CN115068972B - Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor - Google Patents
Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor Download PDFInfo
- Publication number
- CN115068972B CN115068972B CN202110282963.5A CN202110282963A CN115068972B CN 115068972 B CN115068972 B CN 115068972B CN 202110282963 A CN202110282963 A CN 202110282963A CN 115068972 B CN115068972 B CN 115068972B
- Authority
- CN
- China
- Prior art keywords
- mother liquor
- crystallization tank
- ammonium sulfate
- barrel body
- liquor crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention relates to a crystallization tank capable of adjusting the solid-to-liquid ratio of ammonium sulfate mother liquor, which comprises a mother liquor inlet pipeline, a mother liquor crystallization tank upper barrel body, a mother liquor crystallization tank support, a mother liquor crystallization tank lower cone shell and a mother liquor crystallization tank blanking port, wherein the mother liquor inlet pipeline is connected with the mother liquor crystallization tank upper barrel body; the upper barrel body of the mother liquor crystallization tank is welded with the lower cone body of the mother liquor crystallization tank to form a whole, a flange piece is arranged between the whole and the lower cone shell of the mother liquor crystallization tank, two supports are welded on the lower cone shell of the mother liquor crystallization tank and used for fixing the mother liquor crystallization tank on the ground, a blanking opening of the mother liquor crystallization tank is arranged at the lower end of the lower cone shell of the mother liquor crystallization tank, the blanking opening is connected with the lower cone shell in a welding mode, and a mother liquor inlet pipeline is arranged at the upper end of the upper barrel body of the mother liquor crystallization tank, so that the problem of lower solid-to-liquid ratio of ammonium sulfate mother liquor can be effectively solved; meanwhile, the negative influence of production interruption caused by solid-liquid delamination of the ammonium sulfate mother solution can be effectively solved.
Description
Technical Field
The invention relates to a crystallization tank, in particular to a crystallization tank capable of adjusting the solid-to-liquid ratio of ammonium sulfate mother liquor, and belongs to the technical field of coking equipment.
Background
The gas from naphthalene washing device enters into an acid washing tower, ammonium sulfate mother liquor with certain acidity is sprayed in two sections, NH in coke oven gas is sprayed 3 Absorbing down. NH (NH) 3 Combined with sulfuric acid to produce ammonium sulfate, the concentration of ammonium sulfate in the mother liquor is raised, and the ammonium sulfate is sent to an ammonium sulfate crystallization device in an unsaturated state. The unsaturated ammonium sulfate mother liquor is deposited by a mother liquor storage tank and then is sent into a crystallizer, in the crystallizer, the unsaturated ammonium sulfate mother liquor enters a mother liquor heater through a crystallizer circulating pump, and is indirectly heated by steam and then enters the bottom of the crystallizer for circulation, and a part of evaporated water vapor passes through a condenser and then condensate returns to the crystallizer or the condenserThe other part of the mother liquor enters a steam jet pump, is brought into a mother liquor heater to exchange heat with the mother liquor to form condensate liquid, and is sent to a phenol-cyanogen wastewater treatment station; the concentrated ammonium sulfate mother liquor promotes the formation of crystal nucleus and the growth of crystal under the action of a circulating pump and a bottom stirrer. The ammonium sulfate crystals generated in the crystallizer are pumped to a crystallization tank by a crystallization pump, mother liquor in the crystallization tank enters a centrifugal machine from a lower end outlet, the mother liquor is centrifugally separated into filtrate and dehydrated crystals by the centrifugal machine, and the filtrate and clarified liquor are returned to the crystallizer for recycling. The dehydrated crystallization is sent into a vibrating fluidized bed dryer by a screw conveyor, the heated air from a heating section and a hot air heater is subjected to fluidized heat transfer and mass transfer, water is evaporated, the dried water enters a cooling section, and the cooled water is cooled by cold air and then directly enters a storage bin, and the storage bin is packed. However, when the ammonium sulfate mother liquor is separated by a centrifuge, there are the following problems: firstly, the ammonium sulfate mother liquor exists in a solid-liquid two-phase mixed state, so the ammonium sulfate mother liquor has a certain solid-liquid ratio, and because the mother liquor from the crystallizer contains ammonium sulfate crystals, the crystallization residues exist in the pipelines for conveying the mother liquor, and in order to avoid the blockage of the pipelines by the crystals remained in the pipelines, industrial water gaps are reserved on all the pipelines for conveying the mother liquor, and the pipelines for conveying the mother liquor are required to be cleaned by industrial water periodically. Therefore, water inevitably enters the mother liquor, so that the solid-liquid ratio of the mother liquor is lower than 40% of the process requirement. The solid-liquid ratio is controlled between 40% and 60% in the process. If the solid-to-liquid ratio of the ammonium sulfate mother liquor is lower than 40%, the mother liquor contains more water, and the crystallization concentration of the ammonium sulfate mother liquor entering the centrifugal machine is lower, so that the product quality is affected; if the solid-to-liquid ratio of the ammonium sulfate mother liquor is higher than 60%, the water content in the mother liquor is low, the crystallization concentration is higher, and when the mother liquor enters the centrifuge drum for separation, part of ammonium sulfate crystals cannot enter the centrifuge together with the mother liquor, but can be gradually adsorbed on the inner wall of the centrifuge drum, so that unbalance of the