CN101125697A - Method for producing water treatment coagulant by using coal gangue - Google Patents
Method for producing water treatment coagulant by using coal gangue Download PDFInfo
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- CN101125697A CN101125697A CNA2007100185328A CN200710018532A CN101125697A CN 101125697 A CN101125697 A CN 101125697A CN A2007100185328 A CNA2007100185328 A CN A2007100185328A CN 200710018532 A CN200710018532 A CN 200710018532A CN 101125697 A CN101125697 A CN 101125697A
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Abstract
The invention relates to a method to produce water processing coagulant with coal gangue. The method essentially consists of the steps: grinding and processing; calcining; acidizing reaction: the acidic leaching process of the coal gangue; solid-liquid separating, rinsing: the acidized mixture firstly undertakes the solid-liquid separating process, and the acid solution is reserved, and the solid is rinsed; alkalization reaction: the alkaline digestion process of the coal gangue; solid-liquid separating, rinsing; polymerization: the reserved acid solution and the reserved alkaline solution that are diluted, is polymerized under the normal temperature and then dried, thereby, the water processing coagulant is acquired. A chemical method is applied in the method to polymerize and produce water processing coagulant with the coal gangue extracts, thereby making a second time and no-pollution use of the coal gangue, developing the coal gangue by recovering the resource and reducing environmental pollution. The method is also widely applicable to other industrial solid waste processing, thereby more sufficiently and more effectively utilizing the coal gangue, a solid waste.
Description
Technical field
The present invention relates to coal gangue and utilize technical field, especially relate to and a kind of coal gangue is carried out recycling, produces the method for novel material through chemical industry processing.
Background technology
When coal gangue is the colliery digging,, be the solid waste of coal in exploitation and washing process with the mixture of flags such as the top board of coal extraction simultaneously, base plate, dirt band, ore bed, silt.According to pertinent data, coal gangue accounts for 30% of total coal output in mine coal mining process, and the burden of the present coal gangue of China has reached nearly 3,000,000,000 tons, and about 1.5 hundred million tons of average annual growth.A large amount of depleted coal gangues have constituted the dual destruction to ecological and environment.
Coal gangue is a kind of natural resources for development and utilization simultaneously.Coal gangue more or less all contains carbon or other combustiblematerials of some amount, thereby can be used as fuel and use.Element kind contained in the coal gangue is more, wherein SiO
2And Al
2O
3Content is the highest, and other also has some Fe
2O
3, MgO, CaO, SO
3Deng.The main chemical industry purposes of coal gangue is exactly to extract a certain element or production silica-alumina material in the coal gangue by various method.For containing the higher coal gangue of aluminium, the Chemicals of its exploitation mainly contain crystal aluminum chloride, polymerize aluminum chloride, Tai-Ace S 150, zeolite etc.At present to coal gangue to the comprehensive utilization, concentrate on generating mostly, pave the way, refer and synthesize fields such as cement, brickmaking.
Though in every field coal gangue has all been carried out utilizing again, has all had the inadequate problem of utilizing in varying degrees.The method that provides a kind of coal gangue to utilize again just is provided purpose of the present invention, makes every effort to make the utilization of Coal Refuse more abundant, more effective.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, a kind of method of producing water treatment coagulant with coal gangue is provided, the relative prior art of this method, mainly be to utilize chemical process that the extract polymerization in the coal gangue is become the poly aluminium iron silicate coagulating agent that water treatment is used, accomplish that coal gangue does not produce comprehensive, the effectively utilization of secondary pollution, realizes the coal gangue recycling.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of method of producing water treatment coagulant with coal gangue may further comprise the steps:
(1) grinding and processing: two steps broken and in small, broken bits in the branch, lumped coal spoil grinding and processing became the fine powder body of 40～60 mesh sieves the most at last;
(2) calcining;
(3) acidification reaction: the acid process in leaching of coal gangue;
(4) solid-liquid separation, washing: with the mixture of acidified reaction, carry out solid-liquid separation earlier, acid solution stays with stand-by, and solid is washed;
(5) quaternization: the alkaline process in leaching of coal gangue;
(6) solid-liquid separation, washing: will carry out solid-liquid separation earlier through the mixture of quaternization, alkaline solution stays with stand-by, and solid is washed;
(7) polyreaction: stand-by acid solution and stand-by alkaline solution are carried out the polymerized at normal temperature reaction after dilution, make the aluminium silicate polymer ferrous solution, obtain the water treatment coagulating agent after drying.
