CN104591297B - Method and device for preparing polymeric ferric sulfate - Google Patents
Method and device for preparing polymeric ferric sulfate Download PDFInfo
- Publication number
- CN104591297B CN104591297B CN201510009817.XA CN201510009817A CN104591297B CN 104591297 B CN104591297 B CN 104591297B CN 201510009817 A CN201510009817 A CN 201510009817A CN 104591297 B CN104591297 B CN 104591297B
- Authority
- CN
- China
- Prior art keywords
- polymerization reaction
- catalyst
- reaction kettle
- kettle
- pump
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method and a device for preparing polymeric ferric sulfate. The method comprises the following steps: adding water and sulfuric acid at a certain ratio into a ferrous sulfate dissolving kettle, adding a quantitative ferrous sulfate and fully stirring; pumping the ferrous sulfate liquid into a cyclone separator and then feeding into a polymerization reactor; starting a forced-circulating pump of the polymerization reactor and starting a cyclone stirring valve so that the ferrous sulfate liquid is fully dissolved in the polymerization reactor; and adding the quantitative catalyst liquid into the polymerization reactor by virtue of a pressure and introducing oxygen to carry out oxidation reaction. The device comprises the polymerization reactor, the ferrous sulfate dissolving kettle, a catalyst dissolving kettle and the forced-circulating pump, wherein the ferrous sulfate dissolving kettle is connected with a liquid-feeding pump, the liquid-feeding pump is connected with the cyclone separator, the cyclone separator is connected with the polymerization reactor, and the catalyst dissolving kettle is connected with the polymerization reactor by virtue of a chemical agent adding pump and a catalyst chemical agent adding and metering tank.
Description
Technical field
The present invention relates to a kind of preparation method of chemical products and equipment, particularly one kind prepare bodied ferric sulfate method and
Its device.
Background technology
Bodied ferric sulfate is a kind of efficient inorganic high-molecular coagulant adopting, because of its coenocytism, makes it in the process of purified water
In quickly form substantial amounts of positive multinuclear complex ion, the negative charge that can quickly neutralize water-borne glue body microparticle surfaces is allowed to de- steady,
Adhesion, bridge formation, crosslinking can be passed through, roll up and sweep effect in interionic again, so that particle coagulation is formed flco and produce flocculation.Given birth to
Become flocculate ratio great, settling velocity is fast, and flocculating effect is good.Thus polyaluminium sulfate is widely used in urban life drinking water, work
The purified treatment of industry recirculated water, and chemical industry, oil, mine, papermaking, print and dye, brewage, iron and steel, coal gas, the industry such as plating
Industrial wastewater and the purified treatment of city domestic sewage, to different regions variety classes source wastewater treatment, are attained by preferably
Clean-up effect.
The preparation of bodied ferric sulfate mainly has direct oxidation method method and catalytic oxidation.The preparation of most of bodied ferric sulfates
Using direct oxidation method, this method process route is simpler, can reduce equipment investment and production link for commercial production, reduces
Equipment cost, but this production technology is necessarily dependent upon oxidant, such as: h2o2、kclo3、hno3Deng inorganic oxidizer；But it is this
There is oxidizer greatly in method, high cost, and the ion that oxidant introduces need to be separated, and the harmful gass producing in reaction need
Special Equipment absorbs the problems such as process, thus is difficult to popularize in industrialized production and apply.But need a small amount of in experimentation
Bodied ferric sulfate when prepared using such method simple.At present, bodied ferric sulfate in the industrial production more adopts catalysis
Oxidizing process.I.e. with ferrous sulfate and sulphuric acid as raw material, by the effect of catalyst, ferrous sulfate is made to be situated between acid using oxidant
It is oxidized to ferric ion in matter.Then neutralized with sodium hydroxide, adjustment basicity is hydrolyzed, and polyreaction is obtained polymerization
Iron sulfate.
The Chinese patent application of Application No. 2003101059644 is disclosed one kind and is produced by catalytic oxidation titanium dioxide
The method that raw side-product ferrous sulfate prepares bodied ferric sulfate, the method adopts with ferrous sulfate as raw material, adds sulphuric acid, passes through
Air gives oxidation copperas solution, then adds sodium nitrite and pure oxygen, oxidation ferrous sulfate and sulphuric acid to mix from catalytic oxidizer
Close solution, then through compound, the process such as stable, produce solidifying bodied ferric sulfate.But this patent produces titanium dioxide by-product for titanium mineral
In product ferrous sulfate, the inevitable a small amount of gravel retained, it is impossible to process, thus can cause to polymerization reaction kettle to rub, shortens it
Service life.The sulphuric acid adopting in this patent and the ratio of ferrous sulfate lead to reaction not exclusively.Due to catalyst in this patent
Only once add, lead to catalytic effect poor, if added by several times, now because polymerization reaction kettle is reaction under high pressure state, such as
Fruit is using pumping into because in polymerization reaction kettle, pressure is excessive and cause catalyst cannot add, and is first put using traditional approach
Sky, then catalyst is pumped into, this undoubtedly causes oxygen and wastes, and also extends the response time.The urging of addition in this patent
Its catalytic rate of agent itself is low.In addition during the course of the reaction because ferrous sulfate is to be completely dissolved it is possible to can be in polyreaction
Bottom valve goes out to result in blockage and make strong force circulation pump cannot be carried out normal work.
