CN109384236A - Gangue or oil shale slag produce silicon method - Google Patents
Gangue or oil shale slag produce silicon method Download PDFInfo
- Publication number
- CN109384236A CN109384236A CN201710674803.9A CN201710674803A CN109384236A CN 109384236 A CN109384236 A CN 109384236A CN 201710674803 A CN201710674803 A CN 201710674803A CN 109384236 A CN109384236 A CN 109384236A
- Authority
- CN
- China
- Prior art keywords
- gangue
- oil shale
- sulfuric acid
- solid
- carbon dioxide
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
Abstract
The present invention relates to gangues or oil shale slag to produce silicon method, including mainly has gangue, catalyst, sulfuric acid, sodium hydroxide, carbon dioxide and dehydrated alcohol；Using gangue or oil shale waste production technology, make full use of the carbon dioxide that purification is generated in coal gangue combustion property and calcination process, pass through sulfuric acid and the stringent formula of dehydrated alcohol, silicon series of products can be produced, waste utilization reduces environmental pollution, production technology is advanced, the advantages that producing silicon product line can put into production extensively, benefit the society.
Description
Technical field
The present invention relates to chemical industry silicon production technical fields, more specifically refer to gangue or oil shale slag production silicon side
Method.
Background technique
Now utilize gangue or oil shale solid waste, therefore on the basis of carry out refine and chemical technology production, will
Essence in waste produces useful costly chemical raw material with chemical processes, turns waste into wealth fewer.
Since the production method of silicon is more difficult, the side of chemical raw material silicon is extracted in gangue or oil shale
Method is more difficult to accomplish.
Therefore, it is necessary to develop gangue and oil shale slag production silicon method.
Summary of the invention
Present invention aims to overcome that the defect of the prior art, provides gangue or oil shale slag production silicon method, benefit
Silicon production technology is carried out with waste, to achieve the above object, the invention adopts the following technical scheme:
Gangue or oil shale slag of the present invention produce silicon method, including mainly have including mainly have or oil shale slag,
Catalyst, sulfuric acid, sodium hydroxide and carbon dioxide；
The gangue or oil shale slag production silicon method specifically the production method is as follows:
A. by gangue or oil shale slag through graded crushing, be crushed to 80-100 mesh；
B. fluidized bed furnace fluidized calcining is used at a temperature of 600-650 DEG C, fluidized bed furnace dynamic calcining can be by gangue
Carbon, be accompanied by a small amount of combustion catalyst, carry out thermal activation with baking modes, the carbon in raw material can be with completely burned；
C. organic matter therein is removed, the roasting powder that raw material firing is had quite active pozzolanic is stand-by；
D. the sulfuric acid of 25-30% concentration is used, solid-to-liquid ratio 1:3-4, is stirred to react 3-4 hours, until pH value by 90-95 DEG C of temperature
3-4 is acid-leaching reaction terminal；
E. supplement sulfuric acid is to 25-30%, and the reaction was continued, and same operation carries out 3 leachings repeatedly；
F. filtrate is continued to employ after being separated by solid-liquid separation again, and filter residue is the silica crude product of content >=90%, dense with 25-30%
Spend sodium hydroxide solution, solid-to-liquid ratio 1:3-4,95-100 DEG C stirring 2-3 hours, be prepared into qualified modulus sodium silicate solution；
G. gained qualification sodium metasilicate can be prepared into waterglass product through techniques such as agings；
H. the carbon dioxide gas for being about 30-40% with concentration is carried out with the sodium silicate solution for the qualified modulus adjusted
Carburizing reagent, carburizing temperature control is at 35 DEG C hereinafter, making carbonation rate reach 90% or more through multi-stage countercurrent absorption；
I. carbodiimide solution pH value 9-10 is controlled, a certain concentration dehydrated alcohol is added, as carbonization carries out, occurs white in solution
Colloidal precipitation, as hydrated SiO 2 precipitating；
J. it is separated by solid-liquid separation and adjusts pH value with sulfuric acid with after solid washing, be silica after drying, is i.e. white carbon black produces
Silicon product is made in product.
