CN105584997A - Method for producing magnesium hydrogen phosphate Heptahydrate by using boron mud - Google Patents
Method for producing magnesium hydrogen phosphate Heptahydrate by using boron mud Download PDFInfo
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- CN105584997A CN105584997A CN201410504567.2A CN201410504567A CN105584997A CN 105584997 A CN105584997 A CN 105584997A CN 201410504567 A CN201410504567 A CN 201410504567A CN 105584997 A CN105584997 A CN 105584997A
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Abstract
The invention provides a method for producing magnesium hydrogen phosphate heptahydrate by using boron mud, and relates to inorganic chemical industry three-waste management and comprehensive utilization. According to the method, boron mud is subjected to acid leaching recovery and purification synthesis to prepare magnesium hydrogen phosphate heptahydrate and co-produce sodium chloride and calcium hydroxide; in the acid leaching recovery step, the boron mud is heated with steam, the heated boron mud is subjected to liquid-solid separation by using a drying centrifuge, the obtained filtrate adopting boric acid as the main component is additionally processed, the filter cake containing magnesium oxide is added with hydrochloric acid so as to be subjected to a reaction to produce a magnesium chloride, calcium chloride and manganese chloride solution, filtering is performed to obtain the filter cake silica, and the obtained filter cake silica is additionally processed; and in the purification synthesis step, the recovered filtrate is subjected to impurity removing with magnesium hydroxide to make calcium chloride and manganese chloride respectively generate hydroxide precipitates, filtering is performed to obtain calcium hydroxide and manganese hydroxide, sodium hydrogen phosphate is added to the magnesium chloride in the filtrate so as to be subjected to a reaction to obtain a magnesium hydrogen phosphate heptahydrate and sodium chloride mixing solution, filtering is performed to obtain the filtrate cake magnesium hydrogen phosphate heptahydrate product, the filtrate is subjected to pressure reducing distillation, and when the solution achieves a saturated state, cooling is performed to precipitate the sodium chloride crystal. With the method of the present invention, the economic benefits of the boron mud waste treatment are improved.
Description
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly one utilizes boron mud to produce seven water phosphorusThe method of acid hydrogen magnesium.
Background technology
Boron mud is with boromagnesite (2MgOB2O3·H2O) be raw material, by roasting, pulverizing, mix with soda ash, take carbon water lawProduce borax (Na2B4O7·10H2O), washing, crystallization process extract after borax remaining solid waste 7 produce one ton of borax canProduce 4 tons of boron mud, produce the borax plant of 8000 tons per year for one, can produce every year boron mud is 3.2 ten thousand tons. Because the discharge capacity of boron mud is larger,The multiple comprehensive Utilization Ways of current domestic employing, except producing light magnesium carbonate and magnesia and plastic and rubber filler, also produces boronMei Lin composite fertilizer, to make the coal of honeycomb briquette reinforced and do architectural borax etc.
Magnesium in boron mud is all generally to exist with the form of magnesium carbonate, sometimes also has difference along with the mineral products difference of boromagnesite.The component of producing light magnesium carbonate boron mud is such: magnesia accounts for 38%, and silica accounts for 20%, and carbon dioxide accounts for 17%,Boron oxide accounts for 3%, and calcium oxide accounts for 3%, and manganese oxide accounts for 0.11%, and other is moisture content.
One, should improve constantly the value of output object to the utilization of boron mud, some markets of output in short supply, product that added value is large,The economic benefit of utilizing to improve boron mud.
Two, well-known, the utilization of boron mud is relevant with magnesium, and magnesium-containing compound is very extensive in the application of each field, wherein seven waterMagnesium monohydrogen phosphate can be used as nutritional supplement, PH conditioning agent, stabilizing agent, packaging material plasticizer etc., and purposes is very extensive.
Therefore,, processing in the technical scheme of boron mud refuse, should consider the recycling of the compound of boron as far as possible, as produce seven waterMagnesium monohydrogen phosphate.
Summary of the invention
The present invention is intended to for the utilization of boron mud and the market demand, and a kind of method of utilizing boron mud to produce seven water magnesium monohydrogen phosphates is provided.
