CN101723417B - Process for preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method - Google Patents
Process for preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method Download PDFInfo
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- CN101723417B CN101723417B CN2009102486831A CN200910248683A CN101723417B CN 101723417 B CN101723417 B CN 101723417B CN 2009102486831 A CN2009102486831 A CN 2009102486831A CN 200910248683 A CN200910248683 A CN 200910248683A CN 101723417 B CN101723417 B CN 101723417B
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Abstract
The invention provides a process for preparing high dispersivity square blocky superfine magnesium hydroxide by a one-step method, which relates to a process for preparing a chemical material. The process comprises the following steps of: taking magnesium chloride as a raw material; preparing solution of the magnesium chloride; reacting the solution of the magnesium chloride with ammonia gas passed in at a certain speed rate in a bubbling reactor with stirring; controlling the stirring speed and the reaction temperature; and after the reaction, performing constant temperature aging, filtration washing and drying on reaction solution to obtain incompact square blocky (hexahedral structure) superfine magnesium hydroxide powder. An ammonium salt in filtrate can be used for preparing the ammonia gas used in the process of magnesium deposition through ammonia evaporation reactions so as to realize ammonia circulation. The process realizes a technique for synthesizing a magnesium hydroxide fire retarding agent through the one-step method at the normal temperature under a condition that no auxiliary agent is used. Besides, the process has good product quality, needs no hydro-thermal treatment, has simple operating steps, less equipment occupied area, low production cost and small pollutant discharge amount, and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of chemical materials preparation technology, particularly relate to the novel process that a kind of single stage method prepares high dispersivity square blocky superfine particle flame retardant of magnesium hydroxide.
Background technology
Along with fast development and widespread use that macromolecular material is produced, its inflammableness also causes people's attention day by day.For solving the fire-retardant of macromolecular material and pressing down the cigarette problem, people develop flame retardant products such as halogen system, phosphorus system and metal inorganic fire retardant.Though the good flame retardation effect of halogen system, phosphorus flame retardant can produce poisonous and corrosive gases when burning, so its application is restricted more and more.Magnesium hydroxide (MH) is as a kind of " environmental protection " type inorganic combustion inhibitor, have non-volatile, burn into does not produce toxic gas, the decomposition temperature height, press down advantages such as the cigarette ability is strong, at home and abroad obtain developing rapidly and generally pay attention to, and be used for the fire-retardant of macromolecular materials such as electric wire, cable, polyvinyl chloride, polystyrene on a large scale.
Yet the coventional type magnesium hydroxide also has many shortcomings as fire retardant: poor with the superpolymer consistency, heavy addition easily makes its processing characteristics and quality product reduce in substrate material.For improving its performance, the super-refinement of magnesium hydrate powder, crystal formation homogenization, particle size distribution homogenizing are main developing direction.Though at present the domestic and international flame retardant of magnesium hydroxide preparation technology who reports is updating, but still do not break away from that normal temperature is synthetic, hydrothermal treatment consists, surface modification three-steps process.Remain, shortcomings such as temperature and pressure higher, product production little, production cost height long in flow process.The present invention is exactly the deficiency that exists at traditional technology, and proposes a kind of more rational processing method, thereby solution technical process complexity, energy consumption height, the product particle particle diameter is big, size-grade distribution is inhomogeneous, the uneven first-class problem of crystal formation.
Summary of the invention
The object of the present invention is to provide the technology of preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method.Adopt that this method production cost is low, process realizes easily, quality product is high; Can obtain the reaction mass ammonia from heavy magnesium filtrate by the ammonia still process process simultaneously,, reach the effect that reduces cost, reduces pollutant emission so that reaction mass ammonia recycles.
The objective of the invention is to be achieved through the following technical solutions:
The technology of preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, this process using magnesium chloride is raw material, wiring solution-forming and carries out vigorous stirring, again solution is joined in the bubbling style reactor and heat, the precipitation agent ammonia then is passed in this reaction solution with the bubbling form, obtain the block hexahedron structure magnesium hydrate powder in fine four directions of polymolecularity through reaction, ageing and filtration washing and drying treatment, the ammonium salt in the filtrate is used for the magnesium precipitate reaction of back by the ammonia still process reaction to reclaim ammonia.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, reactant ammonia directly enter reaction system and magnesium chloride solution reaction in gas bubbling mode, are settled out magnesium hydroxide products.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, heavy reactive magnesium temperature is 70 ℃～90 ℃, and magnesium chloride solution concentration is 1.0～2.0mol/L, and the reaction times is 2～3h.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, the magnesium hydroxide products particle of preparation are the close cubic block hexahedron structure of the length of side, are the flame-retardant additive of macromolecular material.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, the magnesium hydroxide products grain graininess of preparation is even, laser particle size distribution instrument test average grain footpath D
50Be 0.3～1.0 μ m; The XRD test I
001/ I
101Be 0.8～1.5.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, surfactant-free auxiliary agent, sintetics need not to handle and successive processes production through water-heat process in the heavy reactive magnesium.
