CN101759207A - Process for producing high-purity magnesium hydroxide through brine-lime method - Google Patents
Process for producing high-purity magnesium hydroxide through brine-lime method Download PDFInfo
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- CN101759207A CN101759207A CN200910020974A CN200910020974A CN101759207A CN 101759207 A CN101759207 A CN 101759207A CN 200910020974 A CN200910020974 A CN 200910020974A CN 200910020974 A CN200910020974 A CN 200910020974A CN 101759207 A CN101759207 A CN 101759207A
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- lime
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Abstract
The present invention discloses a process for producing high-purity magnesium hydroxide through brine-lime method. The process produces magnesium hydroxide by means of reaction of saturated lime solution and refined brine which is refined salt lake brine or sea salts or magnesium chloride solution, a mother liquor is obtained after precipitating the magnesium hydroxide resulting from the reaction of saturated lime solution and refined brine and is then submitted to desulfurization to re-digest and re-dissolve lime to prepare saturated lime solution. Conventional calcium hydroxide slurry slag removal technique of whirl flow combined with screening only removes big impurity granules while causing part of lime lost and is incapable of removing small impurities, and the content of calcium hydroxide is in the range of from 80% to 85%; by replacing lime milk with saturated lime solution, the present invention removes insoluble impurities easily and obtains precipitate containing more than 98% of calcium hydroxide and less than 2% of other impurities.
Description
Technical field
The present invention relates to a kind of technology of producing high-purity magnesium hydroxide through brine-lime method.
Background technology
At present, the bittern main technique method of carrying magnesium industry has: lime-bittern method, sodium hydroxide-bittern method, ammonia-bittern method etc.As precipitation agent, water (or hot water) digests lime to lime-bittern method, is diluted to certain concentration with reaction mother liquor again with lime, forms calcium hydroxide slurry.Through sieving, modes such as eddy flow removal of impurities are bigger with some particles again, and the impurity that proportion is bigger is removed, and makes calcium hydroxide emulsion (milk of lime) precipitation agent of slurries shape, and the refining bittern with the process impurity desulfurization reacts then, makes magnesium hydroxide products.Said process seems simply, but will realize this process and obtain highly purified magnesium hydroxide (purity is greater than 98%) product, but is a very thing of difficulty, can be subjected to the influence and the restriction of various factors.This technology can't be removed insoluble detrimental impurity such as lime carbonate in the milk of lime, iron, aluminium, sulphur effectively, the lime utilization ratio is lower, wherein the existence of CaO impurity is to influence one of important factor of product purity and quality, cause the magnesium hydroxide products purity of producing low, the foreign matter content height can't satisfy the needs of middle and high-end market.Because of traditional bittern lime method technology falls behind, quality product is lower, and domestic mid-to high-end product does not have manufacturer to adopt basically, and adopts bittern carbon ammonia method, bittern ammonia process or bittern sodium hydroxide method.But bittern carbon ammonia method, bittern ammonia process or bittern sodium hydroxide method are produced the weak point of magnesium hydroxide: the cost height, product tap density big (influencing use range), and easily form secondary pollution causes production environment and surrounding enviroment to have a strong impact on.
Use the bittern lime method significantly to reduce production costs, can solve the environmental issue in the production process, but the key of problem is to adopt the magnesium hydroxide products purity of bittern lime method production low, of poor quality at present, can't satisfy the needs of middle and high-end market.Causing low, the ropy major cause of product purity is that Wingdale can't be with SiO in the process of calcining digestion formation milk of lime
2, Al
2O
3, Fe
2O
3Remove these impurity and CaCO Deng impurity
3Impurity is mixed in the magnesium hydroxide together, can't effectively separate.Therefore, exploitation bittern lime method production high purity magnesium hydrate new technology is imperative.
Summary of the invention
The technology that the purpose of this invention is to provide a kind of producing high-purity magnesium hydroxide through brine-lime method, traditional technology production product purity is low to overcome, the shortcoming of mass deficiency.
Implementation procedure of the present invention is as follows:
A kind of technology with producing high-purity magnesium hydroxide through brine-lime method uses the reaction of saturated lime solution and refining bittern to produce magnesium hydroxide, and described refining bittern is the magnesium chloride solution of purified salt lake bittern water, sea salt bittern or human configuration; The mother liquor process desulfurization processing that obtains behind saturated lime solution and the refining bittern reaction production magnesium hydroxide is used for digestion once more, dissolving lime prepares saturated lime solution, and the desulfurization processing is to add lime mud in mother liquor, to reach the purpose of removing sulfate radical.
