CN103819936B - Preparation method for compound-type inorganic flame retardation powder material with dual core-shell structure - Google Patents
Preparation method for compound-type inorganic flame retardation powder material with dual core-shell structure Download PDFInfo
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Abstract
The invention discloses a preparation method for a compound-type inorganic flame retardation powder material with a dual core-shell structure, which comprises the following steps: 1) simultaneously and continuously adding a lime milk fluid suspension with 30g/l-150g/l of calcium hydrate content and a brine solution with 50g/l-200g/l of magnesium chloride concentration in a calcium carbonate suspending liquid with 10g/l-50g/l of content, wherein the mol ratio of added magnesium chloride to calcium hydrate is 1.0-1.2: 1.0, and the mol ratio of calcium carbonate to magnesium hydroxide generated by a subsequent reaction is 0.01-0.10: 1.0; 2) reacting magnesium chloride and calcium hydrate in the above mixed liquor, and then insulating and aging to generate a reaction fluid suspension; 3) adding an alkali-silica metal salt solution in the reaction fluid suspension, introducing CO2-containing gas for a carbonization reaction to generate a carbonization fluid suspension; and 4)filtering and drying the carbonization fluid suspension to obtain the inorganic flame retardation powder material. The method has the characteristics of simple process, easy acquisition of raw material and low cost; and the product has the advantages of large granularity, good dispersibility, easy organic modification and good flame retardation effect.
Description
Technical field
The present invention relates to a kind of preparation method of fire-retardant powder body material, the preparation method of the inorganic fire-retarded powder body material of especially a kind of dual-core-shell structure composite type.
Background technology
Magnesium hydroxide is a kind of addition type inorganic combustion inhibitor, has effect that is nontoxic, that eliminate smoke, can overcome the shortcoming of organic halogen containing flame-retardant release Halogen toxic gas; Compared with at present conventional inorganic combustion inhibitor aluminium hydroxide, the degradation production magnesium oxide alkalescence of magnesium hydroxide is comparatively strong, can quickly in and the acidity that produces in Plastics Combustion process and corrosive gases; The decomposition temperature of magnesium hydroxide exceeds 100 DEG C, and the plastics adding flame retardant of magnesium hydroxide can bear higher processing temperature; Mg (OH)
2have higher resolution, thermal capacitance also exceeds 17%, is conducive to improving flame retarding efficiency; Magnesium hydroxide carboniogenesis is strong, and carbonization amount is large, improves flame retarding efficiency, decreases smoke-producing amount.
The preparation of current magnesium hydroxide products is mainly through following two kinds of approach, and one is utilize natural brucite resource, through pulverize obtain, but due to impurity more, belong to after-product; Two is obtained by chemical reaction conversion method by containing magnesium raw material, conventional is with bittern or solubility magnesium salts to precipitate with alkaloids and obtains, comprise ammonia process, sodium hydroxide method and calcium hydroxide method, the magnesium hydroxide products that purity is higher can be obtained, but it is little that the magnesium hydroxide products that chemical method obtains has product cut size, easily reunites, High Temperature High Pressure hydro-thermal method is generally needed to obtain larger powder and granule products, the energy of at substantial, cost is too high; On the other hand, magnesium hydroxide is the mineral compound that a kind of polarity is very strong, has hydrophilic oleophobic property, not good enough with the avidity of polymer molecule; Meanwhile, the generation space, interface of magnesium hydroxide and polymkeric substance, causes its dispersiveness very poor, is difficult to reach the deal that plastic flame needs to add, thus limits its application.In order to improve cohesive force between magnesium hydroxide and polymkeric substance and interface affinity, the better excellent properties playing magnesium hydroxide, need to its modifying surface, to improve magnesium hydroxide surface property.At present, for the method mainly surface chemical modification of magnesium hydroxide surface modifying, conventional surface-modifying agent mainly organosilicon alkanes coupling agent, but it is inadequate directly also to there is bonding force at magnesium hydroxide Surface coating organosilicon alkanes coupling agent, the problem that Surface coating is uneven, makes modified flame retardant of magnesium hydroxide still there is the bad problem of additive effect.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of the inorganic fire-retarded powder body material of a kind of dual-core-shell structure composite type, obtaining macrobead, good dispersity, be beneficial to surface modification, cheap inorganic fire-retarded powder body material.
