CN111760536A - Continuous production process combining magnesium ammonium phosphate and soda ash - Google Patents
Continuous production process combining magnesium ammonium phosphate and soda ash Download PDFInfo
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- CN111760536A CN111760536A CN202010450290.5A CN202010450290A CN111760536A CN 111760536 A CN111760536 A CN 111760536A CN 202010450290 A CN202010450290 A CN 202010450290A CN 111760536 A CN111760536 A CN 111760536A
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Abstract
The invention relates to the technical field of production of magnesium ammonium phosphate, in particular to a continuous production process combining magnesium ammonium phosphate and soda ash, which comprises the following steps: (1) preparing a first reaction solution; (2) preparing a second reaction solution; (3) mixing and reacting; (4) thickening, separating and drying. The device can realize continuous production of the ammonium magnesium phosphate, improves the production efficiency, can be combined with the production of the calcined soda, and reduces the discharge amount of the waste residues of the magnesium hydroxide and the calcium carbonate in the production of the calcined soda.
Description
Technical Field
The invention relates to the technical field of production of magnesium ammonium phosphate, in particular to a continuous production process combining magnesium ammonium phosphate and soda ash.
Background
The magnesium ammonium phosphate contains various nutrient elements required by plants such as nitrogen, phosphorus, magnesium and the like, is directly used for the roots of the plants due to low solubility, does not cause the phenomenon of root burning, releases the amount of the required plants, does not pollute the environment like the traditional soluble fertilizer along with the loss of rainwater, and can be used as a high-quality, high-efficiency and environment-friendly slow-release fertilizer.
The method for producing the magnesium ammonium phosphate by using the sea brine at present comprises the steps of adding phosphate radical ions and ammonium radical ions into the sea brine, then adding alkaline substances, adjusting the pH value to be 7-9, then standing and settling the reacted materials for 1-12 hours, and carrying out solid-liquid separation on the lower-layer solid to obtain a magnesium ammonium phosphate product. The main reaction process of the method needs to be kept stand for settling for 1-12 hours, the batch reaction is carried out, the production efficiency is low, and the method can only be used for small-scale batch production and cannot realize large-scale automatic control industrial production; the method has high cost, the production cost per ton is 4000-5000 yuan, and the obtained product has low purity. In the production of soda by ammonia-soda process, after sea brine is used for dissolving solid sodium chloride, Mg carried in the liquid and the solid2+By adding OH-A method of (3) producing Mg (OH)2Then the waste slag is discharged and stored as waste slag. In the prior art, a continuous production process combining the production process of magnesium ammonium phosphate and the production process of soda by an ammonia-soda process does not exist.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the prior art, the continuous production process combining the production of the magnesium ammonium phosphate and the production of the soda ash is provided, the process can realize the automatic control continuous production of the magnesium ammonium phosphate, improve the production efficiency, facilitate the large-scale production, reduce the production cost, and can be combined with the production of the soda ash to reduce the discharge amount of the waste residues of magnesium hydroxide and calcium carbonate in the production of the soda ash.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a continuous production process combining magnesium ammonium phosphate and soda ash comprises the following steps:
(1) preparation of a first reaction solution: sequentially putting phosphoric acid, tap water, ammonium bicarbonate and sodium hydroxide solution into a liquid storage tank, stirring and mixing, and reacting to obtain a first reaction solution;
(2) preparation of a second reaction solution: sequentially adding deionized water and ammonia water into a liquid storage tank, and stirring and mixing to obtain a second reaction liquid;
(3) mixing and reacting: adding sea brine, a first reaction liquid and a second reaction liquid into a first reactor at the same time, adjusting the pH, carrying out a reaction for a period of time, conveying the reaction liquid to a second reactor, adjusting the pH, and carrying out a reaction for a period of time to obtain magnesium ammonium phosphate crystal slurry;
(4) thickening, separating and drying treatment: after thickening treatment of a thickener and separation treatment of a centrifuge, granulating, drying and packaging the magnesium ammonium phosphate crystal slurry to obtain a magnesium ammonium phosphate product; and conveying the clear liquid discharged by the thickener and the centrifuge to a salt melting barrel on a soda production line.
