CN102502728A - Magnesium hydroxide flame retardant and preparation method thereof - Google Patents
Magnesium hydroxide flame retardant and preparation method thereof Download PDFInfo
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- CN102502728A CN102502728A CN2011103072277A CN201110307227A CN102502728A CN 102502728 A CN102502728 A CN 102502728A CN 2011103072277 A CN2011103072277 A CN 2011103072277A CN 201110307227 A CN201110307227 A CN 201110307227A CN 102502728 A CN102502728 A CN 102502728A
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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 the Chemicals field, the preparation method who relates in particular to a kind of flame retardant of magnesium hydroxide reaches the flame retardant of magnesium hydroxide by this preparing method's gained.
Background technology
Synthetic macromolecule resol occurs in 1907, and indicated the beginning of human use synthesized polymer material.At present, macromolecular material becomes the important materials in science and technology and the economic construction with metallic substance, ceramic.Especially in recent decades; Polymer materialss such as plastics, rubber, synthon and goods thereof obtain flourish; They replace natural polymers such as traditional steel, metal, cement and timber, cotton just rapidly, are widely used in each department of national economy such as industry, agricultural, military affairs.But because that macromolecular material mainly contains carbon, hydrogen, oxygen etc. is elementary composition, most of high molecular polymers belong to flammable, inflammable material, and HRR is big when burning; Calorific value is high; Flame propagation speed is difficult for extinguishing, and also produces thick smoke sometimes and toxic gas; Cause harm, there is huge threat in people's life security environment.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 is meant 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, causes fire easily solving macromolecular material, guarantees that the security aspect that synthetic materials uses plays an important role.
Wherein, flame retardant of magnesium hydroxide is one of most widely used kind in the halogen-free flame retardants.Because Marinco H is in fire-retardant; Also, be widely used in plastics, elastomerics and the elastomeric materials such as SE (PVC), Vestolen PP 7052 (PP), Vilaterm (PE), vinyl acetate (EVA), PS (PS), polyamide (PA) with pressing down characteristics such as cigarette, thermostability, the incarbonization of promotion base material and deacidification ability.Ideal magnesium hydroxide flame retardant profit is added in the polymkeric substance and to be required to have higher purity and suitable size-grade distribution.Because Marinco H needs higher loading level as fire-retardant profit, if the particle of used Marinco H is bigger, add prepared matrix material in the matrix to, between Marinco H and matrix, form crackle easily, thereby influence the overall performance of material.And the purity of Marinco H is one of determinative of matrix material electric property, so the ideal Marinco H all has higher demand as its product purity of fire-retardant filler, each constituent content, particle size range size etc.
The method of producing Marinco H at present mainly contains two kinds: the one, and the direct comminuting method of brucite; The 2nd, contain magnesium raw material reaction conversion method.Because natural brucite purity is lower, adds the decline that tends to cause the matrix material electric property in the macromolecular material to as fire retardant.Can prepare the flame retardant of magnesium hydroxide product of different size through the control different reaction conditions and contain the magnesium raw material conversion method, therefore become the main method of present production flame retardant of magnesium hydroxide.
Utilization contains the main precipitation agent that uses in the prior art of magnesium raw material transformation approach and is sodium hydroxide, ammoniacal liquor, milk of lime.Because separately sodium hydroxide and ammoniacal liquor are as precipitation agent, the products obtained therefrom cost value is higher, is that precipitation agent prepares magnesium hydroxide products so People more and more is tended to the milk of lime that raw material is easy to get.
In a kind of prior art, adopting magnesium chloride, milk of lime is that feedstock production has gone out Marinco H purity greater than 98.5%, and calcium oxide content is less than 0.2% magnesium hydroxide products.This preparation method uses single milk of lime to be precipitation agent, because the character of calcium hydroxide itself is difficult to accurately control some processing parameters in the reaction process in actual production, brings certain difficulty to production operation, thereby influences the final quality of product.
In the another kind of prior art, use saturated lime solution and refining bittern reacted magnesium hydroxide products because the solubleness of calcium hydroxide is lower, in actual production, exist productive rate, the higher shortcoming of low cost.
Summary of the invention
Preparing method's products obtained therefrom purity to the prior art flame retardant of magnesium hydroxide is not high enough, preparation cost is than problems such as height, and the present invention provides the flame retardant of magnesium hydroxide that the sufficiently high flame retardant of magnesium hydroxide preparation method of a kind of products obtained therefrom purity and a kind of purity are enough high, preparation cost is lower.
