CN104787791B - A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product - Google Patents
A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product Download PDFInfo
- Publication number
- CN104787791B CN104787791B CN201510147699.9A CN201510147699A CN104787791B CN 104787791 B CN104787791 B CN 104787791B CN 201510147699 A CN201510147699 A CN 201510147699A CN 104787791 B CN104787791 B CN 104787791B
- Authority
- CN
- China
- Prior art keywords
- product
- microwave
- reaction
- solid
- gangue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses and a kind of utilize gangue to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product, the method comprises the following steps: microwave reaction, microwave acidification, ammonification absorb, neutralize.The present invention is compared with the methods such as domestic molten, the high-temperature calcination of existing acid, response time is greatly shortened, and energy consumption of reaction is greatly lowered, and not only shortens technological process, and whole course of processing low-carbon environment-friendly, really realize the environmentally friendly efficient comprehensive development and utilization of gangue.
Description
Technical field
The present invention relates to comprehensive utilization of energy technical field, be specifically related to one and utilize bastard coal made of stones
Standby cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product.
Background technology
China is coal production state maximum in the world and country of consumption, and the spoil amount of coal mine drainage is very
Greatly, its discharge capacity is about the 15%-20% of colliery raw coal output, is that the current discharge capacity of China is maximum
One of industrial solid castoff, be considered " industrial waste " that the gas, liquid, solid three disasters are various.
Account for the 1/4 of whole nation industrial residue discharge capacity.At present total burden of whole nation gangue oneself reach 30
Hundred million more than t, form hillock more than 1500, and discharge capacity are still increasing year by year.A large amount of coals
Spoil is thrown aside, takies tract.Sulfide effusion or leaching in gangue can be polluted
Air, farmland and water body.Hillock also can spontaneous combustion breaking out of fire, or in avalanche in rainy season, silt up
River causes disaster.
Because the stacking environmental pollution of gangue is badly in need of solving, therefore many gangues
Recycle technique in succession to occur, be most commonly used that the methods such as molten, the high-temperature calcination of acid at present, this
Although a little methods can effectively reduce the heap of gangue high-volume, but there is relatively costly, energy
The problem that consumption is high, technological process is complicated.
Summary of the invention
It is desirable to provide one utilizes gangue to prepare cleaned coal by-product fluosilicic acid ammonium and inclined aluminum
The method of acid sodium product, dirty with the environment solving to be caused seriously because of the bulk deposition of gangue
Dye and ecological disruption problem, this method utilize microwave treatment distribution extract silicon therein, ferrum, aluminum,
Carbon, reaches the current of comprehensive utilization, compares other high temperature methods and have more industrialization promotion
Prospect.
The present invention is achieved by the following technical programs:
A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product,
The method comprises the following steps:
(1) microwave reaction: pulverize coal gangue to 80-200 mesh and auxiliary agent hexafluosilicic acid according to than
Example mixes, and is placed in microwave reaction kettle control material temperature and is 90-110 DEG C and reacts, solid after reaction
Liquid separates, and obtains solid a；
(2) microwave acidification: solid a is proportionally carried out microwave acidification reaction with sulphuric acid, control
Souring temperature processed is 150-300 DEG C, and the acidification reaction time is 20-60min, obtains solid b；
(3) ammonification absorbs: the gas that microwave reaction and microwave acidification produce absorbs through ammonification
Tower, obtains ammonium fluosilicate product；
(4) neutralize: solid b is proportionally mixed homogeneously with sodium hydroxide, control pH value
Reacting, after reaction, solid-liquid separation obtains cleaned coal and sodium metaaluminate product.
In described step (1), gangue and auxiliary agent hexafluosilicic acid are 1t:(1.5-4 according to quality volume)
m3Ratio carry out hybrid reaction, the response time is 20-70min, and the concentration of auxiliary agent hexafluosilicic acid is
15-30%.
In described step (1), microwave power is 1-40kw, and microwave frequency is 200-4000MHz.
