CN103303947B - Preparation method and device for efficiently preparing magnesium hydroxide - Google Patents
Preparation method and device for efficiently preparing magnesium hydroxide Download PDFInfo
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- CN103303947B CN103303947B CN201310248358.1A CN201310248358A CN103303947B CN 103303947 B CN103303947 B CN 103303947B CN 201310248358 A CN201310248358 A CN 201310248358A CN 103303947 B CN103303947 B CN 103303947B
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Abstract
The invention relates to a device for efficiently preparing magnesium hydroxide. The preparation device comprises a material mixing tank, a pressure control linking unit I, a reactor, a pressure control linking unit II, a condenser, a two-position three-way valve, a material storage tank, a pressure control linking unit III and a steam generator, wherein a discharging hole of the material mixing tank is connected with one end of the pressure control linking unit I by a pump; the other end of the pressure control linking unit I is connected with a charging hole of the reactor; the discharging hole of the reactor is connected with one end of the pressure control linking unit II; the other end of the pressure control linking unit II is connected with one end of the condenser; the other end of the condenser is connected with a first interface of the two-position three-way valve; a second interface of the two-position three-way is connected with a material return hole of the material mixing tank; a third interface of the two-position three-way valve is connected with the material storage tank; a steam inlet of the reactor is connected with one end of the pressure control linking unit III; the other end of the pressure control linking unit III is connected with the steam generator. The preparation method and the preparation device for efficiently preparing magnesium hydroxide disclosed by the invention have the beneficial effect of quickly and efficiently preparing magnesium hydroxide sizing agent.
Description
Technical field
The present invention relates to a kind of preparation method and device of efficiently preparing magnesium hydroxide.
Background technology
Magnesium hydroxide, as a kind of green material, is widely used in fire-retardant material, agricultural, environmental protection aspect.The mode of industrial acquisition magnesium hydroxide is generally 5 kinds: 1, with Wingdale and bittern reaction, produce magnesium hydroxide; 2, with sodium hydroxide and bittern, enriched bittern cake, react hydrogen manufacturing magnesium oxide; 3, utilize burnt magnesite, rhombspar and bittern, enriched bittern cake reaction to produce magnesium hydroxide; 4, with ammoniacal liquor and bittern, enriched bittern cake, react hydrogen manufacturing magnesium oxide; 5, utilize magnesium oxide aquation to generate magnesium hydroxide, the magnesium oxide here must be that light-burned product is to guarantee the activity of aquation.The most frequently used is to adopt the mode of aquation light calcined magnesia to obtain magnesium hydroxide, and aquation is all to complete under the condition stirring conventionally, and the condition of aquation is substantially: 30～60 ℃ of hydration temperatures; Magnesium oxide concentration of slurry 5～20%(w/w); Hydration time 1～24h, aquation rate 60～80%.
In sum, magnesium oxide aquation is prepared the problem that magnesium hydroxide technical field exists: due to the longer residence time, traditional magnesium oxide aquation is prepared magnesium hydroxide and is that the volume of batch process, reaction vessel is large, hydration efficiency is not high, aquation rate is lower.
Summary of the invention
The present invention, by control pressure and temperature, makes magnesium oxide and steam reaction, the object of reach stable, efficiently preparing magnesium hydroxide slurry.
The invention provides a kind of device of efficiently preparing magnesium hydroxide, comprise mixing tank, pressure-controlling linkage unit I, reactor, pressure-controlling linkage unit II, condenser, two-position three-way valve, storage tank, pressure-controlling linkage unit III, vapour generator, described mixing tank discharge port is connected by pump with pressure-controlling linkage unit I one end, the pressure-controlling linkage unit I the other end is connected with reactor feed mouth, reactor discharge port is connected with pressure-controlling linkage unit II one end, the pressure-controlling linkage unit II the other end is connected with condenser one end, the condenser the other end is connected with two-position three-way valve first interface, two-position three-way valve the second interface is connected with mixing tank returning charge mouth, two-position three-way valve the 3rd interface is connected with storage tank, reactor vapor entrance is connected with pressure-controlling linkage unit III one end, the pressure-controlling linkage unit III the other end is connected with vapour generator.
Pressure-controlling linkage unit of the present invention is preferably by pressure transmitter and magnetic valve and forms.
In prior art, Water Molecular Adsorption is to magnesium oxide particle surface, the magnesium hydroxide that reaction forms covers on magnesium oxide particle surface, hindered the carrying out of further hydration reaction, when device of the present invention is prepared magnesium hydroxide, high pressure steam directly contacts with solid, and gas-solid reaction occurs, and the magnesium hydroxide generating on magnesium oxide particle surface is peeled off rapidly, magnesium oxide particle continues by aquation, obtains magnesium hydroxide slurry after cooling.