The Chinese invention patent of Application No. 200810300594.2 discloses a kind of synthetic method of bodied ferric sulfate, should
Invention is oxidant using air, oxygen or oxygen-enriched air, with ferrous sulfate, sulphuric acid or titanium dioxide waste acid by sulfuric acid process as raw material, acid
Property nitre iron sulfate be catalyst, synthesizing polymeric ferric sulfate in the enamel reaction still equipped with packed tower；Use at copperas solution
Reason oxidized tail gas, absorb the nitric oxide in oxidized tail gas.The Chinese invention patent of Application No. 201410341013.5 is open
A kind of method that utilization Waste Sulfuric Acid and ferrous sulfate oxygen pressing produce bodied ferric sulfate, this method mainly with Titanium white waste sulfuric acid and
Ferrous sulfate heptahydrate as primary raw material, adds a small amount of sodium nitrite to make catalyst, under the conditions of being passed through oxygen pressing reaction 2～
4 hours, obtain bodied ferric sulfate fluid product.Fluid product is obtained after dried solid, powdery bodied ferric sulfate to produce
Product.
Content of the invention
The purpose of the present invention is for the problems referred to above, provides one kind to prepare bodied ferric sulfate method and its device.
The present invention solves technical problem and be the technical scheme is that a kind of method preparing bodied ferric sulfate at least includes
Following steps:
Step one: water, sulphuric acid are added in ferrous sulfate dissolution kettle according to a certain percentage, adds quantitative sulphuric acid sub-
Ferrum, is then sufficiently stirred for；Solution temperature controls at 20-35 DEG C；
Step 2: copperas solution dosing pump is squeezed into cyclone separator, then squeezes in polymerization reaction kettle, eddy flow divides
The impurity such as gravel are made to be removed from device using ferrous sulfate is different from gravel proportion；Open the strength in polymerization reaction kettle simultaneously
Circulating pump, and open cyclone mixing valve, so that copperas solution is fully dissolved in polymerization reaction kettle；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle of copperas solution by pressure, fully
It is passed through oxygen after stirring and carry out continuous oxidation reaction；Control reactor pressure is 0.3-0.5mpa；Reaction is mended after carrying out 1 hour again
Plus catalyst；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is controlled to 60-80 DEG C；
Step 4: polymerization reaction kettle emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
The each group that described step one is added divides that (mass content is including water, the sulphuric acid of 30 ~ 98% concentration, ferrous sulfate
90%)；The part by weight of three is: 4 ~ 6:1 ~ 5:10 ~ 13.
After described step 2 opens cyclone mixing valve, same along reactor wall located at polymerization reaction kettle bottom at least 3
The nozzle hydrojet in direction, makes reactant liquor carry out same direction rotational flow, plays stirring action.
Described step 2 sets up water-jet pump in polymerization reaction kettle strong cyclic pump discharge, by inside reactor not
The oxygen that can react in time and nitrogen dioxide by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials, when increasing reaction
Between.
Described step 3 catalyst is the catalyst that sodium nitrite and manganese dioxide press 2-3:1 mixed configuration, catalyst
Account for that addition accounts for reaction kettle for reaction thing total amount 0.3 ~ 0.5%；Add 60% catalytic amount for the first time, add 40% second
Catalytic amount, percentage ratio here is weight percentage.
The quantitative catalyst solution of described step 3 by the method that pressure adds polymerization reaction kettle is: first by catalyst
Add catalyst dissolution kettle so that it is fully dissolved, then catalyst is pumped into dosing measuring tank by dosing pump, open and catalyst
Tank connected air compressor machine is measured in dosing, makes the pressure of catalyst dosing measuring tank be more than 0.5mpa so that catalyst is pressed into polymerization
Reactor；The method being passed through oxygen is: the oxygen in liquefied oxygen tank is led to after gasifier gasification, then through spinner flowmeter
Enter to polymerization reaction kettle；
Described step 4 polymerization reaction kettle vent gas treatment, emptying gas is sprayed the process of backward high altitude discharge through alkali liquor
For: polymerization reaction kettle puts into liquid caustic soda spray column gas first, is sent by air-introduced machine after liquid caustic soda spray column alkali liquor spray
Enter smoke stack emission.