For solving the problems of the technologies described above, the processing step that the present invention takes is: (1) is continue in the calcium carbonate suspension liquid of 10g/l ~ 100g/l to add the lime cream soliquoid of calcium hydroxide content 30g/l ~ 150g/l and the aqueous salt brine of density of magnesium chloride 50g/l ~ 200g/l at content simultaneously, in the lime cream soliquoid added and aqueous salt brine, the mol ratio of magnesium chloride and calcium hydroxide is 1.0 ~ 1.2:1.0, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.01 ~ 0.10:1.0;
(2) magnesium chloride in above-mentioned mixed solution and calcium hydroxide react, and are then incubated ageing, generate the reaction suspension of magnesium hydroxide coated caco3 core-shell structure particles;
(3) add silicate base metal salt solution in described reaction suspension, pass into containing CO
2gas carries out carburizing reagent, generates carbonization suspension;
(4) described carbonization suspension after filtration, dry, the inorganic fire-retarded powder body material of dual-core-shell structure composite type can be obtained.
In preferred steps of the present invention (1), in calcium carbonate suspension liquid, the concentration of calcium carbonate is 20g/l ~ 50g/l, and in lime cream soliquoid, the content of calcium hydroxide is 60g/l ~ 100g/l, and in aqueous salt brine, the concentration of magnesium chloride is 80g/l ~ 120g/l; The magnesium chloride added and the mol ratio of calcium hydroxide are 1.05 ~ 1.10:1.0, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.03 ~ 0.08:1.0.
In preferred steps of the present invention (2), temperature of reaction is 30 DEG C ~ 90 DEG C.Preferred, described temperature of reaction is 60 DEG C ~ 80 DEG C.
Aging Temperature in preferred steps of the present invention (2) is 50 DEG C ~ 90 DEG C, and digestion time is 30min ~ 120min.Preferred, described Aging Temperature is 60 DEG C ~ 80 DEG C, and digestion time is 50min ~ 80min.
In preferred steps of the present invention (3), the concentration of silicate base metal salt solution is 10g/l ~ 200g/l, and silicate base metal-salt is water glass and/or potassium silicate; Silicate base metal-salt weight is 0.3% ~ 3.0% of magnesium hydroxide coated caco3 core-shell structure particles weight; Described containing CO
2cO in gas
2volume content is 10% ~ 40%, passes into containing CO
2the time of gas is 10min ~ 90min.
Preferred, the concentration of described silicate base metal salt solution is 30g/l ~ 80 g/l; Silicate base metal-salt weight is 0.5% ~ 1.5% of magnesium hydroxide coated caco3 core-shell structure particles weight; Described containing CO
2cO in gas
2volume content is 15% ~ 30%, passes into containing CO
2the time of gas is 20min ~ 40min.
The preferred carbonation reaction temperature of the present invention is 40 DEG C ~ 80 DEG C.Preferred, described carbonation reaction temperature is 60 DEG C ~ 70 DEG C.
The beneficial effect adopting technique scheme to produce is: (1) the present invention take calcium carbonate as nucleus, lime bittern method is adopted to produce magnesium hydroxide, by changing reinforced order, and control the proportioning of calcium hydroxide and magnesium chloride, make newborn magnesium hydroxide in calcium carbonate surface crystal growth, generate calcium carbonate/magnesium hydroxide nucleocapsid structure inorganic powder material, and the particle generated obviously is greater than the magnesium hydroxide particle of chemical method synthesis, thus solve the problem that current chemical method produces magnesium hydroxide particle undersized, effectively improve its dispersiveness in the polymer.
(2) the present invention is by adopting silicate base metal-salt carborization coated skim silicon-dioxide on calcium carbonate/magnesium hydroxide nucleocapsid powder body material, forms the composite inorganic flame-retardant powder body material of dual-core-shell structure.Powder granule outside surface coated silicon-dioxide there is the silanol base functional group of high reaction activity, be easy to organic modifiers (especially silane coupling agent), dehydration condensation occur and generate more firmly chemical bond, be particularly conducive to the organic modification of fireproof powder surface, improve the combination between fire-retardant powder granule and polymkeric substance.
(3) present invention utilizes lime bittern method raw material to be easy to get and cheap advantage, avoid conventional lime method due to particle fine filter difficulty simultaneously, and cause the problems such as complex process to reduce calcium contents in product, simplify processing step, make product will have obvious price advantage, be conducive to applying.
(4) the calcium carbonate core in the composite inorganic flame retardant that obtains of the present invention and the decomposition temperature of outside surface silicon dioxide film all higher, although can not fire retardation be played at the Plastics Combustion initial stage, also serve the effect of mineral filler; In addition due to the weighting agent that calcium carbonate and thermal oxidation silicon are all rubber and plastics, and the content of calcium hydroxide is less than 8.0%, and the content of silicon-dioxide, about 1.0%, can not have side effects to the flame retardant effect of material.