Further scheme is that the carbon dioxide gas is produced using during lime calcining and during calcined coal gangue
The carbon dioxide gas that concentration is about 30-40% can be obtained in raw gas after gas purification, purification process.
Further scheme is, during the carbonization carries out, passes through the adjustment of the additional amount to dehydrated alcohol, and carbonization
The control of temperature and speed can produce nano-scale white carbon black silicon product line.
Compared with the prior art, the invention has the advantages that: use gangue or oil shale waste production technology, sufficiently benefit
With coal gangue combustion property and and calcination process in generate the carbon dioxide of purification, pass through strictly matching for sulfuric acid and dehydrated alcohol
The advantages that side can produce silicon series of products, and waste utilization reduces environmental pollution, and production technology is advanced, produce silicon product line,
It can put into production extensively, benefit the society.
Detailed description of the invention
Fig. 1 is the flow diagram of the manufacturing process of the specific embodiment of the invention；
Appended drawing reference
Specific embodiment
In order to more fully understand technology contents of the invention, combined with specific embodiments below to technical solution of the present invention into
One step introduction and explanation, but not limited to this.
As shown in Figure 1, specific embodiments of the present invention one, including mainly have or oil shale slag, catalyst, sulfuric acid, hydrogen
Sodium oxide molybdena, carbon dioxide and dehydrated alcohol；
The gangue or oil shale slag production silicon method specifically the production method is as follows:
A. by gangue or oil shale slag through graded crushing, be crushed to 80-100 mesh；
B. fluidized bed furnace fluidized calcining is used at a temperature of 600-650 DEG C, fluidized bed furnace dynamic calcining can be by gangue
Carbon, be accompanied by a small amount of combustion catalyst, carry out thermal activation with baking modes, the carbon in raw material can be with completely burned；
C. organic matter therein is removed, the roasting powder that raw material firing is had quite active pozzolanic is stand-by；
D. the sulfuric acid of 25-30% concentration is used, solid-to-liquid ratio 1:3-4, is stirred to react 3-4 hours, until pH value by 90-95 DEG C of temperature
3-4 is acid-leaching reaction terminal；
E. supplement sulfuric acid is to 25-30%, and the reaction was continued, and same operation carries out 3 leachings repeatedly；
F. filtrate is continued to employ after being separated by solid-liquid separation again, and filter residue is the silica crude product of content >=90%, dense with 25-30%
Spend sodium hydroxide solution, solid-to-liquid ratio 1:3-4,95-100 DEG C stirring 2-3 hours, be prepared into qualified modulus sodium silicate solution；
G. gained qualification sodium metasilicate can be prepared into waterglass product through techniques such as agings；
H. the carbon dioxide gas for being about 30-40% with concentration, carburizing temperature control is at 35 DEG C hereinafter, with the conjunction adjusted
The sodium silicate solution of lattice modulus carries out carburizing reagent, so that carbonation rate is reached 90% or more through multi-stage countercurrent absorption；
I. carbodiimide solution pH value 9-10 is controlled, a certain concentration dehydrated alcohol is added, as carbonization carries out, occurs white in solution
Colloidal precipitation, as hydrated SiO 2 precipitating；
J. it is separated by solid-liquid separation and adjusts pH value with sulfuric acid with after solid washing, be silica after drying, is i.e. white carbon black produces
Silicon product is made in product.
By gangue or oil shale slag through graded crushing, be crushed to 80-100 mesh, at a temperature of 600-650 DEG C using boiling
Furnace fluidized calcining is risen, fluidized bed furnace dynamic calcining can be accompanied by a small amount of combustion catalyst, by the carbon in gangue with the side of roasting
Formula carries out thermal activation, and the carbon in raw material can be completely burned off, removes organic matter therein, raw material firing is had quite active
The roasting powder of pozzolanic is stand-by.It may be omitted with the activation time of a few hours, the heat of generation with fluidized bed furnace active coal gangue
Amount can provide heat source for subsequent reactions.With the sulfuric acid of 25-30% concentration, solid-to-liquid ratio 1:3-4, is stirred to react by 90-95 DEG C of temperature
3-4 hours, until pH value 3-4 is acid-leaching reaction terminal.Pickling repeatedly for three times.Filtrate is continued to employ after being separated by solid-liquid separation, filter residue 25-
30% sodium hydroxide solution when on solid-to-liquid ratio 1:3-4,95-100 DEG C of stirring 2-3, prepares qualified modulus sodium silicate solution.
