CN109956487A - Circulating ammonia coupling reaction is filtered, washed, drying system and method - Google Patents
Circulating ammonia coupling reaction is filtered, washed, drying system and method Download PDFInfo
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- CN109956487A CN109956487A CN201711410349.2A CN201711410349A CN109956487A CN 109956487 A CN109956487 A CN 109956487A CN 201711410349 A CN201711410349 A CN 201711410349A CN 109956487 A CN109956487 A CN 109956487A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/152—Preparation of hydrogels
- C01B33/1525—Preparation of hydrogels from or via fluosilicic acid or salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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Abstract
The invention discloses a kind of circulating ammonia coupling reaction, it is filtered, washed, drying system, including chemical reaction units and physical processing unit, physical processing unit includes Vacuum filtration device, filtrate collecting tank, cleaning solution holding tank, distillation water collecting groove, water stream injection pump, blower device, the first centrifugal pump, the second centrifugal pump, filtrate holding tank, Vacuum filtration device includes the suction filtration cylinder and filtrate collecting tank being arranged above and below, and the pipe branch come out from the second centrifugal pump is the first branch pipe, the second branch pipe and third branch pipe；Chemical reaction units include Leach reaction kettle, ammonia absorption kettle, third centrifugal pump, the 4th centrifugal pump and the second water stream injection pump；Ammonia absorption kettle is connected with suction filtration cylinder by pipeline, and the outlet of third branch pipe connects Leach reaction kettle, and the outlet of filtrate holding tank connects the 5th centrifugal pump by pipeline, and the outlet of the 5th centrifugal pump passes through pipeline and connects Leach reaction kettle.Also disclose the method for carrying out circulating ammonia coupling reaction using the system, being filtered, washed, being dried.
Description
Technical field
The present invention relates to the chemical reaction of chemical field and it is filtered, washed, drying device more particularly to a kind of circulating ammonia
Coupling reaction is filtered, washed, drying system and method.
Background technique
Biological medicine, Chemical Manufacture, mineral processing in product preparation process in, be filtered, washed, dry generally in difference
Equipment in carry out, material needs shifted in different equipment, not only cumbersome, equipment is more, take up a large area, and
Due to being system of opening wide, it is be easy to cause loss of material, leakage, cross contamination, a part volatilization noxious material deteriorates working condition.
Currently, existing filtering, dry, washing all-in-one machine device internal structure complexity, at high cost, maintenance is cumbersome, only uses
In food, pharmacy, fine chemical product production, batch is small, is difficult to make on a large scale in inorganic chemical industry, mineral processing and other fields
With.Meanwhile facility is required to additional washing water, is 3~4 times of filter material quality, not only increases water making device and process,
And more scrub raffinate is generated, and it needs concentration that could discharge, leads to that energy consumption is high, higher cost.
Ammonium salt, which leaches purification magnesium hydroxide, to be added using the oxidation magnesium mineral energy such as light-burning magnesium powder, light dolomite and ammonium salt
Heat or the lower reaction of decompression, obtain magnesium salts and ammonia, generate magnesium hydroxide at normal temperatures and pressures and ammonium salt, ammonium salt recycle.Ammonium
Salt leach purification calcium carbonate be using the calcium carbonates mineral such as lime stone, marble, calcite under heating or reduced pressure with
Ammonium salt reaction obtains calcium salt and ammonia, carbon dioxide, and backward reaction under low temperature retrieves calcium carbonate, and ammonium salt solution circulation makes
With.Ammonium fluoride, which leaches purification silica gel, to be reacted under heating or reduced pressure with ammonium fluoride using quartz mineral, and fluosilicic acid is obtained
Ammonium and ammonia, backward reaction generates silica gel under low temperature, and ammonium fluoride solution is recycled.Thus, it is possible to prepare purification magnesium hydroxide,
The products such as calcium carbonate, silica gel have selectivity by force, at low cost, the high advantage of product purity.
However, above-mentioned technique has following defects that 1) reaction unit leakproofness is poor at present, and ammonia volatility is strong, overflows meeting
Influence operating environment；2) material filtering that this method generates contains ammonia, waste discharge pollution in the washes generated in washing
Water body generates eutrophication；3) chemical precipitation products therefrom suspension fine size, filtration difficulty, easily blocking filtration openings, filters
It is difficult；4) it filters, washing, dry to be generally divided into several operating units, batch production not only forms ammonia volatilization, but also reduces production
Rate.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of circulating ammonia coupling of environmentally friendly, water-saving, continuous integration production
Conjunction reacts, is filtered, washed, drying system and method.