As an improved technical scheme, in the step (1), phosphoric acid, tap water, ammonium bicarbonate and sodium hydroxide solution are sequentially added into a liquid storage tank according to the mass ratio of 1.95-2.25:3.0-3.5:1.1-1.25:1, the reaction temperature is controlled to be 10-30 ℃, wherein the phosphoric acid is 75-85 wt% of phosphoric acid, and the content of sodium hydroxide in the sodium hydroxide solution is 25-35 wt%.
As an improved technical scheme, when the mixing reaction in the step (3) is carried out, the pH value of the reaction system in the first reactor is controlled to be 4.5-6, the reaction time is 30-60min, and PO in the reaction system is controlled4 3+:NH4 +：Mg2+The molar ratio of (1: 1.1) - (1.3: 1.0) - (1.2); the pH value of the reaction system in the second reactor is 6.0-7.5, and the reaction time is 30-50 min.
As an improved technical scheme, the first reactor comprises a barrel body, wherein a first reaction liquid inlet pipe and a sea brine inlet pipe are arranged at the top of the barrel body, a second reaction liquid inlet is arranged at one side of the upper part of the barrel body, a manhole is arranged at one side of the lower part of the barrel body, a discharge hole is arranged at the center of the bottom of the barrel body, and a sewage discharge outlet is arranged at one side of the discharge hole; a stirring frame is arranged inside the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom of the stirring frame, and a plurality of sawteeth are arranged on the scraping plate; the bottom of the barrel body is provided with supporting legs.
As an improved technical scheme, an included angle between the central line of the first reaction liquid inlet pipe and the central line of the sea brine inlet pipe is 16-22 degrees, an included angle between the central line of the second reaction liquid inlet pipe and the central line of the first reaction liquid inlet pipe is 160-175 degrees, and a pipe body of the first reaction liquid inlet pipe extending into the first reactor is provided with a 90-degree bend.
As an improved technical scheme, the shape of the stirring frame is a Chinese character 'zhong', and the stirring frame comprises an upper frame and a lower frame which are detachably connected.
As an improved technical scheme, the second reactor comprises a barrel body, one side of the upper part of the barrel body is provided with a flow guide part communicated with the inside of the barrel body, the bottom of the flow guide part is provided with a first liquid inlet, one side of the top of the barrel body is provided with a second liquid inlet, one side of the lower part of the barrel body is provided with a manhole, the center of the bottom of the barrel body is provided with a discharge hole, one side of the discharge hole is provided with a sewage discharge outlet, the inside of the barrel body is provided with a stirring frame, the stirring frame is driven by a motor, the bottom of the stirring frame is provided with an arc-shaped scraping plate, and; the bottom of the barrel body is provided with supporting legs.
As an improved technical scheme, water conservancy diversion portion is the cuboid of carbon steel material, the inner wall of water conservancy diversion portion is equipped with one deck glass steel layer, the top of water conservancy diversion portion is equipped with can dismantle the top cap, the inside of water conservancy diversion portion is equipped with the pH meter, just the central line of first inlet with the central line of second inlet is parallel to each other.
After the technical scheme is adopted, the invention has the beneficial effects that:
(1) the reaction process of the invention does not need standing sedimentation, the solid content (magnesium ammonium phosphate) of the reaction liquid can be increased through thickening treatment of the thickener, and the separation efficiency of the centrifuge is improved; and the intermittent operation caused by centrifugal separation can be solved, so that the continuous operation of the whole process is ensured. The steady-state continuous reaction is realized, the number of equipment is greatly reduced, the one-time investment of the equipment is further reduced, the utilization rate of the equipment is improved, the liquid-liquid phase automatic control mixing reaction is realized, and the production efficiency is greatly improved.
