CN102502725A - Method for producing flame-retardant magnesium hydroxide - Google Patents
Method for producing flame-retardant magnesium hydroxide Download PDFInfo
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- CN102502725A CN102502725A CN2011103362049A CN201110336204A CN102502725A CN 102502725 A CN102502725 A CN 102502725A CN 2011103362049 A CN2011103362049 A CN 2011103362049A CN 201110336204 A CN201110336204 A CN 201110336204A CN 102502725 A CN102502725 A CN 102502725A
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Abstract
The invention relates to a method for producing flame-retardant magnesium hydroxide, which includes: subjecting raw materials including low-grade magnesium-contained ores such as magnesite, brucite and the like to roasting, levigating and infiltrating in ammonium aqueous solution extraction solvent to obtain ultrapure magnesium-contained aqueous solution, and using ammonia gas as precipitating agent to obtain the flame-retardant magnesium hydroxide. The whole process of producing flame-retardant magnesium hydroxide enables recycling of ammonia gas released during magnesium infiltration and the ammonium aqueous solution for magnesium precipitation. Ammonium-contained filtrate which is separated after precipitation of magnesium hydroxide is used as magnesium extraction solvent, so that obtained magnesium solution needs no extra procedure for removing impurities of Si, Ca, Al, Fe and the like. The preparation process is free of emission of waste water and waste gas, and maximization of low-grade magnesium-contained ore resource utilization, minimization of environment pollution and maximization of economic benefits are completely realized. The method for producing flame-retardant magnesium hydroxide is high in operability and easy in industrialization.
Description
Technical field
The present invention relates to the working method of Marinco H, relate in particular to a kind of working method of Flame Retardant Magnesium Hydroxide.
Background technology
Fire retardant is claimed incombustible agent again, and flame-proofing agent or fireproofing agent are the functional aids of giving the combustible polymers flame retardancy.Be divided into additive flame retardant and reactive flame retardant according to application mode.According to composition, additive flame retardant mainly comprises inorganic combustion inhibitor, halogenated flame retardant (organic chloride and organic bromide), phosphorus flame retardant (red phosphorus, SULPHOSUCCINIC ACID ESTER and halogenated phosphate etc.) and nitrogen flame retardant etc.Mainly be applicable to the plastics of fire-retardant demand, postpone or prevent the especially burning of high score subclass plastics of plastics.Its burning time is increased, light, be difficult to light from putting out.
Since the enhancing of environmental consciousness in addition inorganic combustion inhibitor have cheap, wide material sources, nontoxic, do not have corrosion, when burning, do not cause advantages such as secondary pollution, inorganic combustion inhibitor is by a large amount of uses.Wherein, the U.S., Japan, West Europe inorganic combustion inhibitor consumption account for 60%, 64%, 50% of fire retardant aggregate consumption respectively.And wherein inorganic combustion inhibitor is main with white lake and Marinco H.
Marinco H belongs to the addition type inorganic combustion inhibitor, produce, use and discarded process in all unharmful substance dischargings, and can also in combustion processes in the acidity and the corrosive gases that produce, be a kind of environment-friendly fire retardant.Because Marinco H has been compared many advantages with white lake, so the Marinco H proportion is increasing.According to the foreign data statistics, western developed country flame retardant of magnesium hydroxide consumption accounts for more than 30% of inorganic combustion inhibitor consumption.The U.S., West Europe, Japan a year consumption at present are about 50,000 tons, 80,000 tons, 30,000 tons respectively.Estimate the five-year, the U.S., West Europe, Japan's consumption average growth rate per annum are respectively 12%, 8%, 7%.In view of this, flame retardant of magnesium hydroxide has good development prospect.The domestic production Flame Retardant Magnesium Hydroxide uses raw material to mainly contain magnesium-containing ore (rhombspar, magnesite, brucite mineral etc.) and magnesium chloride bittern at present.
CN 1124982C discloses a kind of technology of magnesium hydroxide directly from magnesite; Comprising that calcining, digestion are synthetic, it is characterized in that, is raw material with magnesite through calcining: digestion is synthetic, removal of impurities, deironing, directly synthetic; And removal of impurities in slurries, deironing, make product reach high-purity.This production technique of inventing disclosed Marinco H needs the purifying step of complicated and power consumption to remove various impurity and unwanted pollutent.