A kind of process units preparing bodied ferric sulfate method of the present invention；Including polymerization reaction kettle, ferrous sulfate
Dissolution kettle and catalyst dissolution kettle, ferrous sulfate dissolution kettle, catalyst dissolution kettle are connected to polymerization reaction kettle by pipeline respectively
Top, polymerization reaction kettle is connected with for strengthen polymerization reaction kettle internal-response liquid circulation strong force circulation pump, this is strong
Power circulating pump two end is connected to top and the bottom of polymerization reaction kettle；Ferrous sulfate dissolution kettle be connected to polymerization reaction kettle it
Between pipeline on be connected with liquid-feeding pump and cyclone separator, the outfan of ferrous sulfate dissolution kettle is connected with liquid-feeding pump, liquid-feeding pump
Outfan be connected with cyclone separator, cyclone separator is connected with polymerization reaction kettle, and ferrous sulfate dissolution kettle reactant liquor is by sending
Liquid pump is pumped into cyclone separator, and the reactant liquor after cyclone separator separates is sent to polymerization reaction kettle；Catalyst dissolution kettle is even
It is connected on the pipeline between polymerization reaction kettle and be connected with dosing pump and catalyst dosing measuring tank, catalyst dissolution kettle and dosing pump
Connect, dosing pump is connected with catalyst dosing measuring tank, and catalyst dosing measuring tank is connected with polymerization reaction kettle, dosing measuring tank
It is connected with air compressor machine, the catalyst of catalyst dissolution kettle is pumped into catalyst dosing measuring tank by dosing pump, enters catalyst and adds
The catalyst of medicine measuring tank is pressed into polymerization reaction kettle；It is provided with water injection vacuum at described strong force circulation pump upper outlet
Pump；Polymerization reaction kettle top is connected with atmospheric valve, and atmospheric valve is connected with liquid caustic soda spray column, and liquid caustic soda spray column alkali is connected with circulation
Pump is used for the circulation of spray liquid in liquid caustic soda spray column, and liquid caustic soda spray column outlet is connected with air-introduced machine, and blower fan is again with chimney even
Connect；It is connected with polymerization reaction kettle and send oxygen device.
The described oxygen device that send includes liquefied oxygen tank, gasifier, spinner flowmeter, and liquefied oxygen tank through gasifier and turns
Subflow gauge is connected with polymerization reaction kettle.
Described polymerization reaction kettle bottom inside is provided with least 3 along the unidirectional nozzle of reactor wall, and nozzle connects
There is eddy flow control valve, eddy flow control valve is connected with strong force circulation pump.
Anti-blocking recoil valve is connected with described strong force circulation pump, anti-blocking recoil valve outlet port is located at polymerization reaction kettle bottom.
Water, sulphuric acid, ferrous sulfate charge door, agitator are connected with ferrous sulfate dissolution kettle of the present invention；Catalysis
Catalyst, water charge door, agitator are connected with agent dissolution kettle.Described catalyst dosing measuring tank is provided with liquidometer, peace
Full valve.Described polymerization reaction kettle top is provided with relief valve.
The invention has the beneficial effects as follows: 1, due to being provided with cyclone separator in ferrous sulfate dissolution kettle, can be by gravel
Carry out separating, to reduce the friction to polymerization reaction kettle system, increase the service life.2nd, catalyst uses compressed air, so that
It can be pressed into polymerization reaction kettle.3rd, add anti-blocking recoil valve in polymerization reaction kettle.By anti-blocking recoil valve to bottom valve around
Carry out strength to recoil, can avoid blocking.4th, increase cyclone mixing valve in polymerization reaction kettle.Increased by polymerization reaction kettle bottom
Plus cyclone mixing valve and reaction pot lower half increase by 3 or 4 along the unidirectional nozzle of reactor wall, so that reactant liquor is carried out
Same direction rotational flow, serves the effect of stirring.5th, increase water injection vacuum in polymerization reaction kettle strong cyclic pump discharge
Pump, the oxygen that can not react in time and nitrogen dioxide inside reactor are sufficiently mixed with reactant liquor by vacuum, improve former material
The utilization rate of material, can achieve the continuous operation of reaction, substantially increases the production capacity of unit interval；Controllable life in simultaneously producing
Produce vent gas treatment, the pollutant that can greatly reduce in production process produce.
Brief description
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment one
As shown in figure 1, a kind of method preparing bodied ferric sulfate of the present invention at least comprises the steps:
Step one: the dilute sulfuric acid that 4.2 tons of water, 2.6 tons of mass concentrations are 50% is added in ferrous sulfate dissolution kettle 18, then
Add 12 tons of ferrous sulfate (mass content is 90%), then be sufficiently stirred for dissolving by three；Solution temperature controls at 35 DEG C；
Step 2: copperas solution dosing pump 19 is squeezed into cyclone separator 20, enters back into polymerization reaction kettle 12, rotation
Stream separator 20 makes the impurity such as gravel be removed using ferrous sulfate is different from gravel proportion；Open polymerization reaction kettle 12 simultaneously
Strong force circulation pump 13, and open cyclone mixing valve 11, so that copperas solution is fully dissolved in polymerization reaction kettle 12；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle 12 of copperas solution by pressure, fills
It is passed through oxygen after dividing stirring and carry out continuous oxidation reaction, control pressure 0.4mpa；Reaction adds second catalysis after carrying out 1 hour
Agent；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is 60 DEG C；
Step 4: polymerization reaction kettle 12 emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
After described step 2 opens cyclone mixing valve 11, located at polymerization reaction kettle 12 bottom at least 3 along reactor wall
Unidirectional nozzle 121 hydrojet, makes reactant liquor carry out same direction rotational flow, plays stirring action.
Described step 2 sets up water-jet pump 8 in polymerization reaction kettle 13 strong force circulation pump 13 outlet, by reactor
The oxygen that can not react in time inside 12 and nitrogen dioxide, by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials, are increased
Plus the response time.
Described step 3 catalyst is the catalyst that sodium nitrite and manganese dioxide press 2.5:1 mixed configuration, catalyst
Account for that addition accounts for reaction-ure mixture in reactor 12 0.3%；Add 60% catalytic amount for the first time, add 40% second
Catalytic amount, percentage ratio here is weight percentage.