Using the gas generated during lime calcining and during calcined coal gangue after gas purification, purification process
The carbon dioxide gas that concentration is about 30-40% is obtained, carries out carburizing reagent with the sodium silicate solution for the qualified modulus adjusted,
Carbonation rate is set to reach 90% or more through multi-stage countercurrent absorption.Control carbodiimide solution pH value 9-10, be added dehydrated alcohol, be carbonized into
It goes, occurs white colloidal precipitating in solution, as hydrated SiO 2 precipitates, and after being separated by solid-liquid separation, uses sulfuric acid after solid washing
PH value is adjusted, is silica, i.e. white carbon black product after drying.During being carbonized progress and by dehydrated alcohol
The adjustment of additional amount can produce nano-scale white carbon black, to realize the series of gangue or oil shale waste production silicon product.
Acid leaching residue is silica crude product by washing, drying, and content reaches 90% or more.Silica is slightly produced
Product are leached with 25-30% sodium hydroxide solution, are stirred to react 3-4 hours under the conditions of 95-100 DEG C, are prepared sodium silicate solution.It utilizes
The gas generated during lime calcining and during calcined coal gangue obtains concentration after gas purification, purification process and is about
The carbon dioxide gas of 30-40%, carburizing temperature control at 35 DEG C hereinafter, with the sodium silicate solution of the qualified modulus adjusted into
Row carburizing reagent makes carbonation rate reach 90% or more through multi-stage countercurrent absorption.Carbodiimide solution pH value 9-10 is controlled, a certain concentration is added
There is white colloidal precipitating as carbonization carries out in dehydrated alcohol in solution, as hydrated SiO 2 precipitates, through being separated by solid-liquid separation
Afterwards, pH value is adjusted with sulfuric acid after solid washing, is silica and white carbon black product after drying.During being carbonized progress
And the adjustment by the additional amount to dehydrated alcohol, nano-scale white carbon black can be produced, to realize that gangue produces silicon
The seriation of product.White carbon black product meets national standard, and the method proposes the white carbon black purity generated up to 99%.
Milk of lime is prepared through digestion after limestone calcination, carries out causticization with the carbodiimide solution after carburizing reagent, that is, sodium carbonate liquor
Reaction, 95-100 DEG C, reacts 2-3 hours, causticizing efficiency reaches 85% or more, and causticization liquid is exactly that hydroxide is molten in Keization reactor
Liquid, this technique are used to recycle sodium hydroxide, make sodium hydroxide Reusability, need to only supplement every time a small amount of.Causticization slag passes through
Product precipitated calcium carbonate is obtained after washing and drying.It is realized in process and sodium hydroxide is recycled, to be greatly lowered white
Carbon black production cost.
The present invention uses gangue or oil shale waste production technology, makes full use of coal gangue combustion property and and calcination process
The middle carbon dioxide for generating purification can produce silicon series of products by sulfuric acid and the stringent formula of dehydrated alcohol, waste utilization,
The advantages that reduction environmental pollution, production technology is advanced, produces silicon product line can put into production extensively, benefit the society.
It is above-mentioned that technology contents of the invention are only further illustrated with embodiment, in order to which reader is easier to understand, but not
It represents embodiments of the present invention and is only limitted to this, any technology done according to the present invention extends or recreation, by of the invention
Protection.Protection scope of the present invention is subject to claims.
