CN101948142A - Method for producing sludge modifier by utilizing coal gangue - Google Patents
Method for producing sludge modifier by utilizing coal gangue Download PDFInfo
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- CN101948142A CN101948142A CN 201010500856 CN201010500856A CN101948142A CN 101948142 A CN101948142 A CN 101948142A CN 201010500856 CN201010500856 CN 201010500856 CN 201010500856 A CN201010500856 A CN 201010500856A CN 101948142 A CN101948142 A CN 101948142A
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- coal gangue
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Abstract
The invention discloses a method for producing sludge modifier by utilizing coal gangue, comprising the following steps: fully and evenly mixing the coal gangue and carbonate, and calcining; soaking the calcined solid matter by water, and filtering to obtain filter residue and alkaline filter liquor; dissolving the filter residue by adopting the acid liquor, and filtering to obtain the alkaline filter liquor; mixing the acidic filter liquor and the alkaline filter liquor; respectively adjusting the alkalinity and the acidity of the mixing system and the concentration of SiO3<3->, Al<3+> and Fe<3+>; carrying out polymerization reaction; carrying out spray drying after the polymerization reaction to obtain the sludge modifier taking polysilicate aluminum iron as a main component. Compared with the prior art, the technical scheme of the invention activates the coal gangue by utilizing a high temperature condition, simultaneously realizes the extraction and separation of Si element, simplifies the production process, and adopts the low-price carbonate as an auxiliary raw material, thus saving the production cost, and multi-element extraction is carried out on the raw materials of the coal gangue, thus improving the use ratio of the raw materials of the coal gangue.
Description
Technical field
The present invention relates to coal gangue and utilize technical field, the method for especially relate to a kind of coal gangue recycling, producing novel material.
Background technology
Coal gangue is the solid waste of discharging in coal washing and the coal separation process, and along with the coal mining amount with to the increase of raw coal washing proportion, the quantity discharged of coal gangue increases with the speed of 10～20 times of raw coal outputs.China is big coal country, and a large amount of for a long time coal gangues is exposed to be stored up, and not only occupies the arable land, and the leaching water polluted underground water and the surface water of coal gangue, and a large amount of H is emitted in the easy spontaneous combustion of coal gangue in addition
2S, SO
2, obnoxious flavour such as CO, the severe contamination atmosphere.Carry out coal gangue comprehensive utilization energetically and not only can increase economic benefit of enterprises, improve the Coal Production structure, and can reduce because of stacking occupying and pollute to the soil.
Owing to contain combustiblecomponents and mineral substance in the coal gangue, be good fuel and industrial raw material.Therefore, the comprehensive utilization of coal gangue for economizing on resources, improves environment, improves economic and social benefit, realizes that resource utilization preparation and Sustainable development are significant.The main component of coal gangue is mineral substance such as kaolinite, montmorillonite, illite, and its main chemical compositions is SiO
2, Al
2O
3, Fe
2O
3, CaO, MgO etc.Comprehensive utilization for coal gangue at present is mainly coal gangue power generation, produces aspects such as building materials, backfill, extraction Chemicals.Extracting aspect the Chemicals, coal gangue utilize mode to produce inorganic polymer coagulant, as polymerize aluminum chloride, poly-sulphur aluminum chloride, aluminium iron polychloride, poly aluminium iron silicate etc.Although the mode of utilizing of coal gangue presents variation, most of modes all exist to be utilized insufficiently, utilizes the cost height, easily produces secondary pollution problems.
Comparatively speaking, produce the mode of utilizing of poly aluminium iron silicate and extracted principal elements such as Si in the coal gangue, Al, Fe, the utilization of coal gangue is more abundant, and the poly aluminium iron silicate of producing has more excellent modified performance for sewage, appropriate pH value wide ranges, and it is rapid to form alumen ustum, flco is thick closely knit, needing the settling time short, is a kind of promising inorganic polymer adjusting material, can be widely used in sewage treatment industry.Utilize the method for coal gangue production poly aluminium iron silicate more at present, but concluding all is that acidleach and alkali soak the mode that combines, the difference of method shows that mainly acidleach and alkali soak the precedence of step, and the selection of acid solution and alkali lye, therefore the essence of these methods is not respectively, shortcoming is also more consistent: preparation process is numerous and diverse, and raw material availability is low, the production cost height.
Summary of the invention
Technical problem to be solved by this invention is to produce at existing coal gangue the deficiency of poly aluminium iron silicate method, and improving with the coal gangue is the method for main material production mud adjusting material, not only improves the utilization ratio of coal gangue, and reduces production costs.
