CN110342558A - Prepare the device and technique of high-purity calcium carbonate - Google Patents
Prepare the device and technique of high-purity calcium carbonate Download PDFInfo
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- CN110342558A CN110342558A CN201910755834.6A CN201910755834A CN110342558A CN 110342558 A CN110342558 A CN 110342558A CN 201910755834 A CN201910755834 A CN 201910755834A CN 110342558 A CN110342558 A CN 110342558A
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- 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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Abstract
The invention discloses a kind of devices for preparing high-purity calcium carbonate, including carburizing reagent slot, distillation water collecting groove, Calcium Carbonate Filtration slot, leached mud lautertuns, the first centrifugal pump, the second centrifugal pump, water stream injection pump, carbon dioxide access port end；Carburizing reagent slot, Calcium Carbonate Filtration slot, first centrifugal pump constitutes closed circuit by pipeline, distill water collecting groove, second centrifugal pump, water stream injection pump constitutes closed circuit, Calcium Carbonate Filtration slot, it is identical that leached mud filters slot structure, it is respectively positioned on right above carburizing reagent slot, it is connected in parallel the first centrifugal pump liquid outlet above, it is connected in parallel a branch of the second centrifugal pump liquid outlet above, the gas access end of water stream injection pump is connected in parallel in side, carburizing reagent slot is connected in bottom, water stream injection pump fluid inlet end connects another of the second outlet of centrifugal pump end branch, distillation water collecting groove immediately below the connection of gas-liquid mixture outlet end, carbon dioxide access port end is connected to carburizing reagent slot top.
Description
Technical field
The invention belongs to chemical machinery fields, and in particular to calcium oxide or the dress of calcium hydroxide preparation purity calcium carbonate
It sets and circulation producing method.
Background technique
Precipitated calcium carbonate is as good pigment and filler, in fields such as plastics, papermaking, rubber, coating, ink, daily use chemicals
It is widely used.Purity, whiteness, the important indicator that granularity is precipitated calcium carbonate, determine the performances such as its dispersibility, oil absorption and application
Field, and high-purity, fine-graded precipitated calcium carbonate are the development trends of industry.
The method for preparing precipitated calcium carbonate is usually to obtain with calcium oxide being main by high-temperature calcinations such as lime stone, calcites
The quick lime of ingredient adds water digestion, is passed through carbon dioxide carbonization, is filtered, is dried to obtain target product, this method technique letter
List, yield are big, at low cost, but entrainment is difficult to the impurity such as iron oxide, the aluminium oxide removed in product, reduce purity and whiteness, produce
Product are lacked competitiveness.
On the other hand, calcium carbide industry a large amount of carbide slags of by-product in production acetylene gas, wherein calcium hydroxide content is reachable
80~90%, the annual carbide slag yield in China is up to 20,000,000 tons or more according to statistics.Carbide slag is in strong basicity, can be used for manufacturing water
Mud, flue gas desulfurization etc., but since carbide slag production capacity is huge, utilization rate is still difficult to more than 30%, most of by after Anti-seeping technology
Landfill causes mineral resources waste and land resource waste.
It using calcined calcium oxide as raw material, is leached with ammonium salt, is filtered to remove insoluble impurities, then be carbonized to obtain carbonic acid
Calcium, ammonium salt reclamation utilize, have been reported (Chen Jiming's round-robin method is prepared high-purity calcium carbonate superfine [J], mineral products comprehensive utilization,
2004,2:15-17,US9725330).This method product purity is high, and meets the green production principle that feedstock circulation utilizes, but
It is generated in production process with ammonium hydroxide, it is right in calcium carbonate, being filtered, washed of leached mud solid, volatile spilling in drying process
Production environment and ecological environment generate adverse effect, meanwhile, need ammonia still, storage the huge of ammonia to set in usual production technology
Standby, investment is big, takes up a large area.
Summary of the invention
The present invention is directed to the above technological deficiency and not perfect place, provides the device and application method for preparing calcium carbonate,
Both it can guarantee that ammonia sealed, and prevented volatilization pollution air, while guaranteeing to prepare fine grain purity calcium carbonate, purposes prospect is wide
It is general.
