CN103964482B - A kind of method that gangue silicon aluminum carbon works in coordination with utilization - Google Patents
A kind of method that gangue silicon aluminum carbon works in coordination with utilization Download PDFInfo
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Abstract
The present invention relates to a kind of method that gangue silicon aluminum carbon works in coordination with utilization.The method includes through hydro-thermal method High Temperature High Pressure acidleach, gangue is carried aluminum, prepare aluminium polychlorid, then utilization carries waste slag of aluminum and sodium silicate solution is prepared in sodium hydroxide solution reaction in autoclave, make carbon enrichment then FLOTATION SEPARATION, it is substantially reduced ash in carbon, sodium silicate solution 10～12 ° of B é of regulation will be obtained and prepare white carbon by carbonation decompsition process.The present invention takes full advantage of the aluminum in gangue, silicon, carbon, improves the comprehensive utilization ratio of gangue.
Description
Technical field
The present invention relates to Technology of Comprehensive Utilization of Coal Gangue, be specifically related to a kind of method that gangue silicon aluminum carbon works in coordination with utilization.
Background technology
Gangue is one of trade waste of China's annual emissions and accumulative volume of cargo in storage maximum.According to statistics, China's gangue is the most tired
Meter is stored up and is reached more than 50 hundred million tons, floor space about 58,000,000 square metres, and respectively with the generation amount continuation discharge being often close on 200000000 tons.
Owing to comprehensive development and utilization can not get due attention, substantial amounts of gangue land occupation, pollute environment.On the other hand, gangue
In containing multiple utilizable component, such as carbon, aluminium oxide and silicon dioxide.In today that resource is the poorest, from gangue
The materials such as middle extraction aluminium oxide, silicon oxide are the effective ways making gangue turn waste into wealth, comprehensively utilizing, and have good society
Benefit and economic benefit.
At present bastard coal comprehensive Utilization Ways made of stones mainly utilizes with coal gangue power generation, making coal gangue brick, gangue low value of reclaiming etc.
Means are main.Existing higher value application means mainly have (1) to extract the aluminium element such as patent documentation in gangue, and " one utilizes coal
Spoil produces the method (CN102311136A) of low iron aluminum sulfate " use the aluminum in sulphuric acid extraction gangue for aluminum sulfate；" a kind of
Gangue is utilized to produce aluminum chloride, silicon chloride and the method (publication number CN102923747A) of iron chloride " use chlorine and gangue
In carbon, the element reaction such as aluminum prepare aluminum chloride；" plant slag, gangue is utilized to produce polyaluminum ferric chloride composite water purification agent
Method (publication number CN101559987A) " react with the ferro-aluminum in gangue with hydrochloric acid, and prepare polymerization with reacted solution
Aluminium chloride ferrum.(2) extract sial element such as patent documentation in gangue " gangue eco-utilization coproduction aluminium oxide white carbon
The method (publication number CN1903727) of low ash carbon " first react with gangue with sulphuric acid, obtain the filtrate containing aluminum for preparing oxygen
Change aluminum, siliceous filtering residue dipping by lye, obtain silicate solutions and carbon containing filtering residue, and utilize silicate solutions to prepare white carbon；" one
Plant the calcining thermal activation of gangue anaerobic and prepare the method (publication number CN102701220A) of white carbon " first use pyrolysis oven at anaerobic bar
Thermal activated coal gangue under part, then reacts with the gangue after acid and activation, obtains filtrate for preparing sodium metaaluminate, filtering residue and
Sodium hydroxide solution prepares sodium silicate solution, and utilizes sodium silicate solution to prepare white carbon.The patent documentation that above-mentioned gangue utilizes
Middle comprehensive utilization silicon, aluminum, carbon have " gangue eco-utilization coproduction aluminium oxide white carbon the method (publication number of low ash carbon
CN1903727) " although this patent documentation make use of the silicon aluminum carbon in gangue, but the method adds fluoride, increase
The problem that follow-up water processes, and its aluminium oxide preparation process is the most complex.And " a kind of gangue anaerobic calcining thermal activation preparation is white
The method (publication number CN102701220A) of white carbon black " gangue need to be carried out activation processing, and activation equipment is required higher,
Needing special pyrolysis oven, this increases production cost undoubtedly, and the enrichment degree of the method carbon is low does not reaches the degree directly utilized,
Its side-product is that sodium metaaluminate market value is relatively low.
Summary of the invention
It is an object of the invention to provide the gangue comprehensive utilization that a kind of equipment is simple, added value of product is high, gangue utilization rate is high
Method.
