CN109133102B - Method for directly utilizing low-grade magnesite surface modification chemistry - Google Patents
Method for directly utilizing low-grade magnesite surface modification chemistry Download PDFInfo
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- CN109133102B CN109133102B CN201810722576.7A CN201810722576A CN109133102B CN 109133102 B CN109133102 B CN 109133102B CN 201810722576 A CN201810722576 A CN 201810722576A CN 109133102 B CN109133102 B CN 109133102B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/12—Preparation of carbonates from bicarbonates or bicarbonate-containing product
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
- C01F5/32—Preparation of anhydrous magnesium chloride by chlorinating magnesium compounds
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D7/00—Fertilisers producing carbon dioxide
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Abstract
The invention relates to a method for directly utilizing low-grade magnesite surface modification chemistry, in particular to a method for modifying low-grade magnesite, which adopts a mechanical modification method and a chemical modification method to modify the surface of high-silicon high-calcium low-grade magnesite mineral powder, and then the modified low-grade magnesite mineral powder reacts with sulfuric acid to generate magnesium sulfate heptahydrate and release carbon dioxide; reacting part of the carbon dioxide with an ammonia solution of sodium chloride to generate sodium bicarbonate and ammonium chloride, and continuously reacting the ammonium chloride with the light-burned magnesia powder to generate magnesium chloride hexahydrate and ammonia gas for recycling; the product sodium bicarbonate can be used as a raw material for modifying the surface of low-grade magnesite, the cost is saved, the filtered residue is mixed with magnesium sulfate monohydrate to be used as a medium-trace element fertilizer, and part of carbon dioxide products are compressed to be used as a gas fertilizer for greenhouses.
Description
Technical Field
The invention relates to a method for modifying low-grade magnesite, in particular to a method for directly utilizing the surface modification chemistry of low-grade magnesite.
Background
In the prior art, light calcined powder is obtained by calcining magnesite, and then the light calcined powder is used as a raw material to produce a magnesium chemical raw material, the energy consumption in the calcining process is high, the other half of magnesite is combined into carbon dioxide to be directly discharged in the calcining process, the carbon dioxide is not utilized, the carbon emission requirement is not met, and the environmental pollution is serious. Excessive pursuit of high grade and high quality of magnesium oxide is the result of the development of magnesia refractory materials for many years, which causes damage and waste to magnesite mines, magnesite below 40% (magnesium oxide) is not suitable to be used as the raw material of refractory materials, and is directly abandoned and abandoned, the statistics shows that the magnesite with high quality and high content is nearly exhausted, the utilization of low grade magnesite with over 50% of reserve becomes the urgent need at present, and is also the necessary supplement for prolonging the service life of mines, and is necessary for the reformation of magnesite supply side structures.
In the use of the magnesite in China, in order to produce refractory materials, the problems that the magnesite with high quality is excessively exploited and used, and the magnesite with low grade or fine ore and tailings cannot be fully utilized exist. The problem of recovering vegetation in the mine is serious, and the comprehensive utilization degree of resources is not high. Not only the product variety is less, but also the product grade is not high.
So far, the chemical utilization of magnesite only takes light calcined magnesia of magnesite as a raw material, then the light calcined magnesia reacts with sulfuric acid or hydrochloric acid to generate magnesium sulfate heptahydrate or magnesium chloride hexahydrate, carbon dioxide is directly discharged in the calcining process and is not utilized, so that energy is consumed, resources are wasted, and the environment is polluted. Furthermore, the calcination is to obtain raw materials for producing refractory materials, and most of low-grade magnesite, tailings, fine ore and the like are not utilized.
The chemical engineering technical characteristics are utilized to carry out mechanical and surface chemical modification on low-grade magnesite, and the low-grade magnesite is directly and chemically utilized under the low-temperature condition, so that the transformation and supply side structure reformation of the magnesite industry is quickened while the refractory raw materials are utilized in a protective manner, the carbon dioxide in the magnesite is chemically utilized, the problem of carbon dioxide emission is solved, and the double utilization values of magnesium and carbon of the magnesite are exerted. The comprehensive utilization is really realized, and the significance is great.
