CN103449483A - Impurity removing method in process of preparing alumina from fly ash by utilizing acid method - Google Patents
Impurity removing method in process of preparing alumina from fly ash by utilizing acid method Download PDFInfo
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- CN103449483A CN103449483A CN2012101706605A CN201210170660A CN103449483A CN 103449483 A CN103449483 A CN 103449483A CN 2012101706605 A CN2012101706605 A CN 2012101706605A CN 201210170660 A CN201210170660 A CN 201210170660A CN 103449483 A CN103449483 A CN 103449483A
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Abstract
The invention relates to an impurity removing method in a process of preparing alumina from fly ash by utilizing an acid method. The method comprises following steps: by utilizing the characteristic that iron (III) dimethyldithiocarbamate does not precipitate in an alkaline environment condition, adjusting the pH value of the system to the alkaline range by adding ammonia water, ammonia gas, or sodium hydroxide to precipitate iron in the form of iron hydroxide, then subjecting the reaction liquid to a filtration separation treatment so as to obtain an aluminium salt solution without iron, crystallizing the aluminium salt solution without iron to precipitate, filtrating to separate so as to obtain aluminium salt crystals and filtration liquid, burning the aluminium salt crystals so as to obtain purified alumina. The method solves the technical problems of complicated technologies and difficult separation of impurities in the conventional acid method, and has the advantages of prominent iron-removing effect, simple technology, easy operation, and low technology cost.
Description
Technical field
The present invention relates to a kind of impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing that adopt.
Background technology
Thermal power generation occupies dominant position in the electrification structure of China, and coal-fired thermal power generation occupies absolute ratio in thermal power generation, and flyash is the solid waste that coal-burning power plant dumps.
In recent years, development along with power industry, the quantity discharged sharp increase of flyash, according to the report in January, 2009 of Chinese coal TIA, the producing coal total amount of China in 2008 is 27.16 hundred million tons, and wherein most of for generating, the annual emissions of China's flyash is over 200,000,000 tons, the accumulative total volume of cargo in storage surpasses 2,500,000,000 tons, taken a large amount of arable lands, on a large scale ground contamination environment.Therefore; carry out the comprehensive utilizating research of flyash, realize its resource utilization, be not only and be related to the significant problem urgently to be resolved hurrily that China's power industry and related industries Sustainable development face; and, to protection land resources, minimizing and elimination environmental pollution, realize that recycling economy is significant.
The major ingredient contained in flyash has: Al
2o
3, SiO
2, Fe
2o
3, FeO, TiO
2, CaO, K
2o, MgO etc., wherein the content of aluminum oxide generally can reach 20%～40%, reaches as high as more than 50%, can replace bauxite to become a kind of good alumina resource.Because flyash is the product of high-temp combustion in burner hearth, so most flyash is to exist with the vitreum form, its topology convergence degree is large, and chemical property is very stable.
Both at home and abroad by the method for the standby aluminum oxide of coal ash for manufacturing, be mainly acid system, alkaline process at present.
Acid system (sulfuric acid directly leaches method, solubilization of ammonium fluoride method, exsiccated ammonium alum etc.) is with the acidic aqueous solution of the mineral acid such as sulfuric acid, hydrochloric acid or the corresponding aluminium salt that obtains as the strong acid weak base salts such as ammonium sulfate processing aluminum-containing raw material while producing aluminum oxide, then produces aluminum oxide.Its shortcoming is to need expensive acid-resistant system, the recovery more complicated of acid and from aluminum salt solution deironing also more difficult.
Alkaline process (limestone sintering is from efflorescence method, soda-lime sintering process, sodium carbonate roasting method etc.) is to utilize alkali to extract aluminum oxide from flyash, due to silicon, with aluminium, is dissolved in alkaline solution, needs the idea desiliconization.When flyash adopts alkaline process to extract aluminum oxide during the alkali Aluminum, the foreign ion not strippings substantially such as magnesium, calcium, iron, but whole technology chain is longer, and facility investment is large, and energy consumption is high, and the quantity of slag is large; While adopting acid system to extract aluminum oxide, aluminium, iron are miscible in dissolution fluid, and impurity iron is difficult to separate, and has a strong impact on the alumina product quality.Acid system flyash is produced the manque deironing impurity removal process of aluminum oxide at present.