In sum, the present invention has that technique is simple, raw material is easy to get, cheap feature; The powder body material obtained has that grain graininess is comparatively large, good dispersity, be easy to organically-modified and the advantage of good flame retardation effect.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is the dual-core-shell structural representation of product of the present invention;
Fig. 3 is the stereoscan photograph of product of the present invention;
Fig. 4 is the outside surface X-ray energy spectrum figure of product of the present invention;
Fig. 5 is the infrared spectrum of product of the present invention.
Embodiment
Shown in embodiment 1: Fig. 1, the inorganic fire-retarded powder body material of this dual-core-shell structure composite type adopts following processing step to be prepared from.
(1) in the synthesis reactor of band stirring, compound concentration is the calcium carbonate suspension liquid of 20g/l; Compound concentration is the lime cream soliquoid of 75g/l, squeezes into milk of lime elevated dosing vessel; Preparation aqueous salt brine, makes its density of magnesium chloride reach 80g/l, then squeezes in magnesium chloride elevated dosing vessel, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.08:1.0.
(2) the calcium carbonate suspension liquid in reactor is heated to 70 DEG C, under whipped state, to reactor, aqueous salt brine and lime cream soliquoid is slowly added respectively from two elevated dosing vessels, what control two strands of materials adds inbound traffics to ensure that the magnesium chloride that adds in reactor and calcium hydroxide meet ratio requirement, and the mol ratio of magnesium chloride and the total add-on of calcium hydroxide is 1.05:1.Magnesium chloride and calcium hydroxide generation chemical reaction in the reactor; Then make reaction suspension be incubated at 80 DEG C, ageing 80min, makes it generate the core-shell structure particles of the homogeneous magnesium hydroxide coated caco3 of granular size.
(3) the above-mentioned reaction suspension containing core-shell structure particles is proceeded in carbonization reactor.Compound concentration is the sodium silicate solution of 50g/l, and the water glass weight in solution is 2.0% of magnesium hydroxide coated caco3 core-shell structure particles weight.Join disposable for the sodium silicate solution of preparation in carbonization reactor, and to adjust mixeding liquid temperature be 60 DEG C; Pass into containing volume percent 20.0%CO from the bottom of carbonization reactor
2air 30min, make CO
2water glass generation carburizing reagent with mixed solution, at core-shell structure particles Surface Creation silicon dioxide film, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry and dry method modification, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the mean particle size of the present embodiment gained inorganic combustion inhibitor powder granule is 2.3 μm, and specific surface is 12m
2/ g, stereoscan photograph is shown in accompanying drawing 3(a).Adopt S4800-I type field emission scanning electron microscope to Mg (OH)
2/ SiO
2the distribution situation of composite particles surface composition and element M g, Si, O carries out microcell scanning, and X-ray energy spectrum figure is shown in accompanying drawing 4.Comprise Si, O, Mg and C element in the known composite particles of interpretation of result, wherein occur C element be a part of magnesium hydroxide and Carbon Dioxide in Air react generate magnesiumcarbonate institute extremely; The existence of Mg element is because magnesium hydroxide surface coating layer is thinner and the X-ray transmission degree of depth comparatively large, therefore can conclude that the surface coated of magnesium hydroxide is layer of silicon dioxide film.The FTIR spectrogram of sample (a) and sample (b) afterwards before figure 5 provides coated silica, wherein the charateristic avsorption band of O-H appears at 3683.9 cm
-1, wave number is at 1021.8 cm
-1for the contracting second month in a season of Si-O-Si key unsymmetrically vibrates the strong absorption band caused, 873.8cm
-1, 420.6 cm
-1the absorption peak at place is then relevant with the flexural vibration of Si-O key.Chemical composition analysis is carried out to sample, the results are shown in subordinate list 1.
Table 1: various substances content analysis in this powder body material
Comprehensive above information, the structure of this powder body material is the calcium hydroxide shown in Fig. 2/magnesium hydroxide/silicon dioxide dual-core-shell structure; In Fig. 2,1 is calcium carbonate core, and 2 is magnesium hydroxide housing, and 3 is silicon-dioxide adventitia.
Embodiment 2: the fire-retardant powder body material of this composite inorganic adopts following processing step to be prepared from.