In described step (2), solid a and sulphuric acid are 1t:(0.2-1 according to quality volume) m3's
Ratio carries out microwave acidification reaction, and sulfuric acid concentration is 50-98%.
In described step (2), microwave power is 1-30kw, and microwave frequency is 200-4000MHz.
In described step (4), solid b and sodium hydroxide are 1:(1-5 according to mass volume ratio)
m3Ratio hybrid reaction, control PH is 6-8, and the control response time is 10-70min, hydrogen-oxygen
The concentration changing sodium is 10-30%.
The beneficial effects of the present invention is: after gangue and auxiliary agent acid are sufficiently mixed, in industry
Reacting in microwave equipment, solid-liquid separation after reaction, solid adds sulphuric acid and carries out microwave acidification
Reaction, the gas produced during microwave reaction and microwave acidification prepares fluorine silicon by ammonification absorption
Acid ammonium, the solid after microwave acidification adds sodium hydroxide and is neutralized reaction, and reaction obtains after terminating
To solid be head coal product, liquid is sodium metaaluminate product, the present invention and domestic existing acid is molten,
The methods such as high-temperature calcination are compared, and the response time is greatly shortened, and energy consumption of reaction is greatly lowered, no
Only shorten technological process, and whole course of processing low-carbon environment-friendly, really realize bastard coal stone ring
The efficient comprehensive development and utilization of border friendly.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is further described, but wants
The scope asking protection is not limited to described.
Embodiment one
Pulverize coal gangue to 80 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 15% is according to quality volume
For 1t:1.5m3Ratio mix, be placed in microwave reaction kettle control material temperature be 90 DEG C, micro-
Wave power is 2kw, and microwave frequency is that 200MHz reacts, and the response time is 20min, instead
Should solid-liquid separation afterwards, obtain solid a, be that the sulphuric acid of 50% is according to mass body by solid a with concentration
Amass as 1t:0.2m3Ratio carry out microwave acidification reaction, controlling souring temperature is 150 DEG C, micro-
Wave power is 2kw, and microwave frequency is 300MHz, and the acidification reaction time is 20min, consolidate
The gas that body b, microwave reaction and microwave acidification produce, through ammonification absorption tower, obtains hexafluosilicic acid
Ammonium product, by solid b and concentration be the sodium hydroxide of 10% be 1t:1m according to mass volume ratio3
Ratio mixing, controlling pH value is 6 to react, and the response time is 10min, solid after reaction
Liquid isolated cleaned coal and sodium metaaluminate product.
Embodiment two
Pulverize coal gangue to 80 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 15% is according to quality volume
For 1t:1.5m3Ratio mix, be placed in microwave reaction kettle control material temperature be 90 DEG C, micro-
Wave power is 5kw, and microwave frequency is that 1000MHz reacts, and the response time is 20min,
Solid-liquid separation after reaction, obtains solid a, is that the sulphuric acid of 70% is according to quality by solid a and concentration
Volume is 1t:0.7m3Ratio carry out microwave acidification reaction, controlling souring temperature is 150 DEG C,
Microwave power is 5kw, and microwave frequency is 915MHz, and the acidification reaction time is 30min, obtains
The gas that solid b, microwave reaction and microwave acidification produce, through ammonification absorption tower, obtains fluorine silicon
Acid ammonium product, by solid b and concentration be the sodium hydroxide of 20% be 1t:4m according to mass volume ratio3
Ratio mixing, controlling pH value is 7 to react, and the response time is 30min, solid after reaction
Liquid isolated cleaned coal and sodium metaaluminate product.
