CN102060314B - Preparation method for synthesizing platy flame-retardant magnesium hydroxide by using light burned magnesia powder - Google Patents
Preparation method for synthesizing platy flame-retardant magnesium hydroxide by using light burned magnesia powder Download PDFInfo
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- CN102060314B CN102060314B CN2010105659394A CN201010565939A CN102060314B CN 102060314 B CN102060314 B CN 102060314B CN 2010105659394 A CN2010105659394 A CN 2010105659394A CN 201010565939 A CN201010565939 A CN 201010565939A CN 102060314 B CN102060314 B CN 102060314B
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Abstract
The invention relates to a preparation method for synthesizing platy flame-retardant magnesium hydroxide by using light burned magnesia powder. The method comprises the following steps of: preparing MgSO4 solution from light burned magnesia serving as a magnesium ion providing source by using sulfuric acid, filtering to remove impurities, controlling the ratio of [NH3.H2O] to [Mg<2+>] to be 1.5-1 and the ratio of [OH<->] to the [Mg<2+>] to be 2-1.5 by using ammonia water and NaOH solution as precipitating agents, and synthesizing the platy flame-retardant magnesium hydroxide by a two-step method, wherein the temperature of the ammonia water precipitating stage is between 50 and 60 DEG C, the temperature of the NaOH solution precipitating stage is between 120 and 160 DEG C, and the hydrothermal reaction time is 2 to 10 hours. The obtained platy magnesium hydroxide has the primary particle size of 0.5 to 1mu m and the magnesium hydroxide content of over 97 percent. The method is low in cost and high in added value; the prepared magnesium hydroxide has high purity, a stable structure and narrow particle size distribution; and a good way is provided for highly utilizing magnesium hydroxide and even magnesite resources. The magnesium hydroxide product prepared by the method can be used as a flame retardant in the industries of rubber, plastic, electric wires and cables, building materials and the like.
Description
Technical field
The present invention relates to a kind of preparation method of sheet flame-proof magnesium hydroxide, being specifically related to a kind of light-magnesite powder that adopts is that magnesium source, ammoniacal liquor and sodium hydroxide are the method for preparing the sheet flame-proof magnesium hydroxide of precipitation agent, belongs to technical field of inorganic chemical industry.
Background technology
China has abundant magnesite resource; Wherein the proven reserve of magnesite resource in Liaoning Province reach 3,000,000,000 tons; Magnesite is widely used as the raw material of refractory materials, is respectively applied for preparation light calcined magnesia, heavy burned magnesium oxide and electric molten magnesite, and is used to prepare various magnesium salts on a small quantity.But, the utilization of magnesite is all existed get the poor problem of rich house for many years, and in recovery process, produce the fine ore of quantity huge (accounting for the 25%-35% of extracted ore).Just utilize the maximum light calcined magnesia of magnesite production; Present stage, the economic value added of product was very low; And produce and also can produce the discarded powder of partially oxidation magnesium in the process of other magnesium Chemicals; Therefore be badly in need of developing a kind of novel method that can improve the light-magnesite powder economic worth, thus the magnesium Chemicals of production high added value.
Along with the development of macromolecular materials such as plastics, rubber, synthon production and the expansion of Application Areas thereof, its inflammableness also causes people's attention day by day.Especially when macromolecular material and electrical equipment are used in combination (like plastic products such as electric wires), owing under conditions such as high pressure, heating, discharge, work, the initiation fire that burns easily produces a large amount of smog and toxic gas simultaneously, causes damage to property and casualties.People work out anti-combustion and but the cigarette problem that various fire retardants solve macromolecular material for this reason.Marinco H has flame-retardant smoke inhibition, thermostability high (decomposition temperature is 340～490 ℃), characteristics such as nontoxic, especially is fit to polymkeric substance such as the PP higher with processing temperature, PA, POM and is used.Therefore, in various magnesium products, the research and development of high-performance, high added value Marinco H are just becoming the focus of attention both domestic and external.The most size-grade distribution of prior oxyhydrogen magnesium products is wide, agglomeration is serious, purity low (Marinco H content is lower than 90～96%), makes its price cheap, and application surface is limited; And added value is higher, the market requirement increases faster that high-purity lamellar magnesium hydroxide fire retardant output is very little, causes the required high-performance flame retardant of magnesium hydroxide of industry such as plastics, rubber, electric wire, forms a sharp contrast with a large amount of idle magnesium resource present situations.
Because Marinco H is the very strong mineral compound of a kind of surface polarity; Its plane of crystal possess hydrophilic property; And normal temperature condition adopts traditional technology synthetic Marinco H surface polarity stronger down, and the formation particle diameter that is easy to reunite is the offspring of 10-100 μ m, has very big surface-area; Dispersiveness and consistency are all relatively poor when directly adding in the superpolymer, influence the processing characteristics of matrix material.In order to prepare dispersiveness Marinco H preferably, it is structurally-modified to adopt suitable process means that normal temperature synthetic Marinco H is carried out, to reduce crystalline microstress and surface polarity, the preparation high purity magnesium hydroxide product that specific surface area is little, particle diameter is moderate.