Summary of the invention
Prepare alumina technology complexity, impurity iron and be difficult to the technical problem of separating in order to solve existing acid system, the invention provides a kind of impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing that adopt, adopt Sodium dimethyldithiocarbamate 40min or potassium dimethyldithiocarbamate to remove as precipitation agent the new process that flyash is produced iron ion in the acidic aqueous solution of aluminium salt in alumina process, its de-ferrous effect is remarkable, technique is simple, easy handling, and precipitation agent can be processed reuse, and process costs is low.
Technical solution of the present invention is:
Adopt the impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing, its special character is: comprise the following steps:
1] under agitation the precipitation agent Sodium dimethyldithiocarbamate 40min is pressed to Fe
3+: Na
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, and reaction produces the black precipitate ferric dimethyl dithiocarbamate, collects filtrate through filtering separation and obtains aluminum salt solution after deironing; The acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains;
2], by the aluminum salt solution crystallization after deironing, filtering separation, obtain aluminium salt crystal and collect filtrate for later use;
3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
Also comprise step 4]:
By step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] the filtrate of collection in, and by adding sodium hydroxide, potassium hydroxide or ammoniacal liquor, adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, reclaim its use of storage, and the filtrate that collection contains regeneration precipitation agent Sodium dimethyldithiocarbamate 40min is for step 1].
Above-mentioned steps 4] pH value adjusted is 9～13.
Upper step 1] in add precipitation agent amount for according to Fe
3+: Na
+the molar mass ratio is 1: 2～4.
The another kind of impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing that adopt, its special character is: comprise the following steps:
1] under agitation the precipitation agent potassium dimethyldithiocarbamate is pressed to Fe
3+: K
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, and reaction produces the black precipitate ferric dimethyl dithiocarbamate, collects filtrate through filtering separation and obtains aluminum salt solution after deironing; The acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains;
2], by the aluminum salt solution crystallization after deironing, filtering separation, obtain aluminium salt crystal and collect filtrate for later use;
3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
Also comprise step 4]:
By step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] the filtrate of collection in, and by adding sodium hydroxide, potassium hydroxide, ammoniacal liquor or ammonia, adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, reclaim its use of storage, and the filtrate that collection contains regeneration precipitation agent potassium dimethyldithiocarbamate is for step 1].
Above-mentioned steps 4] pH value adjusted is 9～13.
Above-mentioned steps 1] in add precipitation agent amount for according to Fe
3+: K
+the molar mass ratio is 1: 2～4.
Of the present invention had advantage is:
1, the present invention precipitates the foreign ions such as deironing with Sodium dimethyldithiocarbamate 40min or potassium dimethyldithiocarbamate in the process of acidic process flyash as precipitation agent, solve iron contamination in the acid technological process treated coal ash and removed difficult problem, its sedimentation speed is fast, one-tenth solid impurity particle great Yi removes, de-ferrous effect is remarkable, technique is simple, easy handling.
2, the present invention recycles used precipitation agent by reaction, turns waste into wealth, and the removal of impurities cost is low.
The accompanying drawing explanation
The schema that Fig. 1 is removal of impurities in acidic process flyash technique of the present invention.
Embodiment
A kind of impurity-removing method that adopts the acid system aluminum oxide standby by coal ash for manufacturing, comprise the following steps: 1] under agitation the precipitation agent Sodium dimethyldithiocarbamate 40min is pressed to Fe
3+: Na
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, reaction produces the black precipitate ferric dimethyl dithiocarbamate, aluminum salt solution after filtering separation collection filtrate obtains deironing, the acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains; 2] by the aluminum salt solution crystallization after deironing, filtering separation, to aluminium salt crystal collect filtrate for later use; 3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
Also comprise step 4] by step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] and the filtrate or water of collection in, and by adding sodium hydroxide, potassium hydroxide or ammoniacal liquor etc., adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, and it is used to reclaim storage, and collect filtrate for step 1], now in filtrate, contain regeneration precipitation agent Sodium dimethyldithiocarbamate 40min.
Described step 4] pH value adjusted is 9～13.
Step 1] in add precipitation agent amount for according to Fe
3+: Na
+mol ratio is 1: 2～4.