Technical scheme is as follows:
A kind of circulating ammonia coupling reaction is filtered, washed, drying system, including chemical reaction units and physical treatment list
Member, the physical processing unit include Vacuum filtration device, filtrate collecting tank, cleaning solution holding tank, distillation water collecting groove, water spray
Pump, blower device, the first centrifugal pump, the second centrifugal pump, filtrate holding tank are penetrated, the Vacuum filtration device includes upper and lower setting
Suction filtration cylinder and filtrate collecting tank, the blower device connect with filtrate collecting tank by pipeline, filtrate collecting tank and the filter
Liquid holding tank, the first centrifugal pump, suction filtration cylinder are in turn connected to form a circuit, filtrate collecting tank and the water injection by pipeline
Pump, distillation water collecting groove are sequentially connected by pipeline, and distillation water collecting groove also passes through pipeline successively with the second centrifugal pump, suction filtration cylinder
Connection, the filtrate holding tank are connect with filtrate collecting tank by pipeline, and the pipe branch come out from the second centrifugal pump is first
Branch pipe, the second branch pipe and third branch pipe, first branch pipe are connected to the second centrifugal pump and water stream injection pump, the second branch pipe connection
Second centrifugal pump is provided with the first valve, the second branch pipe on the pipeline between filtrate collecting tank and filtrate holding tank with suction filtration cylinder
On be provided with the second valve, distillation water collecting groove peripheral hardware is equipped with water-bath cooling housing；
The chemical reaction units include Leach reaction kettle, ammonia absorption kettle, third centrifugal pump, the 4th centrifugal pump and the second water
Jet pump, the Leach reaction kettle, third centrifugal pump, ammonia absorption kettle are sequentially connected by pipeline, Leach reaction kettle, the spray of the second water
Penetrate pump, ammonia absorption kettle is sequentially connected by pipeline, the 4th centrifugal pump passes through pipeline with ammonia absorption kettle and the second water stream injection pump respectively
Connection is so that three forms a circuit；
The ammonia absorption kettle is connected with suction filtration cylinder by pipeline, and the outlet of the third branch pipe connects Leach reaction kettle, institute
The outlet for stating filtrate holding tank connects the 5th centrifugal pump by pipeline, and the outlet of the 5th centrifugal pump is connected by pipeline leaches
Reaction kettle.
Preferably, the Vacuum filtration device is structure as a whole, and is provided with one in the middle part of the main body of Vacuum filtration device
Main body is divided into the suction filtration cylinder and underlying filtrate collecting tank being located above, the leakproofness of Vacuum filtration device by block filter plate
Good, suction filtration effect is good, and structure is simple, easily fabricated.
Preferably, it is provided with heating water bath housing outside the filtrate collecting tank and Leach reaction kettle, it can be to filter
Liquid collecting tank is heated, and the moisture in filtrate collecting tank is evaporated.Pressure gauge, thermometer are provided on Leach reaction kettle
Pressure, the temperature in reaction kettle can be monitored with exhaust valve, guarantee being normally carried out for chemical reaction.
Preferably, it is provided with agitating device in the suction filtration cylinder, filters and is provided with the first blow-off valve on cylinder, filters cylinder
It is additionally provided with heating water bath housing outside, makes material washing effect more preferable with heating water bath, the material after having handled can be direct
It is discharged to obtain from the first blow-off valve.
Preferably, it is provided with pressure gauge and exhaust valve on the distillation water collecting groove, is set on the filtrate collecting tank
It is equipped with exhaust valve and the second blow-off valve, exhaust valve can help to adjust the air pressure in filtrate collecting tank, guarantee to filter effect.
Preferably, the pipeline between the Leach reaction kettle and third centrifugal pump is at Leach reaction kettle one end
Equipped with conical filter tip, it is equipped with filter cloth in filter tip, prevents the particulate matter in reaction kettle from entering pipeline and causes to block.
A kind of circulating ammonia coupling reaction, the method for being filtered, washed, drying, are carried out, including as follows using above-mentioned system
Step:
1) Leach reaction, ammonia absorb synchronous carry out: ammonium salt A and material B to be leached being added in Leach reaction kettle, inhales in ammonia
Corresponding salting liquid C after material B to be leached and ammonium salt A reaction is added in kettle is received, chemical reaction units are opened, carries out leaching and ammonia
Absorption operation, reaction are finished, and are opened ammonia absorption kettle and are filtered the valve between cylinder, the product D and ammonium salt A suspension in ammonia absorption kettle into
Enter to filter cylinder, close the valve, open third centrifugal pump, salting liquid C enters ammonia absorption kettle, opens the second centrifugal pump and third branch
Valve on pipe washs filter residue, and filtrate is pumped into ammonia absorption kettle, and deslagging closes slag notch；
2) Leach reaction, ammonia absorb and the dry synchronous progress of filtration washing: ammonium salt A are added in Leach reaction kettle and wait soak
Material B out, open chemical reaction units, carry out leach and ammonia absorption operation, meanwhile, open physical processing unit be filtered,