CN 101850994 A disclose a kind of method of manufacture of flame-proof magnesium hydroxide, may further comprise the steps: A1: the building-up reactions step is a raw material with sal epsom, is transforming agent with sodium hydroxide, in synthesizer, carries out building-up reactions; A2: activation step, adding precipitation agent and acvator carry out activation in the mixed solution that steps A 1 obtains, and the activation completion is after the press filtration of high pressure automatic diaphragm pressure filter uses the vaal water washing to obtain A type Marinco H; A3: modification procedure, through high temperature modified, the mixed solution after the modification filters through high pressure automatic diaphragm pressure filter again with said A type Marinco H, uses the vaal water washing, makes the Type B Marinco H; A4: the drying and crushing step, with said Type B Marinco H process drying and crushing, the flame-proof magnesium hydroxide finished product that can obtain.This preparing method's process is complicated, be difficult for accomplishing scale production, and used starting material can't be recycled in the preparation process, are unfavorable for economizing on resources.
CN 101723418 A disclose a kind of method of utilizing magnesium chloride to prepare ultra-fine magnesium hydroxide flame retardant, and comprise the steps: a reaction: take by weighing 15～200 parts of deionized waters by weight, purity is 10～20 parts in 95-99% solid magnesium chloride; Add in the reaction kettle; In temperature is that 150～200 ℃, pressure are under the 0.4-1.5MPa condition, and dripping percentage concentration is the 25%-30% sodium hydroxide solution, and rate of addition is the 4-6 ml/min; Drip 20-23 part, process magnesium hydrate precipitate; The b hydro-thermal: being 150～200 ℃ in temperature is the condition fore-telling of 0.4-1.5MPa with pressure, and hydro-thermal 6-12h is cooled to 50 ℃ of dischargings; C filters: the Marinco H slurry that will go up step reaction generation is under the 0.7-0.9MPa condition in vacuum tightness, carries out vacuum filtration; D washing: with the hot wash of filter cake with 70-80 ℃, wash to wash in the rear filtrate can not check cl ions with Silver Nitrate till; E is dry: the filter cake after will washing is put into drying machine and is foretold 95-105 ℃ of condition, is dried to constant weight; The f packing: dried material, vacuum-packed with combined package bag.Preparing method's complex process that this invention provided, raw materials cost is high, is difficult for suitability for industrialized production.
Summary of the invention
To the deficiency of prior art, the object of the present invention is to provide a kind of method of utilizing low-grade magnesium-containing ore production Flame Retardant Magnesium Hydroxide.
Working method of the present invention comprises the steps:
(1) with the levigate magnesium oxide powder that obtains of the magnesium-containing ore after the roasting;
(2) magnesium oxide powder with step (1) gained places reaction vessel,, stirs and makes its reaction as leaching solvent with the ammonium class aqueous solution, then reaction solution is naturally cooled to room temperature and gets magma;
(3) magma that step (2) is obtained filters, and removes insoluble impurities, obtains Mg-bearing water solution;
(4) the Mg-bearing water solution that step (3) is obtained places reaction crystalizer, handles with ammonia, is settled out Marinco H;
(5) reacting liquid filtering that step (4) is obtained obtains Marinco H, and washing, drying obtain Flame Retardant Magnesium Hydroxide.
As optimal technical scheme, the maturing temperature described in the step (1) is 300～890 ℃, preferred 450～650 ℃.The roasting magnesium ore is so that obtain easy dissolved magnesium oxide powder, and the selection of maturing temperature can influence the use properties of the flame retardant of magnesium hydroxide that finally obtains, and it is 300～890 ℃ that the present invention selects maturing temperature, preferred 450～650 ℃.
Used magnesium-containing ore is low-grade magnesium ore deposits such as magnesite, brucite mineral in the step (1).China's magnesium-containing ore abundant raw material; Used magnesium-containing ore is low-grade magnesium ore deposits such as magnesite, brucite mineral among the present invention; A kind of low-grade magnesium-containing ore of how developing and make full use of is provided thus; Make full use of resource to reach, make the production Flame Retardant Magnesium Hydroxide method of maximization of economic benefit.Certainly, magnesium-containing ore of the present invention is not limited to low-grade magnesium ore deposit, and the same available method provided by the present invention of ore that contains the other types of magnesium prepares Flame Retardant Magnesium Hydroxide.
As optimal technical scheme, the reaction vessel described in the step (2) is a reaction kettle.Ammonium class described in the step (2) is ammonium chloride, ammonium sulfate, monoammonium sulfate or an ammonium nitrate, or its mixture.Use this type of ammonium class solution so that the magnesium oxide powder that step (1) obtains forms mg ion soluble in water among the present invention, so that sedimentaryly carry out smoothly.And the magnesium chloride solution that utilizes the ammonium class aqueous solution to obtain as the leaching solvent does not need the extra Si that removes, Ca, and Al, the operation of impurity such as Fe, thus practiced thrift operation, reduced energy consumption.
