CN106012024A - Method and apparatus for production of basic magnesium carbonate and magnesium oxide whisker from magnesite - Google Patents
Method and apparatus for production of basic magnesium carbonate and magnesium oxide whisker from magnesite Download PDFInfo
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- CN106012024A CN106012024A CN201510584662.2A CN201510584662A CN106012024A CN 106012024 A CN106012024 A CN 106012024A CN 201510584662 A CN201510584662 A CN 201510584662A CN 106012024 A CN106012024 A CN 106012024A
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- carbonization
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Abstract
The invention relates to a method and apparatus for production of basic magnesium carbonate and magnesium oxide whisker from magnesite. The invention utilizes non-acidolysis and non-alkalifying of magnesite to synthesize a precursor, then calcination is carried out to obtain magnesium oxide whisker, magnesite can be utilized to automatically synthesize basic magnesium carbonate and magnesium oxide whisker. The method consists of: taking magnesite as the raw material, carrying out calcination, powdering, carbonization and deslagging on the raw material to obtain a heavy magnesium solution, resolving the heavy magnesium solution to obtain a precursor, and drying the precursor to obtain magnesium carbonate whisker. The method does not involved acid or alkali, can enable automatic synthesis of the precursor and magnesium oxide whisker from magnesite, in the future the industrialized operation can be safer, and the equipment and pipeline can realize material carbon tempering. Also the carbon dioxide and water produced in the process can be recycled, thus realizing a green process.
Description
Technical field
The invention belongs to inorganic salt preparation field, a kind of magnesite synthesis basic magnesium carbonate and magnesia crystal whisker of utilizing
Method and apparatus.
Background technology
Whisker is a kind of draw ratio mono-crystlling fibre material more than 10, and whisker atomic structural arrangement when crystallization is orderly, internal flaw
Few, therefore its intensity and modulus are all close to the theoretical value of perfect crystal material, are the benefits of the composite that a kind of performance is the most superior
Strong agent.
Magnesia crystal whisker has good thermostability, resistance to acids and bases, insulating properties, heat conductivity, stability and strengthening and toughening,
Thermal conductivity is three times of aluminium oxide, and heat resisting temperature is up to 1600 DEG C, and hot strength is 980MPa, thermal conductivity 260W/M.K,
Can be used for composite.Magnesium oxide and polrvinyl chloride with the use of, mechanical strength and the heat stability of goods can be improved；With cement
With the use of time, flexural strength and the impact strength of goods can be improved；Can be used as raw material for refractory；Also act as absorption
Agent, sound-absorbing material, fire proofing, resistant material etc..
Magnesia crystal whisker preparation method has: one be magnesium-containing mineral be raw material add industrial acids dissolvings, remove impurity, interpolation alkali, then general
Reactant liquor puts into high-pressure bottle, is passed through oxygen, carries out heat treatment under 98-147MPa pressure, and the scrubbed dehydration of product exists
1100-1200 DEG C is burnt till, and obtains magnesia crystal whisker；Two is with magnesium salt and halogenide as raw material, is mixed, at 650-900 DEG C
Under add heat fusing 1-6hr, generate fused salt, then be heated to 700-900 DEG C, be passed through steam simultaneously, magnesia crystal whisker separates out
And grow up, scrubbed isolated relatively pure zirconia magnesium whisker；Three is the mixture formed with magnesium sulfate and halogenide, at 550 DEG C
Lower dehydration, 0.5-5h, then burnt till in the solution of 700-900 DEG C under the gas phase of water vapour, obtained magnesia crystal whisker heat time heating time；
Four is that patent of invention CN 1676682 of Xue Dongfeng, Wang Xiaoli utilizes magnesite acidolysis, remove impurity, adds alkali and generate predecessor
MgCO3 3H2O, generates magnesia crystal whisker by the calcining of its predecessor.
The preparation method of above-mentioned magnesia crystal whisker adds industrial acids, alkali, easy etching apparatus pipeline, it is impossible to realize material carbon steel
Change；And complex manufacturing, operating difficulties, production cost is high, and produces a large amount of waste material waste gas in production process, is also unfavorable for
Environmental conservation.
