CN218854292U - System for continuous production liquid polyferric sulfate - Google Patents
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- CN218854292U CN218854292U CN202223382784.8U CN202223382784U CN218854292U CN 218854292 U CN218854292 U CN 218854292U CN 202223382784 U CN202223382784 U CN 202223382784U CN 218854292 U CN218854292 U CN 218854292U
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Abstract
The utility model belongs to the technical field of liquid water purification agent preparation, concretely relates to system for serialization production liquid polyferric sulfate. The device comprises a ferrous solution batching tank, a sodium nitrite batching tank and a primary pre-oxidation reaction kettle provided with a gas-liquid mixer, wherein the ferrous solution batching tank is connected with the gas-liquid mixer through a preheater, the sodium nitrite batching tank is connected with the gas-liquid mixer, the gas-liquid mixer is connected with an oxygen pipeline, the primary pre-oxidation reaction kettle is connected with the upper part of a secondary pre-oxidation reaction kettle through an overflow pipeline on the upper part, a pipeline connected with a kettle bottom valve of the secondary pre-oxidation reaction kettle and the overflow pipeline on the upper part are connected with the top end of a packing layer of a tower reactor through a filter, the oxygen pipeline is connected with the bottom of the packing layer of the tower reactor, the top end of the tower reactor is provided with an exhaust port and connected to a gas-liquid separator, and the bottom of the gas-liquid separator is connected with the tower reactor through a pipeline; system, process flow is short, the conversion rate is high, product quality is stable homogeneous, easily industrialization, energy-concerving and environment-protective.
Description
Technical Field
The utility model belongs to the technical field of liquid water purification agent preparation, concretely relates to system for serialization production liquid polyferric sulfate.
Background
Polyferric sulfate (PFS for short) is a novel, high-quality and high-efficiency ferric salt inorganic polymeric flocculant. Can be used for the feed water pretreatment of power production, the treatment of domestic sewage and industrial wastewater, and has wide application in the aspects of wastewater recycling, casting, papermaking, medicine, leather making and the like.
At present, the domestic method for preparing the liquid polymeric ferric sulfate mainly comprises a direct oxidation method and a catalytic oxidation method. The direct oxidation method takes ferrous sulfate and titanium dioxide waste sulfuric acid as raw materials, directly oxidizes ferrous ions into ferric ions through a strong oxidant, has quick reaction and simple operation, but the ferrous ions are quickly oxidized, the temperature is instantly increased to be more than 100 ℃, the materials are easy to flee in a boiling pot, great hidden danger is generated to the safety of operators, and the production cost is higher. The catalytic oxidation method is to oxidize ferrous ions by oxygen under the action of a catalyst, and the specific principle is as follows: ferrous sulfate and titanium white waste sulfuric acid are used as raw materials, under the action of a catalyst (sodium nitrite), and oxygen is used as an oxidant to enable the ferrous sulfate to be subjected to oxidation, hydrolysis and polymerization in an acid medium to prepare liquid polymeric ferric sulfate. The oxidation reaction is the first step in a three series of reactions, which is slow and controls the overall reaction process.
The principle of a unit loop reactor is mostly adopted in domestic production of liquid polymeric ferric sulfate by adopting a catalytic oxidation method, namely, a circulating reaction is carried out in a closed reaction kettle by a pipeline jet pump and introducing oxygen. The oxidation time of the process is about 50-120min under the condition that the catalyst participates in the reaction, particularly, in the later period of the oxidation reaction, the oxidation rate of ferrous ions is low, the reaction can be completely carried out only by frequently adding the catalyst, and the defects of long production period, frequent operation, low production efficiency, unstable quality and the like are caused.