For achieving the above object, a kind of technical scheme of the method that boron mud produces seven water magnesium monohydrogen phosphates of utilizing of the present invention is as follows:
Utilize boron mud to produce a method for seven water magnesium monohydrogen phosphates, boron mud, by acidleach recovery, purifying synthesis technique, is made to sevenWater magnesium monohydrogen phosphate, simultaneously co-producing calcium hydroxide and sodium chloride:
Described acidleach recovery process is: boron is maintained to 1.1～2.1 hours in Steam Heating to 61～81 DEG C for mud, then with dryingThe liquid-solid separation of centrifuge, obtains taking boric acid as main filtrate deep processing separately; Magnesia and hydrochloric acid in filter cake boron mud are pressed pure materialThe mass ratio 1: 1.61～2.05 of meter, reacts in the first corrosion-resistant reactor, stirs; Reaction generates magnesium chloride, calcium chlorideAnd manganese chloride solution; Filtration obtains the deep processing separately of filter cake silica; The filtrate of clarification is done further purifying;
Described purifying synthesis technique is: appropriate magnesium hydroxide impurity and purification for the clear filtrate obtaining through acidleach recovery process, makeCalcium chloride and manganese chloride generate respectively precipitation of hydroxide, and washing after filtration, drying and crushing, sizing screening, packaging obtain respectivelyCalcium hydroxide and manganous hydroxide product; Gained filtrate is magnesium chloride clarified solution; In clarified solution, magnesium chloride and dibastic sodium phosphate are pressed pure materialThe mass ratio 1: 1.61～2.05 of meter reacts in the second corrosion-resistant reactor, stirs; Obtain seven water magnesium monohydrogen phosphate and sodium chlorideMixed liquor; Filter, filter cake is through washing drying, drying and crushing, being packaged to be seven water magnesium monohydrogen phosphate products; Filtrate is sent into decompression and is steamedHeat up in a steamer device and carry out decompression distillation, in the time that solution reaches capacity concentration, distillate is ejected, through being cooled to sodium chloride crystallization, warpWashing, drying, pulverizing obtain sodium chloride crystal product.
The present invention's boron mud used is to produce the boron mud of light magnesium carbonate, and its component is: magnesia, silica, carbon dioxide,Boron oxide, calcium oxide, manganese oxide and moisture. Certainly it is standby that, other boron mud of similar components also can adapt to the present invention's use boric sludgeThe method of basic magnesium carbonate coproduction calcium and manganese hydroxide.
Chemical equation of the present invention is:
MgO+2HCl＝MgCl2+H2O
CaO+2HCl＝CaCl2+H2O
MnO+2HCl＝MnCl2+H2O
CaCl2+Mg(OH)2＝MgCl2+Ca(OH)2
MnCl2+Mg(OH)2＝MgCl2+Mn(OH)2
MgCl2+Na2HPO3+7H2O＝MgHPO3·7H2O+2NaCl
Beneficial effect of the present invention is: one, provides a kind of method of utilizing boron mud to produce seven water magnesium monohydrogen phosphates, Ke YiyouEffect is processed boron mud waste material. Its two, preparation comprises seven water magnesium monohydrogen phosphates, calcium hydroxide and sodium chloride, all serve many purposes,Remarkable in economical benefits, has improved the economic benefit of processing boron mud waste material. Its three, preparation purity is high, quality is guaranteed.
Detailed description of the invention
Embodiment mono-
Utilize boron mud to produce a method for seven water magnesium monohydrogen phosphates, boron mud, by acidleach recovery, purifying synthesis technique, is made to sevenWater magnesium monohydrogen phosphate, simultaneously co-producing calcium hydroxide and sodium chloride; The present invention's boron mud used is the boron mud of producing light magnesium carbonate, its groupBe divided into: magnesia 38%, silica 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture.
