CN102502728B - Magnesium hydroxide flame retardant and preparation method thereof - Google Patents
Magnesium hydroxide flame retardant and preparation method thereof Download PDFInfo
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- CN102502728B CN102502728B CN201110307227.7A CN201110307227A CN102502728B CN 102502728 B CN102502728 B CN 102502728B CN 201110307227 A CN201110307227 A CN 201110307227A CN 102502728 B CN102502728 B CN 102502728B
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Abstract
The invention provides magnesium hydroxide flame retardant and a preparation method thereof. The preparation method of the magnesium hydroxide flame retardant comprises the following steps: adding magnesium chloride into a reactor to form magnesium chloride solution, and heating correspondingly to the set temperature T; adding composite precipitant formed by mixing calcium oxide, magnesium hydroxide, sodium hydroxide with water; continuing to carry out constant-temperature reaction at the set temperature T after finishing adding all the composite precipitant, and washing and filtering chloride ions in the filtering reactor; repulping a magnesium hydroxide filter cake; and finally, physically crushing the repulped magnesium hydroxide filter cake to obtain the magnesium hydroxide flame retardant. The magnesium hydroxide in the magnesium hydroxide flame retardant prepared by using the preparation method accounts for 99.0% or more.
Description
Technical field
The present invention relates to Chemicals field, relate in particular to a kind of preparation method of flame retardant of magnesium hydroxide and by the flame retardant of magnesium hydroxide of this preparation method's gained.
Background technology
Within 1907, there is synthetic polymer resol, indicate that the mankind apply the beginning of synthesized polymer material.At present, macromolecular material together with metallic substance, ceramic, becomes the important materials in science and technology and economic construction.Especially in recent decades, the polymer materialss such as plastics, rubber, synthon and goods thereof obtain flourish, they replace just rapidly the natural polymers such as traditional steel, metal, cement and timber, cotton, are widely used in each department of the national economy such as industry, agricultural, military affairs.But due to macromolecular material, to mainly contain carbon, hydrogen, oxygen etc. elementary composition, most of high molecular polymers belong to flammable, inflammable material, when burning, heat release rate is large, calorific value is high, flame propagation speed, is difficult for extinguishing, and sometimes also produces thick smoke and toxic gas, cause the harm to environment, people's life security is existed to huge threat.Therefore the flame retardant resistance that, how to improve synthetic polymer and natural polymers material has become a problem of needing solution badly.
Fire retardant refers to the flame retardancy that can improve inflammable substance or combustiblematerials, stops material to be ignited and suppresses a kind of important auxiliary agent of propagation of flame, holds fire hazardous solving macromolecular material, guarantees that the security aspect that synthetic materials is used plays an important role.
Wherein, flame retardant of magnesium hydroxide is one of most widely used kind in halogen-free flame retardants.Because magnesium hydroxide is in fire-retardant, also, with pressing down the characteristics such as cigarette, thermostability, the incarbonization of promotion base material and deacidification ability, be widely used in plastics, elastomerics and the elastomeric materials such as polyvinyl chloride (PVC), polypropylene (PP), polyethylene (PE), vinyl acetate (EVA), polystyrene (PS), polymeric amide (PA).Desirable magnesium hydroxide flame retardant profit is added requirement in polymkeric substance to higher purity and suitable size-grade distribution.Because magnesium hydroxide needs higher loading level as fire-retardant profit, if the particle of magnesium hydroxide used is larger, add prepared matrix material in matrix to, between magnesium hydroxide and matrix, easily form crackle, thereby affect the overall performance of material.And the purity of magnesium hydroxide is one of determinative of matrix material electric property, so desirable magnesium hydroxide all has higher demand as its product purity of fire-retardant filler, each constituent content, particle size range size etc.
The method of producing at present magnesium hydroxide mainly contains two kinds: the one, and the direct comminuting method of brucite; The 2nd, containing magnesium raw material reaction conversion method.Because natural brucite purity is lower, as fire retardant, add the decline that tends to cause matrix material electric property in macromolecular material to.And can prepare the flame retardant of magnesium hydroxide product of different size by controlling different reaction conditionss containing magnesium raw material conversion method, therefore become the main method of current production flame retardant of magnesium hydroxide.
Utilizing containing the main precipitation agent using in the prior art of magnesium raw material transformation approach is sodium hydroxide, ammoniacal liquor, milk of lime.Because separately sodium hydroxide and ammoniacal liquor are as precipitation agent, products obtained therefrom cost value is higher, so people more and more tend to the milk of lime that raw material is easy to get, is that precipitation agent is prepared magnesium hydroxide products.
