CN106564918A - Method and equipment for preparation of magnesium hydroxide - Google Patents
Method and equipment for preparation of magnesium hydroxide Download PDFInfo
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- CN106564918A CN106564918A CN201510662980.6A CN201510662980A CN106564918A CN 106564918 A CN106564918 A CN 106564918A CN 201510662980 A CN201510662980 A CN 201510662980A CN 106564918 A CN106564918 A CN 106564918A
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- magnesium hydroxide
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Abstract
The invention discloses a method and equipment for preparation of magnesium hydroxide and belongs to the field of preparation and purification of inorganic chemical materials. The preparation method comprises the following steps: raw materials including bittern and alkali lye firstly enter a jet mixer at room temperature to be mixed and react for the first time, and pH value is controlled to be 9 and below; secondly, a suspension enters an annular tube to further react with vaporific alkali lye and pH value is controlled to be about 10.5, and after the reaction, pH value of the whole system is regulated to be 12 and above to guarantee complete precipitation of magnesium ions; The suspension stands for 30 min, a supernatant is discharged, magnesium hydroxide paste at the vessel bottom undergoes centrifugal filtration, 5% (volume ratio) of hydrogen peroxide is added while washing, and finally filtration and drying follow successively to obtain the magnesium hydroxide finished product. The method and equipment for preparation of magnesium hydroxide can be directly used for pretreatment of calcium magnesium in raw materials in factories for directly manufacturing magnesium hydroxide or caustic soda factories. By the method and equipment, filtration time is saved and drying cost is saved.
Description
Technical field
The present invention relates to chemistry, chemical industry, medicine, the preparation of environmental protection industry (epi) magnesium hydroxide and purification technique field.
Background technology
Magnesium hydroxide is a kind of important industrial chemicals, as it is a kind of buffering and the excellent alkaline agent of chemisorbed performance, its environmental protection, ceramic material,
Medicine and other fields are widely applied.In recent years, as magnesium hydroxide has, decomposition temperature was high, heat stability is good, nontoxic, smokeless and presses down cigarette
The features such as, become a kind of important inorganic combustion inhibitor, enjoy the attention of researcher and Producer.
Production magnesium hydroxide mainly has two methods.One kind is the levigate method of shepardite, and it is that brucite powder is broken to 150um, further air-flow powder
It is broken to 1-26um；Another kind is chemical synthesiss, and it is reacted in aqueous medium with alkaloids using the salt containing magnesium chloride, halogen ore deposit etc., raw
Into magnesium hydroxide slurry, Jing filtrations, hydrothermal treatment consists, washing, surface treatment, dry prepared magnesium hydroxide.Due to the granule pole that magnesium hydroxide is generated
Which is fine, forms sol system so that the filtration and washing of slurry becomes very difficult, and so as to time-consuming, water consumption, power consumption, cost remains high,
The large-scale production of magnesium hydroxide is constrained seriously.
A filtration difficult problem for magnesium hydroxide is faced, research worker have also been made extensive work.Guizhou University (Li Junqi, five rocs, Liu Liang, Yang Shuhuai, hole
It is numerous to shake, the research that several factors are affected on magnesium hydroxide slurry strainability, Guizhou University of Technology's journal, 2007,32-39) with magnesium chloride as original
Material, sodium hydroxide is precipitant, using adding the method for magnesium hydroxide crystal seed to prepare magnesium hydroxide, have studied crystal seed coefficient, reaction temperature, anti-
Impact between seasonable to slurry filtration performance, and optimum reaction condition have found by orthogonal test, preparing magnesium hydroxide to exploration sodium-hydroxide method has
Certain reference significance；China University of Geosciences (Wang Ping, Du Gaoxiang, Li Fu, the impact flocculated to magnesium hydroxide slurry strainability and clean result,
Chemical industry mineral and processing, 2008,20-22) super fine magnesium hydroxide slurry is flocculated by using polyacrylamide, increase magnesium hydroxide particle
The method of sedimentation velocity is improving the strainability of magnesium hydroxide slurry, while the effect that magnesium hydroxide slurry washing removes sodium ion can also be improved；
Qinghai University (Li Xiaokun, the pass Yunshan Mountain, Yang Zhaojuan, He Zhifei, application of the surface modifier in super fine magnesium hydroxide filtration, inorganic chemicals industry,
2011,57-60) wet modification experiment is carried out to super fine magnesium hydroxide using sodium stearate and water-soluble titanium phosphate ester coupling agent, is improving ultra-fine hydrogen
Strainability can be significantly improved both while the surface property of magnesium oxide；Tsing-Hua University (to orchid, Zhang Junping, Ji Yu, repercussions, Yi Meigui,
2015) a kind of method for preparing High-purity high-activity magnesium hydroxide by calcic magnesium hydroxide, CN104891534A add in calcic reunion state magnesium hydroxide
Enter dispersant, purify magnesium hydroxide, improve strainability.These effort serve certain effect, but exist to production, filtration magnesium hydroxide
The problems such as relatively costly, efficiency is low, has very much the necessity for further improving.