A kind of impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing that adopt comprises the following steps:
1] under agitation the precipitation agent potassium dimethyldithiocarbamate is pressed to Fe
3+: K
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, and reaction produces the black precipitate ferric dimethyl dithiocarbamate, collects filtrate through filtering separation and obtains aluminum salt solution after deironing; The acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains;
2] by the aluminum salt solution crystallization after deironing, filtering separation, to aluminium salt crystal collect filtrate for later use;
3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
Also comprise step 4]: by step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] and the filtrate or water of collection in, and by hydro-oxidation sodium, potassium hydroxide or ammoniacal liquor etc., adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, reclaim its use of storage, and the filtrate that collection contains regeneration precipitation agent potassium dimethyldithiocarbamate is for step 1].
Described step 4] pH value adjusted is 9～13.
Step 1] in add precipitation agent amount for according to Fe
3+: K
+the molar mass ratio is 1: 2～4.
The principle of the invention:
The precipitation agent Sodium dimethyldithiocarbamate 40min mature production technology that the present invention adopts, but be not applied in acidic process flyash process system, the invention belongs to first Application.Itself and iron reaction equation are as follows:
3(CH
3)
2NCSSNa·2H
2O+Fe
3+→C
9H
18FeN
3S
6+3Na
++6H
2O
The present invention utilizes ferric dimethyl dithiocarbamate in the non-setting characteristics of alkaline environment condition, adds ammoniacal liquor, ammonia or sodium hydroxide that the system pH value is adjusted to alkalescence, the form Precipitation by iron with ironic hydroxide.Its reaction equation is as follows:
Fe
3++3OH
-=Fe(OH)
3
Below in conjunction with embodiment, the present invention is described in detail, but protection scope of the present invention is not limited in following implementation column, should comprise the full content in claims.
Embodiment 1
1) at normal temperatures, precipitation agent (Sodium dimethyldithiocarbamate 40min) is pressed to Fe
3+: Na
+mol ratio is under agitation to join acid system flyash at 1: 2 to produce in the acidic aqueous solution of aluminium salt in alumina process, and reaction produces black precipitate (ferric dimethyl dithiocarbamate), and filtering separation obtains aluminum salt solution after deironing.
2), by the aluminum salt solution crystallization after deironing, filtering separation obtains aluminium salt crystal.
3) roasting crystalline aluminium salt is produced aluminum oxide.
4) gained black precipitate ferric dimethyl dithiocarbamate in step 1) is joined to step 2) in solution after aluminium salt crystallization and add sodium hydroxide, adjusting pH value is 10, generate red precipitate (ironic hydroxide), filtering separation, obtain containing Sodium dimethyldithiocarbamate 40min filtrate, for step 1) as precipitation agent.
Embodiment 2
1) at normal temperatures, precipitation agent (potassium dimethyldithiocarbamate) is pressed to Fe
3+: K
+the molar mass ratio is under agitation to join acid system flyash at 1: 4 to produce in the acidic aqueous solution of aluminium salt in alumina process, and reaction produces black precipitate (ferric dimethyl dithiocarbamate), and filtering separation obtains aluminum salt solution after deironing.
2), by the aluminum salt solution crystallization after deironing, filtering separation obtains aluminium salt crystal.
3) roasting crystalline aluminium salt is produced aluminum oxide.
4) by the solution after gained black precipitate (ferric dimethyl dithiocarbamate joins step 2) aluminium salt crystallization in step 1) and add potassium hydroxide, adjusting pH value is 13, generate red precipitate (ironic hydroxide), filtering separation, obtain containing potassium dimethyldithiocarbamate filtrate, for step 1) as precipitation agent.
Claims (8)
1. adopt the impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing, it is characterized in that: comprise the following steps:
1] under agitation the precipitation agent Sodium dimethyldithiocarbamate 40min is pressed to Fe
3+: Na
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, and reaction produces the black precipitate ferric dimethyl dithiocarbamate, collects filtrate through filtering separation and obtains aluminum salt solution after deironing; The acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains;
2], by the aluminum salt solution crystallization after deironing, filtering separation, obtain aluminium salt crystal and collect filtrate for later use;
3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
2. the impurity-removing method of employing acid system according to claim 1 in the standby alumina process of coal ash for manufacturing, is characterized in that: also comprise step 4]:
By step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] the filtrate of collection in, and by adding sodium hydroxide, potassium hydroxide or ammoniacal liquor, adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, reclaim its use of storage, and the filtrate that collection contains regeneration precipitation agent Sodium dimethyldithiocarbamate 40min is for step 1].
3. adopting according to claim 2 the impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing, it is characterized in that: described step 4] pH value adjusted is 9～13.