Acidleach recovery process is: get 500Kg boron mud Steam Heating to 61～81 DEG C and maintain 1.1～2.1 hours, then with getting rid ofThe liquid-solid separation of dry centrifuge, obtains taking boric acid as main filtrate deep processing separately; Magnesia (pure quality is 190Kg) in filter cake boron mud, react in the first corrosion-resistant reactor by the mass ratio of pure material 1: 1.63 with hydrochloric acid, stir; Reaction generation magnesium chloride,Calcium chloride and manganese chloride solution; Filtration obtains the deep processing separately of filter cake silica; The filtrate of clarification is done further purifying;
Purifying synthesis technique is: appropriate magnesium hydroxide impurity and purification for the clear filtrate obtaining through acidleach recovery process, make chlorinationCalcium and manganese chloride generate respectively precipitation of hydroxide, and washing after filtration, drying and crushing, sizing screening, packaging obtain respectively hydrogen-oxygenChange calcium and a small amount of manganous hydroxide product; Gained filtrate is magnesium chloride clarified solution; (previous reaction generates chlorine to magnesium chloride in clarified solution altogetherChanging magnesium pure quality is 403Kg) and dibastic sodium phosphate react at 1: 1.63 in the second corrosion-resistant reactor by the mass ratio of pure material,Stir; Obtain seven water magnesium monohydrogen phosphates and sodium chloride mixed liquor; Filter, filter cake is through washing drying, drying and crushing, being packaged to be sevenWater magnesium monohydrogen phosphate product 1199Kg; Filtrate is sent into decompression distillation device and is carried out decompression distillation, in the time that solution reaches capacity concentration, will distillLiquid ejects, and through being cooled to sodium chloride crystallization, obtains sodium chloride crystal product 610Kg through washing, drying, pulverizing.
Embodiment bis-
Utilize boron mud to produce a method for seven water magnesium monohydrogen phosphates, boron mud, by acidleach recovery, purifying synthesis technique, is made to sevenWater magnesium monohydrogen phosphate, simultaneously co-producing calcium hydroxide and sodium chloride; The present invention's boron mud used is the boron mud of producing light magnesium carbonate, its groupBe divided into: magnesia 38%, silica 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture.
Acidleach recovery process is: get 500Kg boron mud Steam Heating to 61～81 DEG C and maintain 1.1～2.1 hours, then with getting rid ofThe liquid-solid separation of dry centrifuge, obtains taking boric acid as main filtrate deep processing separately; Magnesia (pure quality is 190Kg) in filter cake boron mud, react in the first corrosion-resistant reactor by the mass ratio of pure material 1: 1.83 with hydrochloric acid, stir; Reaction generation magnesium chloride,Calcium chloride and manganese chloride solution; Filtration obtains the deep processing separately of filter cake silica; The filtrate of clarification is done further purifying;
Purifying synthesis technique is: appropriate magnesium hydroxide impurity and purification for the clear filtrate obtaining through acidleach recovery process, make chlorinationCalcium and manganese chloride generate respectively precipitation of hydroxide, and washing after filtration, drying and crushing, sizing screening, packaging obtain respectively hydrogen-oxygenChange calcium and a small amount of manganous hydroxide product; Gained filtrate is magnesium chloride clarified solution; (previous reaction generates chlorine to magnesium chloride in clarified solution altogetherChanging magnesium pure quality is 452Kg) and dibastic sodium phosphate react at 1: 1.83 in the second corrosion-resistant reactor by the mass ratio of pure material,Stir; Obtain seven water magnesium monohydrogen phosphates and sodium chloride mixed liquor; Filter, filter cake is through washing drying, drying and crushing, being packaged to be sevenWater magnesium monohydrogen phosphate product 1510Kg; Filtrate is sent into decompression distillation device and is carried out decompression distillation, in the time that solution reaches capacity concentration, will distillLiquid ejects, and through being cooled to sodium chloride crystallization, obtains sodium chloride crystal product 768Kg through washing, drying, pulverizing.
Embodiment tri-
Utilize boron mud to produce a method for seven water magnesium monohydrogen phosphates, boron mud, by acidleach recovery, purifying synthesis technique, is made to sevenWater magnesium monohydrogen phosphate, simultaneously co-producing calcium hydroxide and sodium chloride; The present invention's boron mud used is the boron mud of producing light magnesium carbonate, its groupBe divided into: magnesia 38%, silica 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture.
