CN100582018C - Method for producing solid polymeric ferric chloride using ferrous chloride crystal as raw material - Google Patents
Method for producing solid polymeric ferric chloride using ferrous chloride crystal as raw material Download PDFInfo
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Abstract
The present invention relates to a preparation method of solid polyferric chloride by ferrous chloride crystal, which comprises the steps of that:(1)the ferrous chloride crystal is added into the reaction kettle and heated into 45~65 DEG C after adding water therein, then the reaction kettle is started, and compressed air is fed into the reaction kettle from the bottom, and then the heating is stopped when the temperature is up to 85~95 DEG C; (2) the alkaline water solution is injected into the reaction kettle from the upper part, and the hydrochloric acid water solution is added under the liquid surface of the reactant, the temperature is controlled at 90~95 DEG C, the filling of alkaline water solution is stopped when the content of Fe2+ is not more than 0.15%, the filling of hydrochloric acid water solution is stopped when the basicity is up to 5~10 %, and then compressed air is fed while agitating, then the material, while hot, is pressed into a tabletting machines to be cooled to solid which is crushed to obtain the solid polyferric chloride with a high content. The solid polyferric chloride of the present invention has stable quality, low cost, excellent stability, no secondary pollution; besides, the procedure does not have waste gases, waste water and waste residue.
Description
Technical field
The invention belongs to the water treatment agent industry in environmental protection field.The production method that relates to a kind of solid polymerization iron(ic) chloride, particularly relating to a kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal.
Background technology
The products molecule formula that the present invention produces is [Fe
2(OH)
nCl
6-n]
mPoly-ferric chloride (PFC) is the inorganic polymer water treatment coagulant of better, the no residual hazard of another performance after polymerize aluminum chloride (PAC) and bodied ferric sulfate (PFS).
Along with global industrialization development and Increase of population, the scarcity of water resources and pollute one of the ecological crisis become countries in the world and faced.And utilize modern science and technology more reasonably to utilize and protect water resources, become the only way of realizing target of sustainable development.Nearest twenty year sequential use along with various environmental protection water treatment agents, water technology brought into play important effect in the development of Treatment of Industrial Water technology.This emerging environmental protection industry (epi) has formed huge market potential, is just presenting flourish trend in China.
Flocculation agent (coagulating agent, water purification agent) is a most important component in the Treatment of Industrial Water medicament, and its effect is to make water-borne glue body particle take off steady and the formation flocs unit, removes to reach the water purifying purpose thereby be able to separate from water.
Flocculation agent commonly used has Tai-Ace S 150, aluminium chlorohydroxide, ferrous sulfate, iron trichloride, bodied ferric sulfate etc.All there is some shortcoming in these water purification agents, as relatively poor to removal effects such as colourity, heavy metal ion, SS, CODcr, BOD and radioactive substances; The water purification agent of aluminium salt series is applied to can bring a large amount of Al in the water treatment
3+
Since the eighties in 20th century since Japan at first synthesizes liquid polymeric iron(ic) chloride (PFC), enjoy people's attention with its good application performance.In existing used mineral-type coagulating agent, poly-ferric chloride has superior coagulation performance, it has intensive charge neutrality cohesion ability and absorption crane span structure ability, significantly improved coagulation effect, not only has safe lifeless matter toxicity, and have flocs unit and form characteristics such as speed is fast, the alumen ustum macrostructure is closely knit, consumption is few, sedimentation is fast, dehydration property is good, and residual, the no deleterious aluminum ion of the water colorless degree after the processing is residual.Especially more have superiority for processing low temperature, low turbidity water, be particularly suitable for the water treatment in winter of northern frore area.The pH value wide ranges (pH4～11, best pH6～9) that it is suitable for, and must not add other coagulant aids.The ability that significant turbidity removal, oil removing, deodorizing, decolouring, reduction COD and BOD are all arranged in the processing of domestic water, process water, municipal wastewater, trade effluent and petroleum waste water.Through equal dosage simultaneous test, purifying water effect is better than inorganic polymer flocculants such as bodied ferric sulfate, polymerize aluminum chloride.