centrifuge drum is caused, vibration of the centrifuge body can be gradually increased, and the centrifuge is triggered to jump, so that production is interrupted. Secondly, an ammonium sulfate crystallization pump pumps out ammonium sulfate mother liquor from the bottom of the crystallizer and conveys the ammonium sulfate mother liquor to an ammonium sulfate crystallization tank. Introducing ammonium sulfate mother liquor into an ammonium sulfate centrifuge from the bottom of the crystallization tank, dehydrating the ammonium sulfate mother liquor in the centrifuge, and separating out dry ammonium sulfateAnd (5) drying ammonium sulfate crystals. The ammonium sulfate mother liquor is in a solid-liquid two-phase mixed state after being conveyed from the ammonium sulfate crystallizer to the crystallization tank, but the mixed liquor can be layered in the crystallization tank, the lower layer of the mixed liquor is ammonium sulfate crystal sediment, and the upper layer of the mixed liquor is saturated ammonium sulfate mother liquor. The ammonium sulfate crystal particles precipitated at the bottom of the crystallization tank are adsorbed on the inner wall of the crystallization tank and gradually block the feed opening of the crystallization tank, so that most of ammonium sulfate mother liquor and a small amount of ammonium sulfate crystals enter the centrifugal machine. Most of ammonium sulfate crystals are all left in the crystallization tank, and the ammonium sulfate crystals adsorbed on the wall of the crystallization tank can fall into the centrifugal machine from time to time along with the time, and massive crystals are extruded into the centrifugal machine to cause unbalanced vibration of the centrifugal machine so as to jump, thereby influencing the stable operation of production. The above problems are urgently needed to be solved by a new technical method.
Disclosure of Invention
The invention aims at the problems in the prior art, and provides the crystallization tank capable of adjusting the solid-liquid ratio of the ammonium sulfate mother liquor.
In order to achieve the above purpose, the technical scheme of the invention is that the crystallization tank with the solid-to-liquid ratio of ammonium sulfate mother liquor adjustable comprises a mother liquor inlet pipeline, a mother liquor crystallization tank upper barrel body, a mother liquor crystallization tank support, a mother liquor crystallization tank lower cone shell and a mother liquor crystallization tank blanking port, wherein the mother liquor crystallization tank upper barrel body and the mother liquor crystallization tank lower cone are welded into a whole, the mother liquor crystallization tank upper barrel body is sleeved in a lining ring flange, and the inner ring of the lining ring flange is welded with the outer ring of the mother liquor crystallization tank upper barrel body; the cone shell at the lower part of the mother liquor crystallization tank is sleeved in the lining ring flange, and the inner ring of the lining ring flange is welded with the outer ring of the cone shell at the lower part of the mother liquor crystallization tank. The gasket is arranged on the contact surface of the upper barrel body of the mother liquor crystallization tank and the lower cone shell of the mother liquor crystallization tank, and the upper barrel body of the mother liquor crystallization tank is connected with the lower cone shell of the mother liquor crystallization tank through a lining ring flange and the gasket by bolts. The upper end of the upper barrel body of the mother liquor crystallization tank is provided with a mother liquor inlet pipeline which is connected with the mother liquor inlet pipeline in a welded mode, and a mother liquor crystallization tank top cover is arranged above the upper barrel body of the mother liquor crystallization tank.
As an improvement of the invention, the crystallization tank further comprises a high-precision online refractometer, wherein the high-precision online refractometer is arranged on the outer side of the barrel wall of the upper barrel body of the mother liquor crystallization tank, the high-precision online refractometer is used for measuring the crystallization concentration of ammonium sulfate in the mother liquor, the high-precision online refractometer is connected with the barrel wall of the mother liquor crystallization tank by adopting a flange, and the detection end of the high-precision online refractometer is immersed in the mother liquor crystallization tank and is used for measuring the solid-to-liquid ratio of the mother liquor; the action value of the refractometer is preset, two pairs of normally open contacts are taken, one pair of normally open contacts is connected in series with the electric heater control loop, the other pair of normally closed contacts is connected in series with the water pump control loop, and the other pair of normally closed contacts is connected in series with the water pump control loop.
As an improvement of the invention, the crystallization tank also comprises an electric heating core, wherein the cone shell at the lower part of the crystallization tank is filled with a filling material for heat transfer, the material is quartz sand, the quartz sand has good heat transfer and insulating properties, the left side and the right side of the cone shell at the lower part of the mother liquor crystallization tank are respectively provided with the electric heating core, after the electric heating core works, heat is transferred to the quartz sand, and the quartz sand transfers the heat to the ammonium sulfate mother liquor in the crystallization tank.
As an improvement of the invention, the crystallization tank further comprises a steam exhaust port and a steam exhaust port top cover, the upper end of the barrel body at the upper part of the mother liquor crystallization tank is provided with the steam exhaust port, the barrel body is connected with the steam exhaust port in a welding mode, the top of the steam exhaust port is provided with the steam exhaust port top cover, the steam exhaust port top cover is connected with the steam exhaust port in a threaded mode, and the top cover is opened manually.