Technical solution used for the above purpose is:
A kind of device preparing high-purity calcium carbonate, it is characterised in that comprise the following structure: carburizing reagent slot, distilled water are collected
Slot, Calcium Carbonate Filtration slot, leached mud lautertuns, the first centrifugal pump, the second centrifugal pump, water stream injection pump, carbon dioxide access port end；
The carburizing reagent slot, Calcium Carbonate Filtration slot, the first centrifugal pump constitute closed circuit by pipeline；The distillation water collecting groove,
Second centrifugal pump, water stream injection pump constitute closed circuit；The Calcium Carbonate Filtration slot, leached mud filtering slot structure are identical, are respectively positioned on
Right above carburizing reagent slot, the first centrifugal pump liquid outlet is respectively connected above, respectively connects the second centrifugal pump above
One branch of liquid outlet, respectively connects the gas access end of water stream injection pump in side, and it is anti-respectively to connect carbonization in bottom
Answer slot；The water stream injection pump fluid inlet end connects another branch at the second outlet of centrifugal pump end, gas-liquid mixture outlet end
Distillation water collecting groove immediately below connecting；Carbon dioxide access port end is connected to carburizing reagent slot top；Described first from
Valve a, the pipeline between the first centrifugal pump and leached mud lautertuns are installed on the pipeline between heart pump and Calcium Carbonate Filtration slot
On valve c is installed；Valve b, the second centrifugal pump are installed on the pipeline between second centrifugal pump and Calcium Carbonate Filtration slot
Valve d is installed on the pipeline between leached mud lautertuns, is equipped on the pipeline between the second centrifugal pump and water stream injection pump
Valve g；Valve e, water stream injection pump and leached mud filtering are installed on the pipeline between the water stream injection pump and Calcium Carbonate Filtration slot
Valve f is installed on the pipeline between slot.
In the above-mentioned technical solutions, Calcium Carbonate Filtration slot and leached mud lautertuns comprise the following structure: filter cake cylinder, filtrate
Cylinder vacuumizes gas outlet end, and solid-liquid arrival end, filtrate (liquid end, dry cake outlet end, mistake are leached in washing water inlet end
Filter plate, agitating device；Filter cake cylinder is separated right above filtrate cylinder with filter plate；The outlet end is located at the side of filtrate canister portion position
Face top, washing water inlet end, leaching solid-liquid arrival end are located at the top of filter cake cylinder, and filtrate (liquid end is located at filtrate cylinder bottom, out
Mouth end is located at filter cake cylinder side lower, and agitating device is located among filter cake cylinder.Outlet end is material outlet end after drying, filter plate
Cartridge filter is divided into two parts up and down, lower part is for temporarily storing filtrate, and upper part is for being filtered, washed, drying and temporarily
Filter cake is stored, agitating device is used for blending filter cake, promotes filtering, the discharge of dry and solid material.
In the above-mentioned technical solutions, Calcium Carbonate Filtration slot and leached mud lautertuns include also water-bath being located at filtrate canister portion position
Heating structure, positioned at the periphery of cylinder, heating water bath can promote calcium carbonate or leached mud dry, improve productivity.
In the above-mentioned technical solutions, Calcium Carbonate Filtration slot and leached mud lautertuns are further including water-bath positioned at filtrate canister portion position
Heating structure, positioned at the periphery of cylinder, heating water bath can promote the water evaporation in lautertuns to enter water collecting groove, guarantee tank water
Amount balance.
In the above-mentioned technical solutions, there are also water-bath temperature control housings for water collecting groove periphery, can be promoted by being heated or cooled
Water stream injection pump generates the ability of negative pressure and reduces the solubility of ammonia in the sink.