(1) in the synthesis reactor of band stirring, compound concentration is the calcium carbonate suspension liquid of 50g/l; Compound concentration is the lime cream soliquoid of 60g/l, squeezes into milk of lime elevated dosing vessel; Preparation aqueous salt brine, makes its density of magnesium chloride reach 100g/l, then squeezes in magnesium chloride elevated dosing vessel, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.05:1.0.
(2) the calcium carbonate suspension liquid in reactor is heated to 80 DEG C, under whipped state, to reactor, aqueous salt brine and lime cream soliquoid is slowly added respectively from two elevated dosing vessels, what control two strands of materials adds inbound traffics to ensure that the magnesium chloride that adds in reactor and calcium hydroxide meet ratio requirement, and the mol ratio of magnesium chloride and the total add-on of calcium hydroxide is 1.1:1.0.Magnesium chloride and calcium hydroxide generation chemical reaction in the reactor; Then make reaction suspension be incubated at 80 DEG C, ageing 60min, makes it generate the core-shell structure particles of the homogeneous magnesium hydroxide coated caco3 of granular size.
(3) the above-mentioned reaction suspension containing core-shell structure particles is proceeded in carbonization reactor.Compound concentration is the sodium silicate solution of 30g/l, and amount of solution is calculate according to 1.5% of magnesium hydroxide coated caco3 core-shell structure particles weight according to wherein water glass.Join disposable for the sodium silicate solution of preparation in carbonization reactor, and to adjust mixeding liquid temperature be 60 DEG C; The CO after purification is after filtration passed into from the bottom of carbonization reactor
2volume content is the stack gas 40min of 15.0%, makes CO
2water glass generation carburizing reagent with mixed solution, at core-shell structure particles Surface Creation silicon dioxide film, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry and dry method modification, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the mean particle size of the present embodiment gained inorganic combustion inhibitor powder granule is 3.8 μm, and specific surface is 8m
2/ g, stereoscan photograph is shown in accompanying drawing 3(b).
Embodiment 3: the fire-retardant powder body material of this composite inorganic adopts following processing step to be prepared from.
(1) in the synthesis reactor of band stirring, compound concentration is the calcium carbonate suspension liquid of 30g/l; Compound concentration is the lime cream soliquoid of 90g/l, squeezes into milk of lime elevated dosing vessel; Preparation aqueous salt brine, makes its density of magnesium chloride reach 150g/l, then squeezes in magnesium chloride elevated dosing vessel, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.04:1.0.
(2) the calcium carbonate suspension liquid in reactor is heated to 90 DEG C, under whipped state, to reactor, aqueous salt brine and lime cream soliquoid is slowly added respectively from two elevated dosing vessels, what control two strands of materials adds inbound traffics to ensure that the magnesium chloride that adds in reactor and calcium hydroxide meet ratio requirement, and the mol ratio of magnesium chloride and the total add-on of calcium hydroxide is 1.2:1.0.Magnesium chloride and calcium hydroxide generation chemical reaction in the reactor; Then make reaction suspension be incubated at 90 DEG C, ageing 50min, makes it generate the core-shell structure particles of the homogeneous magnesium hydroxide coated caco3 of granular size.
(3) the above-mentioned reaction suspension containing core-shell structure particles is proceeded in carbonization reactor.Compound concentration is the sodium silicate solution of 80g/l, and amount of solution is calculate according to 2.5% of magnesium hydroxide coated caco3 core-shell structure particles weight according to wherein water glass.Join disposable for the sodium silicate solution of preparation in carbonization reactor, and to adjust mixeding liquid temperature be 70 DEG C; The CO after purification is after filtration passed into from the bottom of carbonization reactor
2volume content is the stack gas 70min of 12.0%, makes CO
2water glass generation carburizing reagent with mixed solution, at core-shell structure particles Surface Creation silicon dioxide film, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry and dry method modification, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the present embodiment gained inorganic combustion inhibitor powder granule mean particle size is 3.0 μm, and specific surface is 10m
2/ g, stereoscan photograph is shown in accompanying drawing 3(c).
Embodiment 4: the fire-retardant powder body material of this composite inorganic adopts following processing step to be prepared from.
(1) in the synthesis reactor of band stirring, compound concentration is the calcium carbonate suspension liquid of 40g/l; Compound concentration is the lime cream soliquoid of 30g/l, squeezes into milk of lime elevated dosing vessel; Preparation aqueous salt brine, makes its density of magnesium chloride reach 200g/l, then squeezes in magnesium chloride elevated dosing vessel, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.03:1.0.