In a kind of prior art, adopting magnesium chloride, milk of lime is that raw material has been prepared magnesium hydroxide purity and is greater than 98.5%, the magnesium hydroxide products that calcium oxide content is less than 0.2%.This preparation method uses single milk of lime for precipitation agent, due to the character of calcium hydroxide itself, is difficult to accurately control some processing parameters in reaction process in actual production, brings certain difficulty, thereby affect the final quality of product to production operation.
In another kind of prior art, use saturated lime solution react with refining bittern and produce magnesium hydroxide products, because the solubleness of calcium hydroxide is lower, in actual production, exist productive rate compared with, shortcoming that low cost is higher.
Summary of the invention
The problems such as preparation method's products obtained therefrom purity for prior art flame retardant of magnesium hydroxide is not high enough, preparation cost is higher, the invention provides enough high, flame retardant of magnesium hydroxide that preparation cost is lower of the sufficiently high flame retardant of magnesium hydroxide preparation method of a kind of products obtained therefrom purity and a kind of purity.
The invention provides a kind of flame retardant of magnesium hydroxide preparation method, first it comprise the steps:, add magnesium chloride to form magnesium chloride solution, and correspondence is heated to design temperature T in reactor; Then, in reactor, add calcium oxide, magnesium oxide, sodium hydroxide to mix the rear compound precipitants forming with water; Then,, after waiting compound precipitants to add completely, under design temperature T, continue isothermal reaction, then the chlorion in washing and filtering reactor; Moreover, magnesium hydroxide filter cake is starched to processing again; Finally, the magnesium hydroxide filter cake of starching after processing is again carried out to physics break process, obtain flame retardant of magnesium hydroxide.
Preferably, at the massfraction that adds described magnesium chloride in reactor, be between 8%～20%, to form magnesium chloride solution.
Preferably, the massfraction of the magnesium chloride in described magnesium chloride solution is 15%.
Preferably, described design temperature T is 60 degree.
Preferably, in described compound precipitants, the massfraction of wherein said calcium oxide is 15%, and the massfraction of described sodium hydroxide is 0.1%, and described calcium oxide and magnesian mass ratio are 200: 1.
Preferably, the volume of described reactor and the volume ratio of described magnesium chloride solution are 4: 1.
Preferably, when adding compound precipitants toward reactor, the add-on of compound precipitants is that the magnesium ion in mixing solutions precipitates 98.5%～99.5% of required theoretical consumption completely.
Preferably, adding the flow of compound precipitants toward reactor, be 20ml/min.
Preferably, after described compound precipitants adds completely, under design temperature 60 degree, continue isothermal reaction 45min.
Preferably, the volume of described reactor and the volume ratio of described magnesium chloride solution are 4: 1.
Preferably, the magnesium hydroxide pulp density after described slurry is again 40%.
Preferably, described physics break process for being dried after starching the zirconic circulation grinding in ball grinder 60min that the magnesium hydroxide filter cake after processing is 1mm～1.2mm at diameter again again, and obtaining particle diameter is 1.5 μ m, and specific surface area is 5m
2/ g to 10m
2the flame retardant of magnesium hydroxide of/g.
Flame retardant of magnesium hydroxide described in a kind of flame retardant of magnesium hydroxide, it makes by the following method, comprise: the formation magnesium chloride solution that adds magnesium chloride in reactor, and correspondence is heated to design temperature T, the compound precipitants forming after adding calcium oxide, magnesium oxide, sodium hydroxide to mix with water in reactor, after compound precipitants adds completely, under design temperature T, continue isothermal reaction, chlorion in washing and filtering reactor, magnesium hydroxide filter cake is starched to processing again, the magnesium hydroxide filter cake of starching after processing is again carried out to physics break process.
Preferably, the particle size range of described magnesium hydroxide flame retardant profit is within 0.8 μ m～2.5 μ m scope.
Flame retardant of magnesium hydroxide of the present invention and preparation method thereof is by adding in the solution to containing magnesium ion by the mixed compound precipitants of calcium oxide, magnesium oxide, sodium hydroxide and water, by controlling rational processing condition, obtain the flame retardant of magnesium hydroxide that purity is higher again, through many experiments, confirm, the purity of described flame retardant of magnesium hydroxide is more than or equal to 99.0%, and described preparation technology has advantages of that productive rate is high, preparation cost is low.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of preparation method's one preferred embodiment of magnesium hydroxide flame retardant profit of the present invention.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.
