CN104030328B - The method of active porous shape earth silicon material is prepared with serpentine extraction magnesium oxide - Google Patents
The method of active porous shape earth silicon material is prepared with serpentine extraction magnesium oxide Download PDFInfo
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Abstract
The invention discloses the method that a kind of serpentine extraction magnesium oxide prepares active porous shape earth silicon material, comprise step as follows: 1) get serpentine raw material and carry out pre-treatment, be processed into serpentine breeze; 2) mixed with acid salt by the serpentine breeze obtained, roasting obtains product of roasting and tail gas; 3) product of roasting carries out aftertreatment, obtains rough Adlerika and active silica residue; 4) above-mentioned rough Adlerika and active silica residue are processed respectively; Wherein, rough Adlerika step-by-step precipitation method obtains POV magnesium solution; Active porous shape earth silicon material is obtained after active silica residue drying, grinding.Invention selects acid salt as the auxiliary agent removing metal oxide in serpentine, and chemically reactive is high, and technical process is simple, and maturing temperature is low, and roasting time is short, and energy consumption is low, and magnesium oxide leaching rate is high.
Description
Technical field
The present invention relates to the method that a kind of serpentine extraction magnesium oxide prepares active porous shape earth silicon material, belong to Nonmetallic Mineral Industry Exploitation utilization, ceramic, solid waste process and mineral processing and field of environment protection.
Background technology
Serpentine belongs to 1:1 type layered silicate, is made up of, mainly comprises chrysotile, antigorite and lizardite tetrahedral si-o film and magnesia octahedral sheet.Serpentinite, serpentine tailing and asbestos tailings essential mineral consist of serpentine, containing a small amount of magnetite, talcum, brucite, rhombspar, calcite etc.Primary chemical composition is SiO
2, MgO, containing a small amount of Fe
2o
3, Al
2o
3, NiO, Cr
2o
3deng, wherein metal oxide is based on magnesium oxide.
At present, serpentine resourceization utilizes conventional method to be in serpentine raw material, add organic acid and the direct acidleach preparation of mineral acid containing magnesium series compound product, organic acid used has citric acid, oxalic acid, 2-nitro-4-phenylarsonic acid etc., and mineral acid has hydrochloric acid, nitric acid, phosphoric acid, sulfuric acid etc.Serpentine extract the residue after magnesium oxide directly and sodium hydroxide react and prepare the Chemicals such as Starso or white carbon black.
Notification number is that the method disclosing the direct acidleach of a kind of use in the Chinese patent " method of asbestos tailings comprehensive utilization " of 101792184A carries out recycling.Notification number is that to disclose a kind of hydrochloric acid of lower concentration, sulfuric acid or nitric acid of utilizing in the Chinese patent high-efficiency leaching process of metal ion " in a kind of chrysotile nano fiber " of 102352435A be leaching agent, carries out the method for multistage leaching.
The defect of above-mentioned published acidleach method is that acid treatment reaction is insufficient, and magnesium oxide leaching rate is low, easily causes secondary pollution in treating processes; And acid, alkaline solution easily corrodes container, high to equipment requirements, operation corrodibility is large, and cost is high.
For this reason, scientific research personnel develops the method with ammonium salt calcination process serpentine; As the Chinese patent " a kind of method of serpentine processing and utilization " that notification number is 102627302A, disclose one snake stone flour and ammonium salt carries out baking mixed, roasting filtrate and filter residue prepare silicon, magnesium series compound.Notification number is the Chinese patent " a kind of method improving magnesium solubility rate in serpentine ammonium salt product of roasting " of 103496723A, also discloses one serpentine breeze and ammonium salt baking mixed raising magnesium extraction yield.With ammonium salt roasting method comparatively acidleach method advantageously; But the maturing temperature that ammonium salt sinter process requires is high, and range of reaction temperature is little, and acidity is weak, and roasting time is long, energy consumption is large, and raw material granularity requires high.
Up to the present, yet there are no to react with serpentine and acid salt and extract magnesium oxide and prepare active porous shape earth silicon material, its technology is little to equipment corrosion, environmental pollution is little, operate and maturing temperature is low, energy consumption is few, and the open report of this low correlation technique.
Summary of the invention
In order to solve the defect existed in above-mentioned prior art, the object of this invention is to provide a kind of serpentine and acid salt and reacting the method that high efficiency extraction magnesium oxide prepares active porous shape earth silicon material.