Washing, drying: a, transfer product D and ammonium salt A heat filtrate collecting tank, cooling distillation water collecting groove to cylinder is filtered；B, operation the
Two centrifugal pumps generate negative pressure in filtrate collecting tank, filter material to abundant filtering, convey ammonium salt A into filtrate holding tank, fortune
Row blower device separates filter plate with filter cake；C, the second centrifugal pump conveys distilled water washing material D, and heating filters cylinder, and discharge is dry
Material D after dry, shift filtrate collecting tank in cleaning solution into filtrate holding tank；It opens ammonia absorption kettle and filters the valve between cylinder
Door, product D and ammonium salt A suspension enter suction filtration cylinder, close the valve, open third centrifugal pump, and salting liquid C enters ammonia absorption
Kettle opens valve on the second centrifugal pump and third branch pipe, washs filter residue, and filtrate is pumped into ammonia absorption kettle, and deslagging closes slag notch；
3) Leach reaction, ammonia are absorbed carries out with the dry synchronous circulating of filtration washing: the 5th centrifugal pump is opened, by all ammonium salts
A filtrate is pumped into Leach reaction kettle, and material B to be leached is added, and opens chemical reaction units, carries out leaching and ammonia absorption operation,
Meanwhile opening physical processing unit and being filtered, wash, dry: a, transfer product D and ammonium salt A are received to cylinder, heating filtrate is filtered
Collect slot, cooling distillation water collecting groove；B, the second centrifugal pump is run, generates negative pressure in filtrate collecting tank, filters material to abundant
Filtering, the first centrifugal pump convey cleaning solution in cleaning solution holding tank and wash filter cake, and ammonium salt A runs air blast into filtrate holding tank
Device separates filter plate with filter cake；C, the second centrifugal pump conveys distilled water washing material D, and heating filters cylinder, after discharge is dry
Material D, shift filtrate collecting tank in cleaning solution into filtrate holding tank；It opens ammonia absorption kettle and filters the valve between cylinder, product D
And ammonium salt A suspension enters suction filtration cylinder, closes the valve, opens third centrifugal pump, salting liquid C enters ammonia absorption kettle, opens the
Valve on two centrifugal pumps and third branch pipe washs filter residue, and filtrate is pumped into ammonia absorption kettle, and deslagging closes slag notch；
4) step 3) is repeated, into next production cycle.
In the above scheme, when the ammonium salt A is ammonium sulfate, ammonium chloride, ammonium nitrate, leaching material B is light calcined magnesia
Raw material or limestone powder, when the ammonium salt A is ammonium fluoride, the material B to be leached is silica flour.
The principle of the invention includes following reaction formula:
One,
It prepares Mg (OH)2, in Leach reaction kettle, material (B) and ammonium salt solution (A) containing magnesia are in the case where heating reduced pressure
Reaction, is leached to obtain soluble magnesium salt (C) and ammonia:
MgO+2NH4 +=Mg2++2NH3↑+H2O
4th centrifugal pump pump liquid, the second water stream injection pump generate negative pressure close to Leach reaction kettle one end, and absorbing ammonia is so incensed that hydrogen
Magnesia (D)；
Mg2++2NH3+2H2O=Mg (OH)2+2NH4 +
It carries out, is accumulated without ammonia, present apparatus sealing is good simultaneously due to leaching magnesia (B) and generating magnesium hydroxide (D)
It is good, ammonia spilling will not be generated.
Two,
Prepare CaCO3, in Leach reaction kettle, the material and ammonium salt solution (A) of calcium carbonate (B) in the case where heat reduced pressure instead
It answers, is leached to obtain soluble calcium salt (C), ammonia and carbon dioxide gas:
CaCO3+2NH4 +=Ca2++2NH3↑+H2O+CO2↑
4th centrifugal pump pump liquid, the second water stream injection pump generate negative pressure close to Leach reaction kettle one end, absorb ammonia and dioxy
Change carbon and obtains calcium carbonate (D)；
Ca2++2NH3+H2O+CO2=CaCO3↓+2NH4 +
It carries out, is accumulated without ammonia, present apparatus good seal simultaneously due to leaching calcium carbonate (B) and generating calcium carbonate (D),
Ammonia spilling will not be generated.
Three,
Prepare silica gel SiO2·nH2O, in Leach reaction kettle, silica containing material (B) is adding with ammonium fluoride solution (A)
It is reacted under hot reduced pressure, is leached to obtain ammonium fluosilicate (C) and ammonia:
SiO2+6NH4F=(NH4)2SiF6+4NH3↑+2H2O
4th centrifugal pump pump liquid, the second water stream injection pump generate negative pressure close to Leach reaction kettle one end, and absorbing ammonia is so incensed that silicon
Glue SiO2·nH2O(D)；
(NH4)2SiF6+4NH3+(n+2)H2O=SiO2·nH2O↓+6NH4F
It carries out, is accumulated without ammonia, present apparatus good seal simultaneously due to leaching silica (B) and generating silica gel (D),
Ammonia spilling will not be generated.
The beneficial effects of the present invention are: 1) can be formed inside the device of connection circulation it is closed circuit, solve ammonia overflow generate
The problem of pollution；2) washing pure water is self-sufficient in being filtered, washed, drying, and not only simplifies water generator, but also avoids generating newly
Ammonia stripping waste water；3) mineral are leached, product is prepared, are filtered, washing, drying can be carried out simultaneously, is able to achieve from raw material to product
It directly converts, is not only convenient for continuous production, but also can be shortened time raising productivity；4) a variety of reactions can be applicable in, production is flexible, this
The problem of outer to solve magnesium hydroxide, silica-gel materials filtering stickiness is strong, blocks filter opening.