Refer to Fig. 1, the present invention also provides a kind of preparation method of flame retardant of magnesium hydroxide, and the preparation method of described flame retardant of magnesium hydroxide comprises:
First, the magnesium chloride solution that the massfraction that adds magnesium chloride in reactor is 8%～20%, is warming up to design temperature T, and wherein T equals 60 ℃;
Then, in reactor, add calcium oxide, magnesium oxide, sodium hydroxide to mix the rear compound precipitants forming with water.The flow that wherein adds compound precipitants is 20ml/min, and the add-on of described compound precipitants is that the magnesium ion in mixing solutions precipitates 98.5%～99.5% of required theoretical consumption completely;
Then, after waiting described compound precipitants to add completely, at design temperature T, under 60 ℃ of environment, continue isothermal reaction 45min, then washing and filtering is until treat in filtrate without chlorion;
Moreover, magnesium hydroxide filter cake is starched to processing again, form magnesium hydroxide slip;
Finally, the magnesium hydroxide filter cake of starching after processing is again carried out to physics break process, obtain flame retardant of magnesium hydroxide.
Certainly, in formally each composition being joined to reactor before, need to carry out suitable pre-treatment to raw material.For example lime is carried out to fragmentation, digestion process then, then refine.Also have, bischofite is dissolved in water, and remove impurity wherein.
Wherein, reaction equation is:
MgCl
2+CaO+MgO+NaOH+H
2O→Mg(OH)
2+CaCl
2+NaCl
Wherein, in described compound precipitants, the massfraction of calcium oxide is preferably 15%, and the massfraction of sodium hydroxide is preferably 0.1%, and calcium oxide and magnesian mass ratio are preferably 200: 1.
Wherein, the volume of described reactor and the volume ratio of described magnesium chloride solution are preferably 4: 1.
Wherein, the add-on of described compound precipitants is preferably complete 99% of the required theoretical consumption that precipitates of magnesium ion in mixing solutions.
Wherein, the massfraction of the magnesium chloride in described magnesium chloride solution is preferably 15%.
Wherein, the magnesium hydroxide pulp density after described slurry is again preferably 40%.
Wherein, described physics break process for being dried after starching the zirconic circulation grinding in ball grinder 60min that the magnesium hydroxide filter cake after processing is 1mm～1.2mm at diameter again again, and obtaining particle diameter is 1.5 μ m, and specific surface area is 7.451m
2the flame retardant of magnesium hydroxide of/g.Certainly, described physics break process also can be processed for comminution by gas stream.
Embodiment 1
In the reactor of 2L, adding 500mL massfraction is that 8% magnesium chloride solution is warming up to 60 ℃, flow with 20ml/min adds compound precipitants, the calcium oxide massfraction of described compound precipitants is 15%, the massfraction of sodium hydroxide is 0.1%, calcium oxide and magnesian mass ratio are 200: 1, compound precipitants add-on be magnesium ion precipitate required theoretical consumption completely 98.5%, described compound precipitants continues isothermal reaction 45min washing and filtering after adding completely again at 60 ℃, treat in filtrate without till chlorion, magnesium hydroxide filter cake is starched to processing again, obtain magnesium hydroxide slip, making the magnesium hydroxide pulp density after starching is again 40%, then the zirconic circulation grinding in ball grinder 60min that is 1mm at diameter is dry.
Embodiment 2
In the reactor of 2L, adding 500mL massfraction is that 15% magnesium chloride solution is warming up to 60 ℃, flow with 20ml/min adds compound precipitants, the calcium oxide massfraction of compound precipitants is 15%, the massfraction of sodium hydroxide is 0.1%, calcium oxide and magnesian mass ratio are 200: 1, described compound precipitants add-on be magnesium ion precipitate required theoretical consumption completely 99%, described compound precipitants continues isothermal reaction 45min washing and filtering after adding completely again at 60 ℃, treat in filtrate without till chlorion, magnesium hydroxide filter cake is starched to processing again, obtain magnesium hydroxide slip, making the magnesium hydroxide pulp density after starching is again 40%, then the zirconic circulation grinding in ball grinder 60min that is 1mm at diameter is dry.
Embodiment 3
In the reactor of 2L, adding 500mL massfraction is that 20% magnesium chloride solution is warming up to 60 ℃, flow with 20ml/min adds compound precipitants, the calcium oxide massfraction of compound precipitants is 15%, the massfraction of sodium hydroxide is 0.1%, calcium oxide and magnesian mass ratio are 200: 1, described compound precipitants add-on be magnesium ion precipitate required theoretical consumption completely 99.5%, described compound precipitants continues isothermal reaction 45min washing and filtering after adding completely again at 60 ℃, treat in filtrate without till chlorion, magnesium hydroxide filter cake is starched to processing again, obtain magnesium hydroxide slip, making the magnesium hydroxide pulp density after starching is again 40%, then the zirconic circulation grinding in ball grinder 60min that is 1.2mm at diameter is dry.
The embodiment of the present invention provides a kind of magnesium hydroxide flame retardant profit, described flame retardant of magnesium hydroxide can be made by above-mentioned preparation method, described flame retardant of magnesium hydroxide comprises magnesium hydroxide, chlorine and iron, according to mass percent, the content of magnesium hydroxide is more than or equal to 99.0%, and the content of chlorine is less than or equal to 0.05%.