To achieve these goals, the present invention adopts following technical scheme; Serpentine extracts the method that magnesium oxide prepares active porous shape earth silicon material, comprises step as follows:
1) get serpentine raw material and carry out pre-treatment, obtain serpentine breeze; In described serpentine breeze, MgO mass percentage is 30% ~ 45%;
2) by step 1) the serpentine breeze that obtains mix with acid salt after roasting, obtain product of roasting and tail gas; Described serpentine breeze mixes with acid salt and refers to that the mol ratio of MgO and described acid salt in serpentine breeze is 1:0.5 ~ 1:5;
3) by step 2) product of roasting that obtains carries out aftertreatment, obtains rough Adlerika and active porous silicon-dioxide residue;
4) by step 3) in the active porous silicon-dioxide residue that obtains through reprocessing, obtain described active porous shape earth silicon material.
Above-mentioned steps 1) in serpentine raw material used be at least one in serpentinite, serpentine tailing or chrysotile tailing; The granularity of described serpentine breeze is 60 order ~ 600 orders.
Above-mentioned steps 2) in acid salt used can select at least one in monoammonium sulfate, sodium pyrosulfate, ammonium bisulfite or sodium bisulfite; The maturing temperature of described roasting is 110 ~ 800 DEG C, and roasting time is 0.2 ~ 4h; Wherein, react containing serpentine minerals and acid salt the vitriol formed in product of roasting; Described tail gas adopts sulphuric acid soln method to carry out purifying treatment.
Above-mentioned steps 3) in aftertreatment comprise leaching, filter and washing procedure; Described leaching is in described product of roasting, add process water dissolved by vitriol wherein, and the solid-to-liquid ratio of its product of roasting and process water is 1:5 ~ 1:40; Described filtration adopts Filter Press, and filtrate is described rough Adlerika, and filter residue is active silica residue; Described washing is that filter residue is added process water, repeats to rinse and filtration makes its filter residue to neutral, obtains described active porous silicon-dioxide residue.
Above-mentioned steps 4) in reprocessing, be by washing, filter after active porous silicon-dioxide residue, then drying process, drying temperature 110-700 DEG C, then grinding to granularity is 50 order ~ 3250 orders, obtains described active porous shape earth silicon material.
Owing to have employed technique scheme, beneficial effect of the present invention is as follows: chemical assistant 1) used in described preparation method is acid salt; Because its fusing point is low, when baking mixed with serpentine raw material, become molten state, ionize completely and be strongly-acid, remove the metal oxide in mixture under the state existed there being liquid phase, metal oxide leaching rate is greater than 96%; Its technical process is simple, maturing temperature is low, and roasting time is short, and sufficient reacting, energy consumption are low, and leaching time shortens greatly; Have more advantage with making compared with chemical assistant of ammonium salt etc. in prior art.2) raw material selected in the method is serpentinite, serpentine and asbestos tailings, for its recycling provides new approach; Be conducive to changing waste into valuable, active effect played to the environmental pollution of administering above-mentioned mine periphery simultaneously, benefit the nation and the people.3) utilize roasting method of the present invention, the soluble salt that the product of roasting obtained is formed, obtain rough magnesium sulfate salt and active porous silicon-dioxide residue through water logging, washing, filtration; Rough Adlerika Jing Fen Walk precipitation wherein acquires POV magnesium solution, for the preparation of containing magnesium series compound; Active porous silicon-dioxide residue adds basic materials and reacts, and can prepare silicate material; Or drying, grinding to desired particle size prepare active porous shape earth silicon material, its specific surface area is large, and aperture is little, be evenly distributed.4) technical process of whole preparation process is short, and chemical assistant consumption is little, thus also little to mechanical means corrodibility, can reduce the maintenance input cost of mechanical means.
Principle of work of the present invention, for going metal oxide effect, namely removes the metal oxides such as magnesium oxide and the process of retentive activity silicon-dioxide by the method for chemical reaction from serpentine raw material.Because the electropotential difference of the metal oxides such as magnesium oxide in serpentine raw material and silica component is comparatively large, the metal oxide that electrochemical properties is more active dissolves to enter in electrolytic solution and leaves the stable silicon-dioxide remains of electrochemical properties under electrolytical effect.
Embodiment
The present invention prepares the method for active porous shape earth silicon material, comprises step as follows:
1) get serpentine raw material and carry out pre-treatment, serpentine breeze is processed in namely conventional fragmentation, grinding and magnetic separation; The MgO mass percentage contained in this serpentine breeze is 30% ~ 45%; Described pre-treatment comprises conventional fragmentation, grinding, magnetic separation; Serpentine raw material used can select at least one in serpentinite, serpentine tailing or chrysotile tailing; The granularity of serpentine breeze is 60 order ~ 600 orders.