Portion recycles including the washing water energy of physical processing unit of the invention, without multiple additional washing water, generates washing
Waste water is few, while having the function of dried material, be suitable for temperature-sensitive, stickiness, slurry containing volatile matter, with simple structure, it is water-saving,
The advantages of energy-saving and environmental protection；It is filtered, washs, is dried, working efficiency respectively without moving on to material in distinct device
High, pollution is less, at low cost.
Detailed description of the invention
Fig. 1 is circulating ammonia coupling reaction of the invention, is filtered, washed, the structural schematic diagram of drying system.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples:
Embodiment 1 constructs circulating ammonia coupling reaction, is filtered, washed, drying system
A kind of building circulating ammonia coupling reaction as shown in Figure 1 is filtered, washed, drying system, mainly by chemically reacting
Unit and physical processing unit composition.
Physical processing unit include Vacuum filtration device, filtrate collecting tank 2, cleaning solution holding tank 3, distillation water collecting groove 4,
First water stream injection pump 5, blower device 6, the first centrifugal pump 7, the second centrifugal pump 8, filtrate holding tank 15.Vacuum filtration device includes
The suction filtration cylinder 1 and filtrate collecting tank 2 being arranged above and below, Vacuum filtration device is structure as a whole, in the middle part of the main body of Vacuum filtration device
It is provided with one piece of filter plate 1a and main body is divided into the suction filtration cylinder 1 and underlying filtrate collecting tank 2 being located above.Filtrate collecting tank
It is provided with exhaust valve on 2, distills and is provided with pressure gauge and exhaust valve on water collecting groove 4.
It filters and is provided with agitating device in cylinder 1, filter and be provided with the first blow-off valve 1c on cylinder 1, filter and be additionally provided with outside cylinder 1
Heating water bath housing.Blower device 6 is connect with filtrate collecting tank 2 by pipeline, filtrate collecting tank 2 and cleaning solution holding tank 3, the
One centrifugal pump 7, suction filtration cylinder 1 are in turn connected to form a circuit, filtrate collecting tank 2 and the first water stream injection pump 5, distillation by pipeline
Water collecting groove 4 is sequentially connected by pipeline, and distillation water collecting groove 4 is also successively connected with the second centrifugal pump 8, suction filtration cylinder 1 by pipeline
It connects, filtrate holding tank 15 is connect with filtrate collecting tank 2 by pipeline, and the pipe branch come out from the second centrifugal pump 8 is first
Pipe 9, the second branch pipe 10 and third branch pipe 21, the first branch pipe 9 are connected to the second centrifugal pump 8 and the first water stream injection pump 5, the second branch pipe 10
It is connected to the second centrifugal pump 8 and filters cylinder 1, be provided with the first valve on the pipeline between filtrate collecting tank 2 and cleaning solution holding tank 3
, it is provided with the second valve on the second branch pipe 10, is provided with water-bath cooling housing outside distillation water collecting groove 4.
Chemical reaction units include Leach reaction kettle 16, ammonia absorption kettle 17, third centrifugal pump 18, the 4th centrifugal pump 19 and
Two water stream injection pumps 20, Leach reaction kettle 16, third centrifugal pump 18, ammonia absorption kettle 17 are sequentially connected by pipeline, Leach reaction kettle
16, the second water stream injection pump 20, ammonia absorption kettle 17 are sequentially connected by pipeline, the 4th centrifugal pump 19 respectively with ammonia absorption kettle 17 and
Two water stream injection pumps 20 are connected by pipeline so that three forms a circuit.Between Leach reaction kettle 16 and third centrifugal pump 18
Pipeline is being equipped with conical filter tip at 16 one end of Leach reaction kettle, is equipped with filter cloth in filter tip.Filtrate collecting tank 2 and leaching are anti-
It answers and is provided with heating water bath housing outside kettle 16, pressure gauge, thermometer and exhaust valve are provided on Leach reaction kettle 16.
The connection relationship of chemical reaction units and physical processing unit are as follows: ammonia absorption kettle 17 and suction filtration cylinder 1 pass through pipeline and connect
It connects, the outlet of third branch pipe 21 connects Leach reaction kettle 16, and the outlet of filtrate holding tank 15 connects the 5th centrifugal pump by pipeline
22, the outlet of the 5th centrifugal pump 22 connects Leach reaction kettle 16 by pipeline.