Summary of the invention
A kind of method of producing flame-proof magnesium hydroxide with light-magnesite powder that the objective of the invention is to be directed against the existing lower situation of magnesite resource utility value and design; This method has improved the economic use value of light-magnesite powder largely; And sheet flame-proof magnesium hydroxide purity height, Stability Analysis of Structures, the filtration of producing are easy, simple to operate, are easy to suitability for industrialized production.
Concrete step of preparation process is following:
(1) adopting MgO content is raw material in the light-magnesite powder more than 97%, with deionized water it is made into the i.e. [Mg of magnesium ion concentration
2+] be the slip of 1.2～2.0mol/L, under whipped state to wherein adding certain amount of H
2SO
4(control magnesium source slip and H
2SO
4Volume ratio be about 8: 1～10: 1), continue to stir 30～90min, temperature is controlled at 30～50 ℃, promptly makes MgSO
4Solution.
(2) pour in the reactor drum filtrating and to the X 2073 that wherein adds reasonable opinion Marinco H output 0.1%～0.5% after the magnesium source solution that makes in the step 1 is filtered; Controlled temperature is 50～60 ℃; Mixing speed is 200～500r/min, earlier with ammoniacal liquor according to [NH
3H
2O]/[Mg
2+]=1.5～1 ([Mg here
2+] be the magnesium ion concentration in the solution of magnesium source) and ratio add in the reactor drum and react 10～20min, then with NaOH solution according to [OH
-]/[Mg
2+]=2～1.5 ([OH here
-] be merely [OH in the NaOH solution
-], [Mg
2+] be the magnesium ion concentration in the solution of magnesium source) and ratio add in the reactor drum and react 10～20min, promptly get rough Mg (OH)
2Slip suspension-s.
(3) with the Mg that makes in the step 2 (OH)
2Slip is transferred in the reaction kettle and reacts 2～10h at 120～160 ℃, promptly gets and makes with extra care Mg (OH)
2Slip.
(4) with the Mg (OH) that makes in the step (3)
2Promptly get the sheet flame-proof magnesium hydroxide after slurry filtration, washing, the drying.
Above-mentioned ammonia precipitation process stage [Mg
2+] excessive relatively, and NaOH solution precipitation stage [OH
-] excessive relatively.
It is that mg ion provides the source that the present invention adopts light calcined magnesia, is made into MgSO with a certain amount of sulfuric acid earlier
4Solution, filtering and impurity removing matter, utilize ammoniacal liquor and NaOH solution as precipitation agent then, two-step approach synthesizing flaky flame-proof magnesium hydroxide: the first step, with MgSO
4Solution and ammoniacal liquor carry out the normal temperature mix stages, and this process is because [Mg
2+] being in excessive state basically, the nucleation rate of Marinco H is much larger than its growth velocity, so produce a large amount of Marinco H nucleus; In second step, the magnesium magma that the first step is made places reaction kettle, and adds suitably excessive sodium hydroxide solution, and this moment, reaction system was in [OH
-] the high and [Mg of content
2+] state that content is low; So the growth velocity of Marinco H is much larger than its nucleation rate; The flake magnesium hydroxide that fits to should have lower polarity, can make with other organic materialss such as macromolecule resin etc. to have better consistency, has higher industrial application value.
Unusual effect of the present invention is: utilize light-magnesite powder to prepare the sheet flame-proof magnesium hydroxide, well improved the utility value of light-magnesite powder and even magnesite resource, widen its Application Areas; Adopt ammonia process and sodium hydroxide to send out and combine and preparation flame-proof magnesium hydroxide under hydrothermal condition; Both overcome that size distribution broad and the yield of ammonia process process products is on the low side to cause the shortcoming of the Marinco H particle diameter filtration difficulty less than normal of generation easily with sodium hydroxide method, obtained higher, the better dispersed and all controllable Marinco H title product of its pattern, structure and size of productive rate.
Embodiment
Embodiment one:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to the H that wherein adds 5mL49%
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution.
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min earlier, add the NaOH solution 40mL of 2.4mol/L afterwards; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 160 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
Embodiment two:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to the H that wherein adds 4.7mL49%
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution.
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min earlier, add the NaOH solution 40mL of 2.4mol/L afterwards; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 160 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
Embodiment three:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to the H that wherein adds 5mL49%
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution.
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min earlier, add the NaOH solution 25mL (being diluted to 40mL) of 2.4mol/L afterwards with deionized water; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 120 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
Embodiment four:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to the H that wherein adds 5mL49%
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution.