Purpose of the present invention is achieved through the following technical solutions: a kind of method of utilizing coal gangue to produce the mud adjusting material, carry out according to following step:
(1) coal gangue and carbonate thorough mixing are calcined after evenly;
(2) will be soaked in water through the incinerating solid matter in the step (1), filter, obtain filter residue and alkaline filtrate;
(3) adopt acid solution that filter residue is dissolved, filter, obtain acid filtrate;
(4) alkaline filtrate and acid filtrate are mixed, make SiO in the mixed system
3 2-, Al
3+And Fe
3+Mol ratio reach the polymerization requirement, adjusting mixed system simultaneously is strongly-acid, carries out polyreaction;
(5) after polyreaction is finished, carry out spraying drying, promptly obtaining with the poly aluminium iron silicate is the mud adjusting material of main component.
In technical scheme of the present invention, in order to increase the contact area of reactant in the high-temperature calcination process, fast reaction speed, preferably be ground into below the particle diameter 0.4mm lumped coal spoil Powdered, the size of its granularity, have considerable influence for the speed of response and the effective constituent rate of recovery, experiment shows, particle diameter should be controlled at below the 0.4mm.Coal gangue adds two steps broken and in small, broken bits in the work point.In broken employing jaw crusher or hammer mill blocky coal gangue is broken into the little bulk of particle diameter 20～40mm, to satisfy 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 the fine powder body of 0.25～0.4mm.
In technical scheme of the present invention, to calcine after coal gangue and carbonate (as yellow soda ash) powder thorough mixing is even, the residence time and calcining temperature are the principal elements that influences the rate of recovery: at 550～700 ℃, the essential mineral of coal gangue is formed kaolinite (SiO
22Al
2O
32H
2O) remove crystal water and generate metakaolinite (SiO
22Al
2O
3), at 700～800 ℃, metakaolinite decomposes generation SiO
2And have active Al
2O
3SiO
2At 800～900 ℃ of following and Na
2CO
3Reaction generates Na
2SiO
3And overflow CO
2Therefore calcining temperature should be controlled at 800～900 ℃, can adjust calcination time according to the total amount of reactant.Calcining coal gangue can adopt multiple calciners such as shaft kiln, reverberatory furnace, rotary kiln, fluidizing furnace, fluidisation stove.Wherein the fluidisation stove is that to have calcining temperature even, and the residence time is short, the output height, and advantage such as environmental effect is good is a calciner preferably.
In technical scheme of the present invention, need utilize Na
2SiO
3Water-soluble, by in calcinate, adding H
2O is with SiO
3 2-Stripping realizes Si element extraction separation from coal gangue.Therefore when the carbonate of selection and coal gangue mixed calcining, need to consider the solvability of cationic silicate in the carbonate, should select the positively charged ion that silicate can be water-soluble, general yellow soda ash, sodium bicarbonate, salt of wormwood or the saleratus selected, can select to use single carbonate, also can select several mixing of above-mentioned carbonate to use with arbitrary proportion.When determining the add-on of coal gangue and carbonate, need to consider the mol ratio of silicon-dioxide and carbonate in the coal gangue, select in principle that carbonate is excessive slightly to get final product.
Al through high-temperature activation
2O
3And Fe
2O
3Still be present in the filter residue, in filter residue, add acid solution and be used for dissolving Al
2O
3And Fe
2O
3, to form Al
3+And Fe
3+, the mode of stirring can the accelerate dissolution process, and finally the mode by solid-liquid separation is with Al
3+And Fe
3+Separate.In this dissolution process, need to consider the influence of the add-on, reaction times, temperature of reaction etc. of concentration, the acid of kind, the acid of acid to solute effect.
The selection of acid kind influences the speed and the processing safety of dissolution process.Because acid fluid dissolves reaction often needs the acid solution of big concentration, when adopting the dissolving with hydrochloric acid filter residue, HCl is volatile to cause damage and brings environmental pollution; The vitriol oil has strong corrosion, and easily with filter residue in Al and generation passivation reaction such as Fe and hinder to react and proceed.And flocculation mechanism be studies show that SO
4 2-Can improve the flocculating property of adjusting material.Consider from security and economy, select for use hydrochloric acid and vitriolic mixing acid comparatively suitable.
The selection of acid concentration directly influences Al in the filter residue
2O
3And Fe
2O
3Dissolution rate and solubility rate.Generally speaking, with increasing of increasing mixed acid concentration, Al
2O
3And Fe
2O
3Dissolution rate and solubility rate all increase.But under the situation of excessive concentration, mixing acid also faces volatile quantity and increases and safety problem.Take all factors into consideration, selecting the mass percent of acid in the mixed acid solution for use is 30%～35%.