Embodiment 2 using circulating ammonia coupling reaction, be filtered, washed, drying system prepares magnesium hydroxide
Magnesium hydroxide is prepared using the system that embodiment 1 constructs, is operated in accordance with the following steps:
Leach reaction, ammonia absorb synchronous carry out: distilled water being added in distillation water collecting groove 4, adds in Leach reaction kettle 16
Enter ammonium sulfate and light calcined magnesia raw material, Adlerika is added in ammonia absorption kettle 17, heats Leach reaction kettle 16, open
It opens the 4th centrifugal pump 19, ammonium sulfate and magnesia to react under negative pressure heating condition, obtains ammonia and magnesium sulfate suspension, ammonia
It is reacted into ammonia absorption kettle 17 with magnesium sulfate, obtains magnesium hydroxide and ammonium sulfate suspension, open ammonia absorption kettle 17 and filter cylinder 1
Between valve, magnesium hydroxide and ammonium sulphate suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump 18, magnesium sulfate
Solution enters ammonia absorption kettle 17, opens valve on the second centrifugal pump 8 and third branch pipe 21, washs filter residue, and filtrate is pumped into ammonia absorption
Kettle 17, deslagging close slag notch.
2) Leach reaction, ammonia absorb and the dry synchronous progress of filtration washing: in Leach reaction kettle 16 addition ammonium sulfate and
Light calcined magnesia raw material heats Leach reaction kettle 16, opens the 4th centrifugal pump 19, ammonium sulfate and magnesia are in negative pressure heating condition
Lower reaction obtains ammonia and Adlerika, and ammonia enters ammonia absorption kettle 17 and reacts with magnesium sulfate, obtains magnesium hydroxide and sulfuric acid
Ammonium suspension.Meanwhile the second centrifugal pump 8 is opened, it filters cylinder 1 and stirs, the gas in filtrate collecting tank 2 enters distillation water collecting groove
4, the suspension in cylinder 1 is filtered since pressure difference filters on filter plate 1a, and filtrate enters filtrate collecting tank 2, in negative pressure heating condition
The evaporation of lower portion filtrate forms vapor and condenses in distillation water collecting groove 4 and collects, and filtering finishes, open filtrate collecting tank 2 with
Valve between filtrate holding tank 15, filtrate enter filtrate holding tank 15, and from blower device 6, into filtrate collecting tank 2, air blast increases
Pressure, magnesium hydroxide filter cake and filter plate 1a separation, open the valve on the second centrifugal pump 8 and the second branch pipe 10, are washed with distilled water
Filter cake, the magnesium hydroxide filtering after opening the valve washing on the second centrifugal pump 8 and the first branch pipe 9, it is dry that heating filters 1 negative pressure of cylinder
Dry filter cake, stirring filter the magnesium hydroxide filter cake after the discharge drying of cylinder 1, open between filtrate collecting tank 2 and cleaning solution holding tank 3
Valve, cleaning solution enters cleaning solution holding tank 3, opens ammonia absorption kettle 17 and filter the valve between cylinder 1, magnesium hydroxide and sulfuric acid
Ammonium suspension, which enters, filters cylinder 1, closes the valve, opens third centrifugal pump 18, and Adlerika enters ammonia absorption kettle 17, opens
Valve on second centrifugal pump 8 and third branch pipe 21 washs filter residue, and filtrate is pumped into ammonia absorption kettle 17, and deslagging closes slag notch.
3) Leach reaction, ammonia are absorbed with the dry synchronous progress of filtration washing: the 5th centrifugal pump 22 are opened, by all ammonium sulfate
Filtrate is pumped into Leach reaction kettle 16, and light calcined magnesia raw material is added, and heats Leach reaction kettle 16, opens the 4th centrifugal pump 19,
Ammonium sulfate and magnesia react under negative pressure heating condition, obtain ammonia and Adlerika, ammonia enter ammonia absorption kettle 17 with
Magnesium sulfate reaction, obtains magnesium hydroxide and ammonium sulfate suspension.Meanwhile the second centrifugal pump 8 is opened, it filters cylinder 1 and stirs, filtrate is received
Gas in collection slot 2 enters distillation water collecting groove 4, filters the suspension in cylinder 1 and is filtered on filter plate 1a due to pressure difference, filtrate into
Enter filtrate collecting tank 2, portion filtrate evaporates under negative pressure heating condition, forms vapor and condenses receipts in distillation water collecting groove 4
Collection, filtering finishes, and opens the first centrifugal pump 7, wash filter cake with cleaning solution, open filtrate collecting tank 2 and filtrate holding tank 15 it
Between valve, filtrate enters filtrate holding tank 15, and from blower device 6, into filtrate collecting tank 2, air blast is pressurized, magnesium hydroxide filter cake
It is separated with filter plate 1a, opens the valve on the second centrifugal pump 8 and the second branch pipe 10, wash filter cake again with distilled water, open the
The magnesium hydroxide filtering after valve washing on two centrifugal pumps 8 and the first branch pipe 9, heating filter 1 negative pressure drying filter cake of cylinder, stirring
Magnesium hydroxide filter cake after filtering the discharge drying of cylinder 1, opens the valve between filtrate collecting tank 2 and cleaning solution holding tank 3, washing
Liquid enters cleaning solution holding tank 3, open ammonia absorption kettle 17 and filter the valve between cylinder 1, magnesium hydroxide and ammonium sulphate suspension into
Enter to filter cylinder 1, close the valve, open third centrifugal pump 18, Adlerika enters ammonia absorption kettle 17, opens the second centrifugal pump
8 and third branch pipe 21 on valve, wash filter residue, filtrate is pumped into ammonia absorption kettle 17, deslagging, closes slag notch.