The quantitative catalyst solution of described step 3 by the method that pressure adds polymerization reaction kettle 12 is: first will be catalyzed
Agent adds catalyst dissolution kettle 1 so that it is fully dissolved, then pumps into catalyst to dosing measuring tank 4 by dosing pump 2, opens and urges
The air compressor machine 3 that agent dosing measuring tank 4 connects, makes the pressure of catalyst dosing measuring tank 4 be more than 0.5mpa, by catalyst pressure
Enter polymerization reaction kettle 12；The method being passed through oxygen is: the oxygen in liquefied oxygen tank 5 is after gasifier 6 gasification, then process turns
Subflow gauge 7 is passed into polymerization reaction kettle 12；
Described step 4 polymerization reaction kettle 12 vent gas treatment, emptying gas is sprayed the mistake of backward high altitude discharge through alkali liquor
Cheng Wei: 12 gases of polymerization reaction kettle first put into liquid caustic soda spray column 14, passes through after liquid caustic soda spray column 14 alkali liquor spray
Air-introduced machine 16 is sent into chimney 17 and is discharged.
Embodiment two
As shown in figure 1, a kind of method preparing bodied ferric sulfate of the present invention at least comprises the steps:
Step one: the concentrated sulphuric acid that 5.6 tons of water, 1.35 tons of mass concentrations are 98% is added in ferrous sulfate dissolution kettle 18,
Add 10.8 tons of ferrous sulfate (feso4 7h2o, mass content is 90%), then be sufficiently stirred for dissolving by three；Dissolving temperature
Degree controls at 20 DEG C；
Step 2: copperas solution dosing pump 19 is squeezed into cyclone separator 20, enters back into polymerization reaction kettle 12, rotation
Stream separator 20 makes the impurity such as gravel be removed using ferrous sulfate is different from gravel proportion；Open polymerization reaction kettle 12 simultaneously
Strong force circulation pump 13, and open cyclone mixing valve 11, so that copperas solution is fully dissolved in polymerization reaction kettle 12；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle 12 of copperas solution by pressure, fills
It is passed through oxygen after dividing stirring and carry out continuous oxidation reaction, control pressure 0.45mpa；Reaction adds after carrying out 1 hour urges for the second time
Agent；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is 70 DEG C；
Step 4: polymerization reaction kettle 12 emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
After described step 2 opens cyclone mixing valve 11, same along reactor wall located at polymerization reaction kettle bottom at least 3
Nozzle 121 hydrojet in one direction, makes reactant liquor carry out same direction rotational flow, plays stirring action.
Described step 2 sets up water-jet pump 8 in polymerization reaction kettle 12 strong force circulation pump 13 outlet, by reactor
The internal oxygen that can not react in time and nitrogen dioxide, by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials, are increased
Response time.
Described step 3 catalyst is the catalyst that sodium nitrite and manganese dioxide press 2.5:1 mixed configuration, catalyst
Account for that addition accounts for reaction kettle for reaction thing total amount 0.4%；Add for the first time 60% catalytic amount, add 40% urge for second
Agent amount, percentage ratio here is weight percentage.
The quantitative catalyst solution of described step 3 by the method that pressure adds polymerization reaction kettle 12 is: first will be catalyzed
Agent adds catalyst dissolution kettle 1 so that it is fully dissolved, then pumps into catalyst to dosing measuring tank 4 by dosing pump 2, opens and urges
The air compressor machine 3 that agent dosing measuring tank 4 connects, makes the pressure of catalyst dosing measuring tank 4 be more than 0.5mpa, by catalyst pressure
Enter polymerization reaction kettle 12；The method being passed through oxygen is: the oxygen in liquefied oxygen tank 5 is after gasifier 6 gasification, then process turns
Subflow gauge 7 is passed into polymerization reaction kettle 12；
Described step 4 polymerization reaction kettle 12 vent gas treatment, emptying gas is sprayed the mistake of backward high altitude discharge through alkali liquor
Cheng Wei: 12 gases of polymerization reaction kettle first put into liquid caustic soda spray column 14, passes through after liquid caustic soda spray column 14 alkali liquor spray
Air-introduced machine 16 is sent into chimney 17 and is discharged.
Embodiment three
As shown in figure 1, a kind of method preparing bodied ferric sulfate of the present invention at least comprises the steps:
Step one: the dilute sulfuric acid that 4.5 tons of water, 1.95 tons of mass concentrations are 70% is added in ferrous sulfate dissolution kettle 18,
Add 11.5 tons of ferrous sulfate (feso4 7h2o, mass content is 90%), then be sufficiently stirred for dissolving by three；Dissolving temperature
Degree controls at 30 DEG C；
Step 2: copperas solution dosing pump 19 is squeezed into cyclone separator 20, enters back into polymerization reaction kettle 12, rotation
Stream separator 20 makes the impurity such as gravel be removed using ferrous sulfate is different from gravel proportion；Open polymerization reaction kettle 12 simultaneously
Strong force circulation pump 13, and open cyclone mixing valve 11, so that copperas solution is fully dissolved in polymerization reaction kettle 12；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle 12 of copperas solution by pressure, fills
It is passed through oxygen after dividing stirring and carry out continuous oxidation reaction, control pressure 0.3mpa；Reaction adds second catalysis after carrying out 1 hour
Agent；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is 75 DEG C；
Step 4: polymerization reaction kettle 12 emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
After described step 2 opens cyclone mixing valve 11, located at polymerization reaction kettle 12 bottom at least 3 along reactor wall
Unidirectional nozzle 121 hydrojet, makes reactant liquor carry out same direction rotational flow, plays stirring action.