Disclosure of Invention
The invention aims to provide a method for directly utilizing the surface modification chemistry of low-grade magnesite, which is a method for directly utilizing the chemistry after low-grade magnesite is modified by a surfactant after being crushed, ground and screened; the low-grade magnesite (the content of magnesium oxide is less than or equal to 40 percent) is crushed, ground and screened, and then the surface of the low-grade magnesite is modified by adopting composite ammonium salt, so that the modified low-grade magnesite can be directly and chemically utilized under the low-temperature condition.
The purpose of the invention is realized by the following technical scheme:
a method for directly utilizing low-grade magnesite by surface modification chemistry, which comprises the following preparation processes:
firstly, taking low-grade magnesite (the content of magnesium oxide is less than or equal to 40%) as a raw material, wherein the content of silicon oxide is more than or equal to 3%, and the content of calcium oxide is more than or equal to 1.0%;
secondly, crushing, grinding and screening the low-grade magnesite to obtain (200 meshes, not less than 85%) low-grade magnesite powder;
thirdly, controlling a certain pH value of the obtained magnesite powder at room temperature, and modifying the magnesite powder by using a surfactant (composite amine salt);
fourthly, the modified magnesite powder can directly react with sulfuric acid at the temperature of 80-100 ℃ to generate magnesium sulfate heptahydrate, and simultaneously carbon dioxide is discharged;
Fifthly, coupling the carbon dioxide discharged by the reaction with a soda process to produce sodium bicarbonate and ammonium chloride, reacting the ammonium chloride with the light calcined powder to generate magnesium chloride, and recycling the evaporated ammonia gas; sodium bicarbonate generated by the reaction can be used as a raw material for modifying the surface of low-grade magnesite;
and sixthly, filtering the obtained residue containing the active silicon calcium, mixing the residue with the dehydrated magnesium sulfate monohydrate to prepare the medium and trace element fertilizer, wherein part of the recovered carbon dioxide can be used as carbon dioxide fertilizer.
The invention has the advantages and effects that:
the invention realizes the breakthrough of directly utilizing magnesite by a chemical method, has zero discharge in the whole process, really realizes the dry extraction of magnesite and realizes the comprehensive utilization of magnesite. The process technology thoroughly opens the double utilization situation of magnesium and carbon in the magnesite processing industry, and really realizes the comprehensive utilization and even high-efficiency utilization of resources. The technology application drives the magnesite industry to develop, opens up a new chapter for processing and utilizing magnesite, and has wide prospect.
The process realizes the direct chemical utilization of magnesite under low temperature conditions to obtain a large amount of chemical raw materials such as magnesium sulfate heptahydrate, carbon dioxide, sodium bicarbonate, magnesium chloride hexahydrate and the like; meanwhile, the recycling of ammonia gas is realized, and sodium bicarbonate is directly used as a modified raw material; the method can obtain medium trace element fertilizer and carbon dioxide gas fertilizer, the process technology really realizes the dual utilization of magnesium and carbon of low-grade magnesite, the whole process has zero emission, and the method belongs to the green chemical technology.
1. The method takes the low-grade magnesite with high silicon and high calcium as the raw material, does not compete with refractory materials for the raw material, and is a necessary requirement for the development of the magnesite industry and the adjustment of a supply side structure;
2. mechanical modification such as crushing and surfactant modification such as composite ammonium salt are carried out, so that the surface energy and the binding energy of low-grade magnesite are reduced, and direct chemical utilization is realized;
3. the process technology realizes the dual utilization of magnesium and carbon, and really realizes the 'eating, drying and pressing' of low-grade magnesite;
4. the carbon dioxide generated by the chemical reaction has high purity and low temperature, and is combined with the process for producing sodium carbonate from sodium chloride to obtain sodium bicarbonate and magnesium chloride hexahydrate;
5. the evaporated ammonia can be recycled; the product sodium bicarbonate can be used as a modified raw material, so that the cost is saved;
6. the chemical method is adopted to utilize the low-grade magnesite, so that the key technology of carbon dioxide recycling is solved, zero emission of the whole process is realized, and the method belongs to the green chemical technology.