Claims (3)
1. gangue or oil shale slag produce silicon method, it is characterised in that: including mainly having gangue or oil shale slag, urging
Agent, sulfuric acid, sodium hydroxide and carbon dioxide；
The gangue or oil shale slag production silicon method specifically the production method is as follows:
A. by gangue or oil shale slag through graded crushing, be crushed to 80-100 mesh；
B. fluidized bed furnace fluidized calcining is used at a temperature of 600-650 DEG C, fluidized bed furnace dynamic calcining can be by gangue
Carbon is accompanied by a small amount of combustion catalyst, carries out thermal activation with baking modes, the carbon in raw material can be with completely burned；
C. organic matter therein is removed, the roasting powder that raw material firing is had quite active pozzolanic is stand-by；
D. the sulfuric acid of 25-30% concentration is used, solid-to-liquid ratio 1:3-4 90-95 DEG C of temperature, is stirred to react 3-4 hours, until pH value 3-4 is
Acid-leaching reaction terminal；
E. supplement sulfuric acid is to 25-30%, and the reaction was continued, and same operation carries out 3 leachings repeatedly；
F. filtrate is continued to employ after being separated by solid-liquid separation again, and filter residue is the silica crude product of content >=90%, with 25-30% concentration hydrogen
Sodium hydroxide solution, solid-to-liquid ratio 1:3-4,95-100 DEG C stirring 2-3 hours, be prepared into qualified modulus sodium silicate solution；
G. gained qualification sodium metasilicate can be prepared into waterglass product through techniques such as agings；
H. the carbon dioxide gas for being about 30-40% with concentration is carbonized with the sodium silicate solution for the qualified modulus adjusted
Reaction makes carbonation rate reach 90% or more through multi-stage countercurrent absorption；
I. carbodiimide solution pH value 9-10 is controlled, dehydrated alcohol is added, as carbonization carries out, white colloidal precipitating occurs in solution, i.e.,
For hydrated SiO 2 precipitating；
J. it is separated by solid-liquid separation and adjusts pH value with sulfuric acid with after solid washing, be silica, i.e. white carbon black product, system after drying
At silicon product.
2. gangue according to claim 1 or oil shale slag produce silicon method, it is characterised in that: the carbon dioxide
Gas can be obtained after gas purification, purification process using the gas generated during lime calcining and during calcined coal gangue
The carbon dioxide gas for being about 30-40% to concentration.
3. gangue according to claim 1 or oil shale slag produce silicon method, it is characterised in that: the carbonization carries out
In the process, by the adjustment of the additional amount to dehydrated alcohol and the control of carburizing temperature and speed, nanoscale can be produced
White carbon black silicon product line.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710674803.9A CN109384236A (en) | 2017-08-09 | 2017-08-09 | Gangue or oil shale slag produce silicon method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710674803.9A CN109384236A (en) | 2017-08-09 | 2017-08-09 | Gangue or oil shale slag produce silicon method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109384236A true CN109384236A (en) | 2019-02-26 |
Family
ID=65414679
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710674803.9A Pending CN109384236A (en) | 2017-08-09 | 2017-08-09 | Gangue or oil shale slag produce silicon method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109384236A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281820A (en) * | 2000-02-01 | 2001-01-31 | 刘成长 | Technological process for producing aluminium salt and silicate by using coal gangue |
| CN101693538A (en) * | 2009-09-30 | 2010-04-14 | 渤海大学 | Method for preparing white carbon black by using waste bauxite, diatomite and oil shale residue |
| US20100119426A1 (en) * | 2007-04-03 | 2010-05-13 | Qin Jinguo | Process for recovery of silica followed by alumina from coal fly ash |
| CN102583417A (en) * | 2012-03-26 | 2012-07-18 | 西安科技大学 | Method for preparing water glass by using gangue |