Summary of the invention
The technical problem to be solved is to provide one and utilizes magnesite to be directly synthesized forerunner without acid, bases as raw material
Thing and the method and apparatus of magnesia crystal whisker, with it, achieve industrial equipment and the carbon steel of pipeline valve material,
And carbon dioxide, the waste water in production technology can recycle.
In order to solve the problems referred to above, the invention provides a kind of method utilizing magnesite to produce basic magnesium carbonate and magnesia crystal whisker,
Wherein, the method is with magnesite as raw material, carried out calcining, powder, carbonization, slagging-off, and obtain heavy magnesium water, by it
Heavy magnesium water carries out parsing and obtains predecessor, is dried by predecessor and then obtains magnesium carbonate whisker: the calcining of its predecessor is then obtained magnesium oxide brilliant
Must, its preparation process is:
A, calcining: magnesite is sintered into light-burned ore deposit, the ripest breeze；
B, powder: above-mentioned ripe breeze is become light burnt powder；
C, carbonization: light burnt powder and water are mixed into tank, the CO that calcined magnesite is produced2Through cooling, dedusting, air compressor machine supercharging
Deliver to carbonization tank is carried out carbonization, the magnesium oxide of indissoluble is converted into solvable magnesium oxide solution；
D, filtering residue: deliver in filter by above-mentioned carbodiimide solution, obtain heavy magnesium water after slagging-off；
E, parsing: deliver to above-mentioned heavy magnesium water resolve in tank, resolve and obtain predecessor MgCO3·3H2O aqueous solution, generation
CO2Return to suction port of compressor, recycle；
F, separation: by above-mentioned containing MgCO3·3H2O aqueous solution is squeezed in centrifuge, centrifugation, and its water returns carbonation process,
For batch mixing；
G, dry and calcining: by predecessor MgCO obtained above3·3H2O crystal is put in drying machine, 120-180 DEG C with
Under be dried two hours, so that it may obtain basic magnesium carbonate whisker；Place it in Muffle furnace or stainless steel and calcine, calcining temperature
Spend at 750-850 DEG C, 2-3 hour time available MgO whisker.
Further, calcining kiln preheating section temperature controls at 150-200 DEG C, and calcining section temperature controls at 700-900 DEG C, cooling section
Temperature controls at 100-150 DEG C, calcination time 24-32 hour, ripe ore deposit activity≤200S.
Further, light burnt powder is that 120 mesh 90% pass through, and measures its content of MgO after powder, preferably greater than more than 82%, and oxygen
Change calcium less than 1%.
Further, in carbonisation, breeze and water are preferably mixed into tank in the ratio of MgO13-17g/L, and carburizing temperature is less than
20 °, 3-4 atmospheric pressure of carbonization pressure, carbonization time 1.5-2.5 hour.
Further, in the MgO solution of carbonization terminal, soluble M gO reaches 11-15g/L；Preferably reach solvable after filtering residue
The pure liquid of property MgO11-15g/L.
In order to solve above-mentioned technical problem, present invention also offers one and utilize magnesite to produce basic magnesium carbonate and magnesia crystal whisker
Equipment, wherein, this equipment realizes calcining, carbonization, the process that resolves, be dried and calcine to magnesite, thus generates alkali formula
Magnesium carbonate and magnesia crystal whisker, including calcining kiln, powder machine, carbonization tank, filter, parsing tank, compressor, centrifuge,
Drying machine and Muffle furnace or stainless steel, the CO that wherein calcining kiln produces2Through cooling, dedusting, compression device and carbon
Change tank to be connected, resolve the CO generated in tank2Being connected with compression device entrance, the water that centrifuge produces is connected with carbonization tank.
Further, calcining preheating section of kiln temperature controls at 150-200 DEG C, and calcining section temperature controls at 700-900 DEG C, cooling
Duan Wendu controls at 100-150 DEG C, calcination time 24-32 hour, ripe ore deposit activity≤200S.
Further, ripe breeze is become the light burnt powder that 120 mesh 90% pass through by powder machine.
Further, breeze is mixed into carbonization tank with water in the ratio of MgO 13-17g/L, the CO that calcined magnesite produces2Through fall
Temperature, dedusting, supercharging are delivered to carbonization tank and are carried out carbonization, and carbonization terminal is that in solution, soluble M gO reaches 11-15g/L.