Calcining temperature in the step in such scheme (2) is 650～800 ℃, and the calcining and activating time is 1～2.5 hour.
As a kind of preferred implementation of the present invention, in the step (3), the charging in 1: 4 by volume of coal gangue solid and mixing acid, increasing mixed acid concentration as reaction is 25%, the ratio of effective constituent equivalents is below 1.0 in the equivalents of mixing acid and the colliery powder in the stripping, and the reaction times is 1～2 hour.
This acidification reaction carries out under the prerequisite that stirs, and temperature is controlled at 100～120 ℃, and the pH value of reaction mixture is-0.01～0.6.
In the such scheme, after the pH value that the middle solid water of step (4) washes out water reaches more than 6.5, finish washing; The pH value that the middle solid water of step (6) washes out water reaches after 7.5～8, finishes washing.
As another preferred implementation of the present invention, in the step (5), the charging in 1: 5 by volume of coal gangue solid and alkali lye is 12%～15% as the alkaline concentration that reacts, and the reaction times is 1～2 hour.
Its quaternization is carried out under the prerequisite that stirs, and temperature of reaction is 110～130 ℃, and the pH value of reaction mixture is 13.3～13.5.
As another preferred implementation of the present invention, polyreaction described in the step (7) is that the stand-by alkaline solution after diluting through stand-by acid solution after the peroxidation and process is reacted.
Polymerization reaction time will carry out pH value simultaneously and regulate in 1 hour in the reaction process in the step (7), and the pH value of mixing solutions is remained between 1～2.
The beneficial effect that the present invention reached is: 1, utilize aluminium sesquioxide, ferric oxide, silicon-dioxide in the chemical process extraction coal gangue, and its polymerization become the poly aluminium iron silicate coagulating agent that water treatment is used, accomplish not produce the full use of secondary pollution, realize the coal gangue recycling.2, will react the final solid residue that generates, and utilize the online tool moulding of normal temperature glue to produce light building material, unburned pavior brick and impregnating material, coal gangue solid slag will be utilized fully, turn waste into wealth.3, this coal gangue utilizes the coal gangue in the method and technology to produce water conditioner poly aluminium iron silicate technology, also can use in other industrial solid wastes are handled.4, adopt the polymerization technique of producing water conditioner poly aluminium iron silicate technology, the molten reaction technology of mixing acid, the molten reaction technology of alkali, two kinds of solution to realize, package is reasonable, the every intermediate product that produces in the reaction process, heat of release or the like, perhaps finally be converted to enabled production, perhaps reactant, the heating source as next time carries out recycle, accomplishes abundant, effective, full use to all resources.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is that the present invention utilizes the process flow sheet of coal gangue production water treatment with the preferred implementation of coagulating agent.
Embodiment
Fig. 1 is that the present invention utilizes the process flow sheet of coal gangue production water treatment with the preferred implementation of coagulating agent.As shown in the figure,
The first step, grinding and processing: in order to make coal gangue bigger contact area is arranged in subsequent reactions, fast reaction speed, the lumped coal spoil should be processed into the particle of certain particle size earlier.The size of processing granularity all has bigger influence to the solubility rate of effective ingredient and the separating effect of reaction residues.The coal gangue granularity can be selected the particle diameter of 60 mesh sieves for use.Coal gangue adds two steps broken and in small, broken bits in the work point.In broken be to adopt jaw crusher or hammer mill that blocky coal gangue is broken into the little bulk of particle diameter 20～40mm in advance, to adapt to the charging requirement of equipment in small, broken bits.In small, broken bits then is to adopt the fritter shape coal gangue of ball mill or Raymond mill (Suspension roller pulverizer) acquisition in rapid with middle quick short steps to be processed into 40～60 purpose fine powder bodies.