Embodiment three
Pulverize coal gangue to 100 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 25% is according to quality volume
For 1t:1m3Ratio mix, be placed in microwave reaction kettle control material temperature be 100 DEG C, micro-
Wave power is 10kw, and microwave frequency is that 2500MHz reacts, and the response time is 30min,
Solid-liquid separation after reaction, obtains solid a, is that the sulphuric acid of 80% is according to quality by solid a and concentration
Volume is 1t:0.6m3Ratio carry out microwave acidification reaction, controlling souring temperature is 200 DEG C,
Microwave power is 10kw, and microwave frequency is 2450MHz, and the acidification reaction time is 30min,
To solid b, the gas of microwave reaction and microwave acidification generation, through ammonification absorption tower, obtains fluorine
Ammonium silicate product, by solid b with the sodium hydroxide that concentration is 25% according to mass volume ratio be
1t:3m3Ratio mixing, controlling pH value is 8 to react, and the response time is min, after reaction
Solid-liquid separation obtains cleaned coal and sodium metaaluminate product.
Embodiment four
Pulverize coal gangue to 120 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 18% is according to quality volume
For 1t:2.5m3Ratio mix, be placed in microwave reaction kettle control material temperature be 100 DEG C,
Microwave power is 25kw, and microwave frequency is that 1200MHz reacts, and the response time is 35min,
Solid-liquid separation after reaction, obtains solid a, is that the sulphuric acid of 65% is according to quality by solid a and concentration
Volume is 1t:0.6m3Ratio carry out microwave acidification reaction, controlling souring temperature is 200 DEG C,
Microwave power is 6kw, and microwave frequency is 1300MHz, and the acidification reaction time is 35min,
To solid b, the gas of microwave reaction and microwave acidification generation, through ammonification absorption tower, obtains fluorine
Ammonium silicate product, by solid b with the sodium hydroxide that concentration is 18% according to mass volume ratio be
1t:2m3Ratio mixing, controlling pH value is 7 to react, and the response time is 35min, reaction
Rear solid-liquid separation obtains cleaned coal and sodium metaaluminate product.
Embodiment five
Pulverize coal gangue to 150 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 25% is according to quality volume
For 1t:3m3Ratio mix, be placed in microwave reaction kettle control material temperature be 105 DEG C, micro-
Wave power is 30kw, and microwave frequency is that 3200MHz reacts, and the response time is 60min,
Solid-liquid separation after reaction, obtains solid a, is that the sulphuric acid of 75% is according to quality by solid a and concentration
Volume is 1t:0.8m3Ratio carry out microwave acidification reaction, controlling souring temperature is 250 DEG C,
Microwave power is 25kw, and microwave frequency is 3500MHz, and the acidification reaction time is 45min,
To solid b, the gas of microwave reaction and microwave acidification generation, through ammonification absorption tower, obtains fluorine
Ammonium silicate product, by solid b with the sodium hydroxide that concentration is 25% according to mass volume ratio be
1t:4m3Ratio mixing, controlling pH value is 8 to react, and the response time is 60min, reaction
Rear solid-liquid separation obtains cleaned coal and sodium metaaluminate product.
Embodiment six
Pulverize coal gangue to 200 mesh and concentration be that the auxiliary agent hexafluosilicic acid of 30% is according to quality volume
For 1t:4m3Ratio mix, be placed in microwave reaction kettle control material temperature be 110 DEG C, micro-
Wave power is 40kw, and microwave frequency is that 3800MHz reacts, and the response time is 70min,
Solid-liquid separation after reaction, obtains solid a, is that the sulphuric acid of 98% is according to quality by solid a and concentration
Volume is 1t:1m3Ratio carry out microwave acidification reaction, controlling souring temperature is 300 DEG C, micro-
Wave power is 30kw, and microwave frequency is 4000MHz, and the acidification reaction time is 60min, obtains
The gas that solid b, microwave reaction and microwave acidification produce, through ammonification absorption tower, obtains fluorine silicon
Acid ammonium product, by solid b and concentration be the sodium hydroxide of 30% be 1t:5m according to mass volume ratio3
Ratio mixing, controlling pH value is 8 to react, and the response time is 70min, solid after reaction
Liquid isolated cleaned coal and sodium metaaluminate product.