The add-on of acid influences Al in the filter residue equally
2O
3And Fe
2O
3Solubility rate.In practice, with Al in the add-on of acid and the filter residue
2O
3With Fe
2O
3The ratio of mole number sum be defined as and add the acid equivalent ratio.Al
2O
3And Fe
2O
3Solubility rate increase along with the increase that adds the acid equivalent ratio, but when adding acid equivalent than greater than 1.0 the time, the increasing degree of solubility rate diminishes gradually, in order to improve utilization ratio of raw materials, adds acid equivalent than selecting 1～2.
Reaction times directly determines Al in the filter residue
2O
3And Fe
2O
3With H
+Level of response.Al
2O
3And Fe
2O
3Solubility rate increase along with the lengthening in reaction times, but when the reaction times more than 1.0 hours the time, the increase trend of solubility rate is slow.From improving the angle of plant factor, the reaction times was advisable with 1～2 hour.
Temperature of reaction also influences Al
2O
3And Fe
2O
3Dissolution rate.Along with the lifting of temperature of reaction, Al
2O
3And Fe
2O
3Dissolution rate increase, the reaction times shortens.Concentration based on mixing acid is 30%～35%, and is the mixing of sulfuric acid and hydrochloric acid, so controlled temperature is advisable at 100～110 ℃.
Adjusting SiO
3 2-, Al
3+And Fe
3+Concentration before, at first measure SiO in the basic solution
3 2-With Al in the acidic solution
3+, Fe
3+Concentration, adjust according to test result then, general method is dilution or adds corresponding ionic soluble salt that for example the thin up alkaline filtrate adds FeCl
3Increase Fe
3+Content.In order to guarantee the effect of polyreaction, need make SiO in the mixed solution
3 2-, Al
3+And Fe
3+Mol ratio reach the polymerization requirement of poly aluminium iron silicate, i.e. SiO
3 2-With Al
3+And Fe
3+The mol ratio of sum is (1: 1)～(4: 1), and Al
3+With Fe
3+Mol ratio be (1: 1)～(3: 1).
In actual production process, the pH of acid filtrate can reach 2～4, and the pH of alkaline filtrate is generally 8～10 and since alkaline filtrate in SiO
3 2-Be main, Si is an amphoteric element, is SiO in alkaline environment
3 2-, meeting generates the polymkeric substance (be linked at after sloughing a water between the silicic acid and produce the chain thing together, so this reaction process is also referred to as polymerization) of silicic acid in strong acid (the pH value is 0～2) environment.For achieving the above object, need test the pH value of acid filtrate and alkaline filtrate earlier before mixing, mix then, and carry out the adjustment of pH value, so that the pH value of mixed system is a strongly-acid finally, be 0～2 as the pH value.The adjustment of pH value can be adopted following method: increase the acidity of acid filtrate before mixing, perhaps directly mix the acidity (for example dripping dilute hydrochloric acid or dilute sulphuric acid) that the back changes mixed solution.The time of polyreaction generally was controlled at 30～60 minutes, after polyreaction finishes, system was carried out spraying drying, and promptly obtaining with the poly aluminium iron silicate is the mud adjusting material of main component.
Relative prior art, technical scheme of the present invention utilizes hot conditions to activate coal gangue, realized the extraction separation of Si element simultaneously, simplified production technique, adopting cheap carbonate is that auxiliary material has been saved production cost, the coal gangue raw material is carried out multiple element extraction improved its utilization ratio, specifically: 1. utilize chemical process to extract elements such as Si, Al in the coal gangue and Fe, and its polymerization become highly effective sludge adjusting material poly aluminium iron silicate, realize the recycling of waste to greatest extent, significantly reduced the discharging of solid waste; 2. utilize the pyroreaction condition of activated alumina, realize the reaction of silicon-dioxide and yellow soda ash simultaneously, simplified the stripping step of silicon-dioxide; 3. adopt the more cheap carbonate of price as auxiliary material, more cheap than the high density strong base solution that existing technology adopted, reduced production cost; 4. the existing technology of the final solid residue that generates of reaction is few, and is mainly nontoxic materials such as CaO and MgO, can be used to produce light building material, unburned pavior brick and impregnating material, realizes that coal gangue solid slag utilizes fully.
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.
Embodiment 1
Utilize Huairen County, Shaanxi Province coal gangue sample, preparation mud adjusting material.The composition of coal gangue sample and content (wt%) see following table for details:
The coal gangue of use 0.25～0.4mm mixes with powdered sodium carbonate to be calcined, and wherein temperature is 900 ℃, and the time is 50min, and coal gangue and yellow soda ash mass ratio are 2: 1; Solid matter after the calcining is soaked in water, filters, obtain filter residue and alkaline filtrate.