Poly-ferric chloride is compared with traditional low-molecular-weight ferrous sulfate, iron trichloride, has not only improved cleaning water greatly, has reduced dosage, and the heavy corrosion problem to pipe-line equipment is also overcome.
Poly-ferric chloride is compared with bodied ferric sulfate, more has superiority at processing low temperature, low turbidity water.The hidden danger of this product non-secondary pollution in addition.Now mostly the polyaluminum sulfate iron process of producing is with the nitrite to be Catalyst Production, contains nitrite ion in the product, is deleterious to human body when these ion usage quantitys are big.Al
3+Can cause the human brain atrophy, nitrite ion has carcinogenic danger.
In recent years, all at trial production liquid-type poly-ferric chloride, the operational path that is adopted is to be divided into two kinds of operational paths basically both at home and abroad.A kind of is alkalization method, and another kind is a catalytic oxidation.The former is to be that raw material is after being adjusted to certain basicity in the presence of the yellow soda ash with iron trichloride, add stablizer again and get product: the latter is a raw material with iron protochloride liquid and hydrochloric acid, under different strong oxidizer effects such as nitrite, oxymuriate, concentrated nitric acid, hydrogen peroxide, oxygen, react, the control of polymerization basicity is to realize by disposable adding hydrochloric acid, for the shelf lives that guarantees product need add stablizer and could realize.All there is product effective content not high (the total iron content maximum is 13%) in both, and the problem of poor storage stability.
Poly-ferric chloride can replace inorganic polymer coagulants such as existing polymerize aluminum chloride and bodied ferric sulfate fully, can use in multiple water treatment, so wide market application prospect is arranged.The regrettably less stable of liquid polymeric iron(ic) chloride, though added the phosphoric acid salt stablizer in the synthetic fluid poly-ferric chloride, the product stabilising effect of producing in batches is still not very good, so obtain application more widely.Market presses for the high-load solid polymerization iron(ic) chloride product that has high stability and be convenient to transport.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, providing a kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, and technical scheme of the present invention is summarized as follows:
1. one kind is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, it is characterized in that comprising the steps:
(1) in reactor, drops into 500 kilograms of iron protochloride crystal, slow heat temperature raising after adding 10～80 kg of water, when being warmed up to 45-65 ℃, crystal is all molten molten to be liquid, start the reactor agitator, and in reactor bottom by the 80-120 liter/minute flow feed pressurized air continuously or oxygen carries out catalyzed oxidation to material, when temperature rises to 85-95 ℃, stop heating; (2) adding mass percentage concentration at reactor top charging opening with the flow of 0.8-1.2 kg/minute in 4-6 minute is 30～60% initiator solution or suspension liquid, reacted 8～10 minutes, under the reactant liquid level, drip mass percentage concentration and be 5～10 kilograms of the aqueous hydrochloric acids of 20～35% concentration, reacted 8～10 minutes, adding mass percentage concentration at reactor top charging opening with the flow of 0.8-1.2 kg/minute in 4-6 minute again is 30～60% initiator solution or suspension liquid, reacted 8～10 minutes, under the reactant liquid level, drip mass percentage concentration and be 5～10 kilograms of the aqueous hydrochloric acids of 20～35% concentration, reacted 8～10 minutes, so hocket 3-5 time, controlled temperature reacts in 90～95 ℃ of scopes, Fe in detecting reactant
2+Stopped to add initiator solution or suspension liquid at≤0.15% o'clock, reach at 5～10% o'clock at basicity and stop to add aqueous hydrochloric acid, stirred 4-10 minute, feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
Described iron protochloride crystal is Iron dichloride tetrahydrate crystal or six hydration iron protochloride crystal or Iron dichloride dihydrate crystal or a hydration iron protochloride crystal or one of half hydration iron protochloride crystal or the ferrous crystal of anhydrous chlorides of rase.
Described initiator is NaOH or CaO or Ca (OH)
2Or Na
2CO
3In at least a.
The mass percentage concentration of described initiator solution or suspension liquid is 40～50%.
Advantage of the present invention is:
Use the solid polymerization iron(ic) chloride that the present invention produces, steady quality, production cost is low, product stability good, no three wastes generation in the production process, and the hidden danger of product non-secondary pollution is the favorable substitutes of bodied ferric sulfate and polymerize aluminum chloride.
