CN109133102A - The method that a kind of low-grade magnesite surface modified chemical directly utilizes - Google Patents
The method that a kind of low-grade magnesite surface modified chemical directly utilizes Download PDFInfo
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- CN109133102A CN109133102A CN201810722576.7A CN201810722576A CN109133102A CN 109133102 A CN109133102 A CN 109133102A CN 201810722576 A CN201810722576 A CN 201810722576A CN 109133102 A CN109133102 A CN 109133102A
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- magnesite
- low
- grade
- modified
- carbon dioxide
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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
-
- 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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
-
- 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
Abstract
The method that a kind of low-grade magnesite surface modified chemical directly utilizes, it is related to a kind of low-grade magnesite method of modifying, the present invention uses mechanically modifying and chemical modification method, it is modified that surface is carried out to low-grade magnesite miberal powder of high-silicon high calcium, then it with sulfuric acid reaction, generates epsom salt and releases carbon dioxide；A part of carbon dioxide is reacted with the ammonia spirit of sodium chloride, generates sodium bicarbonate and ammonium chloride, continues to react ammonium chloride with light-magnesite powder generating magnesium chloride hexahydrate and ammonia recycle utilization；Product sodium bicarbonate can be used as the modified raw material in low-grade magnesite surface, and save the cost mixes the residue being obtained by filtration as secondary and micro-element fertilizers with magnesium sulfate monohydrate, and partial CO 2 product compresses the gaseous fertilizer as greenhouse.
Description
Technical field
The present invention relates to a kind of low-grade magnesite method of modifying, modified more particularly to a kind of low-grade magnesite surface
The method that chemistry directly utilizes.
Background technique
Previous magnesite has to pass through calcining and first obtains light burnt powder, then produces magnesia industrial chemicals as raw material,
Calcination process energy consumption is higher, and calcination process not utilizes the other half composition carbon dioxide direct emission of magnesite, not only not
Meet carbon emission requirement, and environmental pollution is serious.The high-grade and high quality of excessive pursuit magnesia are magnesia fireproof materials
Expect to develop for many years as a result, this has resulted in the destruction and waste to magnesite mine, be lower than 40%(magnesia) magnesite not
It is suitable for the raw material as refractory material, is directly abandoned, is discarded, the magnesite of high-quality high-content is already close to withered according to statistics
It exhausts, the utilization more than the low-grade magnesite of 50% reserves becomes current urgent need, and extends the necessary of mine age and mend
It fills, even more the certainty of magnesite mine supply side structural reform.
Chinese magnesite exists and uses high-quality magnesite exhaustive exploitation in use, in order to produce refractory material, and right
The problem of low-grade magnesite or fine ore, tailing could not make full use of.Cause recovering plant cover of mine problem serious, resource comprehensive
Producing level is not high.Not only product variety is few, and product specification is not also high.
So far, to the chemical utilization of magnesite, only using the calcined light calcined magnesia of magnesite as raw material, after
And it is reacted with sulfuric acid or hydrochloric acid and generates epsom salt or magnesium chloride hexahydrate, carbon dioxide and directly arranged in calcination process
It puts, does not utilize, not only consume the energy, waste resource, and pollute environment.More notably, calcining is to make in order to obtain
The raw material of refractory material is made, low-grade magnesite, tailing, fine ore etc. are most of not to be utilized.
Using Chemical Engineering Technology feature, mechanical and surface chemical modification is carried out to low-grade magnesite, under cryogenic directly
Chemical utilization is connect, while not only protectiveness utilizes refractory raw material, more accelerates magnesite industrial transformation and supply side structural reform,
To the chemical utilization of carbon dioxide in magnesite, not only solve CO2 emission problem, more played magnesite " magnesium with
Double utility values of carbon ".Really realize comprehensive utilization, it is significant.
Summary of the invention
It is low-grade the purpose of the present invention is to provide the method that a kind of low-grade magnesite surface modified chemical directly utilizes
Magnesite is modified it with surfactant, then the method for direct chemical utilization after broken, milling and screening；It will be low
Grade magnesite (content of magnesia≤40%) is after broken, milling, screening, and modified to its surface using ammonium salt compound, modified is low
Grade magnesite can direct chemical utilization under cryogenic.