As an improvement of the invention, the crystallization tank also comprises a blast pipe and a blast pipe exhaust hole, wherein the two sides of the upper end of the upper barrel body of the mother liquor crystallization tank are respectively provided with a blast pipe, the upper end of the blast pipe extends out of the crystallization tank, and the lower end of the blast pipe is immersed in the ammonium sulfate mother liquor in the crystallization tank; the pipe wall of each bulge pipe is provided with a plurality of exhaust holes; when air enters from the air blowing pipe, the air is discharged through the air discharging hole on the air blowing pipe, and the air blowing pipe is connected with the barrel body on the upper part of the mother liquor crystallization tank in a welding mode.
As an improvement of the invention, the crystallization tank further comprises a water supplementing device, wherein the water supplementing device comprises a water supplementing pipe and a water supplementing pump, the side surface of the upper barrel body of the mother liquor crystallization tank is provided with the water supplementing pipe, the water supplementing pipe is connected with the upper barrel body of the mother liquor crystallization tank by adopting welding, and water can be injected into the mother liquor crystallization tank through the water supplementing pipe; the water supplementing pump is connected with the water supplementing pipe by a flange, and water is injected into the mother liquor crystallization tank by starting the water supplementing pump.
As an improvement of the invention, the crystallization tank also comprises a thermometer, wherein the thermometer is arranged at the upper end of the upper barrel body of the mother liquor crystallization tank, the thermometer is connected with the upper barrel body of the mother liquor crystallization tank by adopting threads, and the detection end of the thermometer is immersed in the mother liquor crystallization tank and is used for measuring the temperature of the mother liquor; the action value of the thermometer is preset, and a pair of normally closed points of the thermometer are connected into the electric heater control loop in series.
Compared with the prior art, the invention has the advantages that 1) the technical proposal introduces two paths of compressed air into the ammonium sulfate mother liquor in the crystallization tank, prevents the layering of the ammonium sulfate mother liquor, prevents the precipitation of ammonium sulfate crystal particles to block the feed opening, and prevents massive ammonium sulfate crystal particles from suddenly falling into the centrifugal machine to influence the stable operation of equipment; 2) According to the technical scheme, the thermometer is additionally arranged for detecting the temperature of the ammonium sulfate mother liquor, the high-precision online refractometer is additionally arranged for detecting the solid-liquid ratio of the mother liquor, the device is not influenced by the color, turbidity, bubbles and the like of materials, and the device has an automatic temperature compensation function and is high in reliability and precision. And (3) evaporating or supplementing water to the ammonium sulfate mother liquor according to the implementation monitoring data, so that the solid-liquid ratio of the ammonium sulfate mother liquor is effectively controlled.
Drawings
FIG. 1 is an overall schematic diagram of a crystallization tank with adjustable solid-to-liquid ratio of ammonium sulfate mother liquor;
FIG. 2 is a diagram of a gas source tube configuration;
FIG. 3 is a block diagram of a refractometer;
FIG. 4 is a diagram of a heater core structure;
fig. 5 is a control schematic diagram of the heater and the water replenishment pump.
In the figure: 1. the mother liquor inlet pipeline, 2, the mother liquor inlet pipeline flange, 3, the steam vent, 4, the steam vent top cap, 5, the air-blowing pipe, 6, the air-blowing pipe exhaust, 7, the air-blowing pipe flange, 8, the mother liquor crystallization tank top cap, 9, the mother liquor crystallization tank upper barrel body, 10, the backing ring flange, 11, the gasket, 12, the mother liquor crystallization tank support, 13, the mother liquor crystallization tank lower cone, 14, the mother liquor crystallization tank lower cone shell, 15, the mother liquor crystallization tank feed opening, 16, the electrical heating core, 17, the heat transfer filler, 18, the mother liquor, 19, ammonium sulfate crystallization, 20, the thermometer, 21, the high-precision online refractometer, 22, the water supplementing pipe, 23, the water supplementing pump.
The specific embodiment is as follows:
in order to enhance the understanding of the present invention, the present embodiment will be described in detail with reference to the accompanying drawings.
Example 1: referring to fig. 1, referring to fig. 1 and 5, a crystallization tank capable of adjusting a solid-to-liquid ratio of an ammonium sulfate mother liquor, the apparatus comprises: the mother liquor inlet pipeline 1, the mother liquor inlet pipeline connecting flange 2, the steam exhaust port 3, the steam exhaust port top cover 4, the air blowing pipe 5, the air blowing pipe exhaust hole 6, the air blowing pipe connecting flange 7, the mother liquor crystallization tank top cover 8, the mother liquor crystallization tank upper barrel body 9, the lining ring flange 10, the gasket 11, the mother liquor crystallization tank support 12, the mother liquor crystallization tank lower cone 13, the mother liquor crystallization tank lower cone shell 14, the mother liquor crystallization tank feed opening 15, the electric heating core 16, the heat transfer filler 17, the mother liquor 18, the ammonium sulfate crystal 19, the thermometer 20, the high-precision online refractometer 21, the water supplementing pipe 22 and the water supplementing pump 23. The upper barrel body of the mother liquor crystallization tank and the lower cone of the mother liquor crystallization tank are welded into a whole, the upper barrel body 9 of the mother liquor crystallization tank is sleeved in the lining ring flange 10, and the inner ring of the lining ring flange 10 and the outer ring of the upper barrel body 9 of the mother liquor crystallization tank are welded together; the lower cone shell 14 of the mother liquor crystallization tank is sleeved in the lining ring flange 10, and the inner ring of the lining ring flange 10 is welded with the outer ring of the lower cone shell 14 of the mother liquor crystallization tank. The gasket 11 is placed on the contact surface of the upper barrel body 9 of the mother liquor crystallization tank and the lower cone shell 14 of the mother liquor crystallization tank, and the upper barrel body 9 of the mother liquor crystallization tank is connected with the lower cone shell 14 of the mother liquor crystallization tank through the lining ring flange 10 and the gasket 11 by bolts. The whole body is connected with the cone shell at the lower part of the mother liquor crystallization tank through a flange piece by bolts. Two supports are welded on the cone shell at the lower part of the mother liquor crystallization tank and are used for fixing the mother liquor crystallization tank on the ground. The lower end of the cone shell at the lower part of the mother liquor crystallization tank is provided with a blanking opening of the mother liquor crystallization tank, and the blanking opening is connected with the cone shell at the lower part in a welding mode. The upper end of the upper barrel body of the mother liquor crystallization tank is provided with a mother liquor inlet pipeline, and the barrel body is connected with the mother liquor inlet pipeline in a welding mode.