Embodiment
The present invention is to be raw material with the iron protochloride crystal, adopting alkaline aqueous solution or suspension liquid under 85～95 ℃ of temperature is reaction initiator, is catalyzer with the pressurized air or the oxygen of continuous feeding, regulates basicity with hydrochloric acid, the polymerization of segmentation catalyzed reaction generates the technology of poly-ferric chloride fast.
Reaction principle:
The adding of initiator alkaline aqueous solution or suspension liquid has destroyed iron protochloride crystalline structure in molten molten iron protochloride, generates unsettled ferrous hydroxide at an easy rate.Airborne oxygen is a kind of very strong oxygenant, and its redox potential is E (O
2/ H
2O)-and 1.23V, can under normal temperature and alkaline condition, at an easy rate unsettled ferrous hydroxide be oxidized to ironic hydroxide, reaction is carried out to generating the ironic hydroxide direction.When the amount of ironic hydroxide generation reaches a certain amount of, can form the very big polymer of viscosity, speed of response is slowed down.Add hydrochloric acid this moment polymer is regulated then some ironic hydroxide generation iron trichloride, unnecessary hydrochloric acid can be oxidized to iron trichloride with iron protochloride under oxygen catalysis.When controlling the adding quantity of hydrochloric acid, will obtain the poly-ferric chloride [Fe of different polymerization degree
2(OH)
nCl
6-n]
mProduct.
Reaction equation is as follows:
FeCl
2+Ca(OH)
2-Fe(OH)
2+CaCl
2
4Fe(OH)
2+O
2+2H
2O-4Fe(OH)
3
Fe(OH)
3+3HCl-FeCl
3+3H
2O
4FeCl
2+4HCl+O
2-4FeCl
3+2H
2O
Above-mentioned being reflected in normal temperature and the air just can be carried out lentamente, if under hot conditions, and then oxidation rapidly, the principle of Here it is direct production solid polymerization iron(ic) chloride.
Because iron protochloride is a catalytic polymerization in liquid phase, its reacted poly-ferric chloride concentration is solid product at normal temperatures, but therefore do not need to reacted material carry out evaporation concentration or spraying drying just direct production go out solid phase prod, save a large amount of energy, belonged to the energy-saving advanced technologies of low power consuming.Because be that solid phase prod is convenient to long-distance transportation, reduced the Product transport cost, and enlarged the sale radius.This Technology is compared with aforesaid two kinds of common processes and is had the following advantages:
Do not use nitrite, concentrated nitric acid, oxymuriate to be catalyzer in the production, so the pollution of nitrogenfree oxide gas, chlorine in the production process, therefore noresidue nitrite in the product can not produce secondary pollution.
Molten molten iron protochloride is thermo-negative reaction with the reaction of alkali lye in the production process, and the reaction of ferric hydroxide colloid and hydrochloric acid is weak thermopositive reaction, and two kinds of raw materials are alternately to add, and generating heat and absorb heat can reach balance substantially, does not have the possibility of heat release bumping rapidly.Therefore when strict control reaction temperature (is no more than 100 ℃) between 90-95 ℃, because hydrochloric acid is to take to drip under the reaction liquid level, enter very fast and material reaction behind the liquid, in closed reaction kettle, can not produce azeotrope (110 ℃ of the azeotropic points) gas evolution of hydrochloric acid and water, therefore can not exist atmospheric pollution.
Is raw material because be with the Iron dichloride tetrahydrate crystal, these raw material sources are in the comprehensive utilization of steel acid lotion, crystallized product purity is higher, alkali lye (or suspension liquid) that adds and hydrochloric acid all are that the product of participating in generation in the solubility raw material of chemical reaction and the reaction all is water-soluble, need not the removal of impurity, therefore there is not the generation of waste residue.
Because reaction is to carry out in molten molten liquid phase, product will become solid after cooling, need not dewater and solid-liquid separation, therefore not have the generation of waste water, and this patent technology three-waste free discharge belongs to cleaner production.