The purpose of the present invention is what is be achieved through the following technical solutions:
The method that a kind of low-grade magnesite surface modified chemical directly utilizes, the method includes following preparation process:
The first step, with low-grade magnesite (content of magnesia≤40%) for raw material, wherein silica content >=3%, calcium oxide contain
Amount >=1.0%；
Second step through broken, ore grinding and after screening, obtains (- 200 mesh, >=85%) low-grade magnesite to above-mentioned low-grade magnesite
Miberal powder；
Third step, the magnesite powder that will be obtained controls certain pH value at room temperature, with surfactant (serotonin
Salt) it is modified；
Modified magnesite powder under the conditions of 80 DEG C~100 DEG C, can be chemically reacted directly with sulfuric acid, generate seven by the 4th step
Water magnesium sulfate, meanwhile, release carbon dioxide；
5th step, the carbon dioxide that reaction is released, couples with soda ash technique, sodium bicarbonate and ammonium chloride is produced, by ammonium chloride
It is reacted with light burnt powder, generates magnesium chloride, and the ammonia steamed can recycle；The sodium bicarbonate that reaction generates can be used as low-grade
The modified raw material in magnesite surface；
6th step, the residue containing active calcium silicon being obtained by filtration, be mixed with the magnesium sulfate monohydrate obtained after dehydration in it is micro-
Secondary element fertilizer, and partially recycled carbon dioxide can be used as CO 2 gas fertilizer.
The advantages and effects of the present invention are:
The present invention realizes the breakthrough that chemical method directly utilizes magnesite, and entire technique zero-emission has been truly realized to magnesite
Eat it is dry squeeze net, realize the comprehensive utilization of magnesite.Technology thoroughly opens " magnesium and the carbon " of magnesite secondary industry
It is double utilize situation, be truly realized comprehensive utilization of resources and even efficiently utilize.The technical application drives magnesite industry development, opens
The new page of magnesite processing and utilization is warded off, technical application there are bright prospects.
Present invention process process realizes the chemistry under magnesite cryogenic conditions and directly utilizes, and obtains epsom salt, two
Large industrial chemicals such as carbonoxide, sodium bicarbonate, magnesium chloride hexahydrate；It is straight that the recycling of ammonia, sodium bicarbonate are realized simultaneously
It connects as modified feedstock；Available secondary and micro-element fertilizers and carbon dioxide gas fertilizer are opened, technology has been truly realized pair
Double utilizations of the magnesium and carbon of low-grade magnesite, entire technique zero-emission belong to green chemical technology.
1, it using the low-grade magnesite of high-silicon high calcium as raw material, does not contend over raw materials with refractory material, is magnesite industry development
With the inevitable requirement of supply side structural adjustment；
2, surfactant-modified by the mechanically modifyings and ammonium salt compound etc. such as broken, reduce the surface energy of low-grade magnesite
With combination energy, chemical directly utilization is realized；
3, technology realizes double utilizations of " magnesium and carbon ", has been truly realized " eating dry squeeze only " to low-grade magnesite；
4, the carbon dioxide that chemical reaction generates, it is not only with high purity, and also temperature is low, in conjunction with sodium chloride production soda ash technique,
Obtain sodium bicarbonate and magnesium chloride hexahydrate；
5, the ammonia steamed can be recycled；Product sodium bicarbonate can be used as modified feedstock, save cost；
6, low-grade magnesite is utilized using chemical method, solves the key technology that carbon dioxide recovery utilizes, entire technique zero
Discharge, belongs to green chemical technology.
Detailed description of the invention
Fig. 1 is the technology of the present invention route block diagram；
Fig. 2 is the infrared spectrum of raw material of the present invention and modified magnesite mine；
Fig. 3 is the FT-IR figure of low-grade magnesite raw ore and modified product；
Fig. 4 is bedded structure oxygen-octahedron group [Si4O10]4-Type structure chart.
Specific embodiment
The following describes the present invention in detail with reference to examples.
As seen from the figure, modified 3428cm-1Place, hydroxyl vibration is remarkably reinforced with N-H stretching vibration, show great amount of hydroxy group with
Amino is attracted to low-grade magnesite surface, in 1047cm-1Place, R-O key is flexible to be remarkably reinforced, and shows that organic ammonium salt is also inhaled
It is attached on low-grade magnesite surface.
The present invention is with low-grade magnesite (content of magnesia≤40%) for raw material, wherein silica content >=3%, oxidation
Calcium content >=1.0%；Through broken, ore grinding and after screening, (- 200 mesh, >=85%) low-grade water chestnut is obtained to above-mentioned low-grade magnesite
Magnesium slag；The magnesite powder that will be obtained controls certain pH value at room temperature, with surfactant (compound amine salt) into
Row is modified；In by modified magnesite powder, under the conditions of 80 DEG C~100 DEG C, it can directly be chemically reacted with sulfuric acid, generate seven water
Magnesium sulfate, meanwhile, release carbon dioxide；The carbon dioxide that reaction is released, couples with soda ash technique, produces sodium bicarbonate and chlorine
Change ammonium, ammonium chloride is reacted with light burnt powder, generates magnesium chloride, and the ammonia steamed can recycle；React the bicarbonate generated
Sodium can be used as the modified raw material in low-grade magnesite surface；The residue containing active calcium silicon being obtained by filtration, and obtains after dehydration
Magnesium sulfate monohydrate be mixed and made into secondary and micro-element fertilizers, and partially recycled carbon dioxide can be used as carbon dioxide gas fertilizer
Material.