The upper end of the barrel body at the upper part of the mother liquor crystallization tank is provided with a steam exhaust port 3, the barrel body is connected with the steam exhaust port in a welding mode, the top of the steam exhaust port is provided with a steam exhaust port top cover 4, the top cover is connected with the exhaust port in a threaded mode, and the top cover is in a normally closed state. The cone shell 14 at the lower part of the crystallization tank is filled with a filling material 17 for heat transfer, and the material is quartz sand which has good heat transfer and insulating properties. The left and right sides of the cone shell of the lower part of the mother liquor crystallization tank are respectively provided with an electric heating core 16, and after the electric heating core is electrically operated, heat is transferred to quartz sand which in turn transfers heat to ammonium sulfate mother liquor 18 in the crystallization tank. The outer of the barrel wall of the upper barrel body of the mother liquor crystallization tank is additionally provided with a high-precision online refractometer which is used as a refractometer 21 for detecting the solid-to-liquid ratio of the mother liquor, when the solid-to-liquid ratio of the ammonium sulfate mother liquor is detected to be lower than a set value, the water content of the mother liquor is larger, certain water is required to be evaporated to adjust the solid-to-liquid ratio of the ammonium sulfate mother liquor, at the moment, a normally open contact of the refractometer is closed, and an electric heating core is electrified to start working. After the electric heating core is electrified to work, the ammonium sulfate mother liquor absorbs heat, water in the mother liquor begins to evaporate, an operator can see that an indicator lamp for the electric heating core to work is on in a central control room, and at the moment, the top cover needs to be manually opened, so that evaporated water vapor is discharged from the exhaust port. Because the evaporation temperature of the ammonium sulfate mother liquor is required not to exceed 65 ℃ in the process, the upper end of the upper barrel body of the mother liquor crystallization tank is additionally provided with a thermometer 20, and the detection end of the thermometer is immersed in the ammonium sulfate mother liquor in the mother liquor crystallization tank and is used for measuring the temperature of the ammonium sulfate mother liquor. And a pair of normally-closed contacts of the thermometer are connected in series into the control loop of the electric heater, once the measured temperature of the ammonium sulfate mother liquor exceeds a set value, the normally-closed contacts of the thermometer are disconnected, the power supply of the electric heater is cut off, and the electric heater stops working, so that the temperature of the ammonium sulfate mother liquor is not increased any more.
The upper end of the upper barrel body of the mother liquor crystallization tank is additionally provided with two air blowing pipes 5, the upper ends of the air blowing pipes extend out of the crystallization tank and are connected with compressed air, and the pressure of the compressed air is 800KPa as an air inlet end; the lower end of the blast pipe is immersed in the ammonium sulfate mother liquor 18 in the crystallization tank; the wall of the air blowing pipe is provided with a plurality of exhaust holes 6; after compressed air enters the air blowing pipe, the compressed air is discharged through the air discharging hole on the air blowing pipe, the compressed air discharged from the air discharging hole is blown into the mother liquor, and precipitated ammonium sulfate crystals 19 are blown up again, so that the ammonium sulfate crystals can be suspended in the mother liquor all the time and are not precipitated, and the phenomenon that a large amount of ammonium sulfate crystals are accumulated at the feed opening of the crystallization tank to cause blockage is avoided. Compressed air is always blown into the ammonium sulfate mother liquor in the production process, so that crystallization and precipitation are prevented.
The side surface of the upper barrel body 9 of the mother liquor crystallization tank is additionally provided with a water supplementing pipe 22 and a water supplementing pump 23. A high-precision online refractometer 21 is additionally arranged outside the barrel wall of the upper barrel body of the mother liquor crystallization tank, and when the refractometer detects that the solid-to-liquid ratio of the ammonium sulfate mother liquor is higher than a set value, the water content in the ammonium sulfate mother liquor is lower and the requirement is not met. A pair of normally open contacts and a pair of normally closed contacts of the refractometer are connected in series into a control loop of the water pump, when the refractometer detects that the solid-to-liquid ratio of ammonium sulfate mother liquor is higher than a set value, the normally open contacts of the refractometer are closed, a water supplementing pump coil is electrified, the water supplementing pump operates, the water supplementing pump is automatically controlled to fill water into a mother liquor crystallization tank, and a pair of normally open contacts of a main contactor of the water pump are connected in parallel with the normally open contacts of the refractometer to serve as self-protection lines of the water pump; when the refractometer detects that the solid-liquid ratio is lower than the set value, the ammonium sulfate mother liquor solid-liquid ratio meets the requirement, the normally closed contact of the refractometer is disconnected, the power supply of the water supplementing pump is cut off, and the water supplementing pump stops supplementing water.