(2) The treatment cost of the method is calculated through continuous production test data, the efficient utilization of the phosphorus source is the key for reducing the treatment cost, the utilization rate of phosphorus in the continuous production process can reach more than 98 percent by controlling the molar ratio of phosphorus to magnesium to be 1:1-1.2 in the reaction process, the content of other phosphates is reduced, the purity of the product is improved, and the production cost of the magnesium ammonium phosphate product is reduced.
(3) After the continuous reaction production is realized, the supernatant fluid after the production of the ammonium magnesium phosphate can be continuously and stably conveyed to the process of soda salt production by the ammonia-soda process, the process meets the process requirements of soda salt production by the ammonia-soda process, the large-scale efficient utilization of the sea brine water resource is realized, the discharge amount of waste residues of magnesium hydroxide and calcium carbonate in the soda production can be reduced, and the cost of waste residue treatment by enterprises is reduced.
The first reactor comprises a barrel body, the top of the barrel body is provided with a first reaction liquid inlet pipe and a sea brine inlet pipe, one side of the upper part of the barrel body is provided with a second reaction liquid inlet, one side of the lower part of the barrel body is provided with a manhole, the center of the bottom of the barrel body is provided with a discharge hole, and one side of the discharge hole is provided with a drain outlet; a stirring frame is arranged inside the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom of the stirring frame, and a plurality of sawteeth are arranged on the scraping plate; the bottom of the barrel body is provided with supporting legs. Inside first reaction liquid, sea brine and second reaction liquid advanced pipe from first reaction liquid respectively, sea brine advanced pipe and second reaction liquid import entered pipe and got into first reactor simultaneously according to a certain proportion respectively, the starter motor operation, stirring frame and scraper blade stir the mixture to the material in the reactor, the inside reaction condition can be observed through the manhole to the producer, inside the slurry after the reaction got into the second reactor from the discharge gate discharge after the reaction finishes. Can will wash water through first inlet when needs wash first reactor, inside sea brine advances pipe or second inlet entering reactor, start the agitator frame, realize the washing to reactor inside, wash the end mouth and pass through the drain and discharge the filth. The design is reasonable, the structure is simple, and the reaction of materials is facilitated; the arc scraper with saw teeth can prevent the bottom of the reactor from scabbing.
Because the included angle between the central line of the first reaction liquid inlet pipe and the central line of the sea brine inlet pipe is 16-22 degrees, and the included angle between the central line of the second reaction liquid inlet and the central line of the first reaction liquid inlet pipe is 160-175 degrees. The design is to ensure that the first reaction liquid and the sea brine firstly contact and react during feeding, and then react with the second reaction liquid, so that the smooth reaction after the three liquids are added is ensured.
Because the shape of stirring frame is chinese character 'zhong', the stirring frame is including upper ledge and the lower frame of dismantling the connection. The novel mixing machine is simple in structure, reasonable in design, convenient to detach and install and capable of promoting sufficient mixing of materials.
The second reactor comprises a barrel body, a flow guide part communicated with the interior of the barrel body is arranged on one side of the upper part of the barrel body, a first liquid inlet is arranged at the bottom of the flow guide part, a second liquid inlet is arranged on one side of the top of the barrel body, a manhole is arranged on one side of the lower part of the barrel body, a discharge hole is arranged in the center of the bottom of the barrel body, a sewage discharge outlet is arranged on one side of the discharge hole, a stirring frame is arranged in the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom; the bottom of the barrel body is provided with supporting legs. Slurry after the reaction of the first reactor enters the second reactor from the first liquid inlet of the flow guide part along the pipeline, the pH is measured, then the rest second reaction liquid is added, and the slurry after the reaction is conveyed to the inside of the buffer tank from the discharge port through stirring and mixing of the stirring frame. In the reaction process, the staff can observe the reaction condition through the manhole, when wasing the second reactor, will wash water direct from first inlet add or the second inlet add can, start the agitator frame, wash reactor inside, the filth is discharged from row's thing mouth after wasing the end. The method has the advantages of reasonable design, simple operation and convenient reaction.