Second step, calcining: will calcine through the coal gangue fine powder body that grinding and processing obtains.The calcining residence time and calcining temperature are the principal elements that influences solubility rate.The dissimilar coal gangues and the coal gangue in the different places of production of the same type have different optimum calcinating temperatures.The solubility rate of various coal gangues under best calcination condition also has nothing in common with each other, thereby will accurately hold wherein calcination condition and calcination time.During calcining, calcining temperature should be controlled at 650～800 ℃, the calcining and activating time is 1～2.5 hour.Calcining coal gangue can adopt multiple calciners such as shaft kiln, reverberatory furnace, rotary kiln, fluidizing furnace, fluidisation stove.Wherein the fluidisation stove is state-of-the art calciner, and it has, and calcining temperature is even, the residence time short, the output advantages of higher, and environmental effect is good, thereby mainly adopts this kind equipment to calcine.
In addition, the waste heat that produces in calcination process is used for generating, builds up the industrial park of cogeneration, fully effective use of energy sources.
The 3rd step, acidification reaction: the acid process in leaching of coal gangue.Acid stripping is to produce one of important procedure of water conditioner with coal gangue, careful assurance.In acidization, the solubility rate that factors such as the concentration of the type of coal gangue, particle diameter, calcination condition, mixing acid, the equivalence ratio (in the stripping in the equivalents of mixing acid and the colliery powder ratio of effective constituent equivalents) that adds acid, dissolution time all can the shadow coal gangue.
The concentration of mixing acid wherein mainly shows on the solubility rate to aluminum oxide, ferric oxide the influence of coal gangue solubility rate.The solubility rate of aluminum oxide, ferric oxide, increasing and increase with increasing mixed acid concentration.But concentration can not be too high simultaneously, because after concentration is greater than 25%, the volatile quantity of mixing acid increases greatly, and concrete operations, environment, yield etc. are all had disadvantageous effect; And concentration is when too low, and aluminum oxide and ferric oxide solubility rate reduce, and simultaneous oxidation aluminium and iron oxide concentration also can reduce, and make aluminum oxide and iron oxide content in the finished product not reach requirement.Consider the volatilization factor of solubility rate and mixing acid, near the concentration 25% when selecting for use mixing acid constant boiling point be advisable (110.58 ℃ of the constant boiling point temperature of mixing acid, relative density 1.286, concentration 24.57%).
The equivalence ratio that adds acid mainly shows the influence of coal gangue solubility rate: the solubility rate of aluminum oxide and ferric oxide increases with the increase that adds acid equivalent, and the basicity of dissolution fluid then reduces with the increase that adds acid equivalent.When adding acid equivalent than 0.9 when above, the solubility rate increasing degree is very little, and it is very fast that basicity then descends, and therefore, for obtaining having the dissolution fluid of certain aluminum oxide and ferric oxide solubility rate and certain basicity, should be controlled at below 1.0 adding the acid equivalent ratio.