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min earlier, add the NaOH solution 40mL of 2.4mol/L afterwards; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 120 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
Claims (6)
1. preparation method who adopts light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide, concrete step of preparation process is following:
(1) adopting MgO content is raw material in the light-magnesite powder more than 97%, with deionized water it is made into the i.e. [Mg of magnesium ion concentration
2+] be the slip of 1.2mol/L, under whipped state to wherein adding a certain amount of 49%H
2SO
4, control magnesium source slip and 49%H
2SO
4Volume ratio be about 8: 1, continue to stir 30～90min, temperature is controlled at 30～50 ℃, promptly makes MgSO
4Solution;
(2) with the MgSO that makes in the step 1
4Pour into filtrating in the reactor drum after solution filters and to the X 2073 that wherein adds reasonable opinion Marinco H output 0.5%, controlled temperature is 50～60 ℃, mixing speed is 200～500r/min, earlier with ammoniacal liquor according to [NH
3H
2O]/[Mg
2+The ratio of]=1.5～1 adds in the reactor drum reacts 10～20min, then with NaOH solution according to [OH
-]/[Mg
2+The ratio of]=2～1.5 adds in the reactor drum reacts 10～20min, promptly gets rough Mg (OH)
2Slip suspension-s;
(3) with the Mg that makes in the step 2 (OH)
2Slip is transferred in the reaction kettle and reacts 2～10h at 120～160 ℃, promptly gets and makes with extra care Mg (OH)
2Slip;
(4) with the Mg that makes in the step 3 (OH)
2Promptly get the sheet flame-proof magnesium hydroxide after slurry filtration, washing, the drying.
2. the preparation method of employing light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide as claimed in claim 1 is characterized in that: ammonia precipitation process stage [Mg
2+] excessive relatively, and NaOH solution precipitation stage [OH
-] excessive relatively.
3. preparation method who adopts light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide is characterized in that concrete step of preparation process and technical qualification:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to wherein adding 5mL 49%H
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution;
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min then, add the NaOH solution 40mL of 2.4mol/L at last; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 160 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
4. preparation method who adopts light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide is characterized in that concrete step of preparation process and technical qualification:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to wherein adding 4.7mL 49%H
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution;
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min then, add the NaOH solution 40mL of 2.4mol/L at last; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 160 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
5. preparation method who adopts light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide is characterized in that concrete step of preparation process and technical qualification:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to wherein adding 5mL 49%H
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution;
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min then, add the NaOH solution 25mL (being diluted to 40mL) of 2.4mol/L at last with deionized water; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 120 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
6. preparation method who adopts light-magnesite powder synthesizing flaky flame-proof magnesium hydroxide is characterized in that concrete step of preparation process and technical qualification:
Take by weighing the 1.98g light-magnesite powder and pour in the beaker, be positioned in the magnetic force heating stirrer after in beaker, adding the 36mL deionized water, controlled temperature is 30 ℃, and mixing speed is 200r/min, stirs behind the 2min to wherein adding 5mL 49%H
2SO
4, continue stirring reaction 30min and promptly get rough MgSO
4Solution;
With common funnel with rough MgSO
4Solution is filtered in the there-necked flask, and after treating to filter fully, the temperature of adjustment magnetic force heating stirrer is 58 ℃; Mixing speed is 200r/min; To the ammoniacal liquor that wherein adds 20mL2%, dropwise back sustained reaction 10min then, add the NaOH solution 40mL of 2.4mol/L at last; Sustained reaction 10min again after dropwising promptly tentatively makes Mg (OH)
2Slip is then with Mg (OH)
2Slip is transferred in the reaction kettle, and temperature is controlled to be 120 ℃ of hydro-thermal reaction 6h, and is last, will make Mg (OH)
2The slip suction filtration, be drying to obtain sheet flame-proof magnesium hydroxide product.
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| CN2010105659394A CN102060314B (en) | 2010-11-30 | 2010-11-30 | Preparation method for synthesizing platy flame-retardant magnesium hydroxide by using light burned magnesia powder |
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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 |
| CN102491380A (en) * | 2011-12-06 | 2012-06-13 | 中国科学院过程工程研究所 | Method for preparing flaky magnesium hydroxide |
| CN103613108B (en) * | 2013-12-02 | 2015-11-18 | 沈阳化工大学 | A kind of ammonia legal system is for the method for flame retardant of magnesium hydroxide |
| CN107128962B (en) * | 2017-05-04 | 2018-07-20 | 四川理工学院 | A kind of preparation method of nano-sized magnesium hydroxide |
| CN111017968A (en) * | 2019-12-27 | 2020-04-17 | 河北邢台冶金镁业有限公司 | Method for preparing pure magnesium sulfate by using light burned bitter soil as raw material without adding any impurity removing agent |
| CN111302672B (en) * | 2020-04-13 | 2021-11-19 | 鞍山盈丰新材料科技有限公司 | Processing raw material of fused magnesia and preparation method thereof |
| CN113881445A (en) * | 2021-09-29 | 2022-01-04 | 白银康宝新型节能建材有限责任公司 | Preparation method of magnesium-based flame-retardant material |
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| JPS55104994A (en) * | 1979-01-30 | 1980-08-11 | Kyowa Chem Ind Co Ltd | Manufacture of fibrous magnesium hydroxide |
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Effective date of registration: 20160621 Address after: Faku Economic Development Zone in Shenyang city of Liaoning Province in 110400 Patentee after: Liaoning Faku County Ceramic Engineering Technology Research Center Address before: Faku Economic Development Zone in Shenyang city of Liaoning Province in 110400 Patentee before: Shenyang Xinjin Powder Engineering Co., Ltd. |
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