Another object of the present invention provides a kind of preparation method who efficiently prepares magnesium hydroxide, and described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank and mixed, obtain magnesium oxide slurries;
Described magnesium oxide accounts for 5～15% of gross weight;
2. magnesium oxide slurries are joined in reactor by pump, open vapour generator, in reactor, pass into steam, reactor heating, it is that 0.2～0.5MPa, pressure-controlling linkage unit II pressure are that 0.2～0.5MPa, pressure-controlling linkage unit III pressure are 0.2～0.5MPa that control pressure is controlled linkage unit I pressure, temperature of reaction is 90～150 ℃, and liquid in reaction is turned back to mixing tank by two-position three-way valve the second interface, then is turned back to and in reactor, formed circulation loop by mixing tank;
3. circulate after 10～35min and close two-position three-way valve the second interface, open two-position three-way valve the 3rd interface, by reaction afterwards liquid join storage tank.
Step of the present invention is 2. for controlling feed pressure by pressure-controlling linkage unit I, the steam that vapour generator produces passes through pressure-controlling linkage unit III and magnesium oxide slurry reaction, the pressure acute variation that the water hammer while controlling reaction by pressure-controlling linkage unit II brings.
Magnesium oxide of the present invention is preferably and accounts for 15% of gross weight.
Pressure-controlling linkage unit I pressure of the present invention is preferably 0.3～0.5MPa.
Pressure-controlling linkage unit II pressure of the present invention is preferably 0.3～0.5MPa.
Pressure-controlling linkage unit III pressure of the present invention is preferably 0.3～0.5MPa.
Temperature of reaction of the present invention is preferably 120～150 ℃.
The ratio of above-mentioned preferential oxidation magnesium, pressure-controlling linkage unit I pressure, pressure-controlling linkage unit II pressure, pressure-controlling linkage unit III pressure and temperature of reaction reach more than 90% magnesium hydroxide reaction conversion ratio.
Beneficial effect of the present invention is:
1. improve the speed of reaction of preparing magnesium hydroxide;
2. improve the reaction conversion ratio of preparing magnesium hydroxide;
3. greatly dwindled the volume of reactor.
Accompanying drawing explanation
Accompanying drawing 1 width of the present invention,
Fig. 1 is for efficiently preparing the structural representation of magnesium hydroxide device;
Wherein, 1, mixing tank, 11, mixing tank discharge port, 12, mixing tank returning charge mouth, 2, pressure-controlling linkage unit I, 3, reactor, 31, reactor feed mouth, 32, reactor discharge port, 33, reactor vapor entrance, 4, pressure-controlling linkage unit II, 5, condenser, 6, two-position three-way valve, 61, two-position three-way valve first interface, 62, two-position three-way valve the second interface, 63, two-position three-way valve the 3rd interface, 7, storage tank, 8, pressure-controlling linkage unit III, 9, vapour generator.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
A kind of device of efficiently preparing magnesium hydroxide, comprise mixing tank 1, pressure-controlling linkage unit I 2, reactor 3, pressure-controlling linkage unit II 4, condenser 5, two-position three-way valve 6, storage tank 7, pressure-controlling linkage unit III 8, vapour generator 9, described mixing tank discharge port 11 is connected by pressure water pump with pressure-controlling linkage unit I 2 one end, pressure-controlling linkage unit I 2 the other ends are connected with reactor feed mouth 31, reactor discharge port 32 is connected with pressure-controlling linkage unit II 4 one end, pressure-controlling linkage unit II 4 the other ends are connected with condenser 5 one end, condenser 5 the other ends are connected with two-position three-way valve first interface 61, two-position three-way valve the second interface 62 is connected with mixing tank returning charge mouth 12, two-position three-way valve the 3rd interface 63 is connected with storage tank 7, reactor vapor entrance 33 is connected with pressure-controlling linkage unit III 8 one end, pressure-controlling linkage unit III 8 the other ends are connected with vapour generator 9, described pressure-controlling linkage unit is comprised of pressure transmitter and magnetic valve.