4) step 3) is repeated, into next production cycle.
Embodiment 3 using circulating ammonia coupling reaction, be filtered, washed, drying system prepares calcium carbonate
Calcium carbonate is prepared using the system that embodiment 1 constructs, is operated in accordance with the following steps:
1) Leach reaction, ammonia absorb synchronous carry out: ammonium chloride and agstone powder stock are added in Leach reaction kettle 16,
Calcium chloride solution is added in ammonia absorption kettle 17, implements to leach and ammonia absorbs, reaction is finished, and is opened ammonia absorption kettle 17 and is filtered cylinder 1
Between valve, calcium carbonate and ammonium chloride suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump 18, calcium chloride is molten
Liquid enters ammonia absorption kettle 17, opens valve on the second centrifugal pump 8 and third branch pipe 21, washs filter residue, and filtrate is pumped into ammonia absorption kettle
17, deslagging closes slag notch.
2) Leach reaction, ammonia absorb and the dry synchronous progress of filtration washing: in Leach reaction kettle 16 addition ammonium chloride and
Agstone powder stock is implemented to leach and ammonia absorbs, meanwhile, it is filtered, washs, drying process referring to 1 step 2) of embodiment,
Dry calcium carbonate is obtained in filtering cylinder 1, discharge obtains ammonium chloride filtrate in filtrate holding tank 15.Open ammonia absorption kettle
Valve between 17 and suction filtration cylinder 1, calcium carbonate and ammonium chloride suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump
18, calcium chloride solution enters ammonia absorption kettle 17, opens valve on the second centrifugal pump 8 and third branch pipe 21, washs filter residue, filtrate pump
Enter ammonia absorption kettle 17, deslagging closes slag notch.
3) Leach reaction, ammonia are absorbed with the dry synchronous progress of filtration washing: the 5th centrifugal pump 22 are opened, by all ammonium chlorides
Filtrate is pumped into Leach reaction kettle 16, and agstone powder stock is added, and implements leaching and ammonia absorption operation, meanwhile, referring to implementation
1 step 3) of example is filtered, washs, drying process, obtains dry calcium carbonate in filtering cylinder 1, and discharge obtains ammonium chloride filter
Liquid obtains cleaning solution in cleaning solution holding tank 3 in filtrate holding tank 15, opens ammonia absorption kettle 17 and filters the valve between cylinder 1
Door, calcium carbonate and ammonium chloride suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump 18, and calcium chloride solution enters
Ammonia absorption kettle 17 opens the second centrifugal pump 8 and third branch pipe 21) on valve, wash filter residue, filtrate is pumped into ammonia absorption kettle 17, arranges
Slag closes slag notch.
4) step 3) is repeated, into next production cycle.
Embodiment 4 using circulating ammonia coupling reaction, be filtered, washed, drying system prepares silica gel
Silica gel is prepared using the system that embodiment 1 constructs, is operated in accordance with the following steps:
1) Leach reaction, ammonia absorb synchronous carry out: ammonium fluoride and quartz powder raw material are added in Leach reaction kettle 16,
Ammonium fluosilicate solution is added in ammonia absorption kettle 17, implements to leach and ammonia absorption operation, reaction is finished, open ammonia absorption kettle 17 and filter
Valve between cylinder 1, silica gel and ammonium fluoride suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump 18, fluosilicic acid
Ammonium salt solution enters ammonia absorption kettle 17, opens valve on the second centrifugal pump 8 and third branch pipe 21, washs filter residue, and filtrate is pumped into ammonia suction
Kettle 17 is received, deslagging closes slag notch.
2) Leach reaction, ammonia absorb and the dry synchronous progress of filtration washing: in Leach reaction kettle 16 addition ammonium fluoride and
Quartz powder raw material implements leaching and ammonia absorption operation, meanwhile, it is filtered referring to 1 step 2) of embodiment, washs, dries behaviour
Make, obtains dry silica gel in filtering cylinder 1, discharge obtains ammonium fluoride filtrate in filtrate holding tank 15.Open ammonia absorption kettle
Valve between 17 and suction filtration cylinder 1, silica gel and ammonium fluoride suspension, which enter, filters cylinder 1, closes the valve, opens third centrifugal pump
18, ammonium fluosilicate solution enters ammonia absorption kettle 17, opens valve on the second centrifugal pump 8 and third branch pipe 21, washs filter residue, filtrate
It is pumped into ammonia absorption kettle 17, deslagging closes slag notch.
