CN106564918B - A kind of method for preparing magnesium hydroxide - Google Patents
A kind of method for preparing magnesium hydroxide Download PDFInfo
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- CN106564918B CN106564918B CN201510662980.6A CN201510662980A CN106564918B CN 106564918 B CN106564918 B CN 106564918B CN 201510662980 A CN201510662980 A CN 201510662980A CN 106564918 B CN106564918 B CN 106564918B
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- magnesium hydroxide
- magnesium
- suspension
- lye
- hydroxide
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Abstract
The invention discloses a kind of method for preparing magnesium hydroxide, belongs to inorganic chemical industry material and prepares and purification field.Raw brine enters the first mixing preparation of jet mixer with lye and reacts side by side at room temperature first, and control ph is below 9；Secondly suspension enters ring pipe further with vaporific alkaline reaction and controlling its pH value 10.5 or so, reaction finishes the pH value for adjusting whole system more than 12, ensures that magnesium ion precipitation is complete.Gained suspension stands 30min, bleeds off supernatant, container bottom pulpous state magnesium hydroxide centrifugal filtration, during washing by washing water volume ratio 5% add 30% hydrogen peroxide, filtering, dry magnesium hydroxide finished product.A kind of disclosed method for preparing magnesium hydroxide can be used for the pretreatment of the factory or production of caustic soda factory of direct preparing magnesium hydroxide to calcium and magnesium in raw material, save filtration time, save drying cost.
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
It is widely applied in environmental protection, ceramic material, medicine and other fields.In recent years, since magnesium hydroxide has decomposition temperature height, heat
The features such as stability is good, nontoxic, smokeless and suppression cigarette, becomes a kind of important inorganic combustion inhibitor, enjoys researcher and production
The attention of person.
Production magnesium hydroxide mainly has two methods.One kind is the levigate method of shepardite, it is to be broken to brucite powder
150um, further air-flow crushing to 1-26um；Another kind is chemical synthesis, it is to utilize the bittern containing magnesium chloride, halogen
Ore deposit etc. is reacted with alkaloids in aqueous medium, generate magnesium hydroxide slurry, filtered, hydro-thermal process, washing, surface treatment,
Dry obtained magnesium hydroxide.Due to magnesium hydroxide generation particle it is extremely fine, formed sol system so that the filtering of slurry and
Washing becomes very difficult, so that time-consuming, water consumption, power consumption, cost remain high, seriously constrains the extensive raw of magnesium hydroxide
Production.
The filtering problem of magnesium hydroxide is faced, researcher have also been made extensive work.Guizhou University (Li Junqi, five rocs, Liu
It is bright, Yang Shuhuai, Kong Fanzhen, the research that several factors influence magnesium hydroxide slurry strainability, Guizhou University of Technology's journal,
2007,32-39) using magnesium chloride as raw material, sodium hydroxide is precipitating reagent, and hydrogen-oxygen is prepared using the method for adding magnesium hydroxide crystal seed
Change magnesium, have studied the influence of crystal seed coefficient, reaction temperature, reaction time to slurry filtration performance, and find by orthogonal test
Optimum reaction condition, preparing magnesium hydroxide to exploring sodium-hydroxide method has certain reference significance；China University of Geosciences (king
Put down, Du Gaoxiang, Li Fu, the influence flocculated to magnesium hydroxide slurry strainability and washing effect, chemical industry mineral and processing,
2008,20-22) flocculate by using polyacrylamide to super fine magnesium hydroxide slurry, increase magnesium hydroxide particle sedimentation
The method of speed improves the strainability of magnesium hydroxide slurry, at the same can also improve magnesium hydroxide slurry washing remove sodium from
The effect of son；(Li Xiaokun, closes the Yunshan Mountain, Yang Zhaojuan, He Zhifei, surface modifier is in super fine magnesium hydroxide filtering for Qinghai University
Application, inorganic chemicals industry, 2011,57-60) using odium stearate with water-soluble titanium phosphate ester coupling agent to super fine magnesium hydroxide
Wet modification experiment is carried out, strainability can be significantly improved both while the surface property of super fine magnesium hydroxide is improved；
Tsinghua University is (a kind of to prepare High-purity high-activity hydroxide by calcic magnesium hydroxide to orchid, Zhang Junping, Ji Yu, repercussions, Yi Meigui
The method of magnesium, CN104891534A, 2015) dispersant is added in calcic reunion state magnesium hydroxide, magnesium hydroxide is purified, is improved
Strainability.These effort play certain effect to producing, filtering magnesium hydroxide, but there is cost is higher, efficiency
, there is the necessity further improved in the problems such as relatively low very much.
