reactor discharge valve and a slurry discharge pump;
simultaneously starting a crystallization dryer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
and (3) 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 structures of the anodic oxidation factory-like waste-disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis system of the present invention.
Referring to FIG. 1, the synthesis system of chemical waste disposal phosphoric acid treatment and 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 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 regulating barrel, the waste liquid is discharged by detecting linkage control, 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; an overflow pipe is arranged at the upper part of the overflow area, and a pipeline is connected to a wastewater treatment station for treating the phosphorus-containing wastewater; the bottom of the rinsing zone is communicated with the overflow zone, and the upper part of the rinsing zone is provided with a cleaning water inlet pipe;
referring to fig. 1, the evaporation and concentration unit is composed of a transfer regulating barrel, an evaporator, a discharge valve, a liquid discharge pump, a condenser, a circulating water tank, a water discharge valve and a water discharge valve, wherein the evaporator is communicated with a liquid inlet valve through a pipeline by the transfer regulating barrel, the output end of the evaporator is sequentially communicated with the discharge valve and the liquid discharge pump through the pipeline, the evaporator is communicated with a condenser through a steam channel, the condenser is communicated with a jet device through the pipeline, the jet device is respectively communicated with the pipeline, and the water discharge valve is connected with 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, the selected chemical polishing waste liquid is discharged into the transfer adjusting barrel, and when the liquid level sensor in the transfer adjusting barrel reaches the set liquid level in the barrel, a signal transmission PLC is used for closing a waste liquid discharge valve of the novel three-level rinsing device; the heterogeneous nucleation reaction unit consists of a nucleation reactor, a stirrer, a second discharge valve, a slurry discharging pump and a feeding valve, wherein an input port of the nucleation reactor is communicated with a liquid discharging pump, the stirrer is arranged in the nucleation reactor, an output port of the nucleation reactor is connected with the second discharge valve, and a feeding valve, which is connected with the other output port of the nucleation reactor, of the nucleation reactor is communicated with a feeding pump and a dosing tank, wherein the feeding pump and the dosing tank are communicated with each other; a feed valve and a feed pump connected with the nucleation reactor; the novel three-stage rinsing device, the evaporation concentration unit, the heterogeneous nucleation reaction unit and the crystallization dryer are in linkage controlled by a PLC; the system also comprises a control circuit, wherein the control circuit comprises a PLC controller, and the PLC controller is used for respectively controlling the novel three-stage rinsing device, the evaporation concentration unit, the heterogeneous nucleation reaction unit and the crystallization dryer in a control signal communication mode.
Referring to fig. 1 to 3, the method for treating chemical waste phosphoric acid and detecting an aluminum phosphate molecular sieve comprises the following steps:
the method comprises the steps that an online specific gravity detector detects total phosphorus concentration in a selection area of a novel three-level rinsing device, and a waste liquid discharge valve is opened after the total phosphorus concentration in the selection area reaches a set value;
when the waste liquid discharge valve is opened, the PLC receives the total phosphorus concentration signal of the selection area, and simultaneously transmits the total phosphorus concentration signal of the phosphorus-containing waste water of the overflow area to the waste water treatment station, so that the adding amount of the phosphorus removing agent is controlled, and the total phosphorus in the waste water is accurately and stably removed;
after the equipment is started, a 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;
after being pressurized by a circulating water pump, distilled water in the circulating water tank returns to the circulating water tank again through the ejector, high-pressure water forms high-speed jet flow in the ejector, 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 is reached in the evaporator, starting a liquid inlet valve; the negative pressure enables the waste liquid in the transfer regulating barrel to enter the evaporator through a liquid inlet valve arranged in a 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;
the steam is sent to a condenser through a steam pipeline, condensed into water in the condenser, pumped into an ejector and then enters 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 the liquid level sensor in the evaporator, the circulating water pump stops working, the emptying valve of the evaporator is opened, after the pressure is emptied, the first discharge valve is opened, and the liquid discharge pump discharges the concentrated liquid to the nucleation reactor;
a feed valve and a feed pump which are sequentially connected through a pipeline are arranged in the nucleation reactor, liquid alkali, alumina monohydrate, a template agent and a mold aid agent are added according to a set proportion after the feed pump is opened, a reaction stirrer is started, and the reaction stirrer is stopped after a set time is reached; the slurry discharging valve is opened, and the nucleation mother solution is discharged into the crystallization dryer through a slurry discharging pump connected with a pipeline;
starting the crystallization dryer, and stopping after the set time is reached;
and (3) backwashing, washing and drying the product in the crystallization dryer to obtain an aluminum phosphate molecular sieve product.