Twice intermediate controlled link is arranged when production process is closed on terminal point, can adjust indexs such as basicities according to the requirement that the user handles different quality, so stable and reliable product quality.
Being equipped with liquid polymeric iron(ic) chloride (PFC) with former oxygen catalyzing liquid phase oxidation legal system compares, because raw material reacts formation ferrous hydroxide earlier easily with alkali lye (or suspension liquid) under the high density condition, ferrous hydroxide is extremely unstable, with have minor amounts of oxygen to exist can to carry out rapid reaction generation ferric hydroxide colloid down, ironic hydroxide and hydrochloric acid rapid reaction are carried out ion-exchange and are generated iron trichloride, it is therefore ferrous that to change into ferric speed of response very fast, the oxygen amount that consumes is few, therefore speed of response is fast, the reaction times that needs is short, the utilization ratio height of oxygen, so consumption is few.
Because alkali lye (or suspension liquid) and hydrochloric acid alternately drip, the new colloid ironic hydroxide that produces forms the back and carries out reactive polymeric with hydrochloric acid at once, can not form a large amount of aggregate and precipitate of colloid ironic hydroxide, therefore the polymerization degree is controlled easily, reaction finishes the back and cools off the repolymerization that has stopped poly-ferric chloride at once, therefore can stablize preservation need not adding under the stablizer condition of phosphorus-containing acid ion solid, stability can reach 2 years.Product inspection method and reference quality standard State Standard of the People's Republic of China " water purification agent---bodied ferric sulfate (II) " are (GB14591-2006).
Solid polymerization iron(ic) chloride technical target of the product
| Sequence number | Index name | Technical indicator |
| 1 | Outward appearance | The tawny pressed powder |
| 2 | Total iron content 〉=% | 19 |
| 3 | Reducing substances is (with ferrous Fe 2+Meter) content≤% | 0.15 |
| 4 | Basicity (basicity) % | 8.0～16.0 |
| 5 | Water-insoluble≤% | 0.5 |
| 6 | PH value (1% solution) | 2.0-3.0 |
| 7 | Arsenic (As) content≤% | 0.0005 |
| 8 | Plumbous (Pb) content≤% | 0.0010 |
The present invention is further illustrated below in conjunction with specific embodiment:
Embodiment 1
With iron protochloride (FeCl
2) content is the by product Iron dichloride tetrahydrate crystal (FeCl that reclaims from steel acid lotion more than 60%
2.4H
2O) in 500 kilograms of input reactors, add after 10 kg of water slowly heat temperature raising, crystal all dissolves when temperature arrives 50 ℃ of left and right sides, start the reactor agitator this moment, and bottom reactor, material is carried out oxidation by 100 liters of/minute flows feeding pressurized air, when slowly being warmed up to 90 ℃, reactant stops heating.Adding mass percentage concentration at reactor top charging opening with the flow of 1 kg/minute is 48% aqueous sodium hydroxide solution, adds 5 kilograms in 5 minutes.React after 10 minutes, dripping mass percentage concentration with the flow of 1 kg/minute under the reactant liquid level is 10 kilograms of 28% technical hydrochloric acids, dropwises the back and keeps reaction 10 minutes.The sodium hydroxide lye that adds 48% concentration with the flow of 1 kg/minute at reactor top charging opening adds 5 kilograms in 5 minutes again.React after 10 minutes, under the reactant liquid level, drip 10 kilograms of the technical hydrochloric acids of 28% concentration, dropwise the back and keep reaction 10 minutes with the flow of 1 kg/minute.So hocket, controlled temperature reacts in 90～95 ℃ of scopes, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, the detection basicity reaches at 5% o'clock and stops to add technical hydrochloric acid, fully stir after 10 minutes, repetition measurement ferrous content basicity, reach and feed pressurized air behind the stability number and material is pressed into to make in the sheet machine while hot is cooled to solid, get 600 kilograms of solid polymerization iron(ic) chloride products, total iron content 〉=22% after the pulverizing.