The content of the invention
It is an object of the invention to the pre-treatment removing calcium and magnesium by-product for industrial production magnesium hydroxide or production of caustic soda factory bittern
Magnesium hydroxide improves production efficiency so that product is washable, easy filter.
To realize above-mentioned target, the technical solution adopted by the present invention is as follows：
1. the first mixing preparation of raw brine and lye：
The bittern of calcic, magnesium is mixed into incident flow side by side at room temperature with prepared concentration for the soda bath of 4mol/l
Clutch 1, and then enter first reaction tank 2, to make to be uniformly mixed, mixed solution is fed into first reaction tank from from bottom
Mouth 3 enters, and be stirred reaction by blender 5 (calculates suspension the bottom of from more than 2 minutes according to the volume of container and flowmeter
Portion to overfall time), the pH value of whole suspension is monitored below 9 by acidometer 4 while reaction, reaction finish from
Discharge gate 6 overflows.
2. suspension is further reacted with alkali：
The suspension of first reaction tank enters second reaction tank 7 after being overflowed by overflow port 6, and suspension initially enters ring
Shape pipe 8 feeds, at the same the lye of 4mol/l by spray nozzle 9 with vaporific addition, the two is stirred reaction, and reaction while leads to
Cross acidometer and monitor the pH value of whole suspension 10.5 or so, to ensure residence time of the suspension in reactor 2, second
Reaction tank discharge port 10 uses automatic control water level valve intermittent discharge mixed liquor, and discharge ensures that residual mixed liquor accounts for entirely when finishing
/ 3rd of reactor, reaction finish mixture and enter from the 3rd reaction tank bottom.
The final adjusting of 3.pH values
To ensure that calcium ions and magnesium ions precipitation is complete, the mixture from second reactor enters the 3rd reaction tank from bottom
11, while the lye of 4mol/l also adds alkali mouth 12 to add by pipeline from bottom, acidometer monitors it to more than pH=12, at this time
Calcium ions and magnesium ions precipitation is complete, and final suspension is overflowed from discharge port 13.
4. the subsequent treatment of pulpous state magnesium hydroxide
From the suspension that the 3rd reaction tank overflows through appropriate sedimentation (about half an hour settles complete), supernatant is bled off, is starched
Shape magnesium hydroxide centrifuges, and is washed by solid-to-liquid ratio 1: 1, in order to enable magnesium hydroxide is easily dried, when washing presses washings
The hydrogen peroxide that the 5% of the volume ratio of amount adds 30% make its solid matter white and formed it is cellular be easy to rapid draing, finally dry,
Crush, pack to obtain finished product magnesium hydroxide.
The key that this patent is implemented is that substep controls the pH value of suspension, using jet mixing arranged side by side, ring-shaped charging with
Spraying plus alkali mixing, prevent that local concentration is too high or too low, so as to further control the crystallization rate of magnesium hydroxide so that hydrogen
Magnesia is easily filtered, 5% adding 30% hydrogen peroxide and magnesium hydroxide can be made loose porous easy to fast by washing water during washing
Rapid-curing cutback is dry.
Brief 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
Attached drawing is the whole process schematic diagram that this patent provides.In above-mentioned figure：(1) jet mixer；(2) first reactions
Pond；(3) first reaction tank feed inlets；(4) acidometer；(5) blender：(6) first reaction tank overflow ports；(7) second reaction tanks；
(8) ring pipe；(9) spray nozzle；(10) second reaction tank discharge ports；(11) the 3rd reaction tanks；(12) the 3rd reaction tanks add alkali mouth；
(13) the 3rd reaction tank discharge ports.
Embodiment：
Specific embodiment 1：
Fig. 1 is a kind of flow for specific embodiment that this patent provides, and prepares magnesium ion concentration about 5g/l's with magnesium chloride
20 liters of solution, enters the first reaction tank by jet mixer side by side with the sodium hydroxide solution of 4mol/l, by adjusting the two
The whole suspension of flow control pH value below 9, more than 2 minutes residence time；Pass through ring pipe in second reaction tank
Charging, playpipe adds vaporific sodium hydroxide and is stirred continuously, and controls whole suspension pH 10.5 or so, 2 minutes residence times
More than；By adding alkali control ph more than 12 after into the 3rd reaction tank, magnesium ion sedimentation is complete, is discharged from upper end overflow port
Suspension bleeds off supernatant, MINI200 type platforms are used in the centrifugation of pulpous state magnesium hydroxide through appropriate sedimentation (about half an hour settles complete)
Formula centrifuge filters, and 4min filterings finish, and are washed by solid-to-liquid ratio 1: 1, in order to enable magnesium hydroxide is easily dried, washing
When 5% added 30% hydrogen peroxide by the volume ratio of washing water and make its solid matter white and formed cellular to be easy to fast rapid-curing cutback
Dry, finally drying, crush to obtain finished product magnesium hydroxide 226.8g.