Because water conservancy diversion portion is the cuboid of carbon steel material, the top of water conservancy diversion portion is equipped with can dismantle the top cap, and the inside of water conservancy diversion portion is equipped with the pH meter. In practical application, the reaction condition can be conveniently observed by opening the top cover, and the pH value of materials in the reactor can be measured.
Drawings
FIG. 1 is a flow chart of a continuous production process of the present invention combining magnesium ammonium phosphate and soda production;
FIG. 2 is a schematic view of the structure of the first reactor in FIG. 1;
FIG. 3 is a top view of FIG. 2;
FIG. 4 is a schematic view of the structure of the second reactor in FIG. 1;
wherein, 1-a first reactor, 13-a first liquid inlet, 14-a sea brine inlet pipe, 15-a second liquid inlet, 16-a manhole, 17-a discharge port, 18-a sewage discharge port, 19-a stirring frame, 190-a scraping plate, 1900-a sawtooth, 20-a motor, 21-a supporting leg, 2-a first reaction liquid storage tank, 3-a second reaction liquid storage tank, 4-a sea brine pipeline, 5-a second reactor, 50-a diversion part, 500-a first liquid inlet, 51-a second liquid inlet, 52-a manhole, 53-a discharge port, 54-a sewage discharge port, 55-a stirring frame, 550-a scraping plate, 5500-a sawtooth, 56-a motor, 57-a supporting leg, 7-a thickener, 8-a centrifuge and 9-a liquid storage tank, 10-alkali dissolving barrel, 11-granulator and 12-dryer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A continuous production process combining magnesium ammonium phosphate and soda ash comprises the following steps:
(1) preparation of a first reaction solution: sequentially adding phosphoric acid (75-85 wt% of phosphoric acid), tap water, ammonium bicarbonate and a sodium hydroxide solution (the content of sodium hydroxide is 25-35 wt%) into a liquid storage tank according to the mass ratio of 1.95:3.0:1.1:1, controlling the reaction temperature to be 10-30 ℃, stirring and mixing, and reacting to obtain a first reaction liquid;
(2) preparation of a second reaction solution: sequentially adding deionized water and ammonia water into a liquid storage tank, and stirring and mixing to obtain a second reaction solution with the pH of 10-13;
(3) mixing and reacting: adding sea brine, the first reaction solution and the second reaction solution into the first reactor at the same time, and controlling PO in the reaction system4 3+:NH4 +：Mg2+The molar ratio of the magnesium phosphate to the ammonium phosphate is 1:1.1-1.3:1.0-1.2, the pH value is adjusted to 4.5-6, the reaction liquid is conveyed to a second reactor after 30-60min of reaction, the pH value is adjusted to 7.0, and the magnesium phosphate ammonium crystal slurry is obtained after 30-50min of reaction.
(4) Thickening, separating and drying treatment: conveying the magnesium ammonium phosphate crystal slurry into a thickener, separating the treated material in a centrifuge (adding deionized water for washing for 15-20min during centrifugal separation), and granulating, drying and packaging the centrifuged material to obtain a magnesium ammonium phosphate product; and conveying clear liquid discharged by the thickener and the centrifuge to an alkali dissolving barrel on a soda production line.
The first reactor comprises a barrel body, a first reaction liquid inlet pipe and a sea brine inlet pipe are arranged at the top of the barrel body, a second reaction liquid inlet is arranged on one side of the upper part of the barrel body, a manhole is arranged on one side of the lower part of the barrel body, a discharge hole is arranged in the center of the bottom of the barrel body, and a drain outlet is arranged on one side of the discharge hole; a stirring frame is arranged in the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom of the stirring frame, and a plurality of sawteeth are arranged on the scraping plate; the bottom of the barrel body is provided with supporting legs. In the actual production, the first reaction liquid, the sea brine (seawater) and the second reaction liquid are respectively and simultaneously arranged at 1650kg/h and 15m from the first reaction liquid inlet pipe, the sea brine inlet pipe and the second reaction liquid inlet respectively3The volume of/h and 2600kg/h enters the first reactor, a motor is started to operate, a stirring frame and a scraper are used for stirring and mixing materials in the reactor, the rotating speed of the stirring frame is 13-20 r/min, a producer can observe the internal reaction condition through a manhole, and slurry after reaction is discharged from a discharge hole and enters the second reactor.