2) by step 1) the serpentine breeze that obtains mixes with acid salt, after the high-temperature roasting 0.2 ~ 4h of 110 ~ 800 DEG C, obtains product of roasting and tail gas; Wherein, be that 1:0.5 ~ 1:5 carries out proportioning by the mol ratio of MgO and acid salt in serpentine breeze when serpentine breeze mixes with acid salt; Tail gas carries out purifying treatment through sulphuric acid soln absorption process.
3) by step 2) product of roasting that obtains carries out aftertreatment, obtains rough Adlerika and active porous silicon-dioxide residue;
4) to step 3) in the rough Adlerika that obtains and active porous silicon-dioxide residue carry out reprocessing respectively; Wherein, rough Adlerika obtains POV magnesium solution through the step-by-step precipitation method of routine; Active porous silicon-dioxide residue drying, grinding, obtain active porous shape earth silicon material.
Above-mentioned steps 2) in acid salt used can select at least one in monoammonium sulfate, sodium pyrosulfate, ammonium bisulfite or sodium bisulfite; Containing vitriol in above-mentioned product of roasting.
Above-mentioned steps 3) in aftertreatment comprise leaching, filter and washing procedure; Wherein, leach for adding process water mixing in product of roasting, the solid-to-liquid ratio of its product of roasting and process water is 1:5 ~ 1:40; Mix and blend generates vitriol lysate; After Filter Press, obtain above-mentioned rough Adlerika and active silica filter residue; Washing adds process water again in filter residue, repeats flushing and make filter residue to neutral, obtain active porous silicon-dioxide residue;
By step 3) the rough Adlerika Jing Fen Walk precipitator method that obtain obtain POV magnesium solution; This POV magnesium solution is used as industrial chemicals, and preparation is containing magnesium series compound; By active porous silicon-dioxide residue after above-mentioned washing procedure, then drying process, drying temperature 110-700 DEG C; Then, grinding obtains active porous shape earth silicon material; Its properties of powder performace is 50 order ~ 3250 orders.
Above-mentioned steps 2) sulphuric acid soln absorption process be carry out purifying treatment by the ammonia in sulphuric acid soln and tail gas, sulphur trioxide and sulfur dioxide gas precursor reactant.
Above-mentioned steps 4) the step-by-step precipitation method of the rough Adlerika of process, specifically start to precipitate pH value according to the solubility product constant calculating metal ion of different metal ion precipitation and carry out fractional precipitation, obtain nickel, chromium, the multiple different hydroxide precipitate of iron (nickel hydroxide, chromium hydroxide, ironic hydroxide) and POV magnesium solution.
Above-mentioned preparation comprises containing magnesium series compound: magnesium hydroxide, magnesium oxide, magnesium basic carbonate, magnesiumcarbonate are containing magnesium series compound.
Below in conjunction with specific examples, technical scheme of the present invention is described in further detail.
Example 1:
This example selects serpentinite to be raw material.
1) serpentinite raw material is carried out fragmentation, grinding, magnetic separation, be processed into serpentine breeze.Its granularity is 60 orders, and MgO mass percentage is 45%; This pre-treatment comprises conventional fragmentation, grinding, magnetic separation operation.
2) by step 1) the serpentinite breeze that obtains is 1:5 calculated mass ratio by MgO and the mol ratio of ammonium bisulfite, weighs material and mixing and stirring; At 800 DEG C after calcination 0.2h, obtain product of roasting and tail gas; Wherein, in tail gas, sulphur trioxide, sulfurous gas or ammonia etc. are collected by conventional sulphuric acid soln absorption process.
3) by step 2) product of roasting that obtains carries out aftertreatment; Wherein, aftertreatment comprises leaching, filters and washing procedure; Described leaching is be that 1:15 mixes in the device of belt stirrer with process water by solid-to-liquid ratio in described product of roasting, the vitriol in leaching product of roasting; After Filter Press, obtain rough Adlerika and filter residue; Washing adds process water in filter residue, repeats flushing and make its filter residue to neutral, obtain active porous silicon-dioxide residue.