Wherein, the particle size range of described magnesium hydroxide flame retardant profit is within 0.8 μ m～2.5 μ m scope, and the specific surface area of described flame retardant of magnesium hydroxide is at 5m
2/ g～10m
2within/g scope.
The preparation method of flame retardant of magnesium hydroxide of the present invention is by adding in the solution to containing magnesium ion by the mixed compound precipitants of calcium oxide, magnesium oxide, sodium hydroxide and water, by controlling rational processing condition, obtain the flame retardant of magnesium hydroxide that purity is higher again, and described preparation technology has advantages of that productive rate is high, preparation cost is low.
These are only preferred case study on implementation of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for flame retardant of magnesium hydroxide, is characterized in that, comprising:
First, in reactor, add magnesium chloride to form magnesium chloride solution, and correspondence is heated to design temperature T;
Then, the compound precipitants forming after adding calcium oxide, magnesium oxide, sodium hydroxide to mix with water in reactor, wherein, the massfraction of described calcium oxide is 15%, the massfraction of described sodium hydroxide is 0.1%, and described calcium oxide and magnesian mass ratio are 200:1;
Then,, after waiting compound precipitants to add completely, under design temperature T, continue isothermal reaction, then the chlorion in washing and filtering reactor;
Moreover, magnesium hydroxide filter cake is starched to processing again, form magnesium hydroxide slip;
Finally, the magnesium hydroxide slip of starching after processing is again carried out to physics break process, obtain flame retardant of magnesium hydroxide.
2. the preparation method of flame retardant of magnesium hydroxide according to claim 1, is characterized in that, when adding magnesium chloride to form magnesium chloride solution in reactor, the massfraction of magnesium chloride solution is between 8%～20%.
3. the preparation method of flame retardant of magnesium hydroxide according to claim 2, is characterized in that, the massfraction of the magnesium chloride in described magnesium chloride solution is 15%.
4. the preparation method of flame retardant of magnesium hydroxide according to claim 1, is characterized in that, described design temperature T is 60 ℃.
5. the preparation method of flame retardant of magnesium hydroxide according to claim 1, is characterized in that, when adding compound precipitants toward reactor, the add-on of compound precipitants is that the magnesium ion in mixing solutions precipitates 98.5%～99.5% of required theoretical consumption completely.
6. the preparation method of flame retardant of magnesium hydroxide according to claim 5, is characterized in that, when adding compound precipitants toward reactor, the flow of compound precipitants is 20mL/min.
7. the preparation method of flame retardant of magnesium hydroxide according to claim 6, is characterized in that, after described compound precipitants adds completely, continues isothermal reaction 45min at 60 ℃ of design temperatures.
8. the preparation method of flame retardant of magnesium hydroxide according to claim 1, is characterized in that, the volume of described reactor and the volume ratio of described magnesium chloride solution are 4:1.
9. the preparation method of flame retardant of magnesium hydroxide according to claim 1, is characterized in that, the magnesium hydroxide pulp density after described slurry is again processed is 40%.
10. the preparation method of flame retardant of magnesium hydroxide according to claim 1, it is characterized in that, described physics break process for being dried after starching the zirconic circulation grinding in ball grinder 60min that the magnesium hydroxide slip after processing is 1mm～1.2mm at diameter again again, obtaining particle diameter is 1.5 μ m, and specific surface area is 5m
2/ g to 10m
2the flame retardant of magnesium hydroxide of/g.
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Families Citing this family (7)
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| CN103387245B (en) * | 2013-07-31 | 2015-10-21 | 中国科学院青海盐湖研究所 | Conversion flow prepares the method for the magnesium hydroxide of different-grain diameter and size-grade distribution |
| CN106632908A (en) * | 2016-09-26 | 2017-05-10 | 高团结 | Preparation method of magnesium hydroxide flame retardant and prepared magnesium hydroxide flame retardant |
| CN110606982B (en) * | 2018-06-15 | 2021-12-17 | 江苏艾特克阻燃材料有限公司 | Basic magnesium borate/magnesium hydroxide composite flame retardant and preparation method thereof |
| CN112390272A (en) * | 2019-08-19 | 2021-02-23 | 唐苑雯 | Water-soluble magnesium hydroxide fire retardant and preparation method thereof |
| CN113150377A (en) * | 2020-10-16 | 2021-07-23 | 南通意特化工有限公司 | Preparation method of magnesium hydroxide flame retardant |
| CN113549245A (en) * | 2021-08-06 | 2021-10-26 | 白银康宝新型节能建材有限责任公司 | Preparation method of inorganic flame retardant |
| CN114832254A (en) * | 2022-05-20 | 2022-08-02 | 山东宙雨消防科技股份有限公司 | Application method of fire extinguishing charcoal without reburning |
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