Described step 2 sets up water-jet pump 8 in polymerization reaction kettle 12 strong force circulation pump 13 outlet, by reactor
The oxygen that can not react in time inside 12 and nitrogen dioxide, by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials, are increased
Plus the response time.
Described step 3 catalyst is the catalyst that sodium nitrite and manganese dioxide press 2.5:1 mixed configuration, catalyst
Account for that addition accounts for reaction kettle for reaction thing total amount 0.3%；Add for the first time 60% catalytic amount, add 40% urge for second
Agent amount, percentage ratio here is weight percentage.
The quantitative catalyst solution of described step 3 by the method that pressure adds polymerization reaction kettle 12 is: first will be catalyzed
Agent adds catalyst dissolution kettle 1 so that it is fully dissolved, then pumps into catalyst to dosing measuring tank 4 by dosing pump 2, opens and urges
The air compressor machine 3 that agent dosing measuring tank 4 connects, makes the pressure of catalyst dosing measuring tank 4 be more than 0.5mpa, by catalyst pressure
Enter polymerization reaction kettle 12；The method being passed through oxygen is: the oxygen in liquefied oxygen tank 5 is after gasifier 6 gasification, then process turns
Subflow gauge 7 is passed into polymerization reaction kettle 12；
Described step 4 polymerization reaction kettle 12 vent gas treatment, emptying gas is sprayed the mistake of backward high altitude discharge through alkali liquor
Cheng Wei: 12 gases of polymerization reaction kettle first put into liquid caustic soda spray column 14, passes through after liquid caustic soda spray column 14 alkali liquor spray
Air-introduced machine 16 is sent into chimney 17 and is discharged.
Example IV
As shown in figure 1, a kind of method preparing bodied ferric sulfate of the present invention at least comprises the steps:
Step one: the concentrated sulphuric acid that 5.6 tons of water, 1.35 tons of mass concentrations are 98% is added in ferrous sulfate dissolution kettle 18, then
Add 10.8 tons of ferrous sulfate (feso4 7h2o, mass content is 90%), then be sufficiently stirred for dissolving by three；Solution temperature
Control at 25 DEG C；
Step 2: copperas solution dosing pump 19 is squeezed into cyclone separator 20, enters back into polymerization reaction kettle 12, rotation
Stream separator 20 makes the impurity such as gravel be removed using ferrous sulfate is different from gravel proportion；Open polymerization reaction kettle 12 simultaneously
Strong force circulation pump 13, and open cyclone mixing valve 11, so that copperas solution is fully dissolved in polymerization reaction kettle 12；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle 12 of copperas solution by pressure, fills
It is passed through oxygen after dividing stirring and carry out continuous oxidation reaction, control pressure 0.35mpa；Reaction adds after carrying out 1 hour urges for the second time
Agent；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is 60 DEG C；
Step 4: polymerization reaction kettle 12 emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
After described step 2 opens cyclone mixing valve 11, located at polymerization reaction kettle 12 bottom at least 3 along reactor wall
Unidirectional nozzle 121 hydrojet, makes reactant liquor carry out same direction rotational flow, plays stirring action.
Described step 2 sets up water-jet pump 8 in polymerization reaction kettle 12 strong force circulation pump 13 outlet, by reactor
The oxygen that can not react in time inside 12 and nitrogen dioxide, by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials, are increased
Plus the response time.
Described step 3 catalyst is the catalyst that sodium nitrite and manganese dioxide press 2.5:1 mixed configuration, catalyst
Account for that addition accounts for reaction-ure mixture in reactor 12 0.3%；Add 60% catalytic amount for the first time, add 40% second
Catalytic amount, percentage ratio here is weight percentage.
The quantitative catalyst solution of described step 3 by the method that pressure adds polymerization reaction kettle 12 is: first will be catalyzed
Agent adds catalyst dissolution kettle 1 so that it is fully dissolved, then pumps into catalyst to dosing measuring tank 4 by dosing pump 2, opens and urges
The air compressor machine 3 that agent dosing measuring tank 4 connects, makes the pressure of catalyst dosing measuring tank 4 be more than 0.5mpa, by catalyst pressure
Enter polymerization reaction kettle 12；The method being passed through oxygen is: the oxygen in liquefied oxygen tank 5 is after gasifier 6 gasification, then process turns
Subflow gauge 7 is passed into polymerization reaction kettle 12；
Described step 4 polymerization reaction kettle 12 vent gas treatment, emptying gas is sprayed the mistake of backward high altitude discharge through alkali liquor
Cheng Wei: 12 gases of polymerization reaction kettle first put into liquid caustic soda spray column 14, passes through after liquid caustic soda spray column 14 alkali liquor spray
Air-introduced machine 16 is sent into chimney 17 and is discharged.