4. the impurity-removing method in the standby alumina process of coal ash for manufacturing according to claim 1 or 2 or 3 described employing acid systems, is characterized in that: step 1] in add precipitation agent amount for according to Fe
3+: Na
+the molar mass ratio is 1: 2～4.
5. one kind adopts the impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing, it is characterized in that: comprise the following steps:
1] under agitation the precipitation agent potassium dimethyldithiocarbamate is pressed to Fe
3+: K
+the molar mass ratio is 1: 1～6 to join in the acidic aqueous solution of aluminium salt, and reaction produces the black precipitate ferric dimethyl dithiocarbamate, collects filtrate through filtering separation and obtains aluminum salt solution after deironing; The acidic aqueous solution of described aluminium salt is for adopting acid system to produce by flyash the intermediate product that aluminum oxide obtains;
2], by the aluminum salt solution crystallization after deironing, filtering separation, obtain aluminium salt crystal and collect filtrate for later use;
3] roasting aluminium salt crystal obtains the aluminum oxide after removal of impurities.
6. the impurity-removing method of employing acid system according to claim 5 in the standby alumina process of coal ash for manufacturing, is characterized in that: also comprise step 4]:
By step 1] gained black precipitate ferric dimethyl dithiocarbamate joins step 2] the filtrate of collection in, and by adding sodium hydroxide, potassium hydroxide, ammoniacal liquor or ammonia, adjusting pH value is 9～14, generate red precipitate, filtering separation, obtain ferric hydroxide precipitate, reclaim its use of storage, and the filtrate that collection contains regeneration precipitation agent potassium dimethyldithiocarbamate is for step 1].
7. adopting according to claim 6 the impurity-removing method of acid system in the standby alumina process of coal ash for manufacturing, it is characterized in that: described step 4] pH value adjusted is 9～13.
8. the impurity-removing method in the standby alumina process of coal ash for manufacturing according to claim 5 or 6 or 7 described employing acid systems, is characterized in that: step 1] in add precipitation agent amount for according to Fe
3+: K
+the molar mass ratio is 1: 2～4.
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150515A (en) * | 2014-08-11 | 2014-11-19 | 航天推进技术研究院 | Method for extracting alumina from fly ash based on ammonium sulfate method |
| CN104528819A (en) * | 2015-01-14 | 2015-04-22 | 辽宁石化职业技术学院 | Method for recycling metal impurities and precipitant in production process of titanium dioxide |
| CN105543506A (en) * | 2016-02-19 | 2016-05-04 | 马桂文 | Method for producing high-purity chromium metal |
| CN106966415A (en) * | 2017-03-29 | 2017-07-21 | 西安航天动力试验技术研究所 | The process of aluminum oxide in a kind of acidity extraction coal-powder boiler flyash |
| CN111762804A (en) * | 2020-07-24 | 2020-10-13 | 眉山顺应动力电池材料有限公司 | Iron removal method for pickle liquor in acid process aluminum extraction |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150515A (en) * | 2014-08-11 | 2014-11-19 | 航天推进技术研究院 | Method for extracting alumina from fly ash based on ammonium sulfate method |
| CN104150515B (en) * | 2014-08-11 | 2015-08-26 | 航天推进技术研究院 | From flyash, the method for aluminum oxide is extracted based on ammonium sulfate method |
| CN104528819A (en) * | 2015-01-14 | 2015-04-22 | 辽宁石化职业技术学院 | Method for recycling metal impurities and precipitant in production process of titanium dioxide |
| CN105543506A (en) * | 2016-02-19 | 2016-05-04 | 马桂文 | Method for producing high-purity chromium metal |
| CN105543506B (en) * | 2016-02-19 | 2017-06-16 | 马桂文 | A kind of method for producing high-purity metal chromium |
| CN106966415A (en) * | 2017-03-29 | 2017-07-21 | 西安航天动力试验技术研究所 | The process of aluminum oxide in a kind of acidity extraction coal-powder boiler flyash |
| CN111762804A (en) * | 2020-07-24 | 2020-10-13 | 眉山顺应动力电池材料有限公司 | Iron removal method for pickle liquor in acid process aluminum extraction |
| CN111762804B (en) * | 2020-07-24 | 2022-09-02 | 四川顺应动力电池材料有限公司 | Iron removal method for pickle liquor in acid process aluminum extraction |
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Application publication date: 20131218 |