The present invention provides a kind of method that gangue silicon aluminum carbon works in coordination with utilization, and step includes:
(1) gangue hydro-thermal method carries aluminum: by gangue and 15～36% hydrochloric acid be placed according to the solid-to-liquid ratio of 1 2～4 and to be contrary
In answering still, and acidleach 1～3 hours at 180～220 DEG C, obtain pickle liquor and acid leaching residue after solid-liquid separation；
(2) prepare aluminium polychlorid: it is 1.0～1.5mol/L that pickle liquor is first concentrated to concentration of aluminum chloride, then add at solution
Calcium aluminate powder to pH value to 3.5～4.5, last solution after 80 DEG C of ripenings 2～3 hours through being spray-dried to obtain aluminium polychlorid finished product；
(3) preparing sodium silicate: acid leaching residue is washed further, filter, filtering residue and sodium hydroxide are placed in autoclave, wherein
Silicon dioxide and the mol ratio 1 0.6～1 of sodium hydroxide, and add water according to solid-to-liquid ratio 1 2～4, react 3～5 at 150～240 DEG C
Hour, by reactant through filtering, isolated sodium silicate solution and filtering residue, filtering residue, through FLOTATION SEPARATION, obtains low ash carbon；
(4) carbon method prepares white carbon: sodium silicate solution obtained above is adjusted to 10～12 ° of B é, is passed through at 85～95 DEG C
Carbon dioxide reaction 1～5 hours, filter, and solid phase, through washing, is dried at 500～600 DEG C, obtains white carbon finished product.
Compared with prior art advantages of the present invention and effect: the present invention is without active coal gangue, thus it is comprehensive to simplify gangue
Utilize technique and reduce energy consumption, improve acid leaching efficiency by the method for high pressure-temperature acidleach.And whole technological process is one
The process of individual enrichment carbon, has not only obtained meeting the white carbon black product of GB, aluminium polychlorid product also obtains after technique terminates
The side-product of enrichment carbon, thus improve gangue comprehensive utilization ratio.
Figure of description
Fig. 1 gangue of the present invention silicon aluminum carbon works in coordination with the process chart of Application way
The white carbon infrared analysis result of Fig. 2 embodiment 1 preparation
Detailed description of the invention
The coal shale in brick making source used in following example respectively from: colliery, the Lu Anguo village, Shanxi, Jia Jiagou colliery, Liulin County,
Zhongyang County Easthome colliery.The Main Ingredients and Appearance of each feed coal spoil and content see attached list 1, and " other " in table 1 are moisture and wave
Send out part.Fig. 1 is shown in the technological process of embodiment.
The Main elements analysis table of table 1 each feed coal spoil
Embodiment 1
Weighing 20g gangue (colliery, the Lu Anguo village) to be placed in homogeneous reaction still, the hydrochloric acid adding 60ml20% is anti-at 200 DEG C
Answer 2 hours, after solid-liquid separation, obtain 12.42g acid leaching residue and about 60ml pickle liquor.Pickle liquor is concentrated into concentration of aluminum chloride is
1.5mol/L, adds 8.08g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, carries out spray drying and obtain 30.89g polymerization chlorine
Change aluminum finished product.Acid leaching residue is washed further, filters, and filtering residue inserts in homogeneous reaction still, and add 5.72g sodium hydroxide, 35
Milliliter distilled water, is warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate, obtain water white
Sodium silicate solution and 3.31g filtering residue, wherein filtering residue ash is 66.3% than the ash 87.8% of raw coal spoil, reduces 21.5%；
FLOTATION SEPARATION filtering residue, obtains low ash carbon, and its ash is 35.3%.Regulation sodium silicate solution, to 11 ° of B é, is heated to 85 DEG C and opens
Beginning to be passed through flow is 160ml/min carbon dioxide, filters after reacting 3 hours at 90 DEG C, and solid phase is through washing, finally 500～600
9.4g white carbon finished product it is dried to obtain at DEG C.Dialogue carbon black sample use ICP measure its dioxide-containing silica is 92.8% and aluminum
Content 0.04% reaches Standard, and the alumina content in aluminium polychlorid is 30.2%, and basicity is 62%, and pH value is 3.8
All meet aluminium polychlorid solid II class Grade A index, and with infrared spectrum analysis white carbon its result such as Fig. 2.