The working process comprises the following steps: referring to fig. 1 and 5, a crystallization tank capable of adjusting the solid-to-liquid ratio of ammonium sulfate mother liquor, the method for detecting and controlling the temperature and the solid-to-liquid ratio of the ammonium sulfate mother liquor comprises the following steps:
1. during normal production, ammonium sulfate crystals generated in the crystallizer are conveyed by a crystallization pump and enter a crystallization tank capable of adjusting the solid-to-liquid ratio of ammonium sulfate mother liquor from a mother liquor inlet pipeline 1.
2. In order to prevent ammonium sulfate from crystallizing and precipitating, the mother liquor in the ammonium sulfate mother liquor crystallization tank is continuously blown by a blowing pipe 5, and the air source is compressed air with the pressure of 800KPa, so that ammonium sulfate crystals in the ammonium sulfate mother liquor are always suspended in the ammonium sulfate mother liquor.
3. A thermometer 20 is additionally arranged at the upper end of the upper barrel body of the mother liquor crystallization tank to measure the temperature of the ammonium sulfate mother liquor; a high-precision on-line refractometer 21 is additionally arranged outside the barrel wall of the upper barrel body of the mother liquor crystallization tank, and the solid-to-liquid ratio of the ammonium sulfate mother liquor is measured.
4. Taking a pair of normally open contacts and a pair of normally closed contacts of the refractometer to be connected in series into a control loop of the water supplementing pump, when the refractometer measures that the solid-to-liquid ratio of the ammonium sulfate mother liquor is higher than 60%, the normally open contacts of the refractometer are closed, the coils of the water supplementing pump are powered on, the water supplementing pump runs, and the water supplementing pump is automatically controlled to water into a mother liquor crystallization tank; in the water replenishing process, once the refractometer measures that the solid-to-liquid ratio of the ammonium sulfate mother liquor is lower than 60%, the normally closed contact of the refractometer is disconnected, the power supply of the water replenishing pump is cut off, and the water replenishing pump stops replenishing water.
5. And a pair of normally open contacts of the refractometer and a pair of normally closed contacts of the thermometer are connected in series into a control loop of the electric heater, when the refractometer measures that the solid-to-liquid ratio of the ammonium sulfate mother liquor is lower than the set 40%, the normally open contacts of the refractometer are closed, the electric heater is powered, and the mother liquor starts to be heated. When the temperature of the ammonium sulfate mother liquor measured by the thermometer is higher than the set 65 ℃, the normally-closed contact of the thermometer is disconnected, the power supply of the electric heater is cut off, the electric heater stops working, the ammonium sulfate mother liquor is not heated, and the temperature of the ammonium sulfate mother liquor in the whole evaporation process is not higher than 65 ℃.
6. The main contactor loop of the water supplementing pump and the electric heater is connected with the working indicator lamp in parallel, so that operators can know the working indicator lamp in the process that the water supplementing pump and the electric heater are powered on.
It should be noted that the above-mentioned embodiments are not intended to limit the scope of the present invention, and equivalent changes or substitutions made on the basis of the above-mentioned technical solutions fall within the scope of the present invention as defined in the claims.
Claims (3)
1. The crystallization tank is characterized by comprising a mother liquor inlet pipeline, a mother liquor crystallization tank upper barrel body, a mother liquor crystallization tank support, a mother liquor crystallization tank lower cone shell and a mother liquor crystallization tank blanking port; the upper barrel body of the mother liquor crystallization tank and the lower cone of the mother liquor crystallization tank are welded into a whole, the upper barrel body of the mother liquor crystallization tank is sleeved in a lining ring flange, and the inner ring of the lining ring flange is welded with the outer ring of the upper barrel body of the mother liquor crystallization tank; the lower cone shell of the mother liquor crystallization tank is sleeved in a lining ring flange, the inner ring of the lining ring flange is welded with the outer ring of the lower cone shell of the mother liquor crystallization tank, a gasket is arranged on the contact surface of the upper barrel body of the mother liquor crystallization tank and the lower cone shell of the mother liquor crystallization tank, the upper barrel body of the mother liquor crystallization tank is connected with the lower cone shell of the mother liquor crystallization tank through the lining ring flange and the gasket through bolts, two supports are welded on the lower cone shell of the mother liquor crystallization tank and used for fixing the mother liquor crystallization tank on the ground, a blanking opening of the mother liquor crystallization tank is arranged at the lower end of the lower cone shell of the mother liquor crystallization tank, the blanking opening is connected with the lower cone shell through welding, a mother liquor inlet pipeline is arranged at the upper end of the upper barrel body of the mother liquor crystallization tank and is connected with the mother liquor inlet pipeline through welding, and a mother liquor crystallization tank top cover is arranged above the upper barrel body of the mother liquor crystallization tank;