The content of the invention
It is an object of the invention to be the pre-treatment removing calcium and magnesium by-product magnesium hydroxide raising production effect of commercial production magnesium hydroxide or production of caustic soda factory salt
Rate so that product is washable, easy filter.
To realize above-mentioned target, the technical solution used in the present invention is as follows：
1. the first mixing preparation of raw brine and alkali liquor：
The soda bath of calcic, the salt of magnesium with the concentration for preparing for 4mol/l is entered into jet mixer 1 at room temperature side by side, and then enters first
Individual reaction tank 2, to make mix homogeneously, mixed solution enters first reaction tank from entering from bottom feed mouth 3, anti-by the stirring mixing of agitator 5
More than 2 minutes (suspension is calculated from the time of bottom to overfall according to the volume and effusion meter of container) is answered, is supervised by acidometer 4 while reaction
The pH value of whole suspension is surveyed below 9, reaction is finished from discharge gate 6 overflows.
2. suspension further with alkali reaction：
The suspension of the first reaction tank enters second reaction tank 7 after the spilling of overfall 6, and suspension initially enters ring pipe 8 and feeds, while
By spray nozzle 9 with vaporific addition, the two stirring hybrid reaction monitors the pH of whole suspension to the alkali liquor of 4mol/l by acidometer while reaction
Value, 10.5 or so, is to ensure the time of staying of the suspension in reactor 2, and the second reaction tank discharging opening 10 is arranged using automatic control water level valve interval
Mixed liquor is put, discharge ensures when finishing that residual mixed liquor accounts for 1/3rd of whole reactor, and reaction finishes mixture and enters from the 3rd reaction tank bottom
Enter.
3. the final regulation of pH value
Complete to ensure calcium ions and magnesium ions precipitation, the mixture from second reactor enters the 3rd reaction tank 11 from bottom, while the alkali of 4mol/l
Liquid also adds alkali mouth 12 to add from bottom by pipeline, and acidometer monitors which to more than pH=12, and now calcium ions and magnesium ions precipitation is complete, final suspension from
Discharging opening 13 overflows.
4. the subsequent treatment of pulpous state magnesium hydroxide
From the suspension Jing of the 3rd reaction tank spilling appropriate sedimentation (about half an hour sedimentation is complete), supernatant is bled off, pulpous state magnesium hydroxide is centrifuged,
And washed by solid-to-liquid ratio 1: 1, in order that magnesium hydroxide is easily dried, the hydrogen peroxide of 5% addition 30% during washing by the washing water yield makes which solid
Body constitution in vain and formed it is cellular be easy to rapid draing, be finally dried, crush, packing and to obtain finished product magnesium hydroxide.
What this patent was implemented it is critical only that substep controls the pH value of suspension, and using jet mixing arranged side by side, ring-shaped charging is mixed with spraying plus alkali, prevented
Local concentration is too high or too low, so as to further control the crystallization rate of magnesium hydroxide so that magnesium hydroxide is easily filtered, 5% (body is added during washing
Product ratio) hydrogen peroxide can make that magnesium hydroxide is loose porous to be easy to rapid draing.