Further, filter obtains the pure liquid of soluble M gO11-15g/L: by soluble M gO11-15g/L after slagging-off
Pure liquid send into resolve tank, resolve and obtain predecessor MgCO3·3H2O aqueous solution；After being performing centrifugal separation on, by predecessor
MgCO3·3H2O crystal is put in drying machine, is dried two hours, can obtain basic magnesium carbonate whisker below 120-180 DEG C；Will
Predecessor MgCO3·3H2O crystal put in Muffle furnace or stainless steel calcine, calcining heat at 750-850 DEG C, time 2-3
Hour can obtain MgO whisker.
Compared with currently existing scheme, what the present invention was obtained has the technical effect that
1, this method anacidity, alkali participate in, and magnesite can be made to be automatically synthesized predecessor and magnesia crystal whisker, and industrial operation is more in the future
Safety, equipment, pipeline can realize material carbon steel.
2, the carbon dioxide recycle produced in this method technique uses, and can realize technique greenization.
3, this method solution can be recycled, and processes and discharge without waste water, can realize the close friendization of man and nature environment.
4, this method predecessor is formed simple, quick, easily realizes project industrialization and scale.
Accompanying drawing explanation
Fig. 1 is Electronic Speculum figure and the grain size distribution of basic magnesium carbonate (sample 1) the D50=4.1 μm of the embodiment of the present invention 1；
Fig. 2 is Electronic Speculum figure and the grain size distribution of basic magnesium carbonate (sample 2) the D50=3.3 μm of the embodiment of the present invention 2.
Detailed description of the invention
The involved in the present invention method utilizing magnesite to be automatically synthesized basic magnesium carbonate and magnesia crystal whisker, is to be former with magnesite
Material, carried out calcining, powder, carbonization, slagging-off, and obtain heavy magnesium water, its heavy magnesium water is carried out parsing obtains predecessor,
Predecessor is dried and then obtains magnesium carbonate whisker；The calcining of its predecessor is then obtained magnesia crystal whisker, and its principles of chemistry are:
A) calcine: MgCO3 → MgO+CO2 ↑ 1.
B) carbonization: MgO+H2O+CO2 → Mg (HCO3) 2 is 2.
C) resolve: Mg (HCO3) 2 → MgCO3.3H2O ↓+CO2 ↑ 3.
D) it is dried: 4MgCO3.3H2O → 3MgCO3.Mg (OH) 2.3H2O+CO2 ↑+3H2O ↑ 4.
E) calcining: MgCO3 3H2O → MgO+CO2 ↑+3H2O ↑ 5.
Currently preferred preparation process includes:
1) calcining: magnesite is sintered into light-burned ore deposit, and calcining kiln preheating section temperature controls at 150-200 DEG C, calcines Duan Wen
Degree controls at 700-900 DEG C, and cooling section temperature controls at 100-150 DEG C, calcination time 24-32 hour, ripe ore deposit activity≤200S.
2) powder: above-mentioned ripe breeze is become the light burnt powder that 120 mesh 90% pass through, and measures its content of MgO, it is desirable to big
In more than 82%.
3) carbonization: breeze and water are mixed into tank in the ratio of MgO13-17g/L, the CO2 that kiln calcined magnesite is produced
(kiln gas) delivers to carry out in carbonization tank carbonization through cooling, dedusting, supercharging, and carbonization terminal is that in solution, soluble M gO reaches
11-15g/L。
4) filtering residue: deliver in filter by above-mentioned carbodiimide solution, obtains the pure liquid of soluble M gO11-15g/L after slagging-off,
It is commonly called as heavy magnesium water.
5) resolve: above-mentioned heavy magnesium water is got in parsing tank, resolve and obtain predecessor MgCO3 3H2O aqueous solution,
The CO2 generated returns to suction port of compressor, recycles.
6) separate: squeezing in centrifuge by the above-mentioned 3H2O aqueous solution containing MgCO3, centrifugation, its water returns carbonization
Operation, for batch mixing.