A method of high-purity calcium carbonate is prepared, is carried out, is included the following steps: using above-mentioned apparatus
1) preparation stage is previously added distilled water in water collecting groove 2；
2) ammonium salt solution is added in carburizing reagent slot 1 in leaching stage, is added in carburizing reagent slot 1 and contains hydroxide
The material of calcium or calcium oxide, stirring generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
3) phase analysis filtering and impurity removing-leaching carries out the stage simultaneously, opens the first centrifugal pump 5, and step 2) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, in carburizing reagent
Ammonium salt solution is added in slot 1, the material containing calcium hydroxide or calcium oxide is added in carburizing reagent slot 1, stirring generates solvable
The solidliquid mixture of property calcium salt, ammonium hydroxide and solid slag；
4) phase analysis filtering and impurity removing-carbonization carries out the stage simultaneously, opens the first centrifugal pump 5, and step 3) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, by step 3) calcium
Salt, which is directed into carburizing reagent slot 1, to be passed through carbon dioxide reaction and obtains the solidliquid mixture of calcium carbonate, ammonium salt solution；
5) Calcium Carbonate Filtration-carbonization carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 4)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 4)
The calcium salt soln of middle leached mud lautertuns 4 is directed into carburizing reagent slot 1, is passed through carbon dioxide carbonization, obtains calcium carbonate and ammonium salt
Solution；
6) Calcium Carbonate Filtration-leaching carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 5)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 5)
Middle 3 ammonium salt solution of Calcium Carbonate Filtration slot is directed into carburizing reagent slot 1, and calcium oxide or calcium hydroxide is added, obtains calcium salt soln；
7) step 3)~6 are repeated), into next reaction time, repeatedly circulation produces calcium carbonate；
8) washing, drying calcium carbonate and leached mud and discharge, Open valve b, valve d open the second centrifugal pump 6, to carbon
Injection distillation water washing in sour calcium lautertuns 3, leached mud lautertuns 4 turns off valve b, valve d for Calcium Carbonate Filtration slot 3, leaching
It slags tap 4 vacuum drying of lautertuns, discharge.
In the above scheme, calcium hydroxide can be carbide slag from a wealth of sources, and carbide slag changing rejected material to useful resource is produced
Calcium carbonate has considerable environmental benefit and economic benefit.
The principle of the invention includes:
Calcium oxide is reacted to obtain calcium hydroxide with water or directly be reacted using calcium hydroxide as raw material with ammonium salt:
Ca(OH)2+2NH4 +=Ca2++2NH3·H2O
After Selectively leaching calcium ion, filtering reaches removal of impurities purpose.
Calcium salt soln and ammonium hydroxide and carbon dioxide reaction after removal of impurities obtain calcium carbonate:
Ca2++2NH3·H2O+CO2=CaCO3↓+2NH4 ++2H2O
It filters, washs in the present apparatus, high-purity, fine grain product can be obtained after dry.
As it can be seen that the function that the present apparatus has removal of impurities concurrently, reacts, is filtered, washed, drying, does not depend on additional washing water, can prevent
Ammonia overflows, and produces convenient, cleaning.
The beneficial effects of the present invention are: 1) ammonia and ammonium salt are recycled in process, actual consumption, does not reduce cost；
2) calcium carbonate product purity is high, partial size is thin, and application potential is wide；3) it is operated under air-proof condition, it is therefore prevented that ammonia overflows environmental protection；4) anti-
It answers, be filtered, washed, drying and can carry out in the same apparatus, it is convenient, it avoids product and transfers the pollution；5) utilization ratio of device is high, follows
In ring running, ammonium salt leached, leached mud filtering, calcium salt carbonization, Calcium Carbonate Filtration alternately, do not occur device shutdown, can be by
Yield maximizes.
Detailed description of the invention
Fig. 1 is the device figure of production calcium carbonate of the invention.
Fig. 2 is Calcium Carbonate Filtration slot or leached mud filtering slot device figure of the invention.
Specific embodiment
Illustrate a specific embodiment of the invention with reference to the accompanying drawing.
The device of the building production high-purity calcium carbonate of embodiment 1
Building prepares the device of high-purity calcium carbonate, comprises the following structure: carburizing reagent slot 1, distillation water collecting groove 2, carbonic acid
Calcium lautertuns 3, leached mud lautertuns 4, the first centrifugal pump 5, the second centrifugal pump 6, water stream injection pump 7, carbon dioxide access port end 8；
The carburizing reagent slot 1, Calcium Carbonate Filtration slot 3, the first centrifugal pump 5 constitute closed circuit by pipeline；The distilled water is collected
Slot 2, the second centrifugal pump 6, water stream injection pump 7 constitute closed circuit；The Calcium Carbonate Filtration slot 3,4 structure phase of leached mud lautertuns
Together, it is respectively positioned on right above carburizing reagent slot 1, respectively connects 5 liquid outlet of the first centrifugal pump above, respectively connection above
One branch of the second centrifugal pump liquid outlet, respectively connects the gas access end of water stream injection pump 7 in side, bottom respectively
Connect carburizing reagent slot 1；Another branch of 7 fluid inlet end of the water stream injection pump connection, 6 outlet end of the second centrifugal pump, gas-liquid
Distillation water collecting groove 2 immediately below the connection of mixture outlet end；Carbon dioxide access port end 8 is connected on carburizing reagent slot
Portion；Valve a, the first centrifugal pump 5 and leached mud are installed on the pipeline between first centrifugal pump 5 and Calcium Carbonate Filtration slot 3
Valve c is installed on the pipeline between lautertuns 4；It is installed on pipeline between second centrifugal pump 6 and Calcium Carbonate Filtration slot 3
There is valve b, valve d, the second centrifugal pump 6 and water injection are installed on the pipeline between the second centrifugal pump 6 and leached mud lautertuns 4
Valve g is installed on pipeline between pump 7；Valve is installed on pipeline between the water stream injection pump 7 and Calcium Carbonate Filtration slot 3
E is equipped with valve f on the pipeline between water stream injection pump 7 and leached mud lautertuns 4.