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 5% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.2～0.3MPa, pressure-controlling linkage unit II 4 pressure are that 0.2～0.3MPa, pressure-controlling linkage unit III 8 pressure are 0.2～0.3MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 90～120 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 1.95L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 1 is in Table 1:
The aquation rate of table 1 embodiment 1
Embodiment 2
Be with embodiment 1 difference:
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 5% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.3～0.5MPa, pressure-controlling linkage unit II 4 pressure are that 0.3～0.5MPa, pressure-controlling linkage unit III 8 pressure are 0.3～0.5MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 120～150 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 1.55L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 2 is in Table 2:
The aquation rate of table 2 embodiment 2
Embodiment 3
Be with embodiment 1 difference:
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 10% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.2～0.3MPa, pressure-controlling linkage unit II 4 pressure are that 0.2～0.3MPa, pressure-controlling linkage unit III 8 pressure are 0.2～0.3MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 90～120 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 1.2L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 3 is in Table 3:
The aquation rate of table 3 embodiment 3
Embodiment 4
Be with embodiment 1 difference:
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 10% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.3～0.5MPa, pressure-controlling linkage unit II 4 pressure are that 0.3～0.5MPa, pressure-controlling linkage unit III 8 pressure are 0.3～0.5MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 120～150 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 2.9L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 4 is in Table 4:
The aquation rate of table 4 embodiment 4
Embodiment 5
Be with embodiment 1 difference:
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 15% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.2～0.3MPa, pressure-controlling linkage unit II 4 pressure are that 0.2～0.3MPa, pressure-controlling linkage unit III 8 pressure are 0.2～0.3MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 90～120 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 3.1L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 5 is in Table 5:
The aquation rate of table 5 embodiment 5
Embodiment 6
Be with embodiment 1 difference:
A preparation method who efficiently prepares magnesium hydroxide, described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank 1 and mixed, described magnesium oxide accounts for 15% of gross weight, obtains magnesium oxide slurries;
2. magnesium oxide slurries are joined in reactor 3 by pump, open vapour generator 9, in reactor 3, pass into steam, reactor heating 3, it is that 0.3～0.5MPa, pressure-controlling linkage unit II 4 pressure are that 0.3～0.5MPa, pressure-controlling linkage unit III 8 pressure are 0.3～0.5MPa that control pressure is controlled linkage unit I 2 pressure, temperature of reaction rises to 120～150 ℃, liquid in reaction is turned back to mixing tank 1 by two-position three-way valve the second interface 62, by mixing tank 1, turned back in reactor 3 and formed circulation loop again, circular flow is 2.75L/min;
3. circulate after 35min and close two-position three-way valve the second interface 62, open two-position three-way valve the 3rd interface 63, by reaction afterwards liquid join storage tank 7.
The experimental result of embodiment 6 is in Table 6:
The aquation rate of table 6 embodiment 6
Experiment conclusion:
1. adopt the method for preparing magnesium hydroxide of the present invention, during 10min, reaction conversion ratio tends towards stability, and after 10min, reaction conversion ratio temporal evolution is less;
When 2. magnesium oxide quality percentage concentration is 10～15%, during 10min, reaction conversion ratio reaches 80～90%.
Comparative example 1
Adopt cup tank experiment contrast the present invention experiment;
The experiment condition of comparative example 1 is in Table 7.
The experiment condition of table 7 comparative example 1
| ? | Magnesium oxide quality percentage concentration | Temperature of reaction | Stirring velocity |
| Comparative example 1 | 10% | 90℃ | 900r/min |
The experimental result of comparative example 1 is in Table 8.
The experiment conclusion of table 8 comparative example 1
| Reaction times (min) | 10 | 20 | 30 | 40 | 50 | 60 | 90 | 120 |
| Aquation rate (%) | 47.1 | 52.0 | 56.7 | 65.1 | 66.0 | 70.0 | 72.8 | 77.7 |
Conclusion: when the hydration time of cup tank experiment is 120min, magnesian reaction conversion ratio is only 77.7%, preparation method of the present invention is under same reaction temperature, reaction 10min obtains more than 80% reaction conversion ratio, therefore, compare with traditional method, the present invention has significant advantage fast and efficiently, because speed of reaction shortens, device of the present invention is greatly reduced compared with conventional apparatus floor space simultaneously.