Leaching solvent described in the step (2) contains NH
4 +The ionic amount of substance is equal to or greater than the amount of substance of institute's dissolved magnesium, preferred NH
4 +The ionic amount of substance is equal to or greater than 2 times of amount of substance of institute's dissolved magnesium.At this control NH
4 +The ionic amount of substance makes its amount of substance that is equal to or greater than institute's dissolved magnesium, be for make the magnesium powder cmpletely change mg ion into, improve the yield of Marinco H.
Leaching solvent described in the step (2) is the filtrating in the step (5).Used leaching solvent is the filtrating that is produced in the working method among the present invention, makes reaction process not have waste water on the one hand and discharges, and has realized the recycle of the ammonium class aqueous solution of heavy magnesium on the other hand, helps economizing on resources, and makes maximizing the benefits.
Churning time in the step (2) is not less than 2h, and temperature of reaction is 0～180 ℃, preferred 105～180 ℃.Control reaction temperature and reaction times fully dissolve in order to make the magnesium body, obtain containing the solution of mg ion.
As optimal technical scheme, the ammonia described in the step (4) is the molten ammonia that discharges in the magnesium oxide powder process that soaks of the ammonium class aqueous solution in the step (2).The used precipitation agent ammonia of the present invention is the waste gas that is produced in the step in present method (2), has realized making full use of of refuse, belongs to the working method of environment-friendly type.
Treating processes described in the step (4) is following: the temperature of control reaction crystalizer; Add X 2073 or cetyl trimethylammonium bromide as surface treatment agent; Feed this solution of ammonia processing and be settled out Marinco H; After reaction finished, the temperature rising with reaction crystalizer continued to stir; As preferably, the temperature of reaction crystalizer is initially and is not less than 40 ℃, is preferably 50～60 ℃; The temperature of the reaction crystalizer after the rising is not less than 80 ℃, is preferably 90～100 ℃; Churning time is not less than 1h, is preferably to be not less than 2h.
Reactive crystallization is meant and carries out the process that chemical reaction produces indissoluble or insoluble solid matter between gas and liquid or liquid and the liquid.Reaction-crystallization method can make some be prone to generate sedimentary material and other compound separation, thereby reaches the purpose of purifying.Reaction crystallization process has the characteristics of highly selective, is usually used in product separation and purifies.It is simple in structure, energy consumption is low, and the grain size number of utilizing mold to obtain is evenly distributed, and is a very big raising to the quality of product.The mold internal temperature is controlled easily, and the present invention comes controls reaction speed through the initial temperature of crystallization control device inside and the temperature after the reaction end, so that obtain performance ideal product.
The invention provides with low-grade magnesium-containing ore (magnesite, brucite mineral etc.) is raw material; Through roasting, levigate, the ammonium class aqueous solution as leach solvent dissolve soak after; The high-purity magnesium solution that obtains directly passes through ammonia recycle method, the method for production Flame Retardant Magnesium Hydroxide.The advantage of this method is, whole process realizes dissolving soaks the ammonia that discharges in the magnesium process and the filtrate cycle utilization behind the heavy magnesium; Adopt the leaching solvent of the ammonium class aqueous solution as magnesium, the magnesium chloride solution that obtains does not need extra Si, Ca, Al, the operation of impurity such as Fe removed; No waste water, exhaust gas emission.Fully realized low-grade magnesium-containing ore utilization of resources maximization, environmental pollution minimizes and maximization of economic benefit.Method of the present invention is workable, is easy to realize industriallization.
Description of drawings
Fig. 1 process flow diagram of the present invention.
Embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment only is used for helping to understand the present invention, should not be regarded as concrete restriction of the present invention.
Fig. 1 is seen in concrete technical process signal of the present invention.
Embodiment one
(1) under 650 ℃ temperature, in retort furnace, with low-grade magnesite calcining 240 minutes.Under this temperature, calcium is still with CaCO in the MgO powder that obtains
3Form exist.With the chemical constitution of chemical analysis assay determination calcining back magnesite, the content of MgO is 90.2% in the MgO powder that after calcining, obtains, and the content of CaO is 3.4%, other impurity (SiO
2, Fe
2O
3Deng) be 6.4%.
(2) the aqueous ammonium chloride solution 1000ml of configuration 4mol/L places reaction kettle, and the temperature of reaction kettle is controlled at 105 ℃, takes by weighing MgO powder 80g that step (1) obtains in reaction kettle, stir 2h after, naturally cool to room temperature.