A kind of device preparing bodied ferric sulfate method of the present invention, molten including polymerization reaction kettle 12, ferrous sulfate
Solution kettle 18 and catalyst dissolution kettle 1.It is anti-that ferrous sulfate dissolution kettle 18, catalyst dissolution kettle 1 are connected to polymerization by pipeline respectively
Answer the top of kettle 12, polymerization reaction kettle 12 is connected with and follows for the strength strengthening the circulation of polymerization reaction kettle 12 internal-response liquid
Ring pump 13, this strong force circulation pump 13 2 end is connected to top and the bottom of polymerization reaction kettle 12；Ferrous sulfate dissolution kettle 18
It is connected on the pipeline between polymerization reaction kettle 12 and be connected with liquid-feeding pump 19 and cyclone separator 20, ferrous sulfate dissolution kettle 18
Outfan is connected with liquid-feeding pump 19, and the outfan of liquid-feeding pump 19 is connected with cyclone separator 20, cyclone separator 20 be polymerized anti-
Kettle 12 is answered to connect, ferrous sulfate dissolution kettle 18 reactant liquor is pumped into cyclone separator 20,20 points of cyclone separator by liquid-feeding pump 19
From after reactant liquor be sent to polymerization reaction kettle 12；Catalyst dissolution kettle 1 is connected to and connects on the pipeline between polymerization reaction kettle 12
It is connected to dosing pump 2 and catalyst dosing measuring tank 4, catalyst dissolution kettle 1 is connected with dosing pump 2, dosing pump 2 and catalyst dosing
Measuring tank 4 connects, and catalyst dosing measuring tank 4 is connected with polymerization reaction kettle 12, and dosing measuring tank 4 is connected with air compressor machine 3, catalysis
The catalyst of agent dissolution kettle 1 is pumped into catalyst dosing measuring tank 4 by dosing pump 2, enters the catalysis of catalyst dosing measuring tank 4
Agent is pressed into polymerization reaction kettle 12；It is provided with water-jet pump 8 at described strong force circulation pump 13 upper outlet；Polymerization is anti-
Kettle 12 top is answered to be connected with atmospheric valve 9, atmospheric valve 9 is connected with liquid caustic soda spray column 14, and liquid caustic soda spray column 14 is connected with circulating pump
15 circulations being used for spray liquid in liquid caustic soda spray column 14, liquid caustic soda spray column 14 outlet is connected with air-introduced machine 16, air-introduced machine 16
It is connected with chimney 17 again；It is connected with polymerization reaction kettle 12 and send oxygen device.
The described oxygen device that send includes liquefied oxygen tank 5, gasifier 6, spinner flowmeter 7, and liquefied oxygen tank 5 is through gasifier
6 and spinner flowmeter 7 be connected with polymerization reaction kettle 12.
Described polymerization reaction kettle 12 bottom inside is provided with least 3 along the unidirectional nozzle of reactor wall 121, nozzle
It is connected to eddy flow control valve 11, eddy flow control valve 11 is connected with strong force circulation pump 13 on 121.
Anti-blocking recoil valve 10 is connected with described strong force circulation pump 13, anti-blocking recoil valve outlet port 122 is located at polyreaction
Kettle 12 bottom.
Water, sulphuric acid, ferrous sulfate charge door, agitator are connected with described ferrous sulfate dissolution kettle 18；Catalyst is molten
It is connected with catalyst, water charge door, agitator on solution kettle 1.
Described catalyst dosing measuring tank 4 is provided with liquidometer, relief valve.Described polymerization reaction kettle 12 top is provided with
Relief valve.
Claims (10)
1. a kind of method preparing bodied ferric sulfate is it is characterised in that the method at least comprises the steps:
Step one: water, sulphuric acid are added in ferrous sulfate dissolution kettle according to a certain percentage, adds quantitative ferrous sulfate, so
After be sufficiently stirred for；Solution temperature controls at 20-35 DEG C；
Step 2: copperas solution dosing pump is squeezed into cyclone separator, then squeezes in polymerization reaction kettle, cyclone separator
The impurity such as gravel are made to be removed using ferrous sulfate is different from gravel proportion；Open the strong cyclic in polymerization reaction kettle simultaneously
Pump, and open cyclone mixing valve, so that copperas solution is fully dissolved in polymerization reaction kettle；
Step 3: quantitative catalyst is added equipped with the polymerization reaction kettle of copperas solution by pressure, is sufficiently stirred for
After be passed through oxygen and carry out continuous oxidation reaction；Control reactor pressure is 0.3-0.5mpa；Reaction is added after carrying out 1 hour again and is urged
Agent；Continue 30 minutes sampling detection ferrous sulfate contents of reaction, qualified blowing；Reaction temperature is controlled to 60-80 DEG C；
Step 4: polymerization reaction kettle emptying gas, waste gas sprays backward high altitude discharge through alkali liquor.
2. the method preparing bodied ferric sulfate according to claim 1 is it is characterised in that what described step one was added
The ferrous sulfate that it is 90% including water, the sulphuric acid of 30 ~ 98% concentration, mass content that each group is divided；The part by weight of three is: 4 ~ 6:1 ~
5:10 ~ 13.
3. the method preparing bodied ferric sulfate according to claim 1, described step 3 catalyst is sodium nitrite, two
Manganese oxide, by 2-3:1 mixed configuration catalyst, catalyst accounts for 0.3 ~ 0.5% that addition accounts for reaction kettle for reaction thing total amount；The
Once add 60% catalytic amount, the catalytic amount that second adds 40%, percentage ratio here is weight percentage.