Calcium Carbonate Filtration slot 3 and leached mud lautertuns 4 comprise the following structure: filter cake cylinder A1, filtrate cylinder A2, vacuumizing gas
Body outlet end A, washing water inlet end B leach solid-liquid arrival end C, filtrate (liquid end D, dry cake outlet end E, filter plate F,
Agitating device G；Filter cake cylinder A1 is separated right above filtrate cylinder A2 with filter plate F；The outlet end A is located at the position filtrate cylinder A2
Side surface upper part, washing water inlet end B, leach solid-liquid arrival end C and be located at the top filter cake cylinder A1, filtrate (liquid end D is located at filtrate
The bottom cylinder A2, outlet end E are located at filter cake cylinder A1 side lower, and agitating device G is located among filter cake cylinder A1.
Calcium Carbonate Filtration slot 3 and leached mud lautertuns 4 are further including heating water bath structure H1, position positioned at the position filter cake cylinder A1
In the periphery of cylinder；Calcium Carbonate Filtration slot 3 and leached mud lautertuns 4 are further including heating water bath structure positioned at the position filtrate cylinder A2
H2, positioned at the periphery of cylinder；There are also water-bath temperature control housings for 2 periphery of water collecting groove.
Embodiment 2 produces high-purity calcium carbonate
High-purity calcium carbonate is produced using the device of embodiment building, is included the following steps:
1) preparation stage is previously added distilled water in water collecting groove 2；
2) solution of containing ammonium chloride 12kg is added in carburizing reagent slot 1, is added in carburizing reagent slot 1 for leaching stage
Calcium hydroxide 7.5kg, stirring generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
3) phase analysis filtering and impurity removing-leaching carries out the stage simultaneously, opens the first centrifugal pump 5, and step 2) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, in carburizing reagent
The solution of containing ammonium chloride 12kg is added in slot 1, calcium hydroxide 7.5kg is added in carburizing reagent slot 1, stirring generates soluble
The solidliquid mixture of calcium salt, ammonium hydroxide and solid slag；
4) phase analysis filtering and impurity removing-carbonization carries out the stage simultaneously, opens the first centrifugal pump 5, and step 3) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, by step 3) calcium
Salt, which is directed into carburizing reagent slot 1, to be passed through carbon dioxide reaction and obtains the solidliquid mixture of calcium carbonate, ammonium salt solution；
5) Calcium Carbonate Filtration-carbonization carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 4)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 4)
The calcium salt soln of middle leached mud lautertuns 4 is directed into carburizing reagent slot 1, is passed through carbon dioxide carbonization, obtains calcium carbonate and ammonium salt
Solution；
6) Calcium Carbonate Filtration-leaching carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 5)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 5)
Middle 3 ammonium salt solution of Calcium Carbonate Filtration slot is directed into carburizing reagent slot 1, and calcium hydroxide 7.5kg is added, obtains calcium salt soln；
7) step 3)~6 are repeated), into next reaction time, 20 times circulation produces calcium carbonate；
8) washing, drying calcium carbonate and leached mud and discharge, Open valve b, valve d open the second centrifugal pump 6, to carbon
Injection distillation water washing in sour calcium lautertuns 3, leached mud lautertuns 4 turns off valve b, valve d for Calcium Carbonate Filtration slot 3, leaching
It slags tap 4 vacuum drying of lautertuns, discharge.
Discharge product calcium carbonate quality is 180kg, and purity respectively is 99.2%, and particle D50 is 2.3 μm.