Contain SO in raw material salt lake bittern water or the sea salt bittern
4 2-, can influence product purity.Available calcium chloride reacts as sulfur elimination, and its chemical reaction equation is:
CaCl
2+MgSO
4+2H
2O→CaSO
4·2H
2O↓+MgCl
2
Separate the sulfate dihydrate calcium deposit that generates, can obtain qualified magnesium chloride stock liquid.All contain CO in the general magnesium salt solution
3 2-, HCO
3 -, add and to generate magnesiumcarbonate behind the alkali and influence product purity, thereby during synthetic high purity magnesium hydroxide, must remove CO earlier
3 2-, can in magnesium salt solution, add CaCl
2Solution generates CaCO
3Precipitation and effectively removing, thus refining to bittern finished.
Beneficial effect of the present invention:
(1) traditional calcium hydroxide slurry deslagging process be eddy flow in conjunction with sieving, only can remove bigger impurity particle, lose part lime simultaneously, can't remove the impurity that particle is less, the content of calcium hydroxide is between 80%--85%.The contriver studied by the several years, found to adopt saturated lime solution replacing lime breast, and insoluble impurities is easy to remove, and obtains calcium hydroxide at the precipitation agent more than 98%, and other foreign matter content is less than 2%.
(2) the lime utilization ratio significantly improves, and impurity-eliminating effect thoroughly, reaction is quick and complete, do not reunite, and can once produce high purity magnesium hydroxide product cheaply.The bittern carbon ammonia method that its cost is more traditional, technology costs such as bittern ammonia process, bittern sodium hydroxide method significantly reduce, and can reach the commercial scale production level of 3000t/a.
(3) use the reaction of high-purity hydrogen calcium oxide precipitation agent and refining bittern, because aqua calcis concentration is low, be difficult for producing the concentration tonsure, reaction is uniformly dispersed, and the product that obtains is difficult for reuniting, good dispersity, easily washing, primary particle size little (about 5-20 micron).Can obtain particle good, be easy to the high purity magnesium hydroxide product that filters, wash, product is amounted to content of magnesia 〉=67.5%, calcium oxide content<0.8%, other foreign matter content<1.2%, tap density≤0.12g/ml.And the direct hybrid reaction of existing technology of employing milk of lime can't guarantee to mix, and easily produces and reunites, and causes the impurity parcel, influences product purity and particle diameter.Product content of magnesia≤62%, particle diameter 10-100 micron, tap density 〉=0.25g/ml, calcium oxide content>2%.
Embodiment
Below in conjunction with embodiment content of the present invention is described further.
Embodiment 1:
Bittern is taken from the Shaanxi deckle, carries out desulfurization, decarburization pre-treatment before the reaction, and adding calcium chloride is done desulfurization, decarburizer reacts, and removes part SO
4 2-, and CO
3 2-, HCO
3 -Thereby, finish refining to bittern, SO in the bittern after refining
4 2-Content is 2.1g/L.
Wingdale is taken from Inner Mongol chessboard well, obtains CaO after 950 ℃ of calcinings, and with 80 ℃ hot water digestion CaO, it is standby to get clear liquid.
The refining bittern of measuring 2000ml is put into there-necked flask, and control reaction temperature is 20 ℃, stirs, saturated lime solution is dripped in the bittern, and control reaction end pH value of solution value is 10.4, stops behind the 2h stirring, filter, washing, 140 ℃ dry magnesium hydrate powder.
Product index: Mg content=67.7%, calcium oxide content=0.4%, other foreign matter content=1.0%, tap density=0.12g/ml.
Contrast is implemented:
Identical with embodiment 1, difference only is: after lime is added the small amount of thermal water-wet and expands, add 80 ℃ of hot water while stirring, incline and get upper strata milk sap and leave standstill, furnishing 100g (lime)/L milk of lime is standby.Use the milk of lime and the bittern reaction of preparation.
Product index: content of magnesia=60.5%, tap density=0.26g/ml, calcium oxide content=2%.
Embodiment 2:
Bittern is taken from Yuncheng, Shanxi, carries out desulfurization, decarburization pre-treatment before the reaction, and adding calcium chloride is done desulfurization, decarburizer reacts, and removes part SO
4 2-, and CO
3 2-, HCO
3 -Thereby, finish refining to bittern, SO in the bittern after refining
4 2-Content is 2.0g/L.
With 70 ℃ hot water digestion CaO, it is standby to get clear liquid.
The refining bittern of measuring 3000ml is put into there-necked flask, and control reaction temperature is 25 ℃, stirs, and Wingdale is dripped in the bittern, and control reaction end pH value of solution value is 10.4, stops behind the 2h stirring, filter, washing, 140 ℃ dry magnesium hydrate powder.
Product index: product index: Mg content=67.6%, calcium oxide content=0.42%, other foreign matter content=1.02%, tap density=0.11g/ml.