Drawings
FIG. 1 is a block diagram of a technical route according to the present invention;
FIG. 2 is an infrared spectrum of the raw material magnesite according to the present invention;
FIG. 3 is a FT-IR diagram of a modified product of low grade magnesite;
FIG. 4 shows a silicon-oxygen tetrahedron group [ Si ] having a layered structure 4 O 10 ] 4- A type structure diagram.
Detailed Description
The present invention will be described in detail with reference to examples.
As can be seen from the figure, 3428cm after modification -1 The hydroxyl vibration and the N-H stretching vibration are obviously enhanced, which shows that a large amount of hydroxyl and amino are adsorbed on the surface of low-grade magnesite1047cm -1 And the R-O bond expansion and contraction are obviously enhanced, which shows that the organic ammonium salt is also adsorbed on the surface of the low-grade magnesite.
The invention takes low-grade magnesite (the content of magnesium oxide is less than or equal to 40 percent) as a raw material, wherein the content of silicon oxide is more than or equal to 3 percent, and the content of calcium oxide is more than or equal to 1.0 percent; crushing, grinding and screening the low-grade magnesite to obtain (200 meshes, more than or equal to 85%) low-grade magnesite powder; controlling a certain pH value of the obtained magnesite powder at room temperature, and modifying by using a surfactant (composite amine salt); the modified magnesite powder can directly react with sulfuric acid at the temperature of 80-100 ℃ to generate magnesium sulfate heptahydrate, and simultaneously, carbon dioxide is discharged; coupling the carbon dioxide discharged by the reaction with a soda process to produce sodium bicarbonate and ammonium chloride, reacting the ammonium chloride with light calcined powder to generate magnesium chloride, and recycling the evaporated ammonia gas; sodium bicarbonate generated by the reaction can be used as a raw material for modifying the surface of low-grade magnesite; filtering to obtain residue containing active silicon calcium, mixing with dehydrated magnesium sulfate monohydrate to obtain medium trace element fertilizer, and partially recovering carbon dioxide as carbon dioxide fertilizer.
A method for directly utilizing low-grade magnesite surface modification chemistry comprises the first step of taking low-grade magnesite (the content of magnesium oxide is less than or equal to 40%) as a raw material, wherein the content of silicon oxide is more than or equal to 3%, and the content of calcium oxide is more than or equal to 1.0%; secondly, crushing, grinding and screening the low-grade magnesite to obtain (200 meshes, not less than 85%) low-grade magnesite powder; thirdly, controlling a certain pH value of the obtained magnesite powder at room temperature, and modifying the magnesite powder by using a surfactant (composite amine salt); fourthly, the modified magnesite powder can directly react with sulfuric acid at the temperature of 80-100 ℃ to generate magnesium sulfate heptahydrate, and simultaneously carbon dioxide is discharged; fifthly, coupling the carbon dioxide discharged by the reaction with a soda process to produce sodium bicarbonate and ammonium chloride, reacting the ammonium chloride with the light calcined powder to generate magnesium chloride, and recycling the evaporated ammonia gas; sodium bicarbonate generated by the reaction can be used as a raw material for modifying the surface of low-grade magnesite; and sixthly, filtering the obtained residue containing the active silicon calcium, mixing the residue with the dehydrated magnesium sulfate monohydrate to prepare the medium and trace element fertilizer, wherein part of the recovered carbon dioxide can be used as carbon dioxide fertilizer.
1. Basic principle of the invention
1) Principle of surface modification
The high-silicon high-calcium mineral in the low-grade magnesite is mainly magnesium silicate mineral with a chemical formula of Mg 3 [Si 4 O 10 ](OH) 2 Expressed as 3 MgO.4SiO by oxide 2 •H 2 And O. Each of [ SiO ] in mineral 4 ] 4- Between three common vertices O 2- Connected, compositionally two-dimensionally extended layers, see FIG. 4, i.e. connected in layers to one another in a plane, in the form of a hexagonal network, so as to be oriented in [ SiO ] form 4 ]4-represents; the other active oxygen in the silicon-oxygen tetrahedron points to one side, and is arranged opposite to the active oxygen in the other hexagonal reticular layer, the two active oxygen layers are connected by magnesium cations, ionic bonds are formed in the layers, and molecular bonds are formed between the layers, as shown in figure 4.