A polymeric ferric sulfate continuous production system is disclosed in patent No. (CN 206985743U): the continuous production system comprises a dissolving tank, a gas-liquid mixer, a gas-liquid separator, a finished product tank and a gas collecting device, wherein the device is used for leading ferrous ions in supersaturated ferrous sulfate heptahydrate solution to be in a catalyst NO 2 Under the action of gas, it is converted into iron ion, and NO 2 The gas is partially converted into NO, the NO reacts with oxygen to generate nitrogen dioxide, the nitrogen dioxide is compressed by a compression pump and then is reused in an oxidation reaction device, the generation of waste gas is well avoided, the production efficiency is gradually improved, the preparation process of the liquid polymeric ferric sulfate comprises three reactions of oxidation, hydrolysis and polymerization, and the three reactions exist in a system at the same time, are mutually influenced and are mutually promoted. Particularly, the ferrous ion oxidation time is long, and the ferrous ion oxidation is difficult to completely realize only through a gas-liquid mixer and a gas-liquid separator, so that the quality of the prepared polymerized ferric sulfate is unstable.
Therefore, how to obtain the liquid polymeric ferric sulfate with stable and uniform quality by reasonably adjusting the process, improving the production efficiency, improving the ferrous conversion rate, reducing the operation labor force and having important significance in the preparation of the polymeric ferric sulfate.
SUMMERY OF THE UTILITY MODEL
For overcoming the not enough of prior art, the utility model provides a system for serialization production liquid polyferric sulfate, process flow is short, reduces the operation labour, and ferrous ion conversion rate is high, easily industrialization, and the preparation process energy consumption is low, and product quality is stable homogeneous, energy-concerving and environment-protective.
In order to solve the above problem, the technical scheme of the utility model is that:
continuous production liquid polyferric sulfate's system, include the ferrous solution proportioning tank with titanium dioxide sulfuric acid waste pipeline connection, the sodium nitrite proportioning tank of being connected with the process water pipeline, be equipped with the one-level preoxidation reation kettle of gas-liquid mixer, the ferrous solution proportioning tank passes through the pre-heater and links to each other with gas-liquid mixer, and the sodium nitrite proportioning tank passes through the pipeline and links to each other with gas-liquid mixer, gas-liquid mixer links to each other with the oxygen pipeline. The mixed material liquid enters a primary pre-oxidation reaction kettle through a bell mouth of a gas-liquid mixer, and about 50 percent of ferrous ions are oxidized into ferric ions in the primary pre-oxidation reaction kettle.
The primary pre-oxidation reaction kettle is connected with the upper part of the secondary pre-oxidation reaction kettle through an overflow pipeline at the upper part, and about 30 percent of ferrous ions in the secondary pre-oxidation reaction kettle are oxidized into ferric ions; the pipeline connected with the kettle bottom valve at the bottom of the secondary pre-oxidation reaction kettle and the overflow pipeline at the upper part are connected with the feed inlet of the filter through a pre-oxidation liquid delivery pump, the discharge outlet of the filter is connected with the top end of the packing layer of the tower reactor, an oxygen pipeline is connected with the bottom of the packing layer of the tower reactor, the top end of the tower reactor is provided with an exhaust port and is connected to a gas-liquid separator, and the bottom of the gas-liquid separator is connected with the tower reactor through a pipeline. The top of the gas-liquid separator is connected with a tail gas absorption tower through a pipeline. The pre-oxidized feed liquid enters a filter through a pre-oxidized liquid conveying pump for filtering, the filtered feed liquid enters the top end of a packing layer of the tower reactor, and oxygen is conveyed from the bottom of the packing layer of the tower reactor through an oxygen pipeline through an oxygen pressure reducing valve; the gas-liquid separator is arranged for separating waste gas from condensate, the waste gas at the top of the gas-liquid separator is conveyed to the tail gas absorption tower, and the condensate flows back to the tower reactor through the bottom of the gas-liquid separator.
The filter is one of a bag filter, a plate filter and a rod filter, and mainly aims to filter mechanical impurities in a ferrous solution, filter crystallized ferrous sulfate which is not completely reacted and avoid blocking a tower reactor.
The tower reactor is a filler reaction tower, and the filler is one of corrosion-resistant stainless steel Raschig rings, ceramic Raschig rings, stainless steel pall rings and ceramic pall rings. In the tower reactor, the incompletely oxidized ferrous solution temporarily stays through a packing bed layer and fully contacts with oxygen, so that ferrous is fully oxidized, hydrolyzed and polymerized; the tower reactor has the advantage of large liquid storage capacity, is more favorable for reducing back mixing and improving reaction rate compared with the traditional kettle reactor, and can obtain higher ferrous ion conversion rate which is up to more than 99.5 percent.