| CN102701220A (en) * | 2012-05-22 | 2012-10-03 | 韩钊武 | Method for preparing white carbon black by oxygen-free high-temperature calcination and thermal activation of coal gangue |
| CN103395793A (en) * | 2013-07-22 | 2013-11-20 | 沈阳鑫博工业技术发展有限公司 | Method for preparing aluminum oxide and white carbon black by utilizing oil shale ash |
-
2017
- 2017-08-09 CN CN201710674803.9A patent/CN109384236A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281820A (en) * | 2000-02-01 | 2001-01-31 | 刘成长 | Technological process for producing aluminium salt and silicate by using coal gangue |
| US20100119426A1 (en) * | 2007-04-03 | 2010-05-13 | Qin Jinguo | Process for recovery of silica followed by alumina from coal fly ash |
| CN101693538A (en) * | 2009-09-30 | 2010-04-14 | 渤海大学 | Method for preparing white carbon black by using waste bauxite, diatomite and oil shale residue |
| CN102583417A (en) * | 2012-03-26 | 2012-07-18 | 西安科技大学 | Method for preparing water glass by using gangue |
| CN102701220A (en) * | 2012-05-22 | 2012-10-03 | 韩钊武 | Method for preparing white carbon black by oxygen-free high-temperature calcination and thermal activation of coal gangue |
| CN103395793A (en) * | 2013-07-22 | 2013-11-20 | 沈阳鑫博工业技术发展有限公司 | Method for preparing aluminum oxide and white carbon black by utilizing oil shale ash |
Non-Patent Citations (2)
| Title |
|---|
| HONGYU GAO ET AL: ""Synthesis Method of White Carbon Black Utilizing Water-Quenching Blast Furnace Slag"", 《ENERGY FUELS》 * |
| 赵瑞彤 等: ""煤矸石酸浸废渣制备白炭黑的工艺研究"", 《无机盐工业》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101570129B1 (en) | Method of producing calcium carbonate from waste and byproducts | |
| CN108149022B (en) | A kind of method of vanadium slag blank roasting ammonium vanadium extraction | |
| CN102897810B (en) | Method for producing aluminum oxide by using fly ash | |
| CN102219257A (en) | Method for preparing vanadium pentoxide | |
| CN101863500A (en) | Method for producing alumina with aluminum-containing metallurgical material | |
| CN102139918A (en) | Method for preparing high-grade synthetic rutile | |
| CN102220478A (en) | Preparation method for vanadium pentoxide | |
| CN103395793B (en) | Method for preparing aluminum oxide and white carbon black by utilizing oil shale ash | |
| CN108642271B (en) | Novel method for producing vanadium dioxide from vanadium-containing shale without ammonium vanadium precipitation | |
| CN101723461A (en) | Neutralization aluminum removing method for sodium chromate alkali solution | |
| CN101244836A (en) | Method for extracting aluminum oxide and white carbon black from bituminous shale waste slag | |
| CN102815730B (en) | Oxidation sweetening-the magnetization of a kind of high-sulfur bauxite removes ferrum preprocess method | |
| CN101306819B (en) | Process for abstracting white carbon black from fly ash or slag | |
| CN109022806A (en) | A method of utilizing the vanadium liquid removal of impurities clay standby vanadic anhydride of vanadium | |
| CN113293297B (en) | Multi-element recycling of residual oil hydrogenation waste catalyst | |
| CN102220499A (en) | Roasting-leaching method of fine vanadium slags | |
| CN108842053A (en) | The method of comprehensive utilization of Low grade manganese ore and electrolytic manganese crystallization double salt | |
| CN109384236A (en) | Gangue or oil shale slag produce silicon method | |
| CN105668597B (en) | The method of flyash soda acid combined extracting aluminium base product and silica-based products | |
| CN102220495A (en) | Method for purifying vanadium-precipitating mother liquor | |
| CN106044820A (en) | Method for producing strontium carbonate from carbon dioxide in exhaust gas | |
| CN113564688B (en) | Preparation method of calcium carbonate whisker | |
| CN111484048A (en) | Treatment method for low-energy-consumption desulfurization and desilication high-efficiency alumina dissolution of refractory bauxite | |
| CN107381585A (en) | Method for extracting aluminum silicon by pyrolyzing fly ash ammonium sulfate roasted clinker | |
| CN109384252A (en) | Coal measures association tailing produces aluminium technique |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190226 |