Embodiment 3 produces high-purity calcium carbonate
High-purity calcium carbonate is produced using the device of embodiment building, is included the following steps:
1) preparation stage is previously added distilled water in water collecting groove 2；
2) solution of the 10kg containing ammonium nitrate is added in carburizing reagent slot 1, is added in carburizing reagent slot 1 for leaching stage
Calcium oxide 6kg, stirring generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
3) phase analysis filtering and impurity removing-leaching carries out the stage simultaneously, opens the first centrifugal pump 5, and step 2) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, in carburizing reagent
The solution of the 10kg containing ammonium nitrate is added in slot 1, calcium oxide 6kg is added in carburizing reagent slot 1, stirs, generation soluble calcium salt,
The solidliquid mixture of ammonium hydroxide and solid slag；
4) phase analysis filtering and impurity removing-carbonization carries out the stage simultaneously, opens the first centrifugal pump 5, and step 3) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, by step 3) calcium
Salt, which is directed into carburizing reagent slot 1, to be passed through carbon dioxide reaction and obtains the solidliquid mixture of calcium carbonate, ammonium salt solution；
5) Calcium Carbonate Filtration-carbonization carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 4)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 4)
The calcium salt soln of middle leached mud lautertuns 4 is directed into carburizing reagent slot 1, is passed through carbon dioxide carbonization, obtains calcium carbonate and ammonium salt
Solution；
6) Calcium Carbonate Filtration-leaching carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 5)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 5)
Middle 3 ammonium salt solution of Calcium Carbonate Filtration slot is directed into carburizing reagent slot 1, and calcium oxide 6kg is added, obtains calcium salt soln；
7) step 3)~6 are repeated), into next reaction time, 20 times circulation produces calcium carbonate；
8) washing, drying calcium carbonate and leached mud and discharge, Open valve b, valve d open the second centrifugal pump 6, to carbon
Injection distillation water washing in sour calcium lautertuns 3, leached mud lautertuns 4 turns off valve b, valve d for Calcium Carbonate Filtration slot 3, leaching
It slags tap 4 vacuum drying of lautertuns, discharge.
Discharge product calcium carbonate quality is 188kg, and purity respectively is 99.1%, and particle D50 is 2.5 μm.
Embodiment 4 produces high-purity calcium carbonate using carbide slag
1) preparation stage is previously added distilled water in water collecting groove 2；
2) solution of containing ammonium chloride 12kg is added in carburizing reagent slot 1, is added in carburizing reagent slot 1 for leaching stage
Carbide slag 10kg containing calcium hydroxide 80%, stirring generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
3) phase analysis filtering and impurity removing-leaching carries out the stage simultaneously, opens the first centrifugal pump 5, and step 2) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, in carburizing reagent
The solution of containing ammonium chloride 12kg is added in slot 1, the carbide slag 10kg containing calcium hydroxide 80% is added in carburizing reagent slot 1, stirs
It mixes, generates the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
4) phase analysis filtering and impurity removing-carbonization carries out the stage simultaneously, opens the first centrifugal pump 5, and step 3) is leached gained solid-liquid
Mixture is pumped into leached mud lautertuns 4, opens the second centrifugal pump 6, in leached mud lautertuns 4 at vacuum, filters, by step 3) calcium
Salt, which is directed into carburizing reagent slot 1, to be passed through carbon dioxide reaction and obtains the solidliquid mixture of calcium carbonate, ammonium salt solution；
5) Calcium Carbonate Filtration-carbonization carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 4)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 4)
The calcium salt soln of middle leached mud lautertuns 4 is directed into carburizing reagent slot 1, is passed through carbon dioxide carbonization, obtains calcium carbonate and ammonium salt
Solution；
6) Calcium Carbonate Filtration-leaching carries out the stage simultaneously, the first centrifugal pump 5 is opened, by the calcium carbonate and ammonium in step 5)
Salting liquid is pumped into Calcium Carbonate Filtration slot 3, opens the second centrifugal pump 6, in Calcium Carbonate Filtration slot 3 at vacuum, filters, by step 5)
Middle 3 ammonium salt solution of Calcium Carbonate Filtration slot is directed into carburizing reagent slot 1, and the carbide slag 10kg containing calcium hydroxide 80% is added, obtains
Calcium salt soln；
7) step 3)~6 are repeated), into next reaction time, 20 times circulation produces calcium carbonate；
8) washing, drying calcium carbonate and leached mud and discharge, Open valve b, valve d open the second centrifugal pump 6, to carbon
Injection distillation water washing in sour calcium lautertuns 3, leached mud lautertuns 4 turns off valve b, valve d for Calcium Carbonate Filtration slot 3, leaching
It slags tap 4 vacuum drying of lautertuns, discharge.