Further, the bottom of the tower reactor is connected with a finished product storage tank through a finished product delivery pump.
Further, an oxygen pressure reducing valve is arranged on the oxygen pipeline, and the oxygen pipeline is connected with the secondary pre-oxidation reaction kettle. Oxygen enters the first-stage pre-oxidation reaction kettle and the second-stage pre-oxidation reaction kettle respectively through oxygen pipelines to maintain constant pressure in the reaction system.
The oxygen pressure reducing valve can effectively control the feeding pressure of the tower reactor, and avoid oxygen waste.
Furthermore, a sodium nitrite solution delivery pump and a sodium nitrite flowmeter are arranged on a connecting pipeline of the sodium nitrite batching tank and the gas-liquid mixer. The feed rate of the sodium nitrite solution was controlled by a flow meter.
The sodium nitrite batching tank is arranged to fully mix and dissolve sodium nitrite and process water into 20-30% sodium nitrite solution which is used as a catalyst for preparing polymeric ferric sulfate.
Furthermore, a ferrous solution delivery pump and a ferrous solution flowmeter are arranged on a connecting pipeline of the ferrous solution batching tank and the gas-liquid mixer.
The ferrous solution batching tank is arranged to fully mix titanium white waste acid and ferrous sulfate to prepare supersaturated ferrous solution: the mass fraction of ferrous ions is 11-13%, and the mass fraction of free acid is 5-8%.
The ferrous solution slurry is conveyed to a preheater through a ferrous solution conveying pump to be preheated to 50-60 ℃ so as to provide the temperature required by ferrous oxidation, which is beneficial to accelerating the ferrous ion oxidation time, and the feeding speed of the ferrous solution is controlled by a ferrous solution flowmeter.
Furthermore, an electric valve is arranged on the overflow line to control the feeding speed of the secondary pre-oxidation reaction kettle.
Further, the first-stage pre-oxidation reaction kettle and the second-stage pre-oxidation reaction kettle are both provided with a speed reducer and a self-suction stirring paddle; the top end of the reaction kettle is provided with a safety discharge device, a pressure gauge and a temperature sensor.
Further, ferrous solution batching groove, sodium nitrite batching groove all are equipped with agitating unit. The dissolution of ferrous iron and sodium nitrite can be accelerated.
And a discharge pipeline is arranged at the bottom of the finished product storage tank, and a finished product loading and unloading pump is arranged on the discharge pipeline. The finished product storage tank is used for storing liquid polyferric sulfate finished products, and the finished product loading and unloading pump is convenient for loading, unloading, packaging and selling the products.
The beneficial effects of the utility model are as follows:
(1) The supersaturated ferrous solution prepared by the utility model enters the preheater for heating through the delivery pump, then fully mixes with the sodium nitrite solution and the oxygen through the gas-liquid mixer to enter the primary pre-oxidation reaction kettle, about 50 percent of ferrous ions are oxidized into ferric ions, the pre-oxidation ferrous solution overflows to the secondary pre-oxidation reaction kettle, about 30 percent of ferrous ions are oxidized into ferric ions, and the overflowed ferrous solution removes impurities through the filter and enters the tower reactor; the incompletely oxidized ferrous solution temporarily stays through a packing bed layer of the reaction tower and fully contacts with oxygen, so that ferrous is fully oxidized, hydrolyzed and polymerized; the tower reactor has large liquid storage capacity, is more favorable for reducing back mixing and improving reaction rate compared with the traditional kettle reactor, can obtain higher ferrous ion conversion rate which is up to more than 99.5 percent, and obtains liquid polymeric ferric sulfate at the tower bottom.
(2) The utility model provides a system for serialization production liquid polyferric sulfate, process flow is short, and ferrous ion conversion rate is high, easily industrial production, and can effectively reduce the operation labour, and its preparation process energy consumption is low, and product quality is stable homogeneous, and is energy-concerving and environment-protective.
Drawings
The accompanying drawings, which are described herein, serve to provide a further understanding of the invention and constitute a part of this specification, and the exemplary embodiments and descriptions thereof are provided for explaining the invention without unduly limiting it. In the drawings:
fig. 1 is a schematic structural diagram of a system for continuously producing liquid polymeric ferric sulfate according to the present invention.