In the embodiment, the ratio of the total phosphorus concentration of the selection area to the total phosphorus concentration of the overflow area of the novel three-stage rinsing device is 5-10:1, when a waste liquid discharge valve is opened, the PLC receives the total phosphorus concentration signal of the selection area, calculates the phosphorus-containing wastewater concentration of the overflow area in equal proportion, transmits the signal to a wastewater treatment station, and the total phosphorus in the wastewater is accurately and stably removed by controlling a metering pump to intelligently adjust the adding amount of the phosphorus remover.
Referring to fig. 5, the method for treating chemical waste phosphoric acid and synthesizing the aluminum phosphate molecular sieve comprises the following steps:
selecting, collecting and cooling the concentration of a waste liquid in chemical polishing by adopting a novel three-level rinsing device;
evaporating and concentrating the waste liquid by adopting a negative pressure evaporation method to obtain an aluminum phosphate molecular sieve synthesis mother solution;
thirdly, adding liquid alkali, alumina monohydrate, a template agent and a mold aid into the mother solution; stirring at normal temperature for reaction, and naturally nucleating;
and fourthly, the nucleated mother solution enters a crystallization dryer, crystallization reaction is completed at 800-910 ℃, crystals are taken out after being cooled to normal temperature, and repeatedly washed and dried, so that the aluminum phosphate molecular sieve product is obtained.
In the embodiment, the step of preparing the novel three-level rinsing device is a three-level countercurrent rinsing device, and the novel three-level countercurrent rinsing device 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 regulating barrel, and the waste liquid discharge valve is used for detecting and controlling the discharge of the chemical throwing waste liquid and is linked with the waste liquid discharge valve of the selection area through a PLC program setting on-line specific gravity signal; 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 discharged waste liquid is controlled to be more than or equal to 10000mg/L; the upper part of the overflow area is provided with an overflow pipe, a pipeline is connected to a wastewater treatment station for treating phosphorus-containing wastewater, 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 step (ii) consists of a transfer regulating barrel, a liquid level sensor arranged in the transfer regulating barrel, a pH meter, an evaporator communicated with a liquid inlet valve through a pipeline, a first discharge valve and a liquid discharge pump which are sequentially communicated with the output end of the evaporator through pipelines, a liquid level sensor arranged in the evaporator, a vacuum meter, an emptying valve, a condenser communicated with the evaporator through a steam channel, a circulating water tank communicated with the condenser through a pipeline and a jet device, and a drain valve connected with a circulating water pump through pipelines respectively; the circulating water pump is communicated with the circulating water tank; the method comprises the steps that waste liquid from selected chemical polishing flows into a transfer adjusting barrel, 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, and a waste liquid discharge valve of a novel three-level rinsing device is closed; when the vacuum degree in the evaporator reaches 0.09Mpa, opening a liquid inlet valve, and sucking liquid inlet through negative pressure; the single liquid inlet amount is more than or equal to 100L, and the concentration ratio is 10% -80%.
In the embodiment, in the step (II), the evaporation concentration unit performs negative pressure evaporation on the selected chemical throwing waste liquid, controls the specific gravity to be 1.2-2.0, evaporates condensate water TP to be less than 50mg/L, and when the evaporation concentrate reaches the low liquid level set by the liquid level sensor, the first discharge valve is opened, and the concentrate is discharged to the heterogeneous nucleation reaction unit through the liquid discharge pump; the evaporating temperature is 30-90 ℃, the negative pressure is 0.09-0.1 Mpa, and the evaporating concentration unit, the waste acid contact heating component 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 and is condensed into water in the condenser, the water is pumped 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, a heterogeneous nucleation reaction unit is disposed in the step of step iii, and the heterogeneous nucleation reaction unit is composed of a nucleation reactor with a stirrer and an input port communicated with a liquid discharge pump, a second discharge valve connected with an output port of the nucleation reactor, a slurry discharge pump, a feed valve with another output port of the nucleation reactor sequentially communicated, a feed pump, and a dosing tank.
In the embodiment, the gel state nucleation mother solution in the step (III) is synthesized by reaction in a nucleation reactor; the evaporation concentrate from the evaporation concentration unit enters the nucleation reactor from a pipeline, a feed valve and a feed pump which are sequentially connected through the pipeline, the feed pump is opened, and the nucleation reaction zone is stirred by a stirrer and is provided with a liquid level sensor and a pH meter; adding caustic soda, alumina monohydrate, a template agent and a molding aid according to a proportion, and stopping after a set time is reached; the second discharge valve is opened, and the slurry is discharged into the 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, and the reaction time is more than or equal to 2H; the pH value is 1.5-8.5.