(3) magma that step (2) is obtained filters, and separates and removes insoluble impurities, after the washing drying, is weighed as 8.1g.The content of magnesium is 1.81mol/L in the magnesium chloride solution that obtains, and the content of calcium is 0.01mol/L;
(4) the magnesium chloride solution 500mL that step (3) is obtained places reaction crystalizer, and the temperature of control reaction crystalizer is 50 ℃, adds X 2073 as surface treatment agent, feeds this solution of ammonia processing and is settled out Marinco H (Mg (OH)
2).After reaction finishes, the temperature of reactive crystallization still is risen to 90 ℃, continue to stir 2h;
(5) magma that step (4) is obtained filters, and obtains the Mg (OH) of flame retardant type through washing, drying
2The purity of final Marinco H is 99.26%, and the content of CaO is 0.3%.
(6) mother liquor after the magma that step (4) is obtained filters returns step (2) as the molten required leaching solvent of low-grade magnesium oxide powder that soaks of selectivity.
Embodiment two
(1) under 450 ℃ temperature, in retort furnace, with low-grade magnesite calcining 240 minutes.Under this temperature, calcium is still with CaCO in the MgO powder that obtains
3Form exist.With the chemical constitution of chemical analysis assay determination calcining back magnesite, the content of MgO is 89.5% in the MgO powder that after calcining, obtains, and the content of CaO is 3.6%, other impurity (SiO
2, Fe
2O
3Deng) be 6.9%.
(2) the aqueous ammonium chloride solution 1000ml of configuration 4mol/L places reaction kettle, and the temperature of reaction kettle is controlled at 180 ℃, takes by weighing MgO powder 80g that step (1) obtains in reaction kettle, stir 2h after, naturally cool to room temperature.
(3) magma that step (2) is obtained filters, and separates and removes insoluble impurities, after the washing drying, is weighed as 9.1g.The content of magnesium is 1.72mol/L in the magnesium chloride solution that obtains, and the content of calcium is 0.009mol/L;
(4) the magnesium chloride solution 500mL that step (3) is obtained places reaction crystalizer, and the temperature of control reaction crystalizer is 60 ℃, adds X 2073 as surface treatment agent, feeds this solution of ammonia processing and is settled out Marinco H (Mg (OH)
2).After reaction finishes, the temperature of reactive crystallization still is risen to 100 ℃, continue to stir 2h;
(5) magma that step (4) is obtained filters, and obtains the Mg (OH) of flame retardant type through washing, drying
2The purity of final Marinco H is 99.08%, and the content of CaO is 0.32%.
(6) mother liquor after the magma that step (4) is obtained filters returns step (2) as the molten required leaching solvent of low-grade magnesium oxide powder that soaks of selectivity.
Embodiment three
(1) under 890 ℃ temperature, in retort furnace, with low-grade brucite mineral calcining 240 minutes.With the chemical constitution of chemical analysis assay determination calcining back magnesite, the content of MgO is 95.1% in the MgO powder that after calcining, obtains, and the content of CaO is 2.9%, other impurity (SiO
2, Fe
2O
3Deng) be 2.0%.
(2) the aqueous ammonium chloride solution 1000ml of configuration 4mol/L places reaction kettle, and the temperature of reaction kettle is controlled at 180 ℃, takes by weighing MgO powder 80g that step (1) obtains in reaction kettle, stir 2h after, naturally cool to room temperature.
(3) magma that step (2) is obtained filters, and separates and removes insoluble impurities, after the washing drying, is weighed as 3.05g.The content of magnesium is 1.81mol/L in the magnesium chloride solution that obtains, and the content of calcium is 0.012mol/L;
(4) the magnesium chloride solution 500mL that step (3) is obtained places reaction crystalizer, and the temperature of control reaction crystalizer is 50 ℃, adds cetyl trimethylammonium bromide as surface treatment agent, feeds this solution of ammonia processing and is settled out Marinco H (Mg (OH)
2).After reaction finishes, the temperature of reactive crystallization still is risen to 90 ℃, continue to stir 2h;
(5) magma that step (4) is obtained filters, and obtains the Mg (OH) of flame retardant type through washing, drying
2The purity of final Marinco H is 99.32%, and the content of CaO is 0.31%.
(6) mother liquor after the magma that step (4) is obtained filters returns step (2) as the molten required leaching solvent of low-grade magnesium oxide powder that soaks of selectivity.