In the figure: 1. a ferrous solution batching tank; 2. a sodium nitrite batching tank; 3. a preheater; 4. a gas-liquid mixer; 5. a first-stage pre-oxidation reaction kettle; 6. a secondary pre-oxidation reaction kettle; 7. a filter; 8. a tower reactor; 9. a gas-liquid separator; 10. a finished product storage tank; 11. a ferrous solution delivery pump; 12. a sodium nitrite solution delivery pump; 13. a pre-oxidation liquid delivery pump; 14. a finished product delivery pump; 15. finished product loading and unloading pump; 16. an electrically operated valve; 17. an oxygen pressure reducing valve; 18. an oxygen line; 19. an overflow line; 20. a sodium nitrite flow meter; 21. a ferrous solution flow meter.
Detailed Description
The present invention will be understood from the following description with reference to the examples.
In one embodiment, as shown in fig. 1, a system for continuously producing liquid polyferric sulfate comprises a ferrous solution dosing tank 1 connected with a titanium white waste sulfuric acid pipeline, a sodium nitrite dosing tank 2 connected with a process water pipeline, and a primary pre-oxidation reaction kettle 5 provided with a gas-liquid mixer 4, wherein the ferrous solution dosing tank 1 is connected with the gas-liquid mixer 4 through a preheater 3, the sodium nitrite dosing tank 2 is connected with the gas-liquid mixer 4 through a pipeline, and the gas-liquid mixer 4 is connected with an oxygen pipeline 18. The mixed material liquid enters a primary pre-oxidation reaction kettle 5 through a bell mouth of a gas-liquid mixer 4, and about 50 percent of ferrous ions are oxidized into ferric ions in the primary pre-oxidation reaction kettle 5.
The primary pre-oxidation reaction kettle 5 is connected with the upper part of a secondary pre-oxidation reaction kettle 6 through an overflow pipeline 19 at the upper part, and about 30 percent of ferrous ions in the secondary pre-oxidation reaction kettle 6 are oxidized into ferric ions; the pipeline that second grade pre-oxidation reation kettle 6 bottom cauldron bottom valve is connected and the overflow pipe on upper portion pass through pre-oxidation liquid delivery pump 13 and connect the feed inlet of filter 7, and 8 packing layers tops of tower reactor are connected to the discharge gate of filter 7, and oxygen pipeline 18 is connected with 8 packing layer bottoms of tower reactor, and 8 tops of tower reactor set up the gas vent and connect to vapour and liquid separator 9, and the pipeline connection tower reactor 8 is passed through to vapour and liquid separator 9 bottoms. The top of the gas-liquid separator 9 is connected with a tail gas absorption tower through a pipeline. The pre-oxidized feed liquid enters a filter 7 through a pre-oxidized liquid delivery pump 13 for filtering, the filtered feed liquid enters the top end of a packing layer of a tower reactor 8, and oxygen is delivered from the bottom of the packing layer of the tower reactor 8 through an oxygen pipeline 18 and an oxygen pressure reducing valve 17; the gas-liquid separator 9 is arranged for separating waste gas from condensate, the waste gas at the top of the gas-liquid separator 9 is conveyed to the tail gas absorption tower, and the condensate flows back to the tower reactor 8 through the bottom of the gas-liquid separator 9.
The pipeline that 5 bottom cauldron bottom valves of one-level pre-oxidation reation kettle connect passes through pre-oxidation liquid delivery pump 13 and connects the feed inlet of filter 7, makes things convenient for the shut down to overhaul the in-process, all transmits remaining material to tower reactor 8 reaction.
The filter 7 is a plate filter, and is mainly used for filtering mechanical impurities in a ferrous solution, filtering out incompletely reacted crystallized ferrous sulfate, and avoiding blocking the tower reactor 8.
The tower reactor 8 is a filler reaction tower, and the filler is a corrosion-resistant stainless steel Raxi ring. The tower reactor 8 is to make the incompletely oxidized ferrous solution stay for a short time through the packing bed layer and fully contact with oxygen to ensure that the ferrous is fully oxidized, hydrolyzed and polymerized; the tower reactor 8 has the advantage of large liquid storage capacity, and is more favorable for reducing back mixing and improving reaction rate compared with the traditional kettle type reactor, and the tower reactor 8 can obtain higher ferrous ion conversion rate which is up to more than 99.5 percent.