4. the method preparing bodied ferric sulfate according to claim 1, after described step 2 opens cyclone mixing valve, if
In polymerization reaction kettle bottom at least 3 along reactor wall unidirectional nozzle hydrojet, reactant liquor is made to carry out same direction rotation
Flowing, plays stirring action；Described step 2 sets up water-jet pump in polymerization reaction kettle strong cyclic pump discharge, will be anti-
Answer the oxygen that can not react in time inside kettle and nitrogen dioxide by being sufficiently mixed with reactant liquor, to improve utilization rate of raw materials,
Increase the response time.
5. the method preparing bodied ferric sulfate according to claim 1, the quantitative catalyst solution of described step 3 leads to
The method of excess pressure addition polymerization reaction kettle is: first catalyst addition catalyst dissolution kettle is made it fully dissolve, then by adding
Teat pipette pumps into catalyst to dosing measuring tank, opens and measures tank connected air compressor machine with catalyst dosing, makes catalyst dosing meter
The pressure of measuring tank is more than 0.5mpa so that catalyst is pressed into polymerization reaction kettle；The method being passed through oxygen is: in liquefied oxygen tank
Oxygen be passed into polymerization reaction kettle after gasifier gasification, then through spinner flowmeter.
6. the method preparing bodied ferric sulfate according to claim 1, described step 4 polymerization reaction kettle vent gas treatment,
Emptying gas through the process that alkali liquor sprays backward high altitude discharge are: polymerization reaction kettle puts into liquid caustic soda spray gas first
Tower, sends into smoke stack emission by air-introduced machine after liquid caustic soda spray column alkali liquor spray.
7. the device preparing bodied ferric sulfate method according to claim 1 is it is characterised in that it is anti-including polymerization
Answer kettle, ferrous sulfate dissolution kettle and catalyst dissolution kettle, ferrous sulfate dissolution kettle, catalyst dissolution kettle are connected by pipeline respectively
To the top of polymerization reaction kettle, the strength for strengthening the circulation of polymerization reaction kettle internal-response liquid is connected with polymerization reaction kettle
Circulating pump, this strong force circulation pump two end is connected to top and the bottom of polymerization reaction kettle；Ferrous sulfate dissolution kettle is connected to
Liquid-feeding pump and cyclone separator, the outfan of ferrous sulfate dissolution kettle and liquid-feeding pump are connected with the pipeline between polymerization reaction kettle
Connect, the outfan of liquid-feeding pump is connected with cyclone separator, and cyclone separator is connected with polymerization reaction kettle, ferrous sulfate dissolution kettle
Reactant liquor is pumped into cyclone separator by liquid-feeding pump, and the reactant liquor after cyclone separator separates is sent to polymerization reaction kettle；Catalysis
Agent dissolution kettle is connected on the pipeline between polymerization reaction kettle and is connected with dosing pump and catalyst dosing measuring tank, catalyst dissolution
Kettle is connected with dosing pump, and dosing pump is connected with catalyst dosing measuring tank, and catalyst dosing measuring tank is connected with polymerization reaction kettle,
Dosing measuring tank is connected with air compressor machine, and the catalyst of catalyst dissolution kettle is pumped into catalyst dosing measuring tank by dosing pump, enters
The catalyst entering catalyst dosing measuring tank is pressed into polymerization reaction kettle；It is provided with described strong force circulation pump upper outlet
Water-jet pump；Polymerization reaction kettle top is connected with atmospheric valve, and atmospheric valve is connected with liquid caustic soda spray column, on liquid caustic soda spray column alkali
It is connected with circulating pump for the circulation of spray liquid in liquid caustic soda spray column, liquid caustic soda spray column outlet is connected with air-introduced machine, blower fan
It is connected with chimney again；It is connected with polymerization reaction kettle and send oxygen device.
8. the device preparing bodied ferric sulfate method according to claim 7 is it is characterised in that described send oxygen device bag
Include liquefied oxygen tank, gasifier, spinner flowmeter, liquefied oxygen tank is connected with polymerization reaction kettle through gasifier and spinner flowmeter
Connect.
9. the device preparing bodied ferric sulfate method according to claim 7 is it is characterised in that polymerization reaction kettle bottom sets
There are at least 3 along the unidirectional nozzle of reactor wall, nozzle is connected with strong force circulation pump by eddy flow control valve；Strong cyclic
Anti-blocking recoil valve is connected with pump, anti-blocking recoil valve outlet port is located at polymerization reaction kettle bottom.