Description of the drawings
In order to be better understood upon the practicality of this patent, three kinds of case study on implementation of this patent are described below
The whole process schematic diagram that accompanying drawing is provided for this patent.In above-mentioned figure：(1) jet mixer；(2) first reaction tanks；(3) first reaction tanks enter
Material mouth；(4) acidometer；(5) agitator：(6) first reaction tank overfalls；(7) second reaction tanks；(8) ring pipe；(9) spray nozzle；
(10) second reaction tank discharging openings；(11) the 3rd reaction tanks；(12) the 3rd reaction tanks add alkali mouth；(13) the 3rd reaction tank discharging openings.
Specific embodiment：
Specific embodiment 1：
A kind of flow process of specific embodiment that Fig. 1 is provided for this patent, prepares 20 liters of the solution of magnesium ion concentration about 5g/l with magnesium chloride, with 4mol/l
Sodium hydroxide solution the first reaction tank is entered by jet mixer side by side, by the pH value of the whole suspension of the flow-control for adjusting the two 9
Hereinafter, the time of staying more than 2 minutes；Fed by ring pipe in second reaction tank, playpipe adds vaporific sodium hydroxide and is stirred continuously, controlled
Whole suspension pH 10.5 or so, more than the 2 minutes time of staying；Into after the 3rd reaction tank by plus alkali control ph more than 12, magnesium
Ion sedimentation is complete, discharges the appropriate sedimentations of suspension Jing (about half an hour sedimentation is complete) from upper end overfall, bleeds off supernatant, pulpous state hydroxide
Magnesium centrifugation is filtered with MINI200 types desk centrifuge, and 4min is filtered and finished, and is washed by solid-to-liquid ratio 1: 1, in order that magnesium hydroxide holds
Easily be dried, make its solid matter white by the hydrogen peroxide of 5% addition 30% of the washing water yield during washing and formed it is cellular be easy to rapid draing, be finally dried,
Crush to obtain finished product magnesium hydroxide 226.8g.
Specific embodiment 2：
A kind of flow process of specific embodiment that Fig. 1 is provided for this patent, prepares 50 liters of the solution of magnesium ion concentration about 10g/l with magnesium chloride, with 4mol/l
Sodium hydroxide solution the first reaction tank is entered by jet mixer side by side, by the pH value of the whole suspension of the flow-control for adjusting the two 9
Hereinafter, the time of staying more than 2 minutes；Fed by ring pipe in second reaction tank, playpipe adds vaporific sodium hydroxide and is stirred continuously, controlled
Whole suspension pH 10.5 or so, more than the 2 minutes time of staying；Into after the 3rd reaction tank by plus alkali control ph more than 12, magnesium
Ion sedimentation is complete, discharges the appropriate sedimentations of suspension Jing (about half an hour sedimentation is complete) from upper end overfall, bleeds off supernatant, pulpous state hydroxide
Magnesium centrifugation is filtered with MINI200 types desk centrifuge, filters 5L pulpous state liquid every time, and 4min is filtered and finished (next round is refiltered after manual cleaning)
And washed by solid-to-liquid ratio 1: 1, in order that magnesium hydroxide is easily dried, the hydrogen peroxide of 5% addition 30% during washing by the washing water yield makes which
Solid matter in vain and formed it is cellular be easy to rapid draing, finally be dried, crush to obtain finished product magnesium hydroxide 1.93kg.
Specific embodiment 3：
A kind of flow process of specific embodiment that Fig. 1 is provided for this patent, prepares 50 liters of the solution of magnesium ion concentration about 30g/l with magnesium chloride, with 4mol/l
Sodium hydroxide solution the first reaction tank is entered by jet mixer side by side, by the pH value of the whole suspension of the flow-control for adjusting the two 9
Hereinafter, the time of staying more than 2 minutes；Fed by ring pipe in second reaction tank, playpipe adds vaporific sodium hydroxide and is stirred continuously, controlled
Whole suspension pH 10.5 or so, more than the 2 minutes time of staying；Into after the 3rd reaction tank by plus alkali control ph more than 12, magnesium
Ion sedimentation is complete, discharges the appropriate sedimentations of suspension Jing (about half an hour sedimentation is complete) from upper end overfall, bleeds off supernatant, pulpous state hydroxide
Magnesium centrifugation is filtered with MINI200 types desk centrifuge, filters 5L pulpous state liquid every time, and 4min is filtered and finished (next round is refiltered after manual cleaning)
And washed by solid-to-liquid ratio 1: 1, in order that magnesium hydroxide is easily dried, the hydrogen peroxide of 5% addition 30% during washing by the washing water yield makes which
Solid matter in vain and formed it is cellular be easy to rapid draing, finally be dried, crush to obtain finished product magnesium hydroxide 3.52kg.