Discharge product calcium carbonate quality is 173kg, and purity respectively is 99.3%, and particle D50 is 3.9 μm.
Claims (7)
1. a kind of device for preparing high-purity calcium carbonate, it is characterised in that comprise the following structure: carburizing reagent slot (1), water collecting groove
(2), Calcium Carbonate Filtration slot (3), leached mud lautertuns (4), the first centrifugal pump (5), the second centrifugal pump (6), water stream injection pump (7),
Carbon dioxide access port end (8)；The carburizing reagent slot (1), Calcium Carbonate Filtration slot (3), the first centrifugal pump (5) pass through pipeline structure
At closed circuit；The water collecting groove (2), the second centrifugal pump (6), water stream injection pump (7) constitute closed circuit；The calcium carbonate mistake
Filter pocket (3), leached mud lautertuns (4) structure are identical, are respectively positioned on right above carburizing reagent slot (1), respectively connection the above
One centrifugal pump (5) liquid outlet, above respectively connection the second centrifugal pump (6) liquid outlet a branch, side respectively
The gas access end for connecting water stream injection pump (7), respectively connects carburizing reagent slot (1) in bottom；Water stream injection pump (7) liquid
Arrival end connects another branch of the second centrifugal pump (6) outlet end, and the water immediately below the connection of gas-liquid mixture outlet end is collected
Slot (2)；Carbon dioxide access port end (8) is connected to carburizing reagent slot top；First centrifugal pump (5) and calcium carbonate mistake
Valve (a) is installed on the pipeline between filter pocket (3), is pacified on the pipeline between the first centrifugal pump (5) and leached mud lautertuns (4)
Equipped with valve (c)；Valve (b) is installed on the pipeline that second centrifugal pump (6) and calcium carbonate are crossed between slot (3), second from
Valve (d), the second centrifugal pump (6) and water stream injection pump (7) are installed on the pipeline between heart pump (6) and leached mud lautertuns (4)
Between pipeline on valve (g) is installed；It is equipped on pipeline between the water stream injection pump (7) and Calcium Carbonate Filtration slot (3)
Valve (e) is equipped with valve (f) on the pipeline between water stream injection pump (7) and leached mud lautertuns (4).
2. a kind of as described in claim 1, device preparing high-purity calcium carbonate, it is characterised in that: Calcium Carbonate Filtration slot (3) and leaching
Lautertuns (4) of slagging tap comprises the following structure: filter cake cylinder (A1), vacuumizes gas outlet end (A), washing water at filtrate cylinder (A2)
Arrival end (B) leaches solid-liquid arrival end (C), filtrate (liquid end (D), dry cake outlet end (E), filter plate (F), stirring dress
Set (G)；Filter cake cylinder (A1) is separated right above filtrate cylinder (A2) with filter plate (F)；The outlet end (A) is located at filtrate cylinder
(A2) side surface upper part at position, washing water inlet end (B), leaching solid-liquid arrival end (C) are located at the top of filter cake cylinder (A1), and filtrate goes out
Mouth end (D) is located at filtrate cylinder bottom (A2), and outlet end (E) is located at filter cake cylinder (A1) side lower, and agitating device (G) is located at filter cake
Cylinder (A1) is intermediate.
3. a kind of as claimed in claim 2, device preparing high-purity calcium carbonate, it is characterised in that: Calcium Carbonate Filtration slot (3) and leaching
Lautertuns (4) of slagging tap is further including heating water bath structure (H1) positioned at the position filter cake cylinder (A1), positioned at the periphery of cylinder.
4. a kind of as claimed in claim 2, device preparing high-purity calcium carbonate, it is characterised in that: Calcium Carbonate Filtration slot (3) and leaching
Lautertuns (4) of slagging tap is further including heating water bath structure (H2) positioned at filtrate cylinder position (A2), positioned at the periphery of cylinder.