The influence in reaction times mainly shows: aluminum oxide and ferric oxide solubility rate increase with the growth in reaction times, but the reaction times is long for example more than 1.0 hours the time, the solubility rate increasing degree is little, for improving plant factor, reaction times can select for use 1～2 hour, and its sour molten reaction equation is:
Al
2O
3+3H
2SO
4→Al
2(SO
4)
3+3H
2O，
Al
2O
3+6HCl→2Al
2Cl
3+3H
2O，
Fe
2O
3+6HCl→2FeCl
3+3H
2O，
Fe
2O
3+3H
2SO
4→Fe
2(SO
4)
3+3H
2O。
To sum up concrete reaction process is: enter acidification reaction after will calcine the material cooling, flue gas is calcined in the thermal utilization that adds of its acidification reaction still, and the solid and the liquid material ratio that enter the acidification reaction still are 1: 4 (volume ratio).Wherein liquid is that mass ratio is 5: 1 a hydrochloric acid (technical grade, content 35%) with the mixing acid of sulfuric acid (technical grade content 98%), and add the long-pending water of triploid and dilute, make that dilution back increasing mixed acid concentration is 25%, in the complex acid device, carry out the configuration of aforementioned mixing acid.Above-mentioned acidification reaction is to carry out under the prerequisite that stirs, and the reaction times is 2 hours, and temperature is controlled at 100～120 ℃, and the pH value of reaction mixture is-0.01～0.6.
The 4th the step, solid-liquid separation, washing: with the mixture of acidified reaction, carry out again solids constituent from, the washing.Acidification reaction carries out solid-liquid separation earlier after finishing, and it is stand-by that supernatant liquor is put into the stand-by storage tank of acid solution; Solid will carry out solid washing, cleans repeatedly with the water of water equipment confession, after the pH value that solid water washes out water reaches more than 6.5, finishes washing.Simultaneously isolated washing water outlet is returned the used complex acid device of acidification reaction, be used for complex acid.
The 5th step, quaternization: the acid process in leaching of coal gangue.Be further to carry out the alkali soaking technology and to handle through the above-mentioned solid coal gangue residue that obtains after the processing steps such as solid-liquid separation, washing with NaOH solution.Its objective is to make abundant Si element and the NaOH effect of content in the coal gangue, generate water glass, become the raw material of preparation active acid in the subsequent technique.
Specifically in this quaternization process, the charge ratio of its quaternization still solid and liquid is 1: 5 (volume ratio), and wherein liquid is to join the sodium hydroxide solution of being joined in the alkali device, contains sodium hydroxide 12%～15%.Earlier alkali lye is diluted, the coal gangue residue that acidleach is obtained later and dilution afterwards afterwards concentration is that 30% NaOH solution mixes by certain solid-to-liquid ratio, under boiling temperature, and 1.5-2.5 hour heating reflux reaction time, obtain sodium silicate solution behind the cold filtration, reaction equation is:
SiO
2+2NaOH→Na
2SiO
3+H
2O。
This quaternization is carried out under stirring condition, and reaction should be controlled at 1～2.5 hour, and control reaction temperature is 110～130 ℃, and the thermal source that heats in the reaction adopts the calcining flue gas to heat equally, and the pH value of reaction soln is 13.3～13.5.
The 6th step, solid-liquid separation, washing: identical with the acidification reaction process, after the quaternization, carry out solid-liquid separation earlier, it is stand-by that its supernatant liquor is put into the alkali lye storage tank.Separate the solid matter that obtains, stand-by after washing.Equally also be to adopt the water supply of water equipment to clean repeatedly, treat that the pH value that solid water washes out water reaches after 7.5～8, finishes washing.Afterwards isolated acid washing water is returned and join the alkali device and be used for joining alkali.Solid residue after the separation stays and settles in separate action.
The 7th step, polyreaction: with the stand-by acid solution that stores in the stand-by storage tank of acid solution and the stand-by alkaline solution of the stand-by storage tank stores of alkali lye, after dilution, carry out the polymerized at normal temperature reaction, make the aluminium silicate polymer ferrous solution, obtain the water treatment coagulating agent after drying.Concrete reaction process is: the stand-by acid solution of the stand-by tank stores of acid solution is put into oxidation reactor, with H
2O
2Carry out oxidizing reaction, make the F in the acid solution
e 2+Iron ion be oxidized to F
e 3+Iron ion.Solution after the oxidation carries out polyreaction with the stand-by alkali lye of the stand-by tank stores of alkali lye again; Thin up is 3 times for alkali lye the time.This polymerization reaction time is in 1 hour, will carry out pH value in the reaction process simultaneously and regulate, and the pH value of mixture is controlled between 1～2.After finishing, polyreaction carries out spraying drying, the heat energy that provides in the calcining process is provided the thermal source that spraying drying is used, the resulting solid of spraying drying is a solid water treating agent. and the gas water that spraying drying is produced carries out the absorption of gas water body simultaneously, and the gas after the absorption of process water body discharges by gas discharging apparatus after reaching emission standard. and the water after the absorption utilizes it as the washing solid water after acidifying and the quaternization again.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not break away from the spirit and scope of technical solution of the present invention.