7) it is dried with calcining: predecessor MgCO3 3H2O crystal obtained above is put in drying machine,
Less than 120-180 DEG C is dried two hours, so that it may obtain basic magnesium carbonate whisker；Place it in Muffle furnace or stainless steel and forge
Burn, calcining heat at 750-850 DEG C, 2-3 hour time available MgO whisker.
The invention still further relates to a kind of equipment utilizing magnesite to produce basic magnesium carbonate and magnesia crystal whisker, this equipment is real to magnesite
Now calcining, carbonization, resolve, be dried and the process of calcining, thus generate basic magnesium carbonate and magnesia crystal whisker, including calcining kiln,
Powder machine, carbonization tank, filter, parsing tank, compressor, centrifuge, drying machine and Muffle furnace or stainless steel, its
Middle calcining kiln is connected with carbonization tank, so that being delivered to through cooling, dedusting, supercharging by the CO2 (kiln gas) that calcined magnesite produces
Carbonization tank carries out carbonization；Resolve tank to be connected with suction port of compressor, so that resolving the CO2 generated to return to suction port of compressor,
Recycle；Centrifuge is connected with carbonization tank, so that the water of centrifugation returns carbonation process, for batch mixing.
Described calcining kiln is to change into magnesium carbonate in magnesite to have certain activated magnesia, and provides finite concentration carbon dioxide
The equipment of (being commonly called as kiln gas).Suitable for reading little, end opening is big, vial-type structure, and suitable for reading have adapter to be connected with scrubbing tower and air compressor machine entrance,
Carbon dioxide channel is inhaled for air compressor machine.
Powder machine is the light burnt powder abrasive blast equipment that ripe breeze becomes 120 mesh 90% pass through.
Carbonization tank is self pressure vessel with cooler Yu agitating device, and indissoluble magnesium oxide is changed into solvable magnesium oxide
Equipment.
Filter is the filter plant for obtaining pure heavy magnesium water after slagging-off；Resolving tank is that the hydrolysis analysis of net net weight magnesium is obtained forerunner
Thing MgCO3 3H2O aqueous solution and the device of carbon dioxide, it connects air compressor machine population with agitator and circulating pump, tank outlet.
Drying machine and calcining furnace: be put in drying machine by predecessor MgCO3 3H2O crystal, be dried two below 120-180 DEG C
Hour, basic magnesium carbonate whisker can be obtained；Being put into by predecessor MgCO3 3H2O crystal in Muffle furnace and calcine, calcining heat exists
750-850 DEG C, 2-3 hour time can obtain MgO whisker, and industrialization can use stainless steel.
Embodiments of the invention 1, magnesite is broken into 13-16 centimetre of size nugget and smokeless coal cinder (calorific capacity 22000 joules/
Kilogram) be added in calcining kiln in 10: 1 ratios, calcining heat controls under 820-860 degree, calcination time 26 hours, obtains ripe
Ore deposit reaches 120 mesh 90% through powder and passes through, and measures content of magnesia 83.5%, activity 185 seconds.By its powder with water by oxidation
Magnesium 15 grams per liter ratio is thrown in carbonization tank, calcining kiln produces carbon dioxide (kiln gas) and delivers to carbon through cooling, dedusting, compression
Changing in tank, Stress control is at 3-4 atmospheric pressure, and temperature controls 10-20 degree, 1.5-2.5 hour response time, measures solubility oxygen
Change magnesium more than 13 grams per liters.By its filter cleaner, obtain pure liquid be commonly called as heavy magnesium water get to parsing tank in, obtain magnesium carbonate crystal,
The carbon dioxide desorbed is delivered to carbonization cycle and is utilized, and magnesium carbonate crystal is delivered in drying machine 120 degree of-180 degree (this experiment control
Temperature processed 130 degree-180 degree) under be dried within 2 hours, obtain basic magnesium carbonate whisker；Crystal is delivered in Muffle furnace under 800 degree
Calcine and obtain magnesia crystal whisker in 2.5 hours, during commercial Application, use stainless steel.