The present invention provides a kind of flame retardant of magnesium hydroxide preparation method, and it comprises the steps: at first, in reactor drum, add magnesium chloride and form magnesium chloride solution, and correspondence is heated to design temperature T; Then, in reactor drum, add quicklime, Natural manganese dioxide, sodium hydroxide and mix the compound precipitants that the back forms with water; Then, wait compound precipitants to add fully after, continuation isothermal reaction, the cl ions in the washing and filtering reactor drum then under design temperature T; Moreover, the Marinco H filter cake is starched processing again; At last, the Marinco H filter cake after slurry is handled is again carried out the physics break process, obtain flame retardant of magnesium hydroxide.
Preferably, be between 8%～20% at the massfraction that in reactor drum, adds said magnesium chloride, to form magnesium chloride solution.
Preferably, the massfraction of the magnesium chloride in the said magnesium chloride solution is 15%.
Preferably, said design temperature T is 60 degree.
Preferably, in the said compound precipitants, the massfraction of wherein said quicklime is 15%, and the massfraction of said sodium hydroxide is 0.1%, and said quicklime and magnesian mass ratio are 200: 1.
Preferably, the volume ratio of the volume of said reactor drum and said magnesium chloride solution is 4: 1.
Preferably, when adding compound precipitants toward reactor drum, the add-on of compound precipitants is that the mg ion in the mixing solutions precipitates 98.5%～99.5% of required theoretical consumption fully.
Preferably, be 20ml/min at the flow that adds compound precipitants toward reactor drum.
Preferably, after said compound precipitants adds fully, lasting isothermal reaction 45min under design temperature 60 degree.
Preferably, the volume ratio of the volume of said reactor drum and said magnesium chloride solution is 4: 1.
Preferably, the Marinco H pulp density behind the said slurry again is 40%.
Preferably, said physics break process is dry again for starching behind the zirconic circulation grinding in ball grinder 60min that Marinco H filter cake after the processing is 1mm～1.2mm at diameter 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.
The said flame retardant of magnesium hydroxide of a kind of flame retardant of magnesium hydroxide; It makes through following method, comprising: in reactor drum, add the formation magnesium chloride solution of magnesium chloride, and correspondence is heated to design temperature T; In reactor drum, add quicklime, Natural manganese dioxide, sodium hydroxide and mix the compound precipitants that the back forms with water; After compound precipitants adding fully, under design temperature T, continue isothermal reaction, the cl ions in the washing and filtering reactor drum; The Marinco H filter cake is starched processing again, the Marinco H filter cake after slurry is handled is again carried out the physics break process.
Preferably, the particle size range of said magnesium hydroxide flame retardant profit is within 0.8 μ m～2.5 mu m ranges.
Flame retardant of magnesium hydroxide of the present invention and preparation method thereof is through adding in the solution that contains mg ion by the mixed compound precipitants of quicklime, Natural manganese dioxide, sodium hydroxide and water; Obtain the higher flame retardant of magnesium hydroxide of purity through the control reasonable process conditions again; Warp is experiment confirm repeatedly; The purity of said flame retardant of magnesium hydroxide is more than or equal to 99.0%, and said preparation technology has productive rate height, advantage that preparation cost is low.
Description of drawings
Fig. 1 is the schematic flow sheet of sharp preparing method's one preferred embodiment of magnesium hydroxide flame retardant of the present invention.
Embodiment
Below in conjunction with accompanying drawing preferred embodiment of the present invention is set forth in detail, thereby protection scope of the present invention is made more explicit defining so that advantage of the present invention and characteristic can be easier to it will be appreciated by those skilled in the art that.
See also Fig. 1, the present invention also provides a kind of preparation method of flame retardant of magnesium hydroxide, and the preparation method of said flame retardant of magnesium hydroxide comprises:
At first, the massfraction that in reactor drum, adds magnesium chloride is 8%～20% magnesium chloride solution, is warming up to design temperature T, and wherein T equals 60 ℃;
Then, in reactor drum, add quicklime, Natural manganese dioxide, sodium hydroxide and mix the compound precipitants that the back forms with water.The flow that wherein adds compound precipitants is 20ml/min, and the add-on of said compound precipitants is that the mg ion in the mixing solutions precipitates 98.5%～99.5% of required theoretical consumption fully;
Then, wait said compound precipitants to add fully after, at design temperature T, promptly 60 ℃ of environment continue isothermal reaction 45min down, washing and filtering is in waiting to filtrate till the no cl ions then;
Moreover, the Marinco H filter cake is starched processing again, form the Marinco H slip;
At last, the Marinco H filter cake after slurry is handled is again carried out the physics break process, obtain flame retardant of magnesium hydroxide.