Embodiment 2
Weigh 20g gangue (Jia Jiagou colliery, Liulin County) to be placed in homogeneous reaction still, add the hydrochloric acid of 60ml20% 200
DEG C reaction 2 hours, solid-liquid separation and wash after obtain 13.31g acidleach propose aluminum slag, and about 60ml pickle liquor.Pickle liquor is dense
Being reduced to concentration of aluminum chloride is 1.5mol/L, adds 8.41g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, is spray-dried
Obtain 34.36g aluminium polychlorid finished product.Acid leaching residue is washed further, filters, and filtering residue is inserted in homogeneous reaction still, and added 4.89g
Sodium hydroxide, 30 milliliters of distilled water, be warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate,
To water white sodium silicate solution and 5.69g filtering residue, wherein filtering residue ash is 40.6% to reduce than the ash 75.2% of raw coal spoil
34.6%；FLOTATION SEPARATION filtering residue, obtaining its ash of low ash carbon is 20.3%.Regulation sodium silicate solution, to 11 ° of B é, is heated to
85 DEG C and to start to be passed through flow be 160ml/min carbon dioxide, filtering after reacting 3 hours at 90 DEG C, solid phase is through washing,
After at 500～600 DEG C, be dried to obtain 7.4g white carbon finished product.Dioxide-containing silica in white carbon is 92.6% and aluminum content
0.05% reaches Standard, and the alumina content in aluminium polychlorid is 31.2%, and basicity is 60%, and pH value is 3.9 equal
Meet aluminium polychlorid solid II class Grade A index.
Embodiment 3
Weigh 20g gangue (Zhongyang County Easthome colliery) to be placed in homogeneous reaction still, add the hydrochloric acid of 60ml20% at 200 DEG C
React 2 hours, obtain 15.48g acidleach after solid-liquid separation washing and propose aluminum slag, and about 60ml pickle liquor.Pickle liquor is concentrated
It is 1.5mol/L to concentration of aluminum chloride, adds 4.79g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, carry out being spray-dried
To 17.44g aluminium polychlorid finished product.Acid leaching residue is washed further, filters, and filtering residue is inserted in homogeneous reaction still, and added 3.25g
Sodium hydroxide, 20 milliliters of distilled water, be warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate,
To water white sodium silicate solution and 10.34g filtering residue, wherein filtering residue ash is 20.1% to drop than the ash 49.8% of raw coal spoil
Low by 29.7%；FLOTATION SEPARATION filtering residue, obtaining its ash of low ash carbon is 10.3%.Regulation sodium silicate solution is to 11 ° of B é, heating
To 85 DEG C and to start to be passed through flow be 160ml/min carbon dioxide, filter after reacting 3 hours at 90 DEG C, solid phase through washing,
Finally at 500～600 DEG C, it is dried to obtain 5.4g white carbon finished product.Dioxide-containing silica in white carbon is 91.8% and aluminum content
0.03% reaches Standard, and the alumina content in aluminium polychlorid is 31.7%, and basicity is 57%, and pH value is 3.8 equal
Meet aluminium polychlorid solid II class Grade A index.
Fig. 2 is the white carbon infrared analysis result of embodiment 1 preparation, and wherein 1 is the collection of illustrative plates of gained white carbon of the present invention, and 2 are
Standard white white carbon black collection of illustrative plates, in figure, 473.25cm-1,800.71cm-1,1099.83cm-1 are the characteristic peak of white carbon, wherein
473.25cm-1 correspondence Si-O-Si bending vibration, 800.71cm-1 correspondence Si-O-Si symmetrical stretching vibration, 1099.83cm-1 pair
Answer Si-O-Si antisymmetric stretching vibration；With standard white white carbon black global similarity in sample peak type, this sample is white carbon in summary.