Embodiments of the invention 2, magnesite is broken into 13-16 centimetre of size nugget and smokeless coal cinder (calorific capacity 21000 joules/
Kilogram) be added in calcining kiln in 10: 1 ratios, calcining heat controls under 800-830 degree, calcination time 27 hours, obtains ripe
Ore deposit reaches 120 mesh 90% through powder and passes through, and measures content of magnesia 85.5%, activity 160 seconds.By its powder with water by oxidation
Magnesium 16 grams per liter ratio is thrown in carbonization tank, calcining kiln produces carbon dioxide (kiln gas) and delivers to carbon through cooling, dedusting, compression
Changing in tank, Stress control is at 3-4 atmospheric pressure, and temperature controls 10-20 degree, 1.5-2.5 hour response time, measures solubility oxygen
Change magnesium more than 14.5 grams per liters.By its filter cleaner, obtain pure liquid be commonly called as heavy magnesium water get to parsing tank in, obtain magnesium carbonate crystal,
The carbon dioxide desorbed is delivered to carbonization cycle and is utilized, and magnesium carbonate crystal is delivered in drying machine 120 degree of-180 degree (this experiment control
Make at 130 degree-170 degree) under dry within 2 hours, obtain basic magnesium carbonate whisker；Crystal is delivered to calcine under 850 degree in Muffle furnace
Within 2.5 hours, obtain magnesia crystal whisker.
Described above illustrate and describes some preferred embodiments of the present invention, but as previously mentioned, it should be understood that the present invention not office
Be limited to form disclosed herein, be not to be taken as the eliminating to other embodiments, and can be used for other combinations various, amendment and
Environment, and can be modified by above-mentioned teaching or the technology of association area or knowledge in invention contemplated scope described herein.
And the change that those skilled in the art are carried out and change are without departing from the spirit and scope of the present invention, the most all should want in right appended by the present invention
In the protection domain asked.
Claims (10)
1. one kind utilizes the method that magnesite produces basic magnesium carbonate and magnesia crystal whisker, it is characterised in that: the method is with magnesite
Ore deposit is raw material, carried out calcining, powder, carbonization, slagging-off, and obtain heavy magnesium water, its heavy magnesium water carried out before parsing obtains
Drive thing, predecessor is dried and then obtains magnesium carbonate whisker；The calcining of its predecessor is then obtained magnesia crystal whisker, and its preparation process is:
A, calcining: magnesite is sintered into light-burned ore deposit, the ripest breeze；
B, powder: above-mentioned ripe breeze is become light burnt powder；
C, carbonization: light burnt powder and water are mixed into tank, the CO that calcined magnesite is produced2Increase through cooling, dedusting, compression device
It is sent in carbonization tank carry out carbonization；
D, filtering residue: deliver in filter by above-mentioned carbodiimide solution, obtain heavy magnesium water after slagging-off；
E, parsing: deliver to above-mentioned heavy magnesium water resolve in tank, resolve and obtain predecessor MgCO3·3H2O aqueous solution, generation
CO2Return to suction port of compressor, recycle；
F, separation: by above-mentioned containing MgCO3·3H2O aqueous solution is squeezed in centrifuge, centrifugation, and its water returns carbonation process,
For batch mixing；
G, dry and calcining: by predecessor MgCO obtained above3·3H2O crystal is put in drying machine, 120-180 DEG C with
Under be dried two hours, so that it may obtain basic magnesium carbonate whisker；Place it in Muffle furnace or stainless steel and calcine, calcining temperature
Spend at 750-850 DEG C, 2-3 hour time available MgO whisker.
Method the most according to claim 1, it is characterised in that calcining kiln preheating section temperature controls at 150-200 DEG C, calcining
Duan Wendu controls at 700-900 DEG C, and cooling section temperature controls at 100-150 DEG C, calcination time 24-32 hour, ripe ore deposit activity≤200S.
Method the most according to claim 2, it is characterised in that light burnt powder is that 120 mesh 90% pass through, and measures it after powder
Content of MgO, preferably greater than more than 82%, calcium oxide is less than 1%.
Method the most according to claim 3, it is characterised in that in carbonisation, breeze and water preferably press MgO13-17g/L
Ratio be mixed into tank, carburizing temperature be less than 20 °, 3-4 atmospheric pressure of carbonization pressure, carbonization time 1.5-2.5 hour.
Method the most according to claim 4, it is characterised in that in the MgO solution of carbonization terminal, soluble M gO reaches
To 11-15g/L；The pure liquid of soluble M gO11-15g/L is preferably reached after filtering residue.