Wherein the included angle between the central line of the first reaction liquid inlet pipe and the central line of the sea brine inlet pipe is 16-22 degrees, the included angle between the central line of the second reaction liquid inlet pipe and the central line of the first reaction liquid inlet pipe is 160-175 degrees, and the pipe body of the first reaction liquid inlet pipe extending into the first reactor is provided with a 90-degree bend. When the materials are fed, the first reaction liquid and the sea brine firstly contact and react, and then the first reaction liquid and the second reaction liquid react, so that smooth reaction after the three liquids are added is ensured.
The stirring frame is in a shape of a Chinese character 'zhong', and comprises an upper frame and a lower frame which are detachably connected.
The second reactor comprises a barrel body, a flow guide part communicated with the interior of the barrel body is arranged on one side of the upper part of the barrel body, a first liquid inlet is formed in the bottom of the flow guide part, a second liquid inlet is formed in one side of the top of the barrel body, a manhole is formed in one side of the lower part of the barrel body, a discharge hole is formed in the center of the bottom of the barrel body, a sewage discharge outlet is formed in one side of the discharge hole, a stirring frame is arranged in the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom; the bottom of the barrel body is provided with supporting legs. And the slurry in the first reactor enters the first reactor from the liquid inlet of the flow guide part, the top cover is opened to detect the pH value of the reaction system in the second reactor, the pH value of the reaction system is adjusted to 7.0 by adding the second reaction liquid, and the rotating speed of the stirring frame is 10-20 r/min.
Wherein water conservancy diversion portion is the cuboid of carbon steel material, and the inner wall of water conservancy diversion portion is equipped with the glass steel layer, and the top of water conservancy diversion portion is equipped with can dismantle the top cap, and the inside of water conservancy diversion portion is equipped with the pH meter, and the central line of first inlet and the central line of second inlet are parallel to each other.
As shown in fig. 2, the first reactor 1 comprises a barrel body, a first reaction liquid inlet 13 and a sea brine inlet pipe 14 are arranged on one side of the top of the barrel body, a manhole and a plurality of spare ports (which are not marked in the drawing) are arranged on the top of the barrel body, a second reaction liquid inlet 15 is arranged on one side of the upper part of the barrel body, a manhole 16 is arranged on one side of the lower part of the barrel body, a discharge port 17 is arranged in the center of the bottom of the barrel body, and a drain outlet 18 is arranged on one side of the discharge port; a middle-shaped stirring frame 19 is arranged inside the barrel body (two sides of the upper frame and the lower frame are respectively provided with a fixing plate, screws penetrate through holes in the fixing plates to assemble the upper frame and the lower frame together), the stirring frame is driven by a motor 20, an arc-shaped scraping plate 190 is arranged at the bottom of the stirring frame 19, and a plurality of saw teeth 1900 are arranged on the scraping plate 190; the bottom of the barrel body is provided with a supporting leg 21. Inside first reaction liquid, sea brine and second reaction liquid advanced pipe from first reaction liquid respectively, sea brine advanced pipe and second reaction liquid import entered pipe and got into first reactor simultaneously according to a certain proportion respectively, the starter motor operation, stirring frame and scraper blade stir the mixture to the material in the reactor, the inside reaction condition can be observed through the manhole to the producer, inside the slurry after the reaction got into the second reactor from the discharge gate discharge after the reaction finishes. Can will wash water through first inlet when needs wash first reactor, inside sea brine advances pipe or second inlet entering reactor, start the agitator frame, realize the washing to reactor inside, wash the end mouth and pass through the drain and discharge the filth.