Claims (6)
1. one kind utilizes gangue to prepare cleaned coal by-product fluosilicic acid ammonium and the side of sodium metaaluminate product
Method, it is characterised in that: the method comprises the following steps:
(1) microwave reaction: pulverize coal gangue to 80-200 mesh and auxiliary agent hexafluosilicic acid according to than
Example mixes, and is placed in microwave reaction kettle control material temperature and is 90-110 DEG C and reacts, solid after reaction
Liquid separates, and obtains solid a；
(2) microwave acidification: solid a is proportionally carried out microwave acidification reaction with sulphuric acid, control
Souring temperature processed is 150-300 DEG C, and the acidification reaction time is 20-60min, obtains solid b；
(3) ammonification absorbs: the gas that microwave reaction and microwave acidification produce absorbs through ammonification
Tower, obtains ammonium fluosilicate product；
(4) neutralize: solid b is proportionally mixed homogeneously with sodium hydroxide, control ph
Reacting, after reaction, solid-liquid separation obtains cleaned coal and sodium metaaluminate product.
The most according to claim 1 utilize gangue prepare cleaned coal by-product fluosilicic acid ammonium and
The method of sodium metaaluminate product, it is characterised in that: gangue and auxiliary agent in described step (1)
Hexafluosilicic acid is 1t:(1.5-4 according to quality volume) m3Ratio carry out hybrid reaction, during reaction
Between be 20-70min, the concentration of auxiliary agent hexafluosilicic acid is 15-30%.
The most according to claim 1 utilize gangue prepare cleaned coal by-product fluosilicic acid ammonium and
The method of sodium metaaluminate product, it is characterised in that: in described step (1), microwave power is
1-40kw, microwave frequency is 200-4000MHz.
The most according to claim 1 utilize gangue prepare cleaned coal by-product fluosilicic acid ammonium and
The method of sodium metaaluminate product, it is characterised in that: in described step (2), solid a presses with sulphuric acid
It is 1t:(0.2-1 according to quality volume) m3Ratio carry out microwave acidification reaction, sulfuric acid concentration is
50-98%.
The most according to claim 1 utilize gangue prepare cleaned coal by-product fluosilicic acid ammonium and
The method of sodium metaaluminate product, it is characterised in that: in described step (2), microwave power is
1-30kw, microwave frequency is 200-4000MHz.
The most according to claim 1 utilize gangue prepare cleaned coal by-product fluosilicic acid ammonium and
The method of sodium metaaluminate product, it is characterised in that: solid b and hydroxide in described step (4)
Sodium is 1t:(1-5 according to mass volume ratio) m3Ratio hybrid reaction, control pH is 6-8, control
Response time processed is 10-70min, and the concentration of sodium hydroxide is 10-30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510147699.9A CN104787791B (en) | 2015-03-31 | 2015-03-31 | A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510147699.9A CN104787791B (en) | 2015-03-31 | 2015-03-31 | A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104787791A CN104787791A (en) | 2015-07-22 |
| CN104787791B true CN104787791B (en) | 2016-08-24 |
Family
ID=53553044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510147699.9A Expired - Fee Related CN104787791B (en) | 2015-03-31 | 2015-03-31 | A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104787791B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536710A (en) * | 2018-11-06 | 2019-03-29 | 李静娴 | A kind of gangue acidification extraction aluminium simple substance technique |
| CN109824074A (en) * | 2019-02-19 | 2019-05-31 | 昆明理工大学 | A kind of production method of aluminium oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288107A (en) * | 2013-05-29 | 2013-09-11 | 如皋市乐恒化工有限公司 | Method for preparing high-purity aluminum oxide from coal gangue |
| CN104457192A (en) * | 2014-11-25 | 2015-03-25 | 贵州远盛钾业科技有限公司 | Potassium-containing shale intermediate microwave processing device |