6. one kind utilizes the equipment that magnesite produces basic magnesium carbonate and magnesia crystal whisker, it is characterised in that: this equipment is to magnesite
Realize calcining, carbonization, resolve, be dried and the process of calcining, thus generate basic magnesium carbonate and magnesia crystal whisker, including calcining
Kiln, powder machine, carbonization tank, filter, parsing tank, compressor, centrifuge, drying machine and Muffle furnace or rustless steel turn
Stove, the CO that wherein calcining kiln produces2It is connected with carbonization tank through cooling, dedusting, compression device, resolves the CO generated in tank2
Being connected with compression device entrance, the water that centrifuge produces is connected with carbonization tank.
Equipment the most according to claim 6, it is characterised in that calcining preheating section of kiln temperature controls, at 150-200 DEG C, to forge
Burning section temperature and control at 700-900 DEG C, cooling section temperature controls at 100-150 DEG C, calcination time 24-32 hour, ripe ore deposit activity
≤200S。
Equipment the most according to claim 7, it is characterised in that it is light-burned that ripe breeze is become that 120 mesh 90% pass through by powder machine
Powder.
Equipment the most according to claim 8, it is characterised in that breeze and water are mixed into carbon in the ratio of MgO 13-17g/L
Change tank, the CO that calcined magnesite produces2Delivering to carbonization tank carry out carbonization through cooling, dedusting, supercharging, carbonization terminal is in solution
Soluble M gO reaches 11-15g/L.
Equipment the most according to claim 9, it is characterised in that obtain soluble M gO11-15g/L after slagging-off in filter
Pure liquid；The pure liquid of soluble M gO11-15g/L is sent into and resolves tank, resolve and obtain predecessor MgCO3·3H2O water
Solution；After being performing centrifugal separation on, by predecessor MgCO3·3H2O crystal is put in drying machine, is dried two below 120-180 DEG C
Individual hour, basic magnesium carbonate whisker can be obtained；By predecessor MgCO3·3H2O crystal is put in Muffle furnace or stainless steel and is calcined,
Calcining heat is at 750-850 DEG C, and 2-3 hour time can obtain MgO whisker.
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| CN201510584662.2A CN106012024A (en) | 2015-09-15 | 2015-09-15 | Method and apparatus for production of basic magnesium carbonate and magnesium oxide whisker from magnesite |
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| CN107641184A (en) * | 2017-09-25 | 2018-01-30 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of thermostable phenolic resin bonding agent |
| CN107687019A (en) * | 2017-06-13 | 2018-02-13 | 岭南师范学院 | A kind of method for preparing hollow tubular basic magnesium carbonate whisker from bittern using solar energy |
| CN108866634A (en) * | 2018-07-27 | 2018-11-23 | 辽宁科技大学 | A method of magnesia crystal whisker is prepared using waste magnesia carbon brick substrate material as raw material |
| CN116003011A (en) * | 2022-12-13 | 2023-04-25 | 辽宁科技大学 | Device and method for preparing non-retarding magnesium phosphate cement by mixing magnesium oxide with liquid carbon dioxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107687019A (en) * | 2017-06-13 | 2018-02-13 | 岭南师范学院 | A kind of method for preparing hollow tubular basic magnesium carbonate whisker from bittern using solar energy |
| CN107641184A (en) * | 2017-09-25 | 2018-01-30 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of thermostable phenolic resin bonding agent |
| CN108866634A (en) * | 2018-07-27 | 2018-11-23 | 辽宁科技大学 | A method of magnesia crystal whisker is prepared using waste magnesia carbon brick substrate material as raw material |
| CN108866634B (en) * | 2018-07-27 | 2019-11-05 | 辽宁科技大学 | A method of magnesia crystal whisker is prepared using waste magnesia carbon brick substrate material as raw material |
| CN116003011A (en) * | 2022-12-13 | 2023-04-25 | 辽宁科技大学 | Device and method for preparing non-retarding magnesium phosphate cement by mixing magnesium oxide with liquid carbon dioxide |
| CN116003011B (en) * | 2022-12-13 | 2023-07-28 | 辽宁科技大学 | Device and method for preparing non-delayed coagulation magnesium phosphate cement |
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