Certainly, before formally joining each composition in the reactor drum, need carry out suitable pre-treatment to raw material.For example lime is carried out fragmentation, digestion process is made with extra care again then.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 the said compound precipitants, the massfraction of quicklime is preferably 15%, and the massfraction of sodium hydroxide is preferably 0.1%, and quicklime and magnesian mass ratio are preferably 200: 1.
Wherein, the volume ratio of the volume of said reactor drum and said magnesium chloride solution is preferably 4: 1.
Wherein, the add-on of said compound precipitants is preferably complete 99% of the required theoretical consumption that precipitates of mg ion in the mixing solutions.
Wherein, the massfraction of the magnesium chloride in the said magnesium chloride solution is preferably 15%.
Wherein, the Marinco H pulp density behind the said slurry again is preferred 40%.
Wherein, said physics break process is dry again for starching behind the zirconic circulation grinding in ball grinder 60min that Marinco H filter cake after the processing is 1mm～1.2mm at diameter 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, said physics break process also can be handled for comminution by gas stream.
Embodiment 1
In the reactor drum of 2L, add the 500mL massfraction and be 8% magnesium chloride solution and be warming up to 60 ℃; Flow with 20ml/min adds compound precipitants, and the quicklime massfraction of said compound precipitants is 15%, and the massfraction of sodium hydroxide is 0.1%; Quicklime and magnesian mass ratio are 200: 1; The compound precipitants add-on be mg ion precipitate required theoretical consumption fully 98.5%, continue isothermal reaction 45min washing and filtering down at 60 ℃ again after said compound precipitants adds fully, in waiting to filtrate till the no cl ions; Starch processing to the Marinco H filter cake again; Obtaining the Marinco H slip, make that again the Marinco H pulp density behind the slurry is 40%, is dry the getting final product of zirconic circulation grinding in ball grinder 60min of 1mm then at diameter.
Embodiment 2
In the reactor drum of 2L, add the 500mL massfraction and be 15% magnesium chloride solution and be warming up to 60 ℃; Flow with 20ml/min adds compound precipitants, and the quicklime massfraction of compound precipitants is 15%, and the massfraction of sodium hydroxide is 0.1%; Quicklime and magnesian mass ratio are 200: 1; Said compound precipitants add-on be mg ion precipitate required theoretical consumption fully 99%, continue isothermal reaction 45min washing and filtering down at 60 ℃ again after said compound precipitants adds fully, in waiting to filtrate till the no cl ions; Starch processing to the Marinco H filter cake again; Obtaining the Marinco H slip, make that again the Marinco H pulp density behind the slurry is 40%, is dry the getting final product of zirconic circulation grinding in ball grinder 60min of 1mm then at diameter.
Embodiment 3
In the reactor drum of 2L, add the 500mL massfraction and be 20% magnesium chloride solution and be warming up to 60 ℃; Flow with 20ml/min adds compound precipitants, and the quicklime massfraction of compound precipitants is 15%, and the massfraction of sodium hydroxide is 0.1%; Quicklime and magnesian mass ratio are 200: 1; Said compound precipitants add-on be mg ion precipitate required theoretical consumption fully 99.5%, continue isothermal reaction 45min washing and filtering down at 60 ℃ again after said compound precipitants adds fully, in waiting to filtrate till the no cl ions; Starch processing to the Marinco H filter cake again; Obtaining the Marinco H slip, make that again the Marinco H pulp density behind the slurry is 40%, is dry the getting final product of zirconic circulation grinding in ball grinder 60min of 1.2mm then at diameter.
The embodiment of the invention provides a kind of magnesium hydroxide flame retardant sharp; Said flame retardant of magnesium hydroxide can be made by above-mentioned preparation method; Comprise Marinco H, chlorine and iron in the said flame retardant of magnesium hydroxide; According to mass percent, the content of Marinco H is more than or equal to 99.0%, and the content of chlorine is smaller or equal to 0.05%.