Claims (8)
1. a device of efficiently preparing magnesium hydroxide, comprise mixing tank (1), pressure-controlling linkage unit I (2), reactor (3), pressure-controlling linkage unit II (4), condenser (5), two-position three-way valve (6), storage tank (7), pressure-controlling linkage unit III (8), vapour generator (9), mixing tank discharge port (11) is connected by pump with pressure-controlling linkage unit I (2) one end, pressure-controlling linkage unit I (2) the other end is connected with reactor feed mouth (31), reactor discharge port (32) is connected with pressure-controlling linkage unit II (4) one end, pressure-controlling linkage unit II (4) the other end is connected with condenser (5) one end, condenser (5) the other end is connected with two-position three-way valve first interface (61), two-position three-way valve the second interface (62) is connected with mixing tank returning charge mouth (12), two-position three-way valve the 3rd interface (63) is connected with storage tank (7), reactor vapor entrance (33) is connected with pressure-controlling linkage unit III (8) one end, pressure-controlling linkage unit III (8) the other end is connected with vapour generator (9).
2. device according to claim 1, is characterized in that: described pressure-controlling linkage unit is comprised of pressure transmitter and magnetic valve.
3. efficiently prepare a preparation method for magnesium hydroxide, it is characterized in that: described method comprises the steps:
1. magnesium oxide and water are joined in mixing tank (1) and mixed, obtain magnesium oxide slurries;
Described magnesium oxide accounts for 5～15% of gross weight;
2. magnesium oxide slurries are joined in reactor (3) by pump, open vapour generator (9), in reactor (3), pass into steam, reactor heating (3), it is that 0.2～0.5MPa, pressure-controlling linkage unit II (4) pressure are that 0.2～0.5MPa, pressure-controlling linkage unit III (8) pressure are 0.2～0.5MPa that control pressure is controlled linkage unit I (2) pressure, temperature of reaction is 90～150 ℃, in reacting, liquid turns back to mixing tank (1) by two-position three-way valve the second interface (62), then turns back to formation circulation loop in reactor (3) by mixing tank (1);
3. circulate after 10～35min and close two-position three-way valve the second interface (62), open two-position three-way valve the 3rd interface (63), by reaction afterwards liquid join storage tank (7).
4. preparation method according to claim 3, is characterized in that: described magnesium oxide accounts for 15% of gross weight.
5. preparation method according to claim 3, is characterized in that: described pressure-controlling linkage unit I (2) pressure is 0.3～0.5MPa.
6. preparation method according to claim 3, is characterized in that: described pressure-controlling linkage unit II (4) pressure is 0.3～0.5MPa.
7. preparation method according to claim 3, is characterized in that: described pressure-controlling linkage unit III (8) pressure is 0.3～0.5MPa.
8. preparation method according to claim 3, is characterized in that: described temperature of reaction is 120～150 ℃.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310248358.1A CN103303947B (en) | 2013-06-19 | 2013-06-19 | Preparation method and device for efficiently preparing magnesium hydroxide |
| EP13887283.3A EP3012222A4 (en) | 2013-06-19 | 2013-07-26 | Preparation method and device for efficiently preparing magnesium hydroxide |
| JP2016520234A JP6212211B2 (en) | 2013-06-19 | 2013-07-26 | Manufacturing method and apparatus for manufacturing magnesium hydroxide |
| PCT/CN2013/080196 WO2014201752A1 (en) | 2013-06-19 | 2013-07-26 | Preparation method and device for efficiently preparing magnesium hydroxide |
| US14/900,334 US9776882B2 (en) | 2013-06-19 | 2013-07-26 | Preparation method and device for efficiently preparing magnesium hydroxide |
| KR1020167001340A KR101795974B1 (en) | 2013-06-19 | 2013-07-26 | Preparation method and device for efficiently preparing magnesium hydroxide |
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| CN201310248358.1A CN103303947B (en) | 2013-06-19 | 2013-06-19 | Preparation method and device for efficiently preparing magnesium hydroxide |
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| CN103303947B true CN103303947B (en) | 2014-09-03 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104108733B (en) * | 2014-07-07 | 2015-12-09 | 新疆大正过程环保科技有限公司 | Highly-purity magnesite wets fire one subtraction unit and prepare the method for highly-purity magnesite |
| CN104925838B (en) * | 2015-07-15 | 2016-12-28 | 后英集团海城市高新技术产品有限公司 | A kind of efficient oxidation magnesium prepares magnesium hydroxide technique |
| CN106365185B (en) * | 2016-10-13 | 2018-03-23 | 大连海事大学 | A kind of efficient aquation of Ultrasound-assisted magnesia prepares the devices and methods therefor of magnesium hydroxide |
| CN109574049B (en) * | 2019-01-23 | 2021-09-21 | 大连海事大学 | Hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate |
| CN112452286A (en) * | 2020-12-15 | 2021-03-09 | 辽宁荣邦科技有限公司 | Preparation device and method of magnesium hydroxide slurry |
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