| CN104457141A (en) * | 2014-11-26 | 2015-03-25 | 贵州远盛钾业科技有限公司 | Method for processing shale containing potassium intermediate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8647400B2 (en) * | 2008-09-03 | 2014-02-11 | Tata Steel Limited | Beneficiation process to produce low ash clean coal from high ash coals |
-
2015
- 2015-03-31 CN CN201510147699.9A patent/CN104787791B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288107A (en) * | 2013-05-29 | 2013-09-11 | 如皋市乐恒化工有限公司 | Method for preparing high-purity aluminum oxide from coal gangue |
| CN104457192A (en) * | 2014-11-25 | 2015-03-25 | 贵州远盛钾业科技有限公司 | Potassium-containing shale intermediate microwave processing device |
| CN104457141A (en) * | 2014-11-26 | 2015-03-25 | 贵州远盛钾业科技有限公司 | Method for processing shale containing potassium intermediate |
Non-Patent Citations (1)
| Title |
|---|
| 微波场中煤矸石酸解制备氧化铝的研究;冯臻;《非金属矿》;20100731;第33卷(第4期);第57-59页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104787791A (en) | 2015-07-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103397128B (en) | Method used for extracting iron from red mud by drastic reduction and method used for preparing gel material from secondary tailings | |
| CN104760976B (en) | A kind of microwave treatment potassium-bearing shale method of comprehensive utilization | |
| CN103086779B (en) | Method for producing alkaline fertilizer by using phosphate rock tailings or low-grade phosphate rock through blast furnace process | |
| CN102358623A (en) | Method for producing aluminum oxide by treating fly ash through ammonia process | |
| CN104310836A (en) | Modified phosphogypsum as well as preparation method and use of modified phosphogypsum | |
| CN105964659A (en) | Comprehensive resource recycling method for waste cathode carbon blocks of aluminum cells | |
| CN103074456A (en) | Method for recycling iron from waste red mud in alumina production | |
| CN105861845B (en) | A kind of method of Combined Treatment copper ashes and slag | |
| CN104004919B (en) | The environment-protective circulating recycling technique of waste residue in a kind of electrolytic manganese production | |
| CN104876250A (en) | Method for extraction of lithium and removal of aluminum by vitriolization of lepidolite | |
| CN105197975A (en) | Method for preparing light calcium carbonate from converter steel slag | |
| CN104162536A (en) | Harmless treatment and resource utilization method of waste cathode | |
| CN103571983A (en) | Autoclaving treatment modification technology for converter steel slag and applications thereof | |
| CN104787791B (en) | A kind of gangue is utilized to prepare cleaned coal by-product fluosilicic acid ammonium and the method for sodium metaaluminate product | |
| CN104291539A (en) | Method for dealkalizing Bayer process red mud by using CO2 and waste acid in combined way | |
| CN101591011B (en) | Method for treating waste acid into calcium hydrophosphate fertilizer | |
| CN108910849A (en) | A method of circulation extracts phosphorus from sludge ash | |
| CN109207658B (en) | Recycling method for phosphorus removal of biomass ash modified converter steel slag | |
| CN103086778A (en) | Method for producing alkaline fertilizer from insoluble potassium-containing rock by kiln process | |
| CN111994937B (en) | Method for recycling calcium fluoride from fluorine-containing sludge | |
| CN106011493A (en) | Roasting method of low-grade vanadium slags | |
| CN103232181A (en) | Preparation method of titanium dioxide slag concrete additive | |
| CN105506292A (en) | Heavy metal sludge innocent treatment and resource utilization method | |
| CN102653403B (en) | Process method for preparing calcium carbide by recycling calcium carbide slag | |
| CN110511072B (en) | Method for preparing nutrient soil by using organic waste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 554200 Transforming Industrial Park in Wanshan District, Tongren City, Guiyang City, Guizhou Province Patentee after: Guizhou Kaisheng Potassium Technology Co.,Ltd. Address before: 554200 Transforming Industrial Park in Wanshan District, Tongren City, Guizhou Province Patentee before: GUIZHOU YUANSHENG POTASSIUM TECHNOLOGY Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160824 |