The technology of described preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method filters out the ammonia that ammonium salt in the filtrate behind the magnesium hydroxide products is further used for the ammonia still process reaction process and recycles.
Advantage of the present invention and effect are:
1. adopting ammonia is reaction mass, and reaction after product mother liquor filters, washing is all easy, and magnesium hydroxide products purity is very high.
2. employing bubbling bed reactor, ammonia directly feeds magnesium chloride solution by the bubbling mode, thus optimizing reaction system macroscopic view and microcosmic mixed effect.
3. obtained product is four directions block (hexahedron structure), and the particle crystal formation is full, homogeneous and good dispersity, and specific surface area is less than the hexagonal flake particle (octahedral structure) with particle diameter.Product particle epigranular (narrow distribution range), median size D
50Less than 1.0 μ m, the largest particle footpath is less than 10.0 μ m.
4. next step is finished to be reflected at relatively mild temperature (being lower than 100 ℃) and pressure (being normal pressure substantially) condition, need not hydrothermal treatment consists, do not need to have used the auxiliary agent (as surface-modifying agent) of regulating the effect of product crystal formation, operation steps is simple, easy realization of required equipment and floor space are few, and can be good at controlling diameter of particle distribution and crystal formation.In reaction process, do not use surface-modifying agent, thereby reduce production costs and external environmental.
5. utilize the ammonia still process process to reclaim ammonia and realize the ammonia circulation, further improved the economic benefit of this technology, reduce pollutant emission from product filtrate.
6. the technology of the present invention's exploitation can single stage method be synthesized the fire-retardant formulation MH product of high quality, and operation steps is simple, and required equipment and floor space are few, and facility investment and productive expense are low, and pollutant discharge amount is few, is suitable for scale production.
Description of drawings
Fig. 1 of the present invention is the block shape synoptic diagram in magnesium hydrate powder particle four directions;
Fig. 2 of the present invention is for introducing magnesium hydrate powder particle hexagonal flake shape synoptic diagram;
Fig. 3 of the present invention is that the magnesium hydroxide products particle characterizes under the present technique condition, SEM photo (amplifying 1500 times);
Fig. 4 of the present invention is that the magnesium hydroxide products particle characterizes under the present technique condition, SEM photo (amplifying 10000 times);
Fig. 5 of the present invention is that the magnesium hydroxide products particle characterizes under the present technique condition, size distribution curve figure;
Fig. 6 of the present invention is that the magnesium hydroxide products particle characterizes under the present technique condition, the XRD graphic representation.
Annotate: accompanying drawing of the present invention is Product Status (result's) aid illustration figure, the whether clear the understanding of the present invention that do not influence of function and photo among the figure.
Embodiment
The present invention at first is made into magnesium chloride certain density solution, join in the bubbling style reactor and fully and directly feed ammonia by certain vapour-liquid ratio in the bubbling mode under the stirring state, control reaction temperature is sunk reactive magnesium in certain limit, reaction certain hour and reacting liquid pH value are about 9.5, filter, wash behind constant temperature ageing 0.5～4h and drying obtains free-running property four directions block superfine magnesium hydroxide powder (hexahedron structure).Ammonium salt can be used for the ammonia still process reaction in the filtrate, thereby ammonia recycles.
It is raw material that the present invention adopts magnesium chloride, is made into certain concentration solution and carries out vigorous stirring.Join above solution in the bubbling style reactor and be heated to certain temperature, the precipitation agent ammonia then is passed in this reaction solution with the bubbling form, obtain block (hexahedron structure) magnesium hydrate powder in fine four directions of polymolecularity through reaction, ageing and filtration washing and drying treatment, the ammonium salt in the filtrate can be used for the magnesium precipitate reaction of back to reclaim ammonia by the ammonia still process reaction.The reactant ammonia directly enters reaction system and magnesium chloride solution reaction in gas bubbling mode, is settled out magnesium hydroxide products.Heavy reactive magnesium temperature is 70 ℃～90 ℃, and magnesium chloride solution concentration is 1.0～2.0mol/L, and the reaction times is 2～3h.The magnesium hydroxide products particle of preparation is block (hexahedron structure is as the signal of accompanying drawing 1) rather than common hexagonal flake (octahedral structure is as the signal of accompanying drawing a 2) body of the close four directions of the length of side, and product can be used as the flame-retardant additive of macromolecular material.The magnesium hydroxide products grain graininess of preparation is even, laser particle size distribution instrument test average grain footpath D
50Be 0.3～1.0 μ m; The product particle good dispersity, the XRD test I
001/ I
101Be 0.8～1.5.Need not to use auxiliary agent, sintetics such as tensio-active agent also to need not to handle through water-heat process again in the heavy reactive magnesium, thereby reduce production costs, reduce production stage and can realize successive processes production.Filter out ammonium salt in the filtrate behind the magnesium hydroxide products and can be further used for the ammonia still process reaction realizing the ammonia recycle of whole process, thereby do not have ammonia consumption, non-pollutant discharge in theory.