In this embodiment, in the step, the material of the crystallization dryer is a hastelloy, and is a strong acid resistant material; step four, the crystallization dryer is a box dryer or a drum dryer, and the reaction temperature is 800-910 ℃; crystallizing nucleation mother liquor in the step of step four in a crystallization dryer, wherein the nucleation mother liquor occupies more than or equal to 60 percent of volume, the operating pressure is 0.1Mpa, the reaction temperature is 800-910 ℃, the reaction time is more than or equal to 48 hours, sulfuric acid is separated during the reaction, and the separated sulfuric acid is absorbed by a drying absorption tower and is recycled 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 foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. The control method for chemical waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis is characterized by comprising the following steps:
the method comprises the steps of powering up and starting a system;
detecting the total phosphorus concentration of the selection area by a three-stage rinsing device;
judging whether the concentration reaches a set value, if so, sending a signal to a PLC, and controlling the opening of a waste liquid discharge valve by the PLC; if not, closing the waste liquid discharge valve and returning to the step (II);
starting vacuumizing and evaporating circulation; the evacuation evaporation cycle includes:
(4.1.1) detecting the liquid level of the transfer regulating 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 operating the circulating water pump to continuously pump out air in the evaporator so as to change the interior of the evaporator into negative pressure;
if not, the liquid level sensor transmits a signal to the PLC, and the PLC controls the circulating water pump to be closed and the vent valve to be opened, 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 larger than a set value, if so, transmitting a signal to a PLC by a vacuum gauge, controlling and starting the evaporator to heat by the PLC, and if not, returning to the step (4.1.4);
(4.1.6) carrying out the step (4.1.2), wherein the negative pressure sucks the waste liquid into the evaporator through the liquid inlet valve, and a liquid level sensor in the evaporator detects the liquid level of 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 (programmable logic controller) by a liquid level sensor in the evaporator, and controlling the PLC to close a liquid inlet valve; 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 by a liquid level sensor in the evaporator, and controlling to close a circulating water pump communicated with a circulating water tank, open a vent valve and a discharge valve by the PLC, and open a liquid discharge pump communicated with the discharge valve;
(4.1.9) judging whether the time reaches a set value, if so, waiting for the set time, discharging the concentrated solution, closing a discharge valve and a discharge valve, discharging the liquid pump, and returning to the step (4.1.2); if not, returning to the step (4.1.8); the evacuated evaporation cycle further 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, entering the following steps:
(4.2.3) a liquid level sensor in the circulating water tank transmits a signal to a PLC, the PLC controls the opening of a drain valve, water is discharged outwards, and the step (4.2.1) is returned;
(4.2.4) carrying out the step (4.2.1), judging whether the water level is lower than the set low water level, and if not, returning to the step (4.2.1); if yes, entering the following steps:
(4.2.5) a liquid level sensor in the circulating water tank transmits a signal to a PLC, the PLC controls the closing of the drain valve, and the step (4.2.1) is returned;
fifthly, discharging the evaporated concentrated solution into a nucleation reactor, controlling a feed valve and a feed pump by a PLC (programmable logic controller) to add liquid alkali, alumina monohydrate, a template agent and a mold aid agent according to a set proportion, and starting a stirrer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
starting a nucleation reactor discharge valve and a slurry discharge pump;
judging whether the set time is reached, if not, returning to the step I; if yes, entering the next step;
closing a nucleation reactor discharge valve and a slurry discharge pump;
simultaneously starting a crystallization dryer;
judging whether the set time is reached, if not, returning to the step; if yes, entering the next step;
and (3) closing the crystallization dryer, taking out the product, and repeatedly washing and drying to obtain the aluminum phosphate molecular sieve product.
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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 |
| CN104474988A (en) * | 2014-12-15 | 2015-04-01 | 温州市索特医药化工工程有限公司 | Neutralization reaction device and automatic control method |
| CN106219507A (en) * | 2016-07-08 | 2016-12-14 | 宿迁久巨环保科技有限公司 | A kind of Application way of electronic material pickling waste phosphoric acid |
| CN111252835A (en) * | 2020-01-16 | 2020-06-09 | 深圳瑞赛环保科技有限公司 | Waste liquid evaporation treatment method and heating and refrigerating method in waste liquid evaporation process |
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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 |
| CN104474988A (en) * | 2014-12-15 | 2015-04-01 | 温州市索特医药化工工程有限公司 | Neutralization reaction device and automatic control method |
| CN106219507A (en) * | 2016-07-08 | 2016-12-14 | 宿迁久巨环保科技有限公司 | A kind of Application way of electronic material pickling waste phosphoric acid |
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