Claims (3)
1. a kind of method and apparatus for preparing magnesium hydroxide, it is characterised in that the stepwise reaction under control ph, mixes feed way, magnesium hydroxide
Washing so that the magnesium hydroxide of generation is easily filtered, is easily dried.
2. the method and apparatus for preparing magnesium hydroxide according to claim 1, it is characterised in that feed side by side and monitor by jet mixer first
Its pH value is less than 9, and further reaction promotes mix homogeneously and keeps pH value 10.5 or so by spraying plus alkali, and gained magnesium hydroxide is easy
In filtration.
3. the method and apparatus for preparing magnesium hydroxide according to claim 1, it is characterised in that add 5% (volume ratio) during washing magnesium hydroxide
Hydrogen peroxide (30%) so that hydroxide is magnesia white, loose porous, is easily dried.
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| CN201510662980.6A CN106564918B (en) | 2015-10-13 | 2015-10-13 | A kind of method for preparing magnesium hydroxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307290A (en) * | 2021-05-20 | 2021-08-27 | 青海盐湖工业股份有限公司 | Agglomerated large-particle-size magnesium hydroxide and preparation method thereof |
| CN114804163A (en) * | 2022-05-16 | 2022-07-29 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by wet dechlorination of industrial-grade magnesium hydroxide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02279515A (en) * | 1989-04-18 | 1990-11-15 | Naikai Engiyou Kk | Superfine granular magnesium hydroxide and its production |
| JP2007137694A (en) * | 2005-11-15 | 2007-06-07 | Ube Material Industries Ltd | Magnesium hydroxide fine power dispersion and method for producing the same |
| CN101125669A (en) * | 2007-07-13 | 2008-02-20 | 马敬环 | Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water |
| CN102417196A (en) * | 2011-09-16 | 2012-04-18 | 沈阳化工大学 | Production method of fire retardant type magnesium hydroxide |
| CN103101936A (en) * | 2013-01-31 | 2013-05-15 | 辽宁红豆杉技术发展有限公司 | Method for preparing magnesium hydrate through ammonia spray method |
| CN204310827U (en) * | 2014-12-10 | 2015-05-06 | 巩义市强宏镁业科技有限责任公司 | High purity magnesium hydrate micronizer mill |
-
2015
- 2015-10-13 CN CN201510662980.6A patent/CN106564918B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02279515A (en) * | 1989-04-18 | 1990-11-15 | Naikai Engiyou Kk | Superfine granular magnesium hydroxide and its production |
| JP2007137694A (en) * | 2005-11-15 | 2007-06-07 | Ube Material Industries Ltd | Magnesium hydroxide fine power dispersion and method for producing the same |
| CN101125669A (en) * | 2007-07-13 | 2008-02-20 | 马敬环 | Method for producing high-pure ultra-thin micro-powder magnesium hydroxide by extracting sea water |
| CN102417196A (en) * | 2011-09-16 | 2012-04-18 | 沈阳化工大学 | Production method of fire retardant type magnesium hydroxide |
| CN103101936A (en) * | 2013-01-31 | 2013-05-15 | 辽宁红豆杉技术发展有限公司 | Method for preparing magnesium hydrate through ammonia spray method |
| CN204310827U (en) * | 2014-12-10 | 2015-05-06 | 巩义市强宏镁业科技有限责任公司 | High purity magnesium hydrate micronizer mill |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307290A (en) * | 2021-05-20 | 2021-08-27 | 青海盐湖工业股份有限公司 | Agglomerated large-particle-size magnesium hydroxide and preparation method thereof |
| CN113307290B (en) * | 2021-05-20 | 2023-03-21 | 青海盐湖工业股份有限公司 | Agglomerated magnesium hydroxide with large particle size and preparation method thereof |
| CN114804163A (en) * | 2022-05-16 | 2022-07-29 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by wet dechlorination of industrial-grade magnesium hydroxide |
| CN114804163B (en) * | 2022-05-16 | 2024-02-13 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by wet dechlorination of industrial magnesium hydroxide |
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