As shown in FIG. 3, the angle between the center line of the first reaction liquid inlet pipe 13 and the center line of the sea brine inlet pipe 14 is 16-22 degrees, the angle between the center line of the second reaction liquid inlet 15 and the center line of the first reaction liquid inlet pipe 13 is 160-175 degrees, and the pipe body of the first reaction liquid inlet pipe extending into the first reactor is provided with a 90-degree bend. The design is to ensure that the first reaction liquid and the sea brine firstly contact and react during feeding, and then react with the second reaction liquid, so that the smooth reaction after the three liquids are added is ensured.
As shown in fig. 4, the second reactor 5 comprises a barrel, a flow guide part 50 communicated with the inside of the barrel is arranged on one side of the upper part of the barrel, a first liquid inlet 500 is arranged at the bottom of the flow guide part 50, a second liquid inlet 51 is arranged on one side of the top of the barrel, a manhole 52 is arranged on one side of the lower part of the barrel, a discharge port 53 is arranged at the center of the bottom of the barrel, a sewage discharge outlet 54 is arranged on one side of the discharge port 53, a stirring frame 55 is arranged inside the barrel, the stirring frame 55 is driven by a motor 56, an arc-shaped scraper 550 is arranged at the bottom of the stirring frame 55; the bottom of the tub is provided with legs 57. Slurry after the reaction of the first reactor enters the second reactor from the first liquid inlet of the flow guide part along the pipeline, the pH is measured, then the rest second reaction liquid is added, and the slurry after the reaction is conveyed to the inside of the buffer tank from the discharge port through stirring and mixing of the stirring frame. In the reaction process, the staff can observe the reaction condition through the manhole, when wasing the second reactor, will wash water direct from first inlet add or the second inlet add can, start the agitator frame, wash reactor inside, the filth is discharged from row's thing mouth after wasing the end.
The water conservancy diversion portion 50 is the cuboid of carbon steel material, and the top of water conservancy diversion portion 50 is equipped with can dismantle top cap 501 (top cap and water conservancy diversion portion card solid coupling), and the inside of water conservancy diversion portion 50 is equipped with the pH meter. In practical application, the reaction condition can be conveniently observed by opening the top cover, and the pH value of materials in the reactor can be measured.
Wherein need to be explained is that the output shaft of the motor on the top cover upper portion of first reactor, second reactor and buffer tank even has the speed reducer, and the speed reducer passes through the shaft coupling and connects the stirring frame.
Example 2
A continuous production process combining magnesium ammonium phosphate and soda ash comprises the following steps:
(1) preparation of a first reaction solution: sequentially adding phosphoric acid (75-85 wt% of phosphoric acid), tap water, ammonium bicarbonate and a sodium hydroxide solution (the content of sodium hydroxide is 25-35 wt%) into a liquid storage tank according to the mass ratio of 2:3.2:1.15:1, controlling the reaction temperature to be 10-30 ℃, stirring and mixing, and reacting to obtain a first reaction liquid;
(2) preparation of a second reaction solution: sequentially adding deionized water and ammonia water into a liquid storage tank, and stirring and mixing to obtain a second reaction solution with the pH of 10-13;
(3) mixing and reacting: adding sea brine, the first reaction solution and the second reaction solution into the first reactor at the same time, and controlling PO in the reaction system4 3+:NH4 +：Mg2+The molar ratio of (1: 1.2: 1.1), adjusting the pH value to 4.5-6, carrying out 45min reaction, then conveying the reaction liquid to a second reactor, adjusting the pH value to 7.5, and carrying out 30-50min reaction to obtain the magnesium ammonium phosphate crystal slurry.