The magnesium silicate mineral has a surface isoelectric point pH (2-3.5), and therefore exhibits a strong electronegativity at a pH of 7 or more. The composite ammonium salt belongs to a cationic surfactant, can be adsorbed on the surface of magnesium silicate minerals through electrostatic physical action and ion exchange action, reduces the binding energy of silicon and magnesium, and provides a powerful condition for direct chemical utilization under a low-temperature condition.
2) Principle of chemical reaction
MgCO 3 .SiO 2 .CaO+NH4-R+OH-→ (1)
MgCO 3 +H 2 SO 4 +7H 2 O →MgSO 4 .7H 2 O+CO 2 (2)
CO 2 +NaCl+NH 3 +H 2 O→NaHCO 3 +NH 4 Cl (3)
NH 4 Cl+MgO+H 2 O→MgCl 2 +NH 3 ↑ (4)
SiO2.CaSO 4 +MgSO 4 H2O → (SMgCaSi) fertilizer (5).
2. Basic embodiment of the invention
Firstly, taking low-grade magnesite (the content of magnesium oxide is less than or equal to 40%) as a raw material, wherein the content of silicon oxide is more than or equal to 3%, and the content of calcium oxide is more than or equal to 1.0%; secondly, crushing, grinding and screening the low-grade magnesite to obtain (200 meshes, not less than 85%) low-grade magnesite powder; thirdly, controlling a certain pH value of the obtained magnesite powder at room temperature, and modifying the magnesite powder by using a surfactant (composite amine salt); fourthly, the modified magnesite powder can directly react with sulfuric acid at the temperature of 80-100 ℃ to generate magnesium sulfate heptahydrate, and simultaneously carbon dioxide is discharged; fifthly, coupling the carbon dioxide discharged by the reaction with a soda process to produce sodium bicarbonate and ammonium chloride, reacting the ammonium chloride with the light calcined powder to generate magnesium chloride, and recycling the evaporated ammonia gas; sodium bicarbonate generated by the reaction can be used as a raw material for modifying the surface of low-grade magnesite; and sixthly, filtering the obtained residue containing the active silicon calcium, mixing the residue with the dehydrated magnesium sulfate monohydrate to prepare the medium and trace element fertilizer, wherein part of the recovered carbon dioxide can be used as carbon dioxide fertilizer.
3. The technical method of the invention
The invention adopts mechanical modification and chemical modification methods to carry out surface modification on high-silicon high-calcium low-grade magnesite ore powder, and then the high-silicon high-calcium low-grade magnesite ore powder reacts with sulfuric acid to generate magnesium sulfate heptahydrate and release carbon dioxide; reacting part of the carbon dioxide with an ammonia solution of sodium chloride to generate sodium bicarbonate and ammonium chloride, and continuously reacting the ammonium chloride with the light-burned magnesia powder to generate magnesium chloride hexahydrate and ammonia gas for recycling; the product sodium bicarbonate can be used as a raw material for modifying the surface of low-grade magnesite, the cost is saved, the filtered residue is mixed with magnesium sulfate monohydrate to be used as a medium-trace element fertilizer, and part of carbon dioxide products are compressed to be used as a gas fertilizer for greenhouses.
4. Specific embodiments of the invention
(1) The low-grade magnesite is mechanically modified (crushed, ground and sieved to obtain 200-mesh low-grade magnesite powder with the particle size of more than or equal to 85%.
(2) Weighing 0.035g of anhydrous sodium carbonate, dissolving in 100ml of distilled water, transferring into a 500ml beaker, adding 0.01g of composite ammonium salt (dodecylamine, oxalic amine and the like), stirring uniformly, adding 100g of mechanically modified low-grade magnesite powder, continuing to stir for 5min, filtering, and taking a filter cake.
(3) Weighing 30g of NaCl solid, weighing 200ml of ammonia water and 200ml of distilled water, uniformly stirring in a 500ml beaker, and adding into a wide-mouth bottle.