Reactor is the closed reactor that has rot-resistant and have heating, cooling, agitating function, a charging opening on reactor top is provided with the fluid drips feeder apparatus, another charging opening is provided with extension tubing, length can reach 30 centimeters under the molten liquid level after molten of iron protochloride crystal, does not expose material liquid surface to guarantee it in the stirring reaction process.Reactor bottom is provided with a ventpipe, makes pressurized air can enter into molten molten reaction mass.
Embodiment 2:
With iron protochloride (FeCl
2) content is the by product six water iron protochloride crystal (FeCl that reclaim from steel acid lotion more than 55%
2.6H
2O) in 500 kilograms of input reactors, slow heat temperature raising, crystal all dissolves when temperature arrives 50 ℃ of left and right sides, start the reactor agitator this moment, and bottom reactor, material is carried out oxidation by 100 liters of/minute flows feeding pressurized air, when slowly being warmed up to 90 ℃, reactant stops heating.Add the sodium hydroxide lye of 48% concentration at reactor top charging opening with the flow of 1 kg/minute, add 5 kilograms in 5 minutes.React after 10 minutes, under the reactant liquid level, drip 8 kilograms of the technical hydrochloric acids of 30% concentration, dropwise the back and keep reaction 10 minutes with the flow of 1 kg/minute.The sodium hydroxide lye that adds 48% concentration with the flow of 1 kg/minute at reactor top charging opening adds 5 kilograms in 5 minutes again.React after 10 minutes, under the reactant liquid level, drip 8 kilograms of the technical hydrochloric acids of 30% concentration, dropwise the back and keep reaction 10 minutes with the flow of 1 kg/minute.So hocket, controlled temperature reacts in 90～95 ℃ of scopes, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, the detection basicity reaches at 10% o'clock and stops to add technical hydrochloric acid, fully stir after 10 minutes, repetition measurement ferrous content basicity, reach and feed pressurized air behind the stability number and material is pressed into to make in the sheet machine while hot is cooled to solid, get 550 kilograms of solid polymerization iron(ic) chloride products, total iron content 〉=22% after the pulverizing.
Embodiment 3:
With iron protochloride (FeCl
2) content is the by product two water iron protochloride crystal (FeCl that reclaim from steel acid lotion more than 70%
2.2H
2O) in 500 kilograms of input reactors, add after 45 kg of water slowly heat temperature raising, crystal all dissolves when temperature arrives 55 ℃ of left and right sides, start the reactor agitator this moment, and bottom reactor, material is carried out oxidation by 100 liters of/minute flows feeding pressurized air, when slowly being warmed up to 90 ℃, reactant stops heating.Add the aqueous sodium hydroxide solution of 48% concentration at reactor top charging opening with the flow of 1 kg/minute, add 5 kilograms in 5 minutes.React after 10 minutes, under the reactant liquid level, drip 10 kilograms of the technical hydrochloric acids of 31% concentration, dropwise the back and keep reaction 10 minutes with the flow of 1 kg/minute.The sodium hydroxide lye that adds 48% concentration with the flow of 1 kg/minute at reactor top charging opening adds 10 kilograms in 5 minutes again.React after 10 minutes, under the reactant liquid level, drip 10 kilograms of the technical hydrochloric acids of 31% concentration, dropwise the back and keep reaction 10 minutes with the flow of 1 kg/minute.So hocket, controlled temperature reacts in 90～95 ℃ of scopes, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, the detection basicity reaches at 10% o'clock and stops to add technical hydrochloric acid, fully stir after 10 minutes, repetition measurement ferrous content basicity, reach and feed pressurized air behind the stability number and material is pressed into to make in the sheet machine while hot is cooled to solid, get 650 kilograms of solid polymerization iron(ic) chloride products, total iron content 〉=25% after the pulverizing.