It will be appreciated that the bottom of the column reactor 8 is connected to a product storage tank 10 by a product transfer pump 14.
It is understood that the oxygen line 18 is provided with an oxygen pressure reducing valve 17, and the oxygen line 18 is connected with the secondary pre-oxidation reaction kettle 6. Oxygen enters the first-stage pre-oxidation reaction kettle 5 and the second-stage pre-oxidation reaction kettle 6 through an oxygen pipeline 18 respectively to maintain constant pressure in the reaction system.
The oxygen pressure reducing valve 17 can effectively control the feeding pressure of the tower reactor 8, and oxygen waste is avoided.
It can be understood that the sodium nitrite solution delivery pump 12 and the sodium nitrite flow meter 20 are arranged on the connecting pipeline of the sodium nitrite dosing tank 2 and the gas-liquid mixer 4. The feed rate of the sodium nitrite solution was controlled by a flow meter.
The sodium nitrite batching tank 2 is arranged to fully mix and dissolve sodium nitrite and process water into 20-30 percent sodium nitrite solution which is used as a catalyst for preparing polymeric ferric sulfate.
It can be understood that the connection pipeline of the ferrous solution batching tank 1 and the gas-liquid mixer 4 is provided with a ferrous solution delivery pump 11 and a ferrous solution flow meter 21.
The ferrous solution batching tank 1 is arranged to fully mix titanium white waste acid and ferrous sulfate and prepare supersaturated ferrous solution: the mass fraction of ferrous ions is 11-13%, and the mass fraction of free acid is 5-8%.
The ferrous solution slurry is conveyed to the preheater 3 through the ferrous solution conveying pump 11 to be preheated to 50-60 ℃, the temperature required by ferrous oxidation is provided, the ferrous ion oxidation time is favorably accelerated, and the feeding speed of the ferrous solution is controlled through the ferrous solution flowmeter 21.
It can be understood that the overflow line 19 is provided with an electric valve 16 for controlling the feeding rate of the secondary pre-oxidation reactor 6.
As can be understood, the first-stage pre-oxidation reaction kettle 5 and the second-stage pre-oxidation reaction kettle 6 are both provided with a speed reducer and a self-suction stirring paddle; the top end of the reaction kettle is provided with a safety discharge device, a pressure gauge and a temperature sensor.
It can be understood that ferrous solution dosing tank 1, sodium nitrite dosing tank 2 all are equipped with speed reducer and stirring rake. The dissolution of ferrous iron and sodium nitrite can be accelerated.
And a discharge pipeline is arranged at the bottom of the finished product storage tank 10, and a finished product loading and unloading pump 15 is arranged on the discharge pipeline. The finished product storage tank 10 is used for storing a liquid polyferric sulfate finished product, and the finished product loading and unloading pump 15 is convenient for loading, unloading, packaging and selling the product.