The method that a kind of low-grade magnesite surface modified chemical directly utilizes, the first step, with low-grade magnesite (oxidation
Content of magnesium≤40%) it is raw material, wherein silica content >=3%, calcium oxide content >=1.0%；Second step, to above-mentioned low-grade water chestnut
Magnesium mine obtains (- 200 mesh, >=85%) low-grade magnesite powder through broken, ore grinding and after screening；Third step, the magnesite that will be obtained
Miberal powder controls certain pH value at room temperature, is modified with surfactant (compound amine salt)；4th step will be modified
Magnesite powder afterwards can be chemically reacted directly with sulfuric acid under the conditions of 80 DEG C~100 DEG C, generate epsom salt, meanwhile, it puts
Carbon dioxide out；5th step, the carbon dioxide that reaction is released, couples with soda ash technique, produces sodium bicarbonate and ammonium chloride, will
Ammonium chloride is reacted with light burnt powder, generates magnesium chloride, and the ammonia steamed can recycle；The sodium bicarbonate that reaction generates can be used as
The modified raw material in low-grade magnesite surface；6th step, the residue containing active calcium silicon that is obtained by filtration and obtain after dehydration
Magnesium sulfate monohydrate is mixed and made into secondary and micro-element fertilizers, and partially recycled carbon dioxide can be used as CO 2 gas fertilizer.
1. basic principle of the invention
1) surface modification theory
High-silicon high calcium mineral in low-grade magnesite are based on magnesia silicate mineral, chemical formula Mg3[Si4O10](OH)2,
3MgO 4SiO is expressed as with oxide2•H2O.[SiO each in mineral4]4-Between three common angles tops O2-It is connected, composition
The stratiform to extend to dual space, is shown in Fig. 2, i.e., be connected to each other stratification in the plane, netted at six sides, so with [SiO4] 4- table
Show；Another active oxygen in oxygen-octahedron is directed to a side, is arranged relative to each other with the active oxygen of another six sides lamina reticularis, it
Between be connected by magnesium cation, be ionic bond in layer, interlayer is molecular link, as shown in Figure 4.
The surface isoelectric pH (2-3.5) of magnesia silicate mineral, so showing strong bear under the conditions of pH >=7
Electrically.Ammonium salt compound belongs to cationic surface active agent can be adsorbed on by electrostatic physical action and ion exchange
The surface of magnesia silicate mineral reduces the combination energy of silicon and magnesium, directly utilizes and has provided for the chemistry under cryogenic conditions
The condition of power.
2) chemical principle
MgCO3.SiO2.CaO+NH4-R+OH-→ (1)
MgCO3+H2SO4+7H2O →MgSO4.7H2O+CO2 (2)
CO2+NaCl+NH3+H2O→NaHCO3+NH4Cl (3)
NH4Cl+MgO+H2O→MgCl2+NH3↑ (4)
SiO2.CaSO4+MgSO4.H2O → (SMgCaSi) fertilizer (5).
2. basic scheme of the invention
The first step, with low-grade magnesite (content of magnesia≤40%) for raw material, wherein silica content >=3%, calcium oxide contain
Amount >=1.0%；Second step through broken, ore grinding and after screening, obtains (- 200 mesh, >=85%) low product to above-mentioned low-grade magnesite
Position magnesite powder；Third step, the magnesite powder that will be obtained control certain pH value, at room temperature with surfactant
(compound amine salt) is modified；4th step, can directly and sulfuric acid under the conditions of 80 DEG C~100 DEG C by modified magnesite powder
Chemical reaction generates epsom salt, meanwhile, release carbon dioxide；5th step, the carbon dioxide that reaction is released, with soda ash
Technique coupling, produces sodium bicarbonate and ammonium chloride, ammonium chloride is reacted with light burnt powder, generation magnesium chloride, and the ammonia energy steamed
It recycles；The sodium bicarbonate that reaction generates can be used as the modified raw material in low-grade magnesite surface；6th step, is obtained by filtration
Residue containing active calcium silicon is mixed and made into secondary and micro-element fertilizers with the magnesium sulfate monohydrate obtained after dehydration, and partially recycled
Carbon dioxide can be used as CO 2 gas fertilizer.