Applicant's statement; The present invention explains detailed process parameter of the present invention and technical process through the foregoing description; But the present invention is not limited to above-mentioned detailed process parameter and technical process, does not mean that promptly the present invention must rely on above-mentioned detailed process parameter and technical process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. the working method of a Flame Retardant Magnesium Hydroxide comprises the steps:
(1) with the levigate magnesium oxide powder that obtains of the magnesium-containing ore after the roasting;
(2) magnesium oxide powder with step (1) gained places reaction vessel,, stirs and makes its reaction as leaching solvent with the ammonium class aqueous solution, then reaction solution is naturally cooled to room temperature and gets magma;
(3) magma that step (2) is obtained filters, and removes insoluble impurities, obtains Mg-bearing water solution;
(4) the Mg-bearing water solution that step (3) is obtained places reaction crystalizer, handles with ammonia, is settled out Marinco H;
(5) reacting liquid filtering that step (4) is obtained obtains Marinco H, and washing, drying obtain Flame Retardant Magnesium Hydroxide.
2. method according to claim 1 is characterized in that, the maturing temperature described in the step (1) is 300～890 ℃, preferred 450～650 ℃.
3. method according to claim 1 is characterized in that, used magnesium-containing ore is low-grade magnesium ore deposits such as magnesite, brucite mineral in the step (1).
4. method according to claim 1 is characterized in that, the reaction vessel described in the step (2) is a reaction kettle.
5. method according to claim 1 is characterized in that, the ammonium class described in the step (2) is ammonium chloride, ammonium sulfate, monoammonium sulfate or an ammonium nitrate, or its mixture.
6. method according to claim 1 is characterized in that, the leaching solvent described in the step (2) contains NH
4 +The ionic amount of substance is equal to or greater than the amount of substance of institute's dissolved magnesium, preferred NH
4 +The ionic amount of substance is equal to or greater than 2 times of amount of substance of institute's dissolved magnesium.
7. method according to claim 1 is characterized in that, the leaching solvent described in the step (2) is the filtrating in the step (5).
8. method according to claim 1 is characterized in that, the churning time in the step (2) is not less than 2h, and temperature of reaction is 0～180 ℃, preferred 105～180 ℃.
9. method according to claim 1 is characterized in that, the ammonia described in the step (4) is the molten ammonia that discharges in the magnesium oxide powder process that soaks of the ammonium class aqueous solution in the step (2).
10. method according to claim 1; It is characterized in that the treating processes described in the step (4) is following: the temperature of control reaction crystalizer adds X 2073 or cetyl trimethylammonium bromide as surface treatment agent; Feed this solution of ammonia processing and be settled out Marinco H; After reaction finished, the temperature rising with reaction crystalizer continued to stir;
Preferably, the temperature of reaction crystalizer is initially and is not less than 40 ℃, is preferably 50～60 ℃; The temperature of the reaction crystalizer after the rising is not less than 80 ℃, is preferably 90～100 ℃; Churning time is not less than 1h, is preferably to be not less than 2h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104743585A (en) * | 2015-03-04 | 2015-07-01 | 上海应用技术学院 | Method for preparing flame retardant grade magnesium hydroxide |
| CN106590689A (en) * | 2016-12-26 | 2017-04-26 | 荆门市格林美新材料有限公司 | Method for preparing composite flame retardant through recovering aluminum and magnesium from different types of sludge |
| CN109133822A (en) * | 2018-10-08 | 2019-01-04 | 苏州市泽镁新材料科技有限公司 | A kind of combined oxidation magnesium-based curing agent, preparation method and application |
| CN114249340A (en) * | 2021-12-07 | 2022-03-29 | 郑州大学 | Preparation method of nanorod magnesium hydroxide flame retardant based on microcrystalline magnesite |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104743585A (en) * | 2015-03-04 | 2015-07-01 | 上海应用技术学院 | Method for preparing flame retardant grade magnesium hydroxide |
| CN104743585B (en) * | 2015-03-04 | 2016-08-17 | 上海应用技术学院 | A kind of method preparing flame-proof magnesium hydroxide |
| CN106590689A (en) * | 2016-12-26 | 2017-04-26 | 荆门市格林美新材料有限公司 | Method for preparing composite flame retardant through recovering aluminum and magnesium from different types of sludge |
| CN106590689B (en) * | 2016-12-26 | 2018-06-19 | 荆门市格林美新材料有限公司 | The method that magnalium prepares composite flame-retardant agent is recycled from different sludge |
| CN109133822A (en) * | 2018-10-08 | 2019-01-04 | 苏州市泽镁新材料科技有限公司 | A kind of combined oxidation magnesium-based curing agent, preparation method and application |
| CN114249340A (en) * | 2021-12-07 | 2022-03-29 | 郑州大学 | Preparation method of nanorod magnesium hydroxide flame retardant based on microcrystalline magnesite |
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Application publication date: 20120620 |