5. a kind of as described in claim 1, device preparing high-purity calcium carbonate, it is characterised in that: water collecting groove (2) periphery is also
Water-bath temperature control housing.
6. a kind of method for preparing high-purity calcium carbonate is included the following steps: using Claims 1 to 5 described device
1) preparation stage is previously added distilled water in water collecting groove (2)；
2) ammonium salt solution is added in leaching stage in carburizing reagent slot (1), is added in carburizing reagent slot (1) and contains hydroxide
The material of calcium or calcium oxide, stirring generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
3) phase analysis filtering and impurity removing-leaching carries out the stage simultaneously, opens the first centrifugal pump (5), and it is mixed that step 2) is leached gained solid-liquid
It closes object to be pumped into leached mud lautertuns (4), open the second centrifugal pump (6), in leached mud lautertuns (4) at vacuum, filter, be carbonized
Ammonium salt solution is added in reactive tank (1), the material containing calcium hydroxide or calcium oxide is added in carburizing reagent slot (1), stirs,
Generate the solidliquid mixture of soluble calcium salt, ammonium hydroxide and solid slag；
4) phase analysis filtering and impurity removing-carbonization carries out the stage simultaneously, opens the first centrifugal pump (5), and it is mixed that step 3) is leached gained solid-liquid
It closes object to be pumped into leached mud lautertuns (4), open the second centrifugal pump (6), in leached mud lautertuns (4) at vacuum, filter, by step
3) calcium salt, which is directed into, is passed through carbon dioxide reaction in carburizing reagent slot (1) and obtains the solidliquid mixture of calcium carbonate, ammonium salt solution；
5) Calcium Carbonate Filtration-carbonization carries out the stage simultaneously, opens the first centrifugal pump (5), by the calcium carbonate and ammonium salt in step 4)
Solution is pumped into Calcium Carbonate Filtration slot (3), is opened the second centrifugal pump (6), in Calcium Carbonate Filtration slot (3) at vacuum, is filtered, will be walked
It is rapid 4) in the calcium salt soln of leached mud lautertuns (4) be directed into carburizing reagent slot (1), be passed through carbon dioxide carbonization, obtain carbonic acid
Calcium and ammonium salt solution；
6) Calcium Carbonate Filtration-leaching carries out the stage simultaneously, opens the first centrifugal pump (5), by the calcium carbonate and ammonium salt in step 5)
Solution is pumped into Calcium Carbonate Filtration slot (3), is opened the second centrifugal pump (6), in Calcium Carbonate Filtration slot (3) at vacuum, is filtered, will be walked
It is rapid 5) in Calcium Carbonate Filtration slot (3) ammonium salt solution be directed into carburizing reagent slot (1), calcium oxide or calcium hydroxide is added, obtains calcium
Salting liquid；
7) step 3)~6 are repeated), into next reaction time, repeatedly circulation produces calcium carbonate；
8) washing, drying calcium carbonate and leached mud and discharge, Open valve (b), valve (d) are opened the second centrifugal pump (6), to
Injection distillation water washing in Calcium Carbonate Filtration slot (3), leached mud lautertuns (4) turns off valve (b), valve (d) for calcium carbonate
Lautertuns (3), leached mud lautertuns (4) vacuum drying, discharge.
7. a kind of method for preparing high-purity calcium carbonate as claimed in claim 6, it is characterised in that calcium hydroxide source is in carbide slag.
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|---|---|---|---|---|
| CN106219586A (en) * | 2016-08-02 | 2016-12-14 | 王延军 | A kind of be raw material production nanometer grade calcium carbonate with carbide slag device and method |
| CN109956487A (en) * | 2017-12-23 | 2019-07-02 | 张旭 | Circulating ammonia coupling reaction is filtered, washed, drying system and method |
| CN210559432U (en) * | 2019-08-15 | 2020-05-19 | 张旭 | Device for preparing high-purity calcium carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106219586A (en) * | 2016-08-02 | 2016-12-14 | 王延军 | A kind of be raw material production nanometer grade calcium carbonate with carbide slag device and method |
| CN109956487A (en) * | 2017-12-23 | 2019-07-02 | 张旭 | Circulating ammonia coupling reaction is filtered, washed, drying system and method |
| CN210559432U (en) * | 2019-08-15 | 2020-05-19 | 张旭 | Device for preparing high-purity calcium carbonate |
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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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