Claims (9)
1. a method of producing water treatment coagulant with coal gangue is characterized in that, may further comprise the steps:
(1) grinding and processing: two steps broken and in small, broken bits in the branch, lumped coal spoil grinding and processing became the fine powder body of 40～60 mesh sieves the most at last;
(2) calcining;
(3) acidification reaction: the acid process in leaching of coal gangue;
(4) solid-liquid separation, washing: with the mixture of acidified reaction, carry out solid-liquid separation earlier, acid solution stays with stand-by, and solid is washed;
(5) quaternization: the alkaline process in leaching of coal gangue;
(6) solid-liquid separation, washing: will carry out solid-liquid separation earlier through the mixture of quaternization, alkaline solution stays with stand-by, and solid is washed;
(7) polyreaction: stand-by acid solution and stand-by alkaline solution are carried out the polymerized at normal temperature reaction after dilution, make the aluminium silicate polymer ferrous solution, obtain the water treatment coagulating agent after drying.
2. according to the described a kind of method of producing water treatment coagulant with coal gangue of claim 1, it is characterized in that: the calcining temperature in the step (2) is 650～800 ℃, and the calcining and activating time is 1～2.5 hour.
3. according to claim 1 or 2 described a kind of methods of producing water treatment coagulant with coal gangue, it is characterized in that: in the step (3), the charging in 1: 4 by volume of coal gangue solid and mixing acid, increasing mixed acid concentration as reaction is 25%, the ratio of effective constituent equivalents is below 1.0 in the equivalents of mixing acid and the colliery powder in the stripping, and the reaction times is 1～2 hour.
4. according to the described a kind of method of producing water treatment coagulant with coal gangue of claim 3, it is characterized in that: described acidification reaction carries out under the prerequisite that stirs, and temperature is controlled at 100～120 ℃, and the pH value of reaction mixture is-0.01～0.6.
5. according to claim 1 or 2 described a kind of methods of producing water treatment coagulant, it is characterized in that: after the pH value that the middle solid water of step (4) washes out water reaches more than 6.5, finish washing with coal gangue; The pH value that the middle solid water of step (6) washes out water reaches after 7.5～8, finishes washing.
6. according to claim 1 or 2 described a kind of methods of producing water treatment coagulant with coal gangue, it is characterized in that: in the step (5), the charging in 1: 5 by volume of coal gangue solid and alkali lye is 12%～15% as the alkaline concentration that reacts, and the reaction times is 1～2 hour.
7. according to the described a kind of method of producing water treatment coagulant with coal gangue of claim 6, it is characterized in that: described quaternization is carried out under the prerequisite that stirs, and temperature of reaction is 110～130 ℃, and the pH value of reaction mixture is 13.3～13.5.
8. according to claim 1 or 2 described a kind of methods of producing water treatment coagulant with coal gangue, it is characterized in that: in the step (7), described polyreaction is that the stand-by alkaline solution after diluting through stand-by acid solution after the peroxidation and process is reacted.
9. according to the described a kind of method of producing water treatment coagulant with coal gangue of claim 8, it is characterized in that: polymerization reaction time is in 1 hour in the step (7), to carry out pH value in the reaction process simultaneously and regulate, the pH value of mixing solutions is remained between 1～2.
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