Acidleach recovery process is: get 500Kg boron mud Steam Heating to 61～81 DEG C and maintain 1.1～2.1 hours, then with getting rid ofThe liquid-solid separation of dry centrifuge, obtains taking boric acid as main filtrate deep processing separately; Magnesia (pure quality is 190Kg) in filter cake boron mud, react in the first corrosion-resistant reactor by the mass ratio of pure material 1: 2.03 with hydrochloric acid, stir; Reaction generation magnesium chloride,Calcium chloride and manganese chloride solution; Filtration obtains the deep processing separately of filter cake silica; The filtrate of clarification is done further purifying;
Purifying synthesis technique is: appropriate magnesium hydroxide impurity and purification for the clear filtrate obtaining through acidleach recovery process, make chlorinationCalcium and manganese chloride generate respectively precipitation of hydroxide, and washing after filtration, drying and crushing, sizing screening, packaging obtain respectively hydrogen-oxygenChange calcium and a small amount of manganous hydroxide product; Gained filtrate is magnesium chloride clarified solution; (previous reaction generates chlorine to magnesium chloride in clarified solution altogetherChanging magnesium pure quality is 502Kg) and dibastic sodium phosphate react at 1: 2.03 in the second corrosion-resistant reactor by the mass ratio of pure material,Stir; Obtain seven water magnesium monohydrogen phosphates and sodium chloride mixed liquor; Filter, filter cake is through washing drying, drying and crushing, being packaged to be sevenWater magnesium monohydrogen phosphate product 1860Kg; Filtrate is sent into decompression distillation device and is carried out decompression distillation, in the time that solution reaches capacity concentration, will distillLiquid ejects, and through being cooled to sodium chloride crystallization, obtains sodium chloride crystal product 946Kg through washing, drying, pulverizing.
Claims (2)
1. utilize boron mud to produce a method for seven water magnesium monohydrogen phosphates, it is characterized in that: boron mud is synthetic by acidleach recovery, purifyingTechnique, makes seven water magnesium monohydrogen phosphates, simultaneously co-producing calcium hydroxide and sodium chloride: described acidleach recovery process is: by steaming for boron mudVapour is heated to 61～81 DEG C and maintains 1.1～2.1 hours, then with drying the liquid-solid separation of centrifuge, obtains taking boric acid as main filterLiquid is deep processing separately; Magnesia in filter cake boron mud and hydrochloric acid, by the mass ratio of pure material 1: 1.61～2.05, react onIn one corrosion-resistant reactor, stir; Reaction generates magnesium chloride, calcium chloride and manganese chloride solution; Filtration obtains filter cake silicaDeep processing separately; The filtrate of clarification is done further purifying; Described purifying synthesis technique is: what obtain through acidleach recovery process is clearAppropriate magnesium hydroxide impurity and purification for clear filtrate, make calcium chloride and manganese chloride generate respectively precipitation of hydroxide, washing after filtration,Drying and crushing, sizing screening, packaging obtain respectively calcium hydroxide and manganous hydroxide product; Gained filtrate is magnesium chloride clarified solution;In clarified solution, magnesium chloride and dibastic sodium phosphate react in the second corrosion-resistant reactor by the mass ratio of pure material 1: 1.61～2.05,Stir; Obtain seven water magnesium monohydrogen phosphates and sodium chloride mixed liquor; Filter, filter cake is through washing drying, drying and crushing, being packaged to be sevenWater magnesium monohydrogen phosphate product; Filtrate is sent into decompression distillation device and is carried out decompression distillation, in the time that solution reaches capacity concentration, distillate is dischargedCome, through being cooled to sodium chloride crystallization, obtain sodium chloride crystal product through washing, drying, pulverizing.
2. a kind of method of utilizing boron mud to produce seven water magnesium monohydrogen phosphates according to claim 1, is characterized in that: described boronMud, contains magnesia, silica, carbon dioxide, boron oxide, calcium oxide, manganese oxide and moisture in its component.
Priority Applications (1)
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| CN201410504567.2A CN105584997A (en) | 2014-09-16 | 2014-09-16 | Method for producing magnesium hydrogen phosphate Heptahydrate by using boron mud |
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| CN201410504567.2A CN105584997A (en) | 2014-09-16 | 2014-09-16 | Method for producing magnesium hydrogen phosphate Heptahydrate by using boron mud |
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| CN105584997A true CN105584997A (en) | 2016-05-18 |
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| CN201410504567.2A Pending CN105584997A (en) | 2014-09-16 | 2014-09-16 | Method for producing magnesium hydrogen phosphate Heptahydrate by using boron mud |
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Application publication date: 20160518 |
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