Adopt the mix acid liquor of the vitriol oil (massfraction 98%) and concentrated hydrochloric acid (massfraction 36%), the vitriol oil and concentrated hydrochloric acid mass ratio are 1: 5, and the water dilution that adds 3 times of volumes then obtains mixing acid; Adopt mixing acid that filter residue is dissolved, the solid charging in 4: 1 by volume after mixing acid and the calcining is filtered, and obtains acid filtrate, and solvent temperature is 100 ℃, and the time is 60min.
Test the ionic concn in acid filtrate and the alkaline filtrate respectively, according to the ionic concn of test, thin up is to SiO in the alkalitropism filtrate
3 2-Concentration is 0.5mol/L, and thin up is to Al in the oxytropism filtrate
3+Concentration is 0.5mol/L, and drips FeCl in the oxytropism filtrate
3Solution is to Fe
3+Concentration is 0.25mol/L.Alkaline filtrate and acid filtrate are mixed, and the volume ratio of alkaline filtrate and acid filtrate is to mix at 3: 1, and three kinds of ionic mol ratios are SiO in the mixed system
3 2-: Al
3+: Fe
3+=6: 2: 1, mix the back dripping hydrochloric acid to pH to 0.5, stir gently, it is mixed, leave standstill 30min under the room temperature and carry out polyreaction.Carry out spraying drying then, promptly obtaining with the poly aluminium iron silicate is the mud adjusting material of main component.
Embodiment 2
Utilize dooly mountain, Anshun City, Guizhou Province coal gangue sample, preparation mud adjusting material.The composition of coal gangue sample and content (wt%) see following table for details:
The coal gangue of use 0.25～0.4mm mixes with powdered sodium carbonate to be calcined, and wherein temperature is 900 ℃, and the time is 40min, and coal gangue and yellow soda ash mass ratio are 3: 1; Solid matter after the calcining is soaked in water, filters, obtain filter residue and alkaline filtrate.
Adopt the mix acid liquor of the vitriol oil (massfraction 98%) and concentrated hydrochloric acid (massfraction 36%), the vitriol oil and concentrated hydrochloric acid mass ratio are 1: 5, and the water dilution that adds 3 times of volumes then obtains mixing acid; Adopt mixing acid that filter residue is dissolved, the solid charging in 4: 1 by volume after mixing acid and the calcining is filtered, and obtains acid filtrate, and solvent temperature is 100 ℃, and the time is 60min.
Test the ionic concn in acid filtrate and the alkaline filtrate respectively, according to the ionic concn of test, thin up is to SiO in the alkalitropism filtrate
3 2-Concentration is 0.5mol/L, and thin up is to Al in the oxytropism filtrate
3+Concentration is 0.5mol/L, and drips FeCl in the oxytropism filtrate
3Solution is to Fe
3+Concentration is 0.5mol/L.Alkaline filtrate and acid filtrate are mixed, and the volume ratio of alkaline filtrate and acid filtrate is to mix at 2: 1, and three kinds of ionic mol ratios are SiO in the mixed system
3 2-: Al
3+: Fe
3+=2: 1: 1, mix the back dripping hydrochloric acid to pH to 1, stir gently, it is mixed, leave standstill 30min under the room temperature and carry out polyreaction.Carry out spraying drying then, promptly obtaining with the poly aluminium iron silicate is the mud adjusting material of main component.
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 (10)
1. a method of utilizing coal gangue to produce the mud adjusting material is characterized in that, carries out according to following step:
(1) coal gangue and carbonate thorough mixing are calcined after evenly;
(2) will be soaked in water through the incinerating solid matter in the step (1), filter, obtain filter residue and alkaline filtrate;
(3) adopt acid solution that filter residue is dissolved, filter, obtain acid filtrate;
(4) alkaline filtrate and acid filtrate are mixed, make SiO in the mixed system
3 2-, Al
3+And Fe
3+Mol ratio reach the polymerization requirement, adjusting mixed system simultaneously is strongly-acid, carries out polyreaction;
(5) after polyreaction is finished, carry out spraying drying, promptly obtaining with the poly aluminium iron silicate is the mud adjusting material of main component.
2. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (1), the particle diameter of coal gangue is 0.25～0.4mm, and calcining temperature is 800～900 ℃.
3. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that, in the described step (1), described carbonate is at least a in yellow soda ash, sodium bicarbonate, salt of wormwood or the saleratus.
4. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (3), the mass percent of acid is 30%～35% in the acid solution of use
5. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (3), the acid equivalent ratio that adds of acid solution is 1～2.
6. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (3), the temperature of solubilizing reaction is 100～110 ℃.
7. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (3), the time of solubilizing reaction is 1～2 hour.
8. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that, in the described step (4), and SiO in the mixed system
3 2-With Al
3+And Fe
3+The mol ratio of sum is (1: 1)～(4: 1), and Al
3+With Fe
3+Mol ratio be (1: 1)～(3: 1).
9. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (4), the pH value of adjusting mixed system is 0～2.
10. a kind of method of utilizing coal gangue to produce the mud adjusting material according to claim 1 is characterized in that in the described step (4), polymerization time is 30～60 minutes.
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|---|---|---|---|
| CN 201010500856 CN101948142A (en) | 2010-10-09 | 2010-10-09 | Method for producing sludge modifier by utilizing coal gangue |
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|---|---|---|---|
| CN 201010500856 CN101948142A (en) | 2010-10-09 | 2010-10-09 | Method for producing sludge modifier by utilizing coal gangue |
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Cited By (9)
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| CN102531328A (en) * | 2012-01-09 | 2012-07-04 | 济南大学 | Composite inorganic polymeric sludge dehydration conditioner prepared from blast-furnace metallurgical slag |
| CN104148366B (en) * | 2014-07-27 | 2016-01-27 | 甘肃华晨非金属应用科技有限公司 | Gangue after acidifying |
| CN105600895A (en) * | 2015-12-30 | 2016-05-25 | 西安科技大学 | Method using gangue to process slime water |
| CN105858838A (en) * | 2016-04-29 | 2016-08-17 | 绍兴文理学院 | Sludge incineration source flocculating agent and preparing method thereof |
| CN108408858A (en) * | 2018-04-25 | 2018-08-17 | 宁夏宝塔化工中心实验室(有限公司) | A kind of preparation method of polyaluminum ferric chloride |
| CN108496749A (en) * | 2018-03-16 | 2018-09-07 | 辽宁大学 | A kind of gangue suitable for lawn soilless is mixed matrix and application |
| CN109438116A (en) * | 2018-11-30 | 2019-03-08 | 山西大学 | A method of soil conditioner is prepared using gangue and plant ash modification |
| CN109706324A (en) * | 2019-03-14 | 2019-05-03 | 云南方圆矿产资源再生综合利用研究院有限公司 | A method of separating-purifying titanium using coal gangue as raw material |
| CN115108869A (en) * | 2022-06-15 | 2022-09-27 | 华南理工大学 | Method for producing organic-inorganic compound soil conditioner by using coal gangue and product thereof |
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| CN102531328A (en) * | 2012-01-09 | 2012-07-04 | 济南大学 | Composite inorganic polymeric sludge dehydration conditioner prepared from blast-furnace metallurgical slag |
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| CN105858838A (en) * | 2016-04-29 | 2016-08-17 | 绍兴文理学院 | Sludge incineration source flocculating agent and preparing method thereof |
| CN105858838B (en) * | 2016-04-29 | 2019-03-26 | 绍兴文理学院 | A kind of sludge incineration source flocculant and preparation method thereof |
| CN108496749A (en) * | 2018-03-16 | 2018-09-07 | 辽宁大学 | A kind of gangue suitable for lawn soilless is mixed matrix and application |
| CN108408858A (en) * | 2018-04-25 | 2018-08-17 | 宁夏宝塔化工中心实验室(有限公司) | A kind of preparation method of polyaluminum ferric chloride |
| CN109438116A (en) * | 2018-11-30 | 2019-03-08 | 山西大学 | A method of soil conditioner is prepared using gangue and plant ash modification |
| CN109438116B (en) * | 2018-11-30 | 2022-01-07 | 山西大学 | Method for preparing soil conditioner by modifying coal gangue and plant ash |
| CN109706324A (en) * | 2019-03-14 | 2019-05-03 | 云南方圆矿产资源再生综合利用研究院有限公司 | A method of separating-purifying titanium using coal gangue as raw material |
| CN109706324B (en) * | 2019-03-14 | 2022-06-14 | 云南方圆矿产资源再生综合利用研究院有限公司 | Method for separating and purifying titanium by taking coal gangue as raw material |
| CN115108869A (en) * | 2022-06-15 | 2022-09-27 | 华南理工大学 | Method for producing organic-inorganic compound soil conditioner by using coal gangue and product thereof |
| CN115108869B (en) * | 2022-06-15 | 2023-09-26 | 华南理工大学 | Method for producing organic-inorganic compound soil conditioner by using coal gangue and product thereof |
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Application publication date: 20110119 |