Wherein, the particle size range of said magnesium hydroxide flame retardant profit is within 0.8 μ m～2.5 mu m ranges, and the specific surface area of said flame retardant of magnesium hydroxide is at 5m
2/ g～10m
2Within/g the scope.
The preparation method of flame retardant of magnesium hydroxide of the present invention is through adding in the solution that contains mg ion by the mixed compound precipitants of quicklime, Natural manganese dioxide, sodium hydroxide and water; Obtain the higher flame retardant of magnesium hydroxide of purity through the control reasonable process conditions again, and said preparation technology have productive rate height, advantage that preparation cost is low.
More than be merely 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 changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (13)
1. the preparation method of a flame retardant of magnesium hydroxide is characterized in that, comprising:
At first, in reactor drum, add magnesium chloride and form magnesium chloride solution, and correspondence is heated to design temperature T;
Then, in reactor drum, add quicklime, Natural manganese dioxide, sodium hydroxide and mix the compound precipitants that the back forms with water;
Then, wait compound precipitants to add fully after, continuation isothermal reaction, the cl ions in the washing and filtering reactor drum then under design temperature T;
Moreover, the Marinco H filter cake is starched processing again, form the Marinco H slip;
At last, the Marinco H filter cake after slurry is handled is again carried out the physics break process, obtain flame retardant of magnesium hydroxide.
2. the preparation method that magnesium hydroxide flame retardant according to claim 1 is sharp is characterized in that, is between 8%～20% at the massfraction that in reactor drum, adds said magnesium chloride, to form magnesium chloride solution.
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 the said magnesium chloride solution is 15%.
4. the preparation method of flame retardant of magnesium hydroxide according to claim 1 is characterized in that, said design temperature T is 60 degree.
5. the preparation method that magnesium hydroxide flame retardant according to claim 1 is sharp; It is characterized in that in the said compound precipitants, the massfraction of wherein said quicklime is 15%; The massfraction of said sodium hydroxide is 0.1%, and said quicklime and magnesian mass ratio are 200: 1.
6. the preparation method of flame retardant of magnesium hydroxide according to claim 1; It is characterized in that; When adding compound precipitants toward reactor drum, the add-on of compound precipitants is that the mg ion in the mixing solutions precipitates 98.5%～99.5% of required theoretical consumption fully.
7. the preparation method that magnesium hydroxide flame retardant according to claim 6 is sharp is characterized in that, is 20ml/min at the flow that adds compound precipitants toward reactor drum.
8. the preparation method of flame retardant of magnesium hydroxide according to claim 7 is characterized in that, after said compound precipitants adds fully, and lasting isothermal reaction 45min under design temperature 60 degree.
9. the preparation method of flame retardant of magnesium hydroxide according to claim 1 is characterized in that, the volume of said reactor drum and the volume ratio of said magnesium chloride solution are 4: 1.
10. the preparation method of flame retardant of magnesium hydroxide according to claim 1 is characterized in that, the Marinco H pulp density behind the said slurry again is 40%.
11. the preparation method of flame retardant of magnesium hydroxide according to claim 1; It is characterized in that; Said physics break process is dry again for starching behind the zirconic circulation grinding in ball grinder 60min that Marinco H filter cake after the processing is 1mm～1.2mm at diameter 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.
12. a flame retardant of magnesium hydroxide is characterized in that: said flame retardant of magnesium hydroxide is to adopt to make like any described preparation method among the claim 1-11.
13. magnesium hydroxide flame retardant according to claim 12 is sharp, it is characterized in that the particle size range of said flame retardant of magnesium hydroxide is within 0.8 μ m～2.5 mu m ranges.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103387245A (en) * | 2013-07-31 | 2013-11-13 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide with different grain diameters and grain distributions by changing flow |
| CN106632908A (en) * | 2016-09-26 | 2017-05-10 | 高团结 | Preparation method of magnesium hydroxide flame retardant and prepared magnesium hydroxide flame retardant |
| CN110606982A (en) * | 2018-06-15 | 2019-12-24 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103387245A (en) * | 2013-07-31 | 2013-11-13 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide with different grain diameters and grain distributions by changing flow |
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| CN110606982A (en) * | 2018-06-15 | 2019-12-24 | 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 |
| 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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