(4) Pouring 100g of magnesite filter residue with the modified surface into a 500ml three-neck flask, measuring 100ml of concentrated sulfuric acid by using a measuring cylinder, diluting to 50% (mass ratio), dripping into the three-neck flask for 30 drops/min, stirring for 300r/min, heating to 35-85 ℃, and reacting for 1-3 h.
(5) Introducing the discharged carbon dioxide into a wide-mouth bottle filled with sodium chloride and aqueous solution of ammonia water, reacting to generate sodium bicarbonate and ammonium chloride, cooling to 10 ℃, adding sodium chloride to supersaturate, crystallizing to obtain sodium bicarbonate, and recycling the filtrate.
(6) 50g of generated ammonium chloride and 39g of light-burned magnesia powder are dissolved in a 250ml three-necked bottle, and react for 40min at the water bath temperature of 60 ℃ and the stirring speed of 300r/min, and ammonia gas is collected. And obtaining a clear solution after suction filtration. Standing the clear solution at room temperature for 2 days to precipitate white insoluble substances, repeatedly washing with distilled water and ethanol, filtering, and drying to obtain magnesium chloride hexahydrate, and heating ammonia in the solution to evaporate out and recycle.
(7) Dissolving 100g of magnesium sulfate heptahydrate in 200ml of water, performing rotary evaporation to obtain magnesium sulfate monohydrate, and compounding with residues in the technological process to obtain the calcium-magnesium-sulfur secondary element fertilizer.
(8) Compressing the carbon dioxide, and bottling to obtain the gas fertilizer for facility agriculture.
Claims (1)
1. A method for directly utilizing low-grade magnesite surface modification chemistry is characterized by comprising the following preparation processes:
the first step, low-grade magnesite is used as a raw material, and the content of magnesium oxide in the low-grade magnesite is less than or equal to 40%; wherein, the content of silicon oxide is more than or equal to 3 percent, and the content of calcium oxide is more than or equal to 1.0 percent;
secondly, crushing, grinding and screening the low-grade magnesite to obtain 200-mesh low-grade magnesite powder with the particle size of more than or equal to 85%;
thirdly, controlling a certain pH value of the obtained magnesite powder at room temperature, and modifying the magnesite powder by using a surfactant and amine salt;
fourthly, the modified magnesite powder can directly react with sulfuric acid at the temperature of 80-100 ℃ to generate magnesium sulfate heptahydrate, and simultaneously carbon dioxide is discharged;
fifthly, coupling the carbon dioxide discharged by the reaction with a soda process to produce sodium bicarbonate and ammonium chloride, reacting the ammonium chloride with the light calcined powder to generate magnesium chloride, and recycling the evaporated ammonia gas; sodium bicarbonate generated by the reaction can be used as a raw material for modifying the surface of low-grade magnesite;
Sixthly, filtering the obtained residue containing the active silicon calcium, mixing the residue with dehydrated magnesium sulfate monohydrate to prepare a medium trace element fertilizer, wherein part of the recovered carbon dioxide can be used as a carbon dioxide fertilizer;
the compound amine salt is a mixed salt of dodecylamine and ammonium oxalate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107298451A (en) * | 2017-06-12 | 2017-10-27 | 沈阳化工大学 | A kind of double Application ways of low-grade magnesite magnesium carbon |
| CN107311207A (en) * | 2017-06-12 | 2017-11-03 | 沈阳化工大学 | A kind of low-grade magnesite and boron magnesium ore method of comprehensive utilization |
| CN107417146A (en) * | 2017-07-18 | 2017-12-01 | 沈阳化工大学 | A kind of low-grade magnesite method of comprehensive utilization |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107298451A (en) * | 2017-06-12 | 2017-10-27 | 沈阳化工大学 | A kind of double Application ways of low-grade magnesite magnesium carbon |
| CN107311207A (en) * | 2017-06-12 | 2017-11-03 | 沈阳化工大学 | A kind of low-grade magnesite and boron magnesium ore method of comprehensive utilization |
| CN107417146A (en) * | 2017-07-18 | 2017-12-01 | 沈阳化工大学 | A kind of low-grade magnesite method of comprehensive utilization |
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