Contrast is implemented:
Identical with embodiment 2, difference only is: after lime is added the small amount of thermal water-wet and expands, add 70 ℃ of hot water while stirring, incline and get upper strata milk sap and leave standstill, furnishing 100g (lime)/L milk of lime is standby.Use the milk of lime and the bittern reaction of preparation.
Product index: product index: content of magnesia=60.8%, tap density=0.25g/ml, calcium oxide content=2.04%, other foreign matter content=1.01%.
Claims (5)
1. the technology with producing high-purity magnesium hydroxide through brine-lime method is characterized in that: use the reaction of saturated lime solution and refining bittern to produce magnesium hydroxide.
2. according to the technology of the described producing high-purity magnesium hydroxide through brine-lime method of claim 1, it is characterized in that: described refining bittern is purified salt lake bittern water or sea salt bittern or magnesium chloride solution.
3. according to the technology of the described producing high-purity magnesium hydroxide through brine-lime method of claim 2, it is characterized in that: refining bittern is to add calcium chloride solution to obtain behind reaction desulfuration in salt lake brine or sea salt bittern.
4. according to the technology of the described producing high-purity magnesium hydroxide through brine-lime method of claim 1, it is characterized in that: the magnesium hydroxide that saturated lime solution and the reaction of refining bittern obtain obtains mother liquor through post precipitation, be used for digestion, dissolving lime after mother liquor is handled through desulfurization once more, prepare saturated lime solution.
5. according to the technology of the described producing high-purity magnesium hydroxide through brine-lime method of claim 4, it is characterized in that: it is to add lime mud to remove sulfate radical in mother liquor that desulfurization is handled.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102862997A (en) * | 2012-10-09 | 2013-01-09 | 新疆安华矿业投资有限公司 | Method for removing magnesium and sulfate ion in salt lake brine of hexahydric salt-water system |
CN102874851A (en) * | 2012-09-28 | 2013-01-16 | 沈阳化工大学 | Method of utilizing brine to coproduce magnesium hydroxide and calcium sulfate whisker |
CN103551019A (en) * | 2013-09-25 | 2014-02-05 | 林思源 | Desulphurization technology for utilizing sodium salt in salt making bittern as desulfurizer |
CN105271311A (en) * | 2015-10-16 | 2016-01-27 | 华陆工程科技有限责任公司 | Water-saving technology for removing magnesium from lithium chloride solution |
CN111434371A (en) * | 2019-01-14 | 2020-07-21 | *** | Desulfurizing and deslagging agent taking liquid form as raw material and preparation method |
CN112194155A (en) * | 2020-10-14 | 2021-01-08 | 陕西嘉裕化工有限公司 | Method for producing high-purity magnesium oxide by adopting brine-carbide slag method |
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 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1148570A (en) * | 1996-08-20 | 1997-04-30 | 刘品 | Production of magnesium hydroxide and application thereof |
CN101229925A (en) * | 2007-10-11 | 2008-07-30 | 河北科技大学 | Method for preparing magnesium hydroxide with coproduction of calcium chloride |
-
2009
- 2009-01-19 CN CN200910020974A patent/CN101759207B/en not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102874851A (en) * | 2012-09-28 | 2013-01-16 | 沈阳化工大学 | Method of utilizing brine to coproduce magnesium hydroxide and calcium sulfate whisker |
CN102862997A (en) * | 2012-10-09 | 2013-01-09 | 新疆安华矿业投资有限公司 | Method for removing magnesium and sulfate ion in salt lake brine of hexahydric salt-water system |
CN103551019A (en) * | 2013-09-25 | 2014-02-05 | 林思源 | Desulphurization technology for utilizing sodium salt in salt making bittern as desulfurizer |
CN103551019B (en) * | 2013-09-25 | 2015-11-04 | 林思源 | A kind ofly utilize the sodium salt in the old halogen of salt manufacturing as the sulfur removal technology of desulfurizing agent |
CN105271311A (en) * | 2015-10-16 | 2016-01-27 | 华陆工程科技有限责任公司 | Water-saving technology for removing magnesium from lithium chloride solution |
CN111434371A (en) * | 2019-01-14 | 2020-07-21 | *** | Desulfurizing and deslagging agent taking liquid form as raw material and preparation method |
CN112194155A (en) * | 2020-10-14 | 2021-01-08 | 陕西嘉裕化工有限公司 | Method for producing high-purity magnesium oxide by adopting brine-carbide slag method |
CN112194155B (en) * | 2020-10-14 | 2023-11-03 | 陕西航泰镁基材料科技有限公司 | Method for producing high-purity magnesium oxide by brine-carbide slag method |
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 |
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