Embodiment one
The purified magnesium chloride solution of configuration 1.0mol/L, getting this solution 500mL adding volume is in the bubbling style reactor of 2000mL, the interior solution of stirred reactor is also controlled its temperature in 70 ℃, ammonia is directly fed reaction solution with the bubbling form sink reactive magnesium, ammonia flow is 0.20g/min, 70 ℃ of isothermal reaction 2h reacting liquid pH values are about 9.5, obtain the oyster white suspension liquid of magnesium hydroxide and ammonium salt.70 ℃ of constant temperature ageings of product solution 2h, vacuum filtration ageing after product liquid, filter cake with behind the deionized water wash 3 times under 80 ℃ of conditions vacuum-drying 12h, obtain the block superfine magnesium hydroxide powder in crystallization degree good free-running property four directions.Filtrate is returned ammonia steaming device, and replenishes an amount of magnesium source, cyclical operation.
Embodiment two
The purified magnesium chloride solution of configuration 2.0mol/L, getting this solution 500mL adding volume is in the bubbling style reactor of 2000mL, the interior solution of stirred reactor is also controlled its temperature in 90 ℃, ammonia is directly fed reaction solution with the bubbling form sink reactive magnesium, ammonia flow is 0.50g/min, 90 ℃ of isothermal reaction 3h reacting liquid pH values are about 9.5, obtain the oyster white suspension liquid of magnesium hydroxide and ammonium salt.70 ℃ of constant temperature ageings of product solution 1h, vacuum filtration ageing after product liquid, filter cake with behind the deionized water wash 3 times under 80 ℃ of conditions vacuum-drying 12h, obtain the block superfine magnesium hydroxide powder in crystallization degree good free-running property four directions, average diameter of particles D
50Be about 0.7 μ m, maximum particle diameter (second particle) is less than 5.0 μ m.
Claims (2)
1. the technology of preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method, it is characterized in that: this process using magnesium chloride is a raw material, be made into the magnesium chloride solution that concentration is 1.0～2.0mol/L and carry out vigorous stirring, again solution is joined in the bubbling style reactor and heat, the precipitation agent ammonia then is passed in this reaction solution with the bubbling form, heavy reactive magnesium temperature is 70 ℃～90 ℃, reaction times is 2～3h, through reaction, ageing and filtration washing and drying treatment obtain the block hexahedron structure magnesium hydrate powder in fine four directions of polymolecularity, and the ammonium salt in the filtrate is used for the magnesium precipitate reaction of back with the recovery ammonia by the ammonia still process reaction.
2. the technology of preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method as claimed in claim 1, it is characterized in that: the magnesium hydroxide products grain graininess of preparation is even, laser particle size distribution instrument test average grain footpath D
50Be 0.3～1.0 μ m; The XRD test I
001/ I
101Be 0.8～1.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2801733C1 (en) * | 2023-03-15 | 2023-08-15 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extraction of magnesium hydroxide from polycomponent hydromineral raw |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502725A (en) * | 2011-10-28 | 2012-06-20 | 中国科学院过程工程研究所 | Method for producing flame-retardant magnesium hydroxide |
| CN102807238B (en) * | 2012-08-24 | 2014-04-02 | 中国科学院青海盐湖研究所 | Method for preparing spherical magnesium hydroxide |
| CN104071804A (en) * | 2014-07-08 | 2014-10-01 | 中国科学院青海盐湖研究所 | Method for preparing ammonium chloride |
| CN104495883A (en) * | 2014-12-02 | 2015-04-08 | 中国科学院青海盐湖研究所 | Preparation method of magnesium hydrate with high-concentration slurry |
| CN107500351A (en) * | 2017-07-24 | 2017-12-22 | 沈阳化工大学 | A kind of preparation method of zirconium hydroxide |
| CN107758706A (en) * | 2017-09-25 | 2018-03-06 | 沈阳化工大学 | One-step method prepares cubic pieces flame retardant of magnesium hydroxide process |
| CN110240184A (en) * | 2019-05-25 | 2019-09-17 | 邢台镁熙环保材料有限公司 | A kind of production technology of high-purity Nano-class magnesia |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2801733C1 (en) * | 2023-03-15 | 2023-08-15 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extraction of magnesium hydroxide from polycomponent hydromineral raw |
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