the crystallization tank further comprises a high-precision online refractometer, wherein the high-precision online refractometer is arranged on the outer side of the barrel wall of the upper barrel body of the mother liquor crystallization tank and is used for measuring the crystallization concentration of ammonium sulfate in the mother liquor, the high-precision online refractometer is connected with the barrel wall of the mother liquor crystallization tank by adopting a flange, and the detection end of the high-precision online refractometer is immersed in the mother liquor crystallization tank and is used for measuring the solid-to-liquid ratio of the mother liquor; the method comprises the steps of presetting an action value of a refractometer, taking two pairs of normally open contacts of the refractometer, wherein one pair of normally open contacts is connected in series with an electric heater control loop, the other pair of normally closed contacts is connected in series with a water pump control loop, and the other pair of normally closed contacts is connected in series with the water pump control loop;
the crystallization tank further comprises an electric heating core, wherein the cone shell at the lower part of the crystallization tank is filled with a filling material for heat transfer, the filling material is quartz sand, the left side and the right side of the cone shell at the lower part of the mother liquor crystallization tank are respectively provided with an electric heating core, after the electric heating core works, heat is transferred to the quartz sand, and the quartz sand transfers the heat to ammonium sulfate mother liquor in the crystallization tank;
the crystallization tank further comprises an air blowing pipe and an air blowing pipe exhaust hole, two sides of the upper end of the upper barrel body of the mother liquor crystallization tank are respectively provided with an air blowing pipe, the upper end of the air blowing pipe extends out of the crystallization tank, and the lower end of the air blowing pipe is immersed in ammonium sulfate mother liquor in the crystallization tank; the pipe wall of each bulge pipe is provided with a plurality of exhaust holes; when air enters from the air blowing pipe, the air is discharged through the air discharging hole on the air blowing pipe, and the air blowing pipe is connected with the barrel body at the upper part of the mother liquor crystallization tank in a welding mode;
the crystallization tank further comprises a water supplementing device, wherein the water supplementing device comprises a water supplementing pipe and a water supplementing pump, the side surface of the upper barrel body of the mother liquor crystallization tank is provided with the water supplementing pipe, the water supplementing pipe is connected with the upper barrel body of the mother liquor crystallization tank in a welding way, and water is injected into the mother liquor crystallization tank through the water supplementing pipe; the water supplementing pump is connected with the water supplementing pipe by adopting a flange, and water is injected into the mother liquor crystallization tank by starting the water supplementing pump;
the crystallization tank further comprises a thermometer, wherein the thermometer is arranged at the upper end of the upper barrel body of the mother liquor crystallization tank, the thermometer is connected with the upper barrel body of the mother liquor crystallization tank by threads, and the detection end of the thermometer is immersed in the mother liquor crystallization tank and is used for measuring the temperature of the mother liquor; the action value of the thermometer is preset, and a pair of normally closed points of the thermometer are connected into the electric heater control loop in series.
2. The crystallization tank for adjusting the solid-to-liquid ratio of the ammonium sulfate mother solution according to claim 1, wherein the crystallization tank further comprises a steam exhaust port and a steam exhaust port top cover, the upper end of the upper barrel body of the mother solution crystallization tank is provided with the steam exhaust port, the barrel body is connected with the steam exhaust port in a welding mode, the top of the steam exhaust port is provided with the steam exhaust port top cover, the steam exhaust port top cover is connected with the steam exhaust port in a threaded mode, and the top cover is opened manually.