3) Leach reaction, ammonia are absorbed with the dry synchronous progress of filtration washing: Leach reaction, ammonia absorb dry with filtration washing
It is synchronous to carry out: to open the 5th centrifugal pump 22, all ammonium fluoride filtrates are pumped into Leach reaction kettle 16, it is former that quartz powder is added
Material implements leaching and ammonia absorption operation unit, meanwhile, it is filtered, washs, drying process referring to 1 step 3) of embodiment, obtain
In filtering cylinder 1, discharge obtains ammonium fluoride filtrate in filtrate holding tank 15, obtains cleaning solution in cleaning solution dry silica gel
It in holding tank 3, opens ammonia absorption kettle 17 and filters the valve between cylinder 1, silica gel and ammonium fluoride suspension, which enter, filters cylinder 1, closes
The valve opens third centrifugal pump 18, and ammonium fluosilicate solution enters ammonia absorption kettle 17, opens the second centrifugal pump 8 and third branch pipe
21) valve on washs filter residue, and filtrate is pumped into ammonia absorption kettle 17, and deslagging closes slag notch.
4) step 3) is repeated, into next production cycle.
5 product testing of embodiment
Product obtained by embodiment 2-4 is detected, testing result difference is as shown in table 1-3.As shown in Table 1, hydrogen-oxygen
It is high to change magnesium product purity, moisture content is low, stable yield；As shown in Table 2, calcium carbonate product purity is high, moisture content is low, and yield is steady
It is fixed；As shown in Table 3, silica gel product stable yield, silica dry product content and scorching hot decrement can be up to standard.
1 embodiment of table, 2 light-burning magnesium powder extracts magnesium hydroxide operating parameter and resulting information
2 embodiment of table, 3 limestone powder extracts calcium carbonate operating parameter and resulting information
3 embodiment of table, 4 quartz powder extracts silica gel operating parameter and resulting information
Claims (8)
1. a kind of circulating ammonia coupling reaction is filtered, washed, drying system, it is characterised in that: including chemical reaction units and object
Processing unit is managed, the physical processing unit includes Vacuum filtration device, filtrate collecting tank (2), cleaning solution holding tank (3), steams
Distilled water collecting tank (4), the first water stream injection pump (5), blower device (6), the first centrifugal pump (7), the second centrifugal pump (8), filtrate are deposited
Storage tank (15), the Vacuum filtration device include the suction filtration cylinder (1) and filtrate collecting tank (2) being arranged above and below, the blower device
(6) it is connect with filtrate collecting tank (2) by pipeline, filtrate collecting tank (2) and the cleaning solution holding tank (3), the first centrifugal pump
(7), it filters cylinder (1) and a circuit is in turn connected to form by pipeline, filtrate collecting tank (2) and first water stream injection pump (5),
Distillation water collecting groove (4) is sequentially connected by pipeline, and distillation water collecting groove (4) is also logical with the second centrifugal pump (8), suction filtration cylinder (1)
Piping is sequentially connected, and the filtrate holding tank (15) is connect with filtrate collecting tank (2) by pipeline, from the second centrifugal pump (8)
Pipe branch out is the first branch pipe (9), the second branch pipe (10) and third branch pipe (21), and first branch pipe (9) is connected to the
Two centrifugal pumps (8) and the first water stream injection pump (5), the second branch pipe (10) connection the second centrifugal pump (8) and suction filtration cylinder (1), filter
It is provided with the first valve on pipeline between liquid collecting tank (2) and cleaning solution holding tank (3), is provided on the second branch pipe (10)
Two valves, distillation water collecting groove (4) are provided with water-bath cooling housing outside；
The chemical reaction units include Leach reaction kettle (16), ammonia absorption kettle (17), third centrifugal pump (18), the 4th centrifugal pump
(19) and the second water stream injection pump (20), the Leach reaction kettle (16), third centrifugal pump (18), ammonia absorption kettle (17) pass through pipeline
Be sequentially connected, Leach reaction kettle (16), the second water stream injection pump (20), ammonia absorption kettle (17) are sequentially connected by pipeline, the 4th from
Heart pump (19) is connect with ammonia absorption kettle (17) and the second water stream injection pump (20) by pipeline respectively so that three forms a circuit；
The ammonia absorption kettle (17) is connected with suction filtration cylinder (1) by pipeline, and the outlet connection of the third branch pipe (21) is leached anti-
It answers kettle (16), the outlet of the filtrate holding tank (15) connects the 5th centrifugal pump (22), the 5th centrifugal pump by pipeline
(22) outlet connects Leach reaction kettle (16) by pipeline.
2. circulating ammonia coupling reaction as described in claim 1 is filtered, washed, drying system, it is characterised in that: described true
Empty Suction filtration device is structure as a whole, and is provided with one piece of filter plate (1a) in the middle part of the main body of Vacuum filtration device and main body is divided into positioned at upper
The suction filtration cylinder (1) and underlying filtrate collecting tank (2) of side.
3. circulating ammonia coupling reaction as described in claim 1 is filtered, washed, drying system, it is characterised in that: the filter
It is provided with heating water bath housing outside liquid collecting tank (2) and Leach reaction kettle (16), Leach reaction kettle is provided with pressure on (16)
Table, thermometer and exhaust valve.
4. circulating ammonia coupling reaction as described in claim 1 is filtered, washed, drying system, it is characterised in that: the pumping
It is provided with agitating device in filter cylinder (1), filters and is provided with the first blow-off valve (1c) on cylinder (1), filters and is additionally provided with water outside cylinder (1)
Bathe heating jacket.