(2) the calcium carbonate suspension liquid in reactor is heated to 70 DEG C, under whipped state, to reactor, aqueous salt brine and lime cream soliquoid is slowly added respectively from two elevated dosing vessels, what control two strands of materials adds inbound traffics to ensure that the magnesium chloride that adds in reactor and calcium hydroxide meet ratio requirement, and the mol ratio of magnesium chloride and the total add-on of calcium hydroxide is 1.0:1.0.Magnesium chloride and calcium hydroxide generation chemical reaction in the reactor; Then make reaction suspension be incubated at 70 DEG C, ageing 80min, makes it generate the core-shell structure particles of the homogeneous magnesium hydroxide coated caco3 of granular size.
(3) the above-mentioned reaction suspension containing core-shell structure particles is proceeded in carbonization reactor.Compound concentration is the sodium silicate solution of 100g/l, and amount of solution is calculate according to 0.5% of magnesium hydroxide coated caco3 core-shell structure particles weight according to wherein water glass.Join disposable for the sodium silicate solution of preparation in carbonization reactor, and to adjust mixeding liquid temperature be 70 DEG C; The CO after purification is after filtration passed into from the bottom of carbonization reactor
2volume content is the lime-kiln gas 20min of 30.0%, makes CO
2water glass generation carburizing reagent with mixed solution, at core-shell structure particles Surface Creation silicon dioxide film, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry and dry method modification, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the present embodiment gained inorganic combustion inhibitor powder granule mean particle size is 4.2 μm, and specific surface is 3m
2/ g, is shown in accompanying drawing 3(d).
Embodiment 5: the fire-retardant powder body material of this composite inorganic adopts following processing step to be prepared from.
(1) compound concentration is the calcium carbonate suspension liquid of 10g/l, the lime cream soliquoid of 100g/l, density of magnesium chloride reach the aqueous salt brine of 50g/l, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.01:1.0.
(2) calcium carbonate suspension liquid is heated to 60 DEG C, under whipped state, slowly adds aqueous salt brine and lime cream soliquoid, control to add inbound traffics to ensure that the magnesium chloride that adds and calcium hydroxide meet the mol ratio of total add-on for 1.15:1.0; Reaction, at 60 DEG C of insulation ageing 30min, obtains reaction suspension.
(3) the above-mentioned reaction suspension containing core-shell structure particles is proceeded in carbonization reactor, disposablely add the potassium silicate solution that concentration is 200g/l; Solution mesosilicic acid potassium weight is 3.0% of core-shell structure particles weight; Adjustment mixeding liquid temperature is 80 DEG C, passes into CO from the bottom of carbonization reactor
2volume content is air and the carbon dioxide gas mixture 10min of 40.0%, carburizing reagent occurs, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the present embodiment gained inorganic combustion inhibitor powder granule mean particle size is 4.0 μm, and specific surface is 4m
2/ g.
Embodiment 6: the fire-retardant powder body material of this composite inorganic adopts following processing step to be prepared from.
(1) compound concentration is the calcium carbonate suspension liquid of 100g/l, the lime cream soliquoid of 150g/l, density of magnesium chloride reach the aqueous salt brine of 120g/l, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.10:1.0.
(2) calcium carbonate suspension liquid is heated to 30 DEG C, under whipped state, slowly adds aqueous salt brine and lime cream soliquoid, control to add inbound traffics to ensure that the magnesium chloride that adds and calcium hydroxide meet the mol ratio of total add-on for 1.1:1.0; 30 DEG C of reactions, 50 DEG C of insulation ageing 120min, obtain reaction suspension.
(3) proceed in carbonization reactor by the above-mentioned reaction suspension containing core-shell structure particles, the disposable concentration that adds is the water glass of 10g/l and the mixing solutions of potassium silicate; Solution mesosilicic acid sodium and potassium silicate gross weight are 0.3% of core-shell structure particles weight, and the weight ratio of water glass and potassium silicate is 1:1; Adjustment mixeding liquid temperature is 40 DEG C, passes into CO from the bottom of carbonization reactor
2volume content is the air 90min of 10.0%, carburizing reagent occurs, obtains carbonization suspension.
(4) described carbonization suspension after filtration, dry, obtain the composite inorganic flame retardant powder granule with dual-core-shell structure.
After testing, the present embodiment gained inorganic combustion inhibitor powder granule mean particle size is 4.0 μm, and specific surface is 4m
2/ g.