10. the device preparing bodied ferric sulfate method according to claim 7 is it is characterised in that described ferrous sulfate is molten
It is connected with water, sulphuric acid, ferrous sulfate charge door, agitator on solution kettle；Catalyst, water charging are connected with catalyst dissolution kettle
Mouth, agitator；Described catalyst dosing measuring tank is provided with liquidometer, relief valve, and described polymerization reaction kettle top is provided with
Relief valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009817.XA CN104591297B (en) | 2015-01-09 | 2015-01-09 | Method and device for preparing polymeric ferric sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009817.XA CN104591297B (en) | 2015-01-09 | 2015-01-09 | Method and device for preparing polymeric ferric sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104591297A CN104591297A (en) | 2015-05-06 |
| CN104591297B true CN104591297B (en) | 2017-01-18 |
Family
ID=53117414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510009817.XA Expired - Fee Related CN104591297B (en) | 2015-01-09 | 2015-01-09 | Method and device for preparing polymeric ferric sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104591297B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110383A (en) * | 2015-08-18 | 2015-12-02 | 铜陵海陵环保科技有限责任公司 | Polymeric ferric sulfate reaction kettle |
| CN107140693B (en) * | 2017-07-11 | 2019-04-26 | 深圳市长隆科技有限公司 | A kind of bodied ferric sulfate continuous process system and its method |
| CN108751369B (en) * | 2018-06-08 | 2021-03-26 | 高密博宇环保科技有限公司 | Production method of polymeric ferric sulfate |
| CN109081382A (en) * | 2018-10-25 | 2018-12-25 | 马鞍山健鼎化工有限公司 | A kind of processing technology of bodied ferric sulfate |
| CN110468287B (en) * | 2019-08-26 | 2020-05-15 | 中南大学 | Method for removing iron by goethite method by using manganese-containing smoke dust as catalyst |
| CN111672276A (en) * | 2020-06-01 | 2020-09-18 | 深圳市长隆科技有限公司 | Resource utilization process of waste gas in production process of polymeric ferric sulfate |
| CN111762806A (en) * | 2020-08-17 | 2020-10-13 | 刘洪亮 | Aluminum ingot dissolving system |
| CN113955808A (en) * | 2021-03-12 | 2022-01-21 | 衡阳市建衡实业有限公司 | Method for producing polymeric ferric sulfate by using naturally oxidized and deteriorated ferrous sulfate as raw material |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1219706C (en) * | 2003-08-04 | 2005-09-21 | 侯勇 | High concentration high molecular poly iron type water purifier |
| CN1621353A (en) * | 2003-11-26 | 2005-06-01 | 穆顺勇 | Production method of coagulant-polymeric ferric sulfate used for electric power |
| CN201165473Y (en) * | 2007-10-17 | 2008-12-17 | 成都齐力水处理科技有限公司 | Polymeric ferric sulfate production apparatus |
| CN101249987A (en) * | 2008-03-17 | 2008-08-27 | 李绍通 | Method for synthesizing polymeric ferric sulphate |
| CN102515329A (en) * | 2011-12-31 | 2012-06-27 | 山东思源净水科技有限公司 | Polymeric ferric sulfate and production method thereof |
| CN102951713A (en) * | 2012-11-02 | 2013-03-06 | 华南理工大学 | Polymeric ferric sulfate water treatment agent and preparation method thereof |
| CN104071853B (en) * | 2014-07-17 | 2016-04-20 | 广西平果锋华科技有限公司 | Waste Sulfuric Acid and ferrous sulfate oxygen pressing is utilized to produce the method for bodied ferric sulfate |
-
2015
- 2015-01-09 CN CN201510009817.XA patent/CN104591297B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN104591297A (en) | 2015-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104591297B (en) | Method and device for preparing polymeric ferric sulfate | |
| CN104071853B (en) | Waste Sulfuric Acid and ferrous sulfate oxygen pressing is utilized to produce the method for bodied ferric sulfate | |
| CN105692717B (en) | A kind of bodied ferric sulfate and preparation method thereof | |
| CN104843785B (en) | Titanium white continuous acid hydrolysis method and ore deposit used acid premixing groove | |
| CN105129867A (en) | Method used for preparing polymeric ferric sulfate from sulfuric acid waste liquid | |
| CN103864154A (en) | Production method of liquid polymeric ferric sulfate water purifying agent | |
| CN102718268B (en) | Method for producing solid poly ferric sulfate | |
| CN106938866A (en) | A kind of desulfurization wastewater resource utilization system and method | |
| CN103539206B (en) | Wet method for preparing iron oxide red through introducing crystal form accelerant | |
| CN205500803U (en) | Magnesium hydroxide production basic magnesium carbonate's equipment | |
| CN206325543U (en) | Polymeric ferric sulfate production apparatus | |
| CN206985743U (en) | A kind of bodied ferric sulfate continuous process system | |
| CN114804419B (en) | Method for reducing hardness of dust-removing water of converter flue gas by using desulfurization ash of coke oven | |
| CN100484881C (en) | Method of producing iron oxide red using ferrous sulphate | |
| CN111646502B (en) | Slag ore mixing continuous acidolysis leaching method and equipment | |
| CN204569678U (en) | The low BC of a kind of DMTO device is than the advanced treatment apparatus of waste water | |
| CN106007047A (en) | Device and method for treating black water discharged from coal gasification process | |
| CN106396187A (en) | Cyanide wastewater treating and recycling method | |
| CN209602187U (en) | A kind of dyeing and printing sewage processing system based on Fenton's reaction | |
| CN213012149U (en) | Waste water neutralization premixing reaction device and neutralization system | |
| CN206751417U (en) | A kind of scale pressure carbonization device for preparing nano-calcium carbonate | |
| CN106745304B (en) | A method of preparing ferrate solution online | |
| CN218854292U (en) | System for continuous production liquid polyferric sulfate | |
| CN104975339A (en) | Method for preparing nano calcium carbonate whiskers by use of binary complex crystal form control agent of sodium salicylate and ammonium nitrate | |
| CN109678240A (en) | A kind of dyeing and printing sewage processing system and method based on Fenton's reaction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170118 Termination date: 20220109 |