3. technical method of the invention
The present invention uses mechanically modifying and chemical modification method, carries out surface to low-grade magnesite miberal powder of high-silicon high calcium and changes
Property, then with sulfuric acid reaction, generates epsom salt and release carbon dioxide；By the ammonium hydroxide of a part of carbon dioxide and sodium chloride
Solution reaction generates sodium bicarbonate and ammonium chloride, continue to react ammonium chloride with light-magnesite powder generation magnesium chloride hexahydrate and
Ammonia recycle utilizes；Product sodium bicarbonate can be used as the modified raw material in low-grade magnesite surface, and save the cost will be obtained by filtration
Residue mixed with magnesium sulfate monohydrate as secondary and micro-element fertilizers, partial CO 2 product compresses the gas as greenhouse
Body fertilizer.
4. specific embodiment of the present invention
(1) low-grade magnesite is obtained into 200 mesh, >=85% low-grade water chestnut by mechanically modifying (broken, milling), screening
Magnesium slag.
(2) it weighs 0.035g natrium carbonicum calcinatum to be dissolved in 100ml distilled water, shift in 500ml beaker, be added
0.01g ammonium salt compound (lauryl amine+oxamide etc.), is stirring evenly and then adding into the low-grade magnesite powder of 100g mechanically modifying, after
Continuous stirring 5min., filtering take filter cake.
(3) NaCl solid 30g is weighed, 200ml ammonium hydroxide is measured, 200ml distilled water stirs evenly in 500ml beaker, adds
Enter in wide-mouth bottle.
(4) the modified magnesite filter residue in the surface 100g is taken, is poured into 500ml three-necked flask, by concentrated sulfuric acid graduated cylinder amount
100ml is taken, 50% (mass ratio) is diluted to, 30 drops/minute are added dropwise in three-necked flask, open stirring 300r/min., are warming up to 35
DEG C -85 DEG C, react 1~3h.
(5) carbon dioxide released is passed through in the wide-mouth bottle equipped with sodium chloride and ammonia aqueous solution, and reaction generates bicarbonate
Sodium and ammonium chloride are cooled to 10 DEG C, and addition sodium chloride supersaturation, crystallization obtains sodium bicarbonate, and filtrate cycle utilizes.
(6) the ammonium chloride 50g of generation is dissolved into 250ml there-necked flask, with 39g light-magnesite powder in bath temperature
60 DEG C, mixing speed react 40min when being 300 r/min, collect ammonia.Clear solution is obtained after suction filtration.Clear solution is existed
2 days are stood at room temperature, white insoluble matter is precipitated, is washed repeatedly using distilled water, ethyl alcohol, filters, dries, therefore obtain six water
Magnesium chloride, the ammonia in heated solution, which steams, to be recycled.
(7) it by epsom salt 100g, is dissolved in 200ml water, rotary evaporation to magnesium sulfate monohydrate, with technical process
Residue compounding, is made calcium and magnesium sulphur secondary nutrients.
(8) by carbon dioxide compression, the gaseous fertilizer bottled as industrialized agriculture.
Claims (1)
1. the method that a kind of low-grade magnesite surface modified chemical directly utilizes, which is characterized in that the method includes following
Preparation process:
The first step, with low-grade magnesite (content of magnesia≤40%) for raw material, wherein silica content >=3%, calcium oxide contain
Amount >=1.0%；
Second step through broken, ore grinding and after screening, obtains (- 200 mesh, >=85%) low-grade magnesite to above-mentioned low-grade magnesite
Miberal powder；
Third step, the magnesite powder that will be obtained controls certain pH value at room temperature, with surfactant (serotonin
Salt) it is modified；
Modified magnesite powder under the conditions of 80 DEG C~100 DEG C, can be chemically reacted directly with sulfuric acid, generate seven by the 4th step
Water magnesium sulfate, meanwhile, release carbon dioxide；
5th step, the carbon dioxide that reaction is released, couples with soda ash technique, sodium bicarbonate and ammonium chloride is produced, by ammonium chloride
It is reacted with light burnt powder, generates magnesium chloride, and the ammonia steamed can recycle；The sodium bicarbonate that reaction generates can be used as low-grade
The modified raw material in magnesite surface；
6th step, the residue containing active calcium silicon being obtained by filtration, be mixed with the magnesium sulfate monohydrate obtained after dehydration in it is micro-
Secondary element fertilizer, and partially recycled carbon dioxide can be used as CO 2 gas fertilizer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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