Claims (1)
1. the method that a gangue silicon aluminum carbon works in coordination with utilization, it is characterised in that comprise the steps of:
The gangue weighing colliery, the 20g Lu Anguo village is placed in homogeneous reaction still, adds the hydrochloric acid of 60mL20% 200 DEG C of reactions
2 hours, after solid-liquid separation, obtain 12.42g acid leaching residue and 60mL pickle liquor；It is 1.5mol/L that pickle liquor is concentrated into concentration of aluminum chloride,
Add 8.08g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, carry out spray drying and obtain 30.89g aluminium polychlorid
Product；Acid leaching residue is washed further, filters, and filtering residue is inserted in homogeneous reaction still, and added 5.72g sodium hydroxide, 35 milliliters of steamings
Distilled water, is warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate, obtain water white sodium silicate
Solution and 3.31g filtering residue, wherein filtering residue ash is 66.3% than the ash 87.8% of raw coal spoil, reduces 21.5%；Floating
Choosing separates filtering residue, obtains low ash carbon, and its ash is 35.3%；Regulation sodium silicate solution, to 11 ° of B é, is heated to 85 DEG C and opens
Beginning, to be passed through flow be 160mL/min carbon dioxide, filters after reacting 3 hours at 90 DEG C, solid phase through washing, finally 500～
9.4g white carbon finished product it is dried to obtain at 600 DEG C；
Or comprise the steps of:
The gangue weighing Jia Jiagou colliery, 20g Liulin County is placed in homogeneous reaction still, adds the hydrochloric acid of 60mL20% at 200 DEG C
React 2 hours, obtain 13.31g acidleach after solid-liquid separation washing and propose aluminum slag, and 60mL pickle liquor；Pickle liquor is concentrated into chlorine
Change aluminum concentration is 1.5mol/L, adds 8.41g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, carries out spray drying and obtain
34.36g aluminium polychlorid finished product；Acid leaching residue is washed further, filters, and filtering residue is inserted in homogeneous reaction still, and added 4.89g
Sodium hydroxide, 30 milliliters of distilled water, be warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate,
To water white sodium silicate solution and 5.69g filtering residue, wherein filtering residue ash is 40.6% to drop than the ash 75.2% of raw coal spoil
Low by 34.6%；FLOTATION SEPARATION filtering residue, obtaining its ash of low ash carbon is 20.3%；Regulation sodium silicate solution, to 11 ° of B é, adds
Heat is to 85 DEG C and to start to be passed through flow be 160mL/min carbon dioxide, filters after reacting 3 hours at 90 DEG C, solid phase through washing,
Finally at 500～600 DEG C, it is dried to obtain 7.4g white carbon finished product；
Or comprise the steps of:
Weigh 20g Zhongyang County Easthome mine coal spoil to be placed in homogeneous reaction still, add the hydrochloric acid of 60mL 20% 200 DEG C of reactions
2 hours, obtain 15.48g acidleach after solid-liquid separation washing and propose aluminum slag, and 60mL pickle liquor；Pickle liquor is concentrated into aluminum chloride
Concentration is 1.5mol/L, adds 4.79g calcium aluminate powder, and after 80 DEG C of ripenings 2 hours, carries out spray drying and obtain 17.44g
Aluminium polychlorid finished product；Acid leaching residue is washed further, filters, and filtering residue is inserted in homogeneous reaction still, and added 3.25g hydroxide
Sodium, 20 milliliters of distilled water, be warming up to 200 DEG C, after reacting 5 hours, cools the temperature to room temperature, filters and separate, obtain colourless
Transparent sodium silicate solution and 10.34g filtering residue, wherein filtering residue ash is 20.1% to reduce than the ash 49.8% of raw coal spoil
29.7%；FLOTATION SEPARATION filtering residue, obtaining its ash of low ash carbon is 10.3%；Regulation sodium silicate solution, to 11 ° of B é, is heated to
85 DEG C and to start to be passed through flow be 160mL/min carbon dioxide, filtering after reacting 3 hours at 90 DEG C, solid phase is through washing,
After at 500～600 DEG C, be dried to obtain 5.4g white carbon finished product.
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| CN105800621A (en) * | 2016-03-31 | 2016-07-27 | 王嘉兴 | Silica gel preparation method |
| CN106365173B (en) * | 2016-08-29 | 2018-10-02 | 昆明理工大学 | A kind of method that sial slag prepares White Carbon black and water treatment agent |
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| CN109183194B (en) * | 2018-07-18 | 2020-08-28 | 山西载驰科技有限公司 | Method for preparing high-purity aluminum silicate fiber from coal gangue on large scale |
| CN111170372A (en) * | 2019-09-11 | 2020-05-19 | 沈阳环境科学研究院 | High-added-value comprehensive utilization method of coal gangue |
| CN114314778A (en) * | 2020-09-30 | 2022-04-12 | 中国科学院过程工程研究所 | Method for producing water purifying agent and white carbon black by roasting-free and reinforced acid leaching coal gangue |
| CN114314621B (en) * | 2020-09-30 | 2023-01-10 | 中国科学院过程工程研究所 | Method for producing metallurgical-grade aluminum oxide and white carbon black by roasting-free and reinforced acid leaching coal gangue |
| CN115007321A (en) * | 2022-03-31 | 2022-09-06 | 神华准能资源综合开发有限公司 | Method for recovering carbon from gangue acid leaching residue |
| CN115974119A (en) * | 2022-12-01 | 2023-04-18 | 百色实华环保科技有限公司 | Method for preparing polyaluminum chloride from medium-high aluminum slag in electrolytic aluminum overhaul slag |
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