Embodiment 4:
A kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, comprise the steps: that (1) drop into 500 kilograms of Iron dichloride dihydrate crystal in reactor, after adding 45 kg of water, slow heat temperature raising, crystal all dissolves when temperature arrives 55 ℃ of left and right sides, start the reactor agitator, and by the continuous aerating oxygen of 80 liters/minute flow material is carried out catalyzed oxidation, when temperature rises to 85 ℃, stop heating in the reactor bottom; (2) adding mass percentage concentration at reactor top charging opening with the flow of 1.2 kg/minute in 5 minutes is 30% Na
2CO
36 kilograms of the aqueous solution, reacted 10 minutes, drip mass percentage concentration and be 5 kilograms of the aqueous hydrochloric acids of 35% concentration under the reactant liquid level, reacted 8 minutes, adding mass percentage concentration at reactor top charging opening with the flow of 1.2 kg/minute in 5 minutes again is 30% Na
2CO
36 kilograms of the aqueous solution reacted 10 minutes, dripped mass percentage concentration and be 5 kilograms of the aqueous hydrochloric acids of 35% concentration under the reactant liquid level, reacted 8 minutes, so hocketed 3 times, and controlled temperature reacts at 90 ℃, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, reach at 6% o'clock at basicity and stop to add aqueous hydrochloric acid, stirred 5 minutes, feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
Embodiment 5:
A kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, comprise the steps: that (1) drop into 500 kilogram of one hydration iron protochloride crystal in reactor, delay heat temperature raising after adding 50 kg of water, in the time of 65 ℃, crystal all dissolves, start the reactor agitator, and feed pressurized air in reactor bottom continuously by 90 liters/minute flow material is carried out catalyzed oxidation, when temperature rises to 95 ℃, stop heating; (2) adding mass percentage concentration at reactor top charging opening with the flow of 1 kg/minute in 6 minutes is 60% Ca (OH)
26 kilograms of suspension liquids, reacted 9 minutes, drip mass percentage concentration and be 10 kilograms of the hydrochloric acid solns of 30% concentration under the reactant liquid level, reacted 10 minutes, adding mass percentage concentration at reactor top charging opening with the flow of 1 kg/minute in 5 minutes again is 60% initiator Ca (OH)
2Suspension liquid reacted 8～10 minutes, dripped mass percentage concentration and be 10 kilograms of the hydrochloric acid solns of 30% concentration under the reactant liquid level, reacted 9 minutes, so hocketed 4 times, and controlled temperature reacts at 95 ℃, Fe in detecting reactant
2+Stopped to add Ca (OH) at≤0.2% o'clock
2Suspension liquid reaches at 7% o'clock at basicity and stops to add hydrochloric acid soln, stirs 4 minutes, and feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
Embodiment 6:
A kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, comprise the steps: that (1) drop into 500 kilogram of half hydration iron protochloride crystal in reactor, delay heat temperature raising after adding 60 kg of water, in the time of 65 ℃, crystal all dissolves, start the reactor agitator, and feed pressurized air in reactor bottom continuously by 110 liters/minute flow material is carried out catalyzed oxidation, when temperature rises to 90 ℃, stop heating; (2) adding the reduced mass percentage concentration at reactor top charging opening with the flow of 1.2 kg/minute in 5 minutes is 40% CaO suspension liquid, reacted 8 minutes, under the reactant liquid level, drip mass percentage concentration and be 8 kilograms of the aqueous hydrochloric acids of 28% concentration, reacted 8 minutes, adding the reduced mass percentage concentration at reactor top charging opening with the flow of 1.2 kg/minute in 4 minutes again is 40% initiator CaO suspension liquid, reacted 10 minutes, under the reactant liquid level, drip mass percentage concentration and be 8 kilograms of the aqueous hydrochloric acids of 28% concentration, reacted 8 minutes, so hocket 4 times, controlled temperature reacts at 93 ℃, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, reach at 10% o'clock at basicity and stop to add aqueous hydrochloric acid, stirred 6 minutes, feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
Embodiment 7:
A kind of is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, comprise the steps: that (1) drop into 500 kilograms of ferrous crystal of anhydrous chlorides of rase in reactor, delay heat temperature raising after adding 80 kg of water, in the time of 65 ℃, crystal all dissolves, start the reactor agitator, and feed pressurized air in reactor bottom continuously by 120 liters/minute flow material is carried out catalyzed oxidation, when temperature rises to 92 ℃, stop heating; (2) adding mass percentage concentration at reactor top charging opening with the flow of 0.8 kg/minute in 5 minutes is 4 kilograms of 50% the NaOH aqueous solution, reacted 10 minutes, under the reactant liquid level, drip mass percentage concentration and be 10 kilograms of the aqueous hydrochloric acids of 20% concentration, reacted 10 minutes, adding mass percentage concentration at reactor top charging opening with the flow of 0.8 kg/minute in 5 minutes again is 4 kilograms of 50% the initiator NaOH aqueous solution, reacted 10 minutes, under the reactant liquid level, drip mass percentage concentration and be 10 kilograms of the aqueous hydrochloric acids of 20% concentration, reacted 10 minutes, so hocket 5 times, controlled temperature reacts at 90 ℃, Fe in detecting reactant
2+Stopped to add alkali lye at≤0.2% o'clock, reach at 10% o'clock at basicity and stop to add aqueous hydrochloric acid, stirred 5 minutes, feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
Claims (4)
1. one kind is the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, it is characterized in that comprising the steps:
(1) in reactor, drops into 500 kilograms of iron protochloride crystal, slow heat temperature raising after adding 10～80 kg of water, when being warmed up to 45-65 ℃, crystal is all molten molten to be liquid, start the reactor agitator, and in reactor bottom by the 80-120 liter/minute flow feed pressurized air continuously or oxygen carries out catalyzed oxidation to material, when temperature rises to 85-95 ℃, stop heating; (2) adding mass percentage concentration at reactor top charging opening with the flow of 0.8-1.2 kg/minute in 4-6 minute is 30～60% initiator solution or suspension liquid, reacted 8～10 minutes, under the reactant liquid level, drip mass percentage concentration and be 5～10 kilograms of the aqueous hydrochloric acids of 20～35% concentration, reacted 8～10 minutes, adding mass percentage concentration at reactor top charging opening with the flow of 0.8-1.2 kg/minute in 4-6 minute again is 30～60% initiator solution or suspension liquid, reacted 8～10 minutes, under the reactant liquid level, drip mass percentage concentration and be 5～10 kilograms of the aqueous hydrochloric acids of 20～35% concentration, reacted 8～10 minutes, so hocket 3-5 time, controlled temperature reacts in 90～95 ℃ of scopes, Fe in detecting reactant
2+Stopped to add initiator solution or suspension liquid at≤0.15% o'clock, reach at 5～10% o'clock at basicity and stop to add aqueous hydrochloric acid, stirred 4-10 minute, feeding pressurized air is pressed into material while hot to make in the sheet machine and is cooled to solid, becomes the high content of solid poly-ferric chloride after the pulverizing.
2. according to claim 1 a kind of be the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, it is characterized in that described iron protochloride crystal is Iron dichloride tetrahydrate crystal or six hydration iron protochloride crystal or Iron dichloride dihydrate crystal or a hydration iron protochloride crystal or one of half hydration iron protochloride crystal or the ferrous crystal of anhydrous chlorides of rase.
3. according to claim 1 a kind of be the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, it is characterized in that described initiator is NaOH or Na
2CO
3Or it is at least a among Ca (OH) 2 or the CaO.
4. according to claim 1 a kind of be the method for raw material production solid polymerization iron(ic) chloride with the iron protochloride crystal, the mass percentage concentration that it is characterized in that described initiator solution or suspension liquid is 40～50%.
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| CN105170070A (en) * | 2015-07-08 | 2015-12-23 | 黄立维 | Denitration and desulfurization ferric chloride solid particles and preparation method thereof |
| CN111153477A (en) * | 2020-01-07 | 2020-05-15 | 斯瑞尔环境科技股份有限公司 | Preparation method of powdery polyferric chloride solid |
| CN111170430A (en) * | 2020-01-07 | 2020-05-19 | 斯瑞尔环境科技股份有限公司 | Method for producing blocky polyferric chloride solid |
| CN111847611A (en) * | 2020-06-08 | 2020-10-30 | 江苏沃谱瑞环境科技有限公司 | Method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid |
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| 化学化工大辞典（上、下册）. 《化学化工大辞典》编委会，化学工业出版社物辞书编辑部，1553，化学工业出版社. 2003 |
| 化学化工大辞典（上、下册）. 《化学化工大辞典》编委会，化学工业出版社物辞书编辑部，1553，化学工业出版社. 2003 * |
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