5. circulating ammonia coupling reaction as described in claim 1 is filtered, washed, drying system, it is characterised in that: the steaming
It is provided with pressure gauge and exhaust valve on distilled water collecting tank (4), is provided with exhaust valve on the filtrate collecting tank (2).
6. circulating ammonia coupling reaction as described in claim 1 is filtered, washed, drying system, it is characterised in that: the leaching
The pipeline between reaction kettle (16) and third centrifugal pump (18) is being equipped with cone filter at Leach reaction kettle (16) one end out
Mouth, filter tip is interior to be equipped with filter cloth.
7. a kind of circulating ammonia coupling reaction, the method for being filtered, washed, drying, it is characterised in that: use claim 1 to 6 times
System described in one carries out, and includes the following steps:
1) Leach reaction, ammonia absorb synchronous carry out: ammonium salt A and material B to be leached being added in Leach reaction kettle (16), inhales in ammonia
It receives and material B to be leached and corresponding salting liquid C after ammonium salt A reaction is added in kettle (17), open chemical reaction units, leached
And ammonia absorption operation, reaction are finished, and are opened ammonia absorption kettle (17) and are filtered the valve between cylinder (1), the product D in ammonia absorption kettle (17)
And ammonium salt A suspension enters suction filtration cylinder (1), closes the valve, opens third centrifugal pump (18), salting liquid C enters ammonia absorption kettle
(17), valve on the second centrifugal pump (8) and third branch pipe (21) is opened, filter residue is washed, filtrate is pumped into ammonia absorption kettle (17), arranges
Slag closes slag notch；
2) Leach reaction, ammonia absorb and the dry synchronous progress of filtration washing: ammonium salt A are added in Leach reaction kettle (16) and wait soak
Material B out, open chemical reaction units, carry out leach and ammonia absorption operation, meanwhile, open physical processing unit be filtered,
Washing, drying: a, transfer product D and ammonium salt A are heated filtrate collecting tank (2) to filtering cylinder (1), cooling distillation water collecting groove
(4)；B, the second centrifugal pump (8) are run, negative pressure is generated in filtrate collecting tank (2), filtered material to abundant filtering, convey ammonium salt
For A into filtrate holding tank (15), operation blower device (6) separates filter plate with filter cake；C, the second centrifugal pump (8) conveys distilled water
Washing material D, heating filter cylinder (1), the material D after discharge is dry, and cleaning solution to filtrate stores in transfer filtrate collecting tank (2)
In slot (15)；It opening ammonia absorption kettle (17) and filters the valve between cylinder (1), product D and ammonium salt A suspension, which enter, filters cylinder (1),
The valve is closed, is opened third centrifugal pump (18), salting liquid C enters ammonia absorption kettle (17), opens the second centrifugal pump (8) and third
Valve on branch pipe (21) washs filter residue, and filtrate is pumped into ammonia absorption kettle (17), deslagging, closes slag notch；
3) Leach reaction, ammonia are absorbed carries out with the dry synchronous circulating of filtration washing: the 5th centrifugal pump (22) is opened, by all ammonium salts
A filtrate is pumped into Leach reaction kettle (16), and material B to be leached is added, and opens chemical reaction units, leach and ammonia absorbs behaviour
Make, meanwhile, open physical processing unit and be filtered, wash, dry: a, transfer product D and ammonium salt A are heated to filtering cylinder (1)
Filtrate collecting tank (2), cooling distillation water collecting groove (4)；B, the second centrifugal pump (8) are run, is generated in filtrate collecting tank (2) negative
Pressure filters material to abundant filtering, and the first centrifugal pump (7) conveys cleaning solution in cleaning solution holding tank (3) and washs filter cake, conveys ammonium
For salt A into filtrate holding tank (15), operation blower device (6) separates filter plate with filter cake；C, the second centrifugal pump (8) conveying distillation
Water washing material D, heating filter cylinder (1), the material D after discharge is dry, and cleaning solution to filtrate is deposited in transfer filtrate collecting tank (2)
In storage tank (15)；It opens ammonia absorption kettle (17) and filters the valve between cylinder (1), product D and ammonium salt A suspension enter suction filtration cylinder
(1), close the valve, open third centrifugal pump (18), salting liquid C enters ammonia absorption kettle (17), open the second centrifugal pump (8) and
Valve on third branch pipe (21) washs filter residue, and filtrate is pumped into ammonia absorption kettle (17), deslagging, closes slag notch；
4) step 3) is repeated, into next production cycle.
8. circulating ammonia coupling reaction as claimed in claim 7, the method for being filtered, washed, drying, it is characterised in that: described
Ammonium salt A includes ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium fluoride, and the material B to be leached is light calcined magnesia raw material or lime
Mountain flour powder stock or silica flour.
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| CN110615458A (en) * | 2019-10-08 | 2019-12-27 | 张旭 | Device and process for preparing high-purity calcium carbonate |
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Application publication date: 20190702 |