Specific embodiment 2：
Fig. 1 is a kind of flow for specific embodiment that this patent provides, and prepares magnesium ion concentration about 10g/l's with magnesium chloride
50 liters of solution, enters the first reaction tank by jet mixer side by side with the sodium hydroxide solution of 4mol/l, by adjusting the two
The whole suspension of flow control pH value below 9, more than 2 minutes residence time；Pass through ring pipe in second reaction tank
Charging, playpipe adds vaporific sodium hydroxide and is stirred continuously, and controls whole suspension pH 10.5 or so, 2 minutes residence times
More than；By adding alkali control ph more than 12 after into the 3rd reaction tank, magnesium ion sedimentation is complete, is discharged from upper end overflow port
Suspension bleeds off supernatant, MINI200 type platforms are used in the centrifugation of pulpous state magnesium hydroxide through appropriate sedimentation (about half an hour settles complete)
Formula centrifuge filters, and filters 5L pulpous state liquid every time, and 4min filterings finish and (next round refiltered after manual cleaning) and by solid-to-liquid ratio 1
: 1 is washed, in order to enable magnesium hydroxide is easily dried, during washing by washing water volume ratio 5% add 30% it is double
Oxygen water make its solid matter white and formed it is cellular be easy to rapid draing, finally dry, crush to obtain finished product magnesium hydroxide 1.93kg.
Specific embodiment 3：
Fig. 1 is a kind of flow for specific embodiment that this patent provides, and prepares magnesium ion concentration about 30g/l's with magnesium chloride
50 liters of solution, enters the first reaction tank by jet mixer side by side with the sodium hydroxide solution of 4mol/l, by adjusting the two
The whole suspension of flow control pH value below 9, more than 2 minutes residence time；Pass through ring pipe in second reaction tank
Charging, playpipe adds vaporific sodium hydroxide and is stirred continuously, and controls whole suspension pH 10.5 or so, 2 minutes residence times
More than；By adding alkali control ph more than 12 after into the 3rd reaction tank, magnesium ion sedimentation is complete, is discharged from upper end overflow port
Suspension bleeds off supernatant, MINI200 type platforms are used in the centrifugation of pulpous state magnesium hydroxide through appropriate sedimentation (about half an hour settles complete)
Formula centrifuge filters, and filters 5L pulpous state liquid every time, and 4min filterings finish and (next round refiltered after manual cleaning) and by solid-to-liquid ratio 1
: 1 is washed, in order to enable magnesium hydroxide is easily dried, during washing by washing water volume ratio 5% add 30% it is double
Oxygen water make its solid matter white and formed it is cellular be easy to rapid draing, finally dry, crush to obtain finished product magnesium hydroxide 3.52kg.
Claims (2)
- A kind of 1. method for preparing magnesium hydroxide, it is characterised in that mix raw brine into jet mixer side by side with lye Close, then control ph will obtain suspension and add reaction tank by ring pipe, by lye by spray nozzle with mist below 9 Shape form adds, the two is stirred, and control suspension pH value is 10.5, in order to ensure that calcium ions and magnesium ions precipitate completely, further It is more than 12 to add lye control ph, and obtained magnesium hydrate precipitate is added hydrogen peroxide carries out carrying out washing treatment.
- 2. a kind of method for preparing magnesium hydroxide according to claim 1, it is characterised in that by washing during washing magnesium hydroxide Wash the 5% of the volume ratio of water and add the hydrogen peroxide that concentration is 30% so that hydroxide is magnesia white, loose porous, easily dry.
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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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| CN201510662980.6A CN106564918B (en) | 2015-10-13 | 2015-10-13 | A kind of method for preparing magnesium hydroxide |
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| CN106564918A CN106564918A (en) | 2017-04-19 |
| CN106564918B true CN106564918B (en) | 2018-04-17 |
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| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (2)
| 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 |
| JP5052780B2 (en) * | 2005-11-15 | 2012-10-17 | 宇部マテリアルズ株式会社 | Method for producing magnesium hydroxide fine particle dispersion |
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- 2015-10-13 CN CN201510662980.6A patent/CN106564918B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Granted publication date: 20180417 Termination date: 20211013 |