4) to step 3) in the rough Adlerika that obtains and active porous silicon-dioxide residue carry out reprocessing respectively; Wherein, rough Adlerika, the step-by-step precipitation method through routine obtains POV magnesium solution; The drying process again of active porous silicon-dioxide residue, drying temperature is 400 DEG C, and then grinding obtains active porous shape earth silicon material, and wherein, properties of powder performace is 50 orders.
In this example, magnesian leaching rate is 96.3%; POV magnesium solution can be used for preparing the magnesium series compounds such as magnesium hydroxide, magnesium oxide, magnesium basic carbonate and magnesiumcarbonate; The specific surface area of the active porous shape earth silicon material obtained is 82.5m
2/ g, mean pore size 1.8nm.
Example 2
This embodiment selects serpentine tailing to be raw material; Its preparation method is substantially identical with example 1, does not repeat them here; Its difference is:
1) serpentine tailing is carried out fragmentation, grinding, magnetic separation acquisition serpentine breeze, its granularity is 600 orders, and the MgO mass percentage in serpentine breeze is 30%;
2) by step 1) the serpentine breeze that obtains is 1:0.5 calculated mass ratio by MgO and the mol ratio of monoammonium sulfate, weighs material and mixing and stirring; Inserted in the temperature control reaction unit of tail gas collecting device, calcination 4h at 110 DEG C; By the sulphuric acid soln absorption process of routine, the gas produced in reaction process is collected.
3) by step 2) product of roasting that obtains carries out aftertreatment; Wherein, aftertreatment comprises leaching, filters and washing procedure; Described leaching is be that 1:5 mixes in the device of belt stirrer with process water by solid-to-liquid ratio in described product of roasting, the vitriol in leaching product of roasting; After Filter Press, obtain rough Adlerika and filter residue; Washing adds process water in filter residue, repeats flushing and make its filter residue to neutral, obtain active porous silicon-dioxide residue.
4) to step 3) in the rough Adlerika that obtains and active porous silicon-dioxide residue carry out reprocessing respectively.Wherein, rough Adlerika is obtained POV magnesium solution through the step-by-step precipitation method of routine; The process of active porous silicon-dioxide residue drying, drying temperature is 700 DEG C, and then grinding obtains active porous shape earth silicon material, and wherein, properties of powder performace is 600 orders.
In this example, magnesian leaching rate is 97.1%; POV magnesium solution can prepare the magnesium series compounds such as magnesium hydroxide, magnesium oxide, magnesium basic carbonate and magnesiumcarbonate; The specific surface area of the active porous shape earth silicon material obtained is 156.5m
2/ g, mean pore size 2.6nm.
Example 3
This example selects chrysotile tailing to be raw material.Its preparation method is substantially identical with example 1, does not repeat them here; Its difference is:
1) chrysotile tailing is carried out fragmentation, grinding, magnetic separation acquisition chrysotile tailing breeze, its granularity is 200 orders, and MgO mass percentage is 35%;
2) by step 1) the chrysotile tailing breeze that obtains is 1:3.0 calculated mass ratio by MgO and the mol ratio of sodium pyrosulfate, weighs material and mixing and stirring; Inserted in the temperature control reaction unit of tail gas collecting device, calcination 2h at 380 DEG C; By the sulphuric acid soln absorption process of routine, the tail gas produced in reaction process is collected.
3) by step 2) product of roasting that obtains carries out aftertreatment; Wherein, aftertreatment comprises leaching, filters and washing procedure; Described leaching is be that 1:25 mixes in the device of belt stirrer with process water by solid-to-liquid ratio in described product of roasting, the vitriol in leaching product of roasting; Described filtration adopts Filter Press, obtains rough Adlerika and filter residue after filtration; Described washing is that filter residue is added process water, repeats flushing and makes filter residue to neutral, obtain active porous silicon-dioxide residue.
4) to step 3) in the rough Adlerika that obtains and active porous silicon-dioxide residue carry out reprocessing respectively; Wherein, rough Adlerika obtains POV magnesium solution through the step-by-step precipitation method of routine; The process of active porous silicon-dioxide residue drying, drying temperature is 110 DEG C, and then grinding obtains active porous shape earth silicon material, and wherein, properties of powder performace is 3250 orders.
In the present embodiment, magnesian leaching rate is 96.9%; POV magnesium solution can directly adopt ordinary method to prepare the magnesium series compounds such as magnesium hydroxide, magnesium oxide, magnesium basic carbonate; The specific surface area of the active porous shape earth silicon material obtained is 257.8m
2/ g, mean pore size 2.3nm.