(4) Thickening, separating and drying treatment: conveying the magnesium ammonium phosphate crystal slurry into a thickener, separating the treated material in a centrifuge (adding deionized water for washing for 15-20min during centrifugal separation), and granulating, drying and packaging the centrifuged material to obtain a magnesium ammonium phosphate product; and conveying the clear liquid discharged by the thickener and the centrifuge to a salt melting barrel on a soda production line.
The entire process used the production equipment of example 1 for the preparation of magnesium ammonium phosphate, of which sea, to mention a few, is usedBrine (seawater), first reaction solution and second reaction solution according to 100m3The amount of/h, 1750kg/h and 2800kg/h enters the interior of the first reactor;
example 3
A continuous production process combining magnesium ammonium phosphate and soda ash comprises the following steps:
(1) preparation of a first reaction solution: sequentially adding phosphoric acid (75-85 wt% of phosphoric acid), tap water, ammonium bicarbonate and a sodium hydroxide solution (the content of sodium hydroxide is 25-35 wt%) into a liquid storage tank according to the mass ratio of 2.25:3.5:1.25:1, controlling the reaction temperature to be 10-30 ℃, stirring and mixing, and reacting to obtain a first reaction liquid;
(2) preparation of a second reaction solution: sequentially adding deionized water and ammonia water into a liquid storage tank, and stirring and mixing to obtain a second reaction solution with the pH of 10-13;
(3) mixing and reacting: adding sea brine, the first reaction solution and the second reaction solution into the first reactor at the same time, and controlling PO in the reaction system4 3+:NH4 +：Mg2+The molar ratio of the magnesium phosphate to the ammonium phosphate is 1:1.1-1.3:1.0-1.1, the pH value is adjusted to 4.5-6, the reaction liquid is conveyed to a second reactor after 30-60min of reaction, the pH value is adjusted to 7.5, and the magnesium phosphate ammonium crystal slurry is obtained after 30-50min of reaction.
(4) Thickening, separating and drying treatment: conveying the magnesium ammonium phosphate crystal slurry into a thickener, separating the treated material in a centrifuge (adding deionized water for washing for 15-20min during centrifugal separation), and granulating, drying and packaging the centrifuged material to obtain a magnesium ammonium phosphate product; and conveying clear liquid discharged by the thickener and the centrifuge to an alkali dissolving barrel on a soda production line.
The entire process used the production equipment of example 1 to prepare magnesium ammonium phosphate. Wherein the amount of the first reaction solution and the second reaction solution is 80m3The amounts of 1800kg/h and 2850kg/h were passed into the interior of the first reactor.
The magnesium ammonium phosphate products under the process conditions in examples 1 to 3 and the magnesium ammonium phosphate products under the existing process conditions (the process method in the background art) were tested, and the specific test results are shown in table 1.
TABLE 1
| Examples | Production cost | Purity in product | Production efficiency |
| Example 1 | 3000 | 99.9％ | 35 ton/day |
| Example 2 | 3400 | 99.5％ | 31 ton/day |
| Example 3 | 3200 | 99.2％ | 32 ton/day |
| Comparative example 1 | 4000 | 98.0％ | 5 ton/day |
As can be seen from the data in Table 1, compared with the existing process, the process of the present invention greatly improves the purity of the product, reduces the production cost and improves the production efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A continuous production process combining magnesium ammonium phosphate and soda ash is characterized by comprising the following steps:
(1) preparation of a first reaction solution: sequentially putting phosphoric acid, tap water, ammonium bicarbonate and sodium hydroxide solution into a liquid storage tank, stirring and mixing, and reacting to obtain a first reaction solution;
(2) preparation of a second reaction solution: sequentially adding deionized water and ammonia water into a liquid storage tank, and stirring and mixing to obtain a second reaction liquid;
(3) mixing and reacting: adding sea brine, a first reaction liquid and a second reaction liquid into a first reactor at the same time, adjusting the pH, carrying out a reaction for a period of time, conveying the reaction liquid to a second reactor, adjusting the pH, and carrying out a reaction for a period of time to obtain magnesium ammonium phosphate crystal slurry;
(4) thickening, separating and drying treatment: after thickening treatment of a thickener and separation treatment of a centrifuge, granulating, drying and packaging the magnesium ammonium phosphate crystal slurry to obtain a magnesium ammonium phosphate product; and conveying the clear liquid discharged by the thickener and the centrifuge to a salt melting barrel on a soda production line.