3. The method for detecting and controlling the temperature and the solid-to-liquid ratio of the ammonium sulfate mother liquor by adopting the crystallization tank as claimed in claim 2 comprises the following steps: characterized in that the method comprises the steps of: step 1), a pair of normally closed contacts of a thermometer and a pair of normally open contacts of a refractometer are connected in series into a heater control loop, when the refractometer detects that the solid-to-liquid ratio of the mother liquor is lower than 40%, the water content of the mother liquor is larger, the normally open contacts of the refractometer are closed, the heater works, and the ammonium sulfate mother liquor is heated to evaporate water; because the heating temperature of the ammonium sulfate mother liquor cannot exceed 65 ℃, the action value of a thermometer is preset, when the temperature of the ammonium sulfate mother liquor exceeds a set value, the normally-closed contact of the thermometer is disconnected, the working loop of the heater is cut off, and the heater stops heating; step 2) taking a pair of normally open contacts and a pair of normally closed contacts of the refractometer to be connected in series into a water pump control loop, when the refractometer detects that the solid-to-liquid ratio of the mother liquor is higher than 60%, indicating that the water content of the mother liquor is low, closing the normally open contacts, and starting a water supplementing pump to supplement water into the ammonium sulfate mother liquor; when the refractometer detects that the solid-to-liquid ratio of the mother solution is lower than 60%, the ammonium sulfate mother solution solid-to-liquid ratio meets the production requirement, the normally closed contact of the refractometer is disconnected, and the water pump stops water supplementing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110282963.5A CN115068972B (en) | 2021-03-16 | 2021-03-16 | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110282963.5A CN115068972B (en) | 2021-03-16 | 2021-03-16 | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115068972A CN115068972A (en) | 2022-09-20 |
| CN115068972B true CN115068972B (en) | 2023-08-15 |
Family
ID=83246181
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110282963.5A Active CN115068972B (en) | 2021-03-16 | 2021-03-16 | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115068972B (en) |
Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1350218A (en) * | 1962-02-01 | 1964-01-24 | Phillips Petroleum Co | Separation and purification of multicomponent mixtures |
| DE1237981B (en) * | 1962-02-01 | 1967-04-06 | Phillips Petroleum Co | Process for the separation and purification of a mixture by fractional crystallization |
| US3402047A (en) * | 1964-08-14 | 1968-09-17 | Phillips Petroleum Co | Crystallization separation and purification utilizing fresh feed to reslurry crystals |
| CA1117276A (en) * | 1978-03-09 | 1982-02-02 | Klaus-Dirk Henning | Process for eliminating hydrogen sulfide from gas mixtures |
| CA1166584A (en) * | 1981-03-09 | 1984-05-01 | Gosewinus F. Van Oorschot | Device for separating liquid from liquid-containing compressed gas |
| US6364914B1 (en) * | 1998-03-23 | 2002-04-02 | Ajinomoto Co., Inc. | Method of crystallization with the particle size distribution being controlled |
| DE102007043748A1 (en) * | 2007-09-13 | 2008-09-11 | Basf Se | Method for separating target product i.e. acrylic acid, methacrylic acid, p-xylene or N-vinylpyrrolidone in form of fine crystallized product, involves utilizing heat exchanger, where heat flow is gathered from heat exchanger |
| CN101664214A (en) * | 2009-09-15 | 2010-03-10 | 华南理工大学 | Ultrasonic synergetic crystal growing fruit juice freezing and concentrating method and equipment thereof |
| CN101732886A (en) * | 2010-01-16 | 2010-06-16 | 江阴丰力生化工程装备有限公司 | Continuous crystallizer |
| CN201586401U (en) * | 2010-01-16 | 2010-09-22 | 江阴丰力生化工程装备有限公司 | Continuous crystallizer device |
| CN101342425B (en) * | 2008-08-27 | 2011-06-15 | 武汉大学 | Microwave separation method and apparatus used thereof |
| JP2013184139A (en) * | 2012-03-09 | 2013-09-19 | Asahi Kasei Chemicals Corp | Steam separation membrane and method for manufacturing same |
| CN103335981A (en) * | 2013-06-07 | 2013-10-02 | 广州甘蔗糖业研究所 | Device for on-line detection of concentration during crystallization of cane sugar |
| CN104418779A (en) * | 2013-08-26 | 2015-03-18 | 河南天方药业股份有限公司 | Preparation method of high-purity fudosteine |
| CN104492119A (en) * | 2014-12-19 | 2015-04-08 | 芜湖新兴铸管有限责任公司 | Ammonium sulfate mother liquor crystallization tank |
| CN106399404A (en) * | 2016-12-08 | 2017-02-15 | 辽阳富强食品化工有限公司 | Production method of calcium gluconate |
| CN206778398U (en) * | 2017-05-08 | 2017-12-22 | 浙江华海致诚药业有限公司 | A kind of reactor gas advertises device |
| CN206995915U (en) * | 2017-07-21 | 2018-02-13 | 滨海金海立医药化工有限公司 | A kind of Omeprazole chloride crystallization groove |
| CN207270730U (en) * | 2017-10-09 | 2018-04-27 | 利得环境科技（北京）有限公司 | Evaporating, concentrating and crystallizing system |
| CN208757326U (en) * | 2018-08-31 | 2019-04-19 | 江苏佰健环保科技有限公司 | The linkage control system of lye dissolving tank solid-to-liquid ratio |
| CN210199083U (en) * | 2019-04-24 | 2020-03-27 | 孝感广盐华源制盐有限公司 | Solid-liquid ratio measuring system for vacuum salt production |
| CN211051463U (en) * | 2019-10-29 | 2020-07-21 | 天津长芦海晶集团有限公司 | Feeding box capable of adjusting solid-liquid ratio |
| CN111994923A (en) * | 2020-08-28 | 2020-11-27 | 新兴凌云医药化工有限公司 | Production medicine level large granule sodium bicarbonate crystal system |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9403134B2 (en) * | 2014-04-16 | 2016-08-02 | Gea Egi Energiagazdalkodasi Zrt | Method for producing a material mixture of powder or granular state material and liquid |
| FR3073424B1 (en) * | 2017-11-16 | 2022-03-25 | Novasep Process | REGULATED PROCESS FOR SEPARATION OF A MIXTURE |
-
2021
- 2021-03-16 CN CN202110282963.5A patent/CN115068972B/en active Active
Patent Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1350218A (en) * | 1962-02-01 | 1964-01-24 | Phillips Petroleum Co | Separation and purification of multicomponent mixtures |