Example 4
This example selects serpentinite and chrysotile tailing to be raw material.Its preparation method is substantially identical with example 1, does not repeat them here; Its difference is:
1) serpentinite and chrysotile tailing are carried out fragmentation, grinding, magnetic separation acquisition serpentine breeze, its granularity is 120 orders, and MgO mass percentage is 38.8%;
2) by step 1) the serpentine breeze that obtains is 1:4.0 calculated mass ratio by MgO and the mol ratio of sodium pyrosulfate, weighs material and mixing and stirring; Inserted in the temperature control reaction unit of tail gas collecting device, calcination 1.5h at 400 DEG C; By the sulphuric acid soln absorption process of routine, the tail gas produced in reaction process is collected.
3) by step 2) product of roasting that obtains carries out aftertreatment; Wherein, aftertreatment comprises leaching, filters and washing procedure; Described leaching is be that 1:20 mixes in the device of belt stirrer with process water by solid-to-liquid ratio in described product of roasting, the vitriol in leaching product of roasting; Described filtration adopts Filter Press, obtains rough Adlerika and filter residue after filtration; Described washing is that filter residue is added process water, repeats flushing and makes filter residue to neutral, obtain active porous silicon-dioxide residue.
4) to step 3) in the rough Adlerika that obtains and active porous silicon-dioxide residue carry out reprocessing respectively; Wherein, rough Adlerika obtains POV magnesium solution through the step-by-step precipitation method of routine; The process of active porous silicon-dioxide residue drying, drying temperature is 500 DEG C, and then grinding obtains active porous shape earth silicon material, and wherein, properties of powder performace is 1250 orders.
In the present embodiment, magnesian leaching rate is 97.6%; POV magnesium solution can directly adopt ordinary method to prepare the magnesium series compounds such as magnesium hydroxide, magnesium oxide, magnesium basic carbonate; The specific surface area of the active porous shape earth silicon material obtained is 226.5m
2/ g, mean pore size 2.1nm.
Claims (2)
1. prepare a method for active porous shape earth silicon material with serpentine extraction magnesium oxide, comprise step as follows:
1) get serpentine raw material and carry out pre-treatment acquisition serpentine breeze; In described serpentine breeze, the mass percentage of MgO is 30% ~ 45%;
2) by step 1) the serpentine breeze that obtains mix with acid salt after roasting, obtain product of roasting and tail gas; With mixing of acid salt, described serpentine breeze refers to that the mol ratio of MgO and described acid salt in serpentine breeze is 1:0.5 ~ 1:5;
3) by step 2) described in product of roasting carry out aftertreatment, obtain rough Adlerika and active porous silicon-dioxide residue;
4) by step 3) the active porous silicon-dioxide residue that obtains carries out reprocessing, obtains described active porous shape earth silicon material;
Step 2) described acid salt is at least one in monoammonium sulfate, sodium pyrosulfate, ammonium bisulfite or sodium bisulfite; The maturing temperature of described roasting is 110 ~ 800 DEG C, and roasting time is 0.2 ~ 4h; Containing vitriol in described product of roasting;
Step 3) described in aftertreatment comprise leaching, filter and washing procedure; Described leaching step is in described product of roasting, add process water dissolve vitriol in this product of roasting, and the solid-to-liquid ratio of its product of roasting and process water is 1:5 ~ 1:40; Described filtration is adopted as Filter Press, and the filtrate obtained is described rough Adlerika, and the filter residue obtained adds process water repeated washing and filtration step again, makes the pH value of its filter residue for neutral, obtain described active porous silicon-dioxide residue;
Step 4) described in reprocessing, be by described active porous silicon-dioxide residue, drying process, drying temperature is 110-700 DEG C, and then grinding to granularity is 50 order ~ 3250 orders.
2. method according to claim 1, is characterized in that: step 1) described serpentine raw material is at least one in serpentinite, serpentine tailing or chrysotile tailing; The granularity of described serpentine breeze is 60 order ~ 600 orders.
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| CN115259186B (en) * | 2022-08-24 | 2023-12-26 | 西南科技大学 | Magnesium sulfate solution refined from asbestos tailings and preparation method thereof |
| CN115196657B (en) * | 2022-08-24 | 2023-10-10 | 西南科技大学 | Magnesium sulfate solution refined by asbestos tailing mixed auxiliary agent and preparation method thereof |
| CN116081659A (en) * | 2023-01-19 | 2023-05-09 | 西南科技大学 | Asbestos tailing refined magnesium sulfate solution and method and application thereof |
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