Claims (10)
1. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type, it is characterized in that, it comprises the following steps: (1) is continue in the calcium carbonate suspension liquid of 10g/l ~ 100g/l to add the lime cream soliquoid of calcium hydroxide content 30g/l ~ 150g/l and the aqueous salt brine of density of magnesium chloride 50g/l ~ 200g/l at content simultaneously; In the aqueous salt brine added and lime cream soliquoid, the mol ratio of magnesium chloride and calcium hydroxide is 1.0 ~ 1.2:1.0, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.01 ~ 0.10:1.0;
(2) magnesium chloride in above-mentioned mixed solution and calcium hydroxide react, and are then incubated ageing, generate the reaction suspension of magnesium hydroxide coated caco3 core-shell structure particles;
(3) add silicate base metal salt solution in described reaction suspension, pass into containing CO
2gas carries out carburizing reagent, generates carbonization suspension;
(4) described carbonization suspension after filtration, dry, the inorganic fire-retarded powder body material of dual-core-shell structure composite type can be obtained.
2. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 1, it is characterized in that: in described step (1), in calcium carbonate suspension liquid, the concentration of calcium carbonate is 20g/l ~ 50g/l, in lime cream soliquoid, the content of calcium hydroxide is 60g/l ~ 100g/l, and in aqueous salt brine, the concentration of magnesium chloride is 80g/l ~ 120g/l; The magnesium chloride added and the mol ratio of calcium hydroxide are 1.05 ~ 1.10:1.0, and calcium carbonate and the theoretical mol ratio generated between magnesium hydroxide of subsequent reactions of putting into reactor are in advance 0.03 ~ 0.08:1.0.
3. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 1, is characterized in that: in described step (2), temperature of reaction is 30 DEG C ~ 90 DEG C.
4. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 3, is characterized in that: described temperature of reaction is 60 DEG C ~ 80 DEG C.
5. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 1, is characterized in that: the Aging Temperature in described step (2) is 50 DEG C ~ 90 DEG C, and digestion time is 30min ~ 120min.
6. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 5, is characterized in that: described Aging Temperature is 60 DEG C ~ 80 DEG C, and digestion time is 50min ~ 80min.
7. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 1-6 any one, it is characterized in that: in described step (3), the concentration of silicate base metal salt solution is 10g/l ~ 200g/l, and silicate base metal-salt is water glass and/or potassium silicate; Silicate base metal-salt weight is 0.3% ~ 3.0% of magnesium hydroxide coated caco3 core-shell structure particles weight; Described containing CO
2cO in gas
2volume content is 10% ~ 40%, passes into containing CO
2the time of gas is 10min ~ 90min.
8. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 7, is characterized in that: the concentration of described silicate base metal salt solution is 30g/l ~ 80 g/l; Silicate base metal-salt weight is 0.5% ~ 1.5% of magnesium hydroxide coated caco3 core-shell structure particles weight; Described containing CO
2cO in gas
2volume content is 15% ~ 30%, passes into containing CO
2the time of gas is 20min ~ 40min.
9. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 7, is characterized in that: described carbonation reaction temperature is 40 DEG C ~ 80 DEG C.
10. the preparation method of the inorganic fire-retarded powder body material of dual-core-shell structure composite type according to claim 9, is characterized in that: described carbonation reaction temperature is 60 DEG C ~ 70 DEG C.
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| CN101767974A (en) * | 2010-01-17 | 2010-07-07 | 金同芳 | Mineral-modified organic heat-insulating granules fireproof heated board and manufacture technology thereof |
| EP2441803A1 (en) * | 2010-10-12 | 2012-04-18 | Shin-Etsu Chemical Co., Ltd. | Flame retardant organopolysiloxane composition |
| CN102746533A (en) * | 2012-07-11 | 2012-10-24 | 四川石棉巨丰粉体有限公司 | Heavy calcium carbonate composite packing as well as preparation method and application thereof |
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| CN1033637A (en) * | 1987-12-16 | 1989-07-05 | 青岛建新盐化厂 | Magnesium is inorganic combustion inhibitor and preparation method thereof |
| CN101767974A (en) * | 2010-01-17 | 2010-07-07 | 金同芳 | Mineral-modified organic heat-insulating granules fireproof heated board and manufacture technology thereof |
| EP2441803A1 (en) * | 2010-10-12 | 2012-04-18 | Shin-Etsu Chemical Co., Ltd. | Flame retardant organopolysiloxane composition |
| CN102746533A (en) * | 2012-07-11 | 2012-10-24 | 四川石棉巨丰粉体有限公司 | Heavy calcium carbonate composite packing as well as preparation method and application thereof |
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