The working principle is as follows: the prepared supersaturated ferrous solution enters a preheater 3 through a delivery pump to be heated, then is fully mixed with a sodium nitrite solution and oxygen through a gas-liquid mixer 4 and enters a primary pre-oxidation reaction kettle 5, about 50% of ferrous ions are oxidized into ferric ions, the pre-oxidation ferrous solution overflows to a secondary pre-oxidation reaction kettle 6, and about 30% of ferrous ions are oxidized into ferric ions; the pre-oxidized feed liquid enters a filter 7 through a pre-oxidized liquid delivery pump 13 for filtration, the filtered feed liquid enters the top end of a packing layer of a tower reactor 8, oxygen is delivered from the bottom of the packing layer of the tower reactor 8 through an oxygen pipeline 18 and an oxygen pressure reducing valve 17, and the incompletely oxidized ferrous solution temporarily stays through a packing bed layer of the tower reactor 8 and is fully contacted with the oxygen, so that ferrous is fully oxidized, hydrolyzed and polymerized; the top end of the tower reactor 8 is provided with an exhaust port and is connected to a gas-liquid separator 9; the gas-liquid separator 9 realizes the separation of waste gas and condensate, the waste gas at the top of the gas-liquid separator 9 is conveyed to the tail gas absorption tower, and the condensate flows back to the tower reactor 8 through the bottom of the gas-liquid separator 9. The tower reactor 8 has large liquid storage capacity, is more beneficial to reducing back mixing and improving reaction rate compared with the traditional kettle reactor, the tower reactor 8 can obtain higher ferrous ion conversion rate which is up to more than 99.5 percent, and liquid polymeric ferric sulfate is obtained at the tower bottom. The liquid polymeric ferric sulfate is transported to a finished product storage tank 10 from the bottom of the tower reactor 8 through a finished product delivery pump 14, and the finished product is discharged through a finished product loading and unloading pump 15 through a discharge pipeline at the bottom of the finished product storage tank 10 and packaged for sale.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (9)
1. The system for continuously producing the liquid polymeric ferric sulfate is characterized by comprising a ferrous solution batching tank (1) connected with a titanium white waste sulfuric acid pipeline, a sodium nitrite batching tank (2) connected with a process water pipeline, and a primary pre-oxidation reaction kettle (5) provided with a gas-liquid mixer (4), wherein the ferrous solution batching tank (1) is connected with the gas-liquid mixer (4) through a preheater (3), the sodium nitrite batching tank (2) is connected with the gas-liquid mixer (4) through a pipeline, the gas-liquid mixer (4) is connected with an oxygen pipeline (18), the primary pre-oxidation reaction kettle (5) is connected with the upper part of a secondary pre-oxidation reaction kettle (6) through an overflow pipeline (19) on the upper part, the pipeline connected with a kettle bottom valve at the bottom of the secondary pre-oxidation reaction kettle (6) and the overflow pipeline on the upper part are connected with a feed inlet of a filter (7) through a pre-oxidation liquid conveying pump (13), a discharge port of the filter (7) is connected with the top end of a packing layer of the oxygen pipeline (18) and is connected with the bottom of the reactor (8), the tower type gas-liquid separator (9) through a gas-liquid separator (9), and a gas-liquid separator (9) is connected with the tower type reaction kettle bottom of the tower type reaction kettle (8); the bottom of the tower reactor (8) is connected with a finished product storage tank (10) through a finished product delivery pump (14).
2. The system for continuously producing the liquid polymeric ferric sulfate according to claim 1, wherein the top of the gas-liquid separator (9) is connected with a tail gas absorption tower through a pipeline.
3. The system for continuously producing the liquid polyferric sulfate as claimed in claim 1, wherein the oxygen pipeline (18) is provided with an oxygen pressure reducing valve (17), and the oxygen pipeline (18) is connected with the secondary pre-oxidation reaction kettle (6).
4. The system for continuously producing liquid polyferric sulfate according to claim 1, wherein a sodium nitrite solution delivery pump (12) and a sodium nitrite flow meter (20) are arranged on a connecting pipeline between the sodium nitrite dosing tank (2) and the gas-liquid mixer (4).
5. The system for continuously producing liquid polymeric ferric sulfate according to claim 1, wherein a ferrous solution delivery pump (11) and a ferrous solution flow meter (21) are arranged on a connecting pipeline of the ferrous solution dosing tank (1) and the gas-liquid mixer (4).
6. The system for continuously producing liquid polyferric sulfate according to claim 1, wherein the overflow line (19) is provided with an electric valve (16).
7. The system for continuously producing liquid polymeric ferric sulfate according to claim 1, wherein the first-stage pre-oxidation reaction kettle (5) and the second-stage pre-oxidation reaction kettle (6) are both provided with a speed reducer and a self-priming stirring paddle; the top end of the reaction kettle is provided with a safety discharge device, a pressure gauge and a temperature sensor.
8. The system for continuously producing liquid polymeric ferric sulfate according to claim 1, wherein the ferrous solution dosing tank (1) and the sodium nitrite dosing tank (2) are both provided with stirring devices.
9. The system for continuously producing the liquid polyferric sulfate according to claim 1, wherein a discharge pipeline is arranged at the bottom of the finished product storage tank (10), and a finished product loading and unloading pump (15) is arranged on the discharge pipeline.
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