2. The continuous production process of combining magnesium ammonium phosphate and soda ash according to claim 1, characterized in that: in the step (1), phosphoric acid, deionized water, ammonium bicarbonate and sodium hydroxide solution are sequentially added into a liquid storage tank according to the mass ratio of 1.95-2.25:3.0-3.5:1.1-1.25:1, the reaction temperature is controlled at 10-30 ℃, wherein the phosphoric acid accounts for 75-85 wt% of the phosphoric acid, and the sodium hydroxide content in the sodium hydroxide solution is 25-35 wt%.
3. According toThe continuous production process of magnesium ammonium phosphate and sodium carbonate combined according to claim 1, which is characterized in that: when the mixing reaction in the step (3) is carried out, the pH value of the reaction system in the first reactor is controlled to be 4.5-6, the reaction time is 30-60min, and PO in the reaction system is controlled4 3+:NH4 +：Mg2+The molar ratio of (1: 1.1) - (1.3: 1.0) - (1.2); the pH value of the reaction system in the second reactor is 6.0-7.5, and the reaction time is 30-50 min.
4. The continuous production process of combining magnesium ammonium phosphate and soda ash according to claim 1, characterized in that: the first reactor comprises a barrel body, a first reaction liquid inlet pipe and a sea brine inlet pipe are arranged at the top of the barrel body, a second reaction liquid inlet is arranged on one side of the upper part of the barrel body, a manhole is arranged on one side of the lower part of the barrel body, a discharge hole is arranged in the center of the bottom of the barrel body, and a sewage discharge outlet is arranged on one side of the discharge hole; a stirring frame is arranged inside the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom of the stirring frame, and a plurality of sawteeth are arranged on the scraping plate; the bottom of the barrel body is provided with supporting legs.
5. The continuous production process of magnesium ammonium phosphate and soda ash combined according to claim 4, characterized in that: the included angle between the central line of the first reaction liquid inlet pipe and the central line of the sea brine inlet pipe is 16-22 degrees, the included angle between the central line of the second reaction liquid inlet pipe and the central line of the first reaction liquid inlet pipe is 160-175 degrees, and the pipe body of the first reaction liquid inlet pipe extending into the first reactor is provided with 90-degree bending.
6. The continuous production process of magnesium ammonium phosphate and soda ash combined according to claim 4, characterized in that: the shape of stirring frame is the font in, the stirring frame is including upper ledge and the lower frame of dismantling the connection.
7. The continuous production process of combining magnesium ammonium phosphate and soda ash according to claim 1, characterized in that: the second reactor comprises a barrel body, wherein a flow guide part communicated with the interior of the barrel body is arranged on one side of the upper part of the barrel body, a first liquid inlet is arranged at the bottom of the flow guide part, a second liquid inlet is arranged on one side of the top of the barrel body, a manhole is arranged on one side of the lower part of the barrel body, a discharge hole is arranged in the center of the bottom of the barrel body, a sewage discharge outlet is arranged on one side of the discharge hole, a stirring frame is arranged in the barrel body and driven by a motor, an arc-shaped scraping plate is arranged at the bottom of the stirring frame, and a plurality of saw; the bottom of the barrel body is provided with supporting legs.
8. The continuous production process of magnesium ammonium phosphate and soda ash combined according to claim 7, wherein: the water conservancy diversion portion is the cuboid of carbon steel material, the inner wall of water conservancy diversion portion is equipped with one deck glass steel layer, the top of water conservancy diversion portion is equipped with can dismantle the top cap, the inside of water conservancy diversion portion is equipped with the pH meter, just the central line of first inlet with the central line of second inlet is parallel to each other.
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