| DE1237981B (en) * | 1962-02-01 | 1967-04-06 | Phillips Petroleum Co | Process for the separation and purification of a mixture by fractional crystallization |
| US3402047A (en) * | 1964-08-14 | 1968-09-17 | Phillips Petroleum Co | Crystallization separation and purification utilizing fresh feed to reslurry crystals |
| CA1117276A (en) * | 1978-03-09 | 1982-02-02 | Klaus-Dirk Henning | Process for eliminating hydrogen sulfide from gas mixtures |
| CA1166584A (en) * | 1981-03-09 | 1984-05-01 | Gosewinus F. Van Oorschot | Device for separating liquid from liquid-containing compressed gas |
| US6364914B1 (en) * | 1998-03-23 | 2002-04-02 | Ajinomoto Co., Inc. | Method of crystallization with the particle size distribution being controlled |
| DE102007043748A1 (en) * | 2007-09-13 | 2008-09-11 | Basf Se | Method for separating target product i.e. acrylic acid, methacrylic acid, p-xylene or N-vinylpyrrolidone in form of fine crystallized product, involves utilizing heat exchanger, where heat flow is gathered from heat exchanger |
| CN101342425B (en) * | 2008-08-27 | 2011-06-15 | 武汉大学 | Microwave separation method and apparatus used thereof |
| CN101664214A (en) * | 2009-09-15 | 2010-03-10 | 华南理工大学 | Ultrasonic synergetic crystal growing fruit juice freezing and concentrating method and equipment thereof |
| CN101732886A (en) * | 2010-01-16 | 2010-06-16 | 江阴丰力生化工程装备有限公司 | Continuous crystallizer |
| CN201586401U (en) * | 2010-01-16 | 2010-09-22 | 江阴丰力生化工程装备有限公司 | Continuous crystallizer device |
| JP2013184139A (en) * | 2012-03-09 | 2013-09-19 | Asahi Kasei Chemicals Corp | Steam separation membrane and method for manufacturing same |
| CN103335981A (en) * | 2013-06-07 | 2013-10-02 | 广州甘蔗糖业研究所 | Device for on-line detection of concentration during crystallization of cane sugar |
| CN104418779A (en) * | 2013-08-26 | 2015-03-18 | 河南天方药业股份有限公司 | Preparation method of high-purity fudosteine |
| CN104492119A (en) * | 2014-12-19 | 2015-04-08 | 芜湖新兴铸管有限责任公司 | Ammonium sulfate mother liquor crystallization tank |
| CN106399404A (en) * | 2016-12-08 | 2017-02-15 | 辽阳富强食品化工有限公司 | Production method of calcium gluconate |
| CN206778398U (en) * | 2017-05-08 | 2017-12-22 | 浙江华海致诚药业有限公司 | A kind of reactor gas advertises device |
| CN206995915U (en) * | 2017-07-21 | 2018-02-13 | 滨海金海立医药化工有限公司 | A kind of Omeprazole chloride crystallization groove |
| CN207270730U (en) * | 2017-10-09 | 2018-04-27 | 利得环境科技（北京）有限公司 | Evaporating, concentrating and crystallizing system |
| CN208757326U (en) * | 2018-08-31 | 2019-04-19 | 江苏佰健环保科技有限公司 | The linkage control system of lye dissolving tank solid-to-liquid ratio |
| CN210199083U (en) * | 2019-04-24 | 2020-03-27 | 孝感广盐华源制盐有限公司 | Solid-liquid ratio measuring system for vacuum salt production |
| CN211051463U (en) * | 2019-10-29 | 2020-07-21 | 天津长芦海晶集团有限公司 | Feeding box capable of adjusting solid-liquid ratio |
| CN111994923A (en) * | 2020-08-28 | 2020-11-27 | 新兴凌云医药化工有限公司 | Production medicine level large granule sodium bicarbonate crystal system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115068972A (en) | 2022-09-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115068972B (en) | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor | |
| CN107128950A (en) | The apparatus and method that refined salt is extracted in the waste liquid produced from wet method ISS J desulfurization | |
| CN208667148U (en) | A kind of high-salt wastewater crystalline mother solution drying device | |
| CN105435482B (en) | A kind of multi-stage vacuum adiabatic flash continuous crystallisation process and equipment | |
| CN114159824A (en) | High-purity manganese sulfate crystallization drying system | |
| CN105776294B (en) | A kind of energy-efficient alchlor production method | |
| KR101264823B1 (en) | Reaction system for silicon powder | |
| CN208635487U (en) | A kind of lotus leaf tea production leaf abscission machine | |
| CN204767470U (en) | Concentrated crystallization device of ammonium nitrate | |
| CN207129963U (en) | The device of refined salt is extracted from waste liquid caused by wet method ISS J desulfurization | |
| CN206680209U (en) | A kind of sewage disposal thin film evaporator | |
| CN105013410A (en) | Production system for phosphorylation reaction | |
| CN104368278A (en) | Filter type sulfur melting kettle | |
| CN210448159U (en) | Vacuum evaporation crystallization device is used in sodium metasilicate pentahydrate production | |
| CN103691191A (en) | Online vacuum oil-filtering treatment machine of oil | |
| CN207886707U (en) | A kind of methanol prepares the evaporator of formaldehyde | |
| JP5330920B2 (en) | Operation method of horizontal continuous conduction heat dryer | |
| CN208770862U (en) | Interior heat cycles vaporising device and vapo(u)rization system | |
| CN208700598U (en) | A kind of continuous crystallizing system of ferrous sulfate | |
| CN207307239U (en) | A kind of crystallization apparatus that secondary crystallization is carried out to kojic acid raw material | |
| CN220507464U (en) | Vacuum drying device for preventing triethylene diamine from caking | |
| CN110155952A (en) | A kind of molten sulphur device of energy conservation and environmental protection | |
| CN204563658U (en) | A kind of crystallizing tank with pellicle | |
| CN112742051B (en) | Sucrose-6-ester uninterrupted preparation device and production method | |
| CN212141513U (en) | Film scraper evaporator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |