CN102167370A - Method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge - Google Patents
Method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge Download PDFInfo
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- CN102167370A CN102167370A CN2010105616651A CN201010561665A CN102167370A CN 102167370 A CN102167370 A CN 102167370A CN 2010105616651 A CN2010105616651 A CN 2010105616651A CN 201010561665 A CN201010561665 A CN 201010561665A CN 102167370 A CN102167370 A CN 102167370A
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- magnesium chloride
- boric sludge
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Abstract
The invention belongs to the technical field of three-waste disposal and comprehensive utilization in the inorganic chemical industry, in particular relating to a method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge. The method mainly comprises the following steps: firstly, heating the boric sludge by steam, separating and then reacting the obtained boric sludge with hydrochloric acid; and after filtering, reacting the filtrate with magnesium hydroxide, thus finally obtaining the products of anhydrous magnesium chloride, manganic hydroxide and calcium hydroxide. The method ensures that the boric sludge waste residue can be thoroughly removed, so that the environment pollution caused by the boric sludge waste residue can be reduced; the valuable anhydrous magnesium chloride, manganic hydroxide and calcium hydroxide can be prepared, so that the method has remarkable social benefits and economic benefits; and furthermore, the technique and production equipment are simple, so that the method is a more practical treatment and utilization method.
Description
Technical field
The invention belongs to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly a kind of method that is equipped with Magnesium Chloride Anhydrous coproduction manganous hydroxide and calcium hydroxide with boric sludge.
Technical background
Producing the waste residue that products such as boric acid, borax produce, is with szaibelyite (MgOB
2O
3H
2O) be raw material, by roasting, pulverizing, mix, take the carbon water law to produce borax (Na with soda ash
2B
4O
710H
2O), washing again, crystallisation process extract the solid waste that is left behind the borax; This solid waste is canescence, yellow-white powdery solid, is alkalescence, contains components such as boron oxide and magnesium oxide, is commonly called as " boron mud ".One ton of borax of boron mud production can produce 4 tons of boron mud, and a borax of producing 8000 tons produces, and can produce 3.2 ten thousand tons in boron mud every year.The disposal of storing up of boron mud not only takies a large amount of soils, and can make near the alkalization of soils the stockyard and cause that the migration of boron transforms, and causes environmental pollution.Because the quantity discharged of boron mud is bigger, the present domestic multiple comprehensive Utilization Ways of taking except that producing Magnesium Carbonate Light 41-45 and magnesium oxide and plastic and rubber filler, also has the coal of producing boron magnesium phosphorus composite fertilizer, making honeycomb briquette to add labor and materials and do architectural borax etc.Though these methods are handled filter residue certain effect being arranged, all is to want buy-birth production art complexity, or the product that generates is comparatively single; Boric sludge also of no use is equipped with the relevant report of the method for Magnesium Chloride Anhydrous coproduction manganous hydroxide and calcium hydroxide at present.
Summary of the invention
The invention provides the method that is equipped with Magnesium Chloride Anhydrous coproduction manganous hydroxide and calcium hydroxide with boric sludge, this method can not only effectively be handled waste residue, can also make multiple value product.
To achieve the above object, technical scheme of the present invention is:
A kind ofly be equipped with the method for Magnesium Chloride Anhydrous coproduction manganous hydroxide and calcium hydroxide, it is characterized in that, comprise being prepared as follows step with boric sludge:
Steps A, boron mud is transferred in the reactor, heats, when temperature reaches 60 ℃～80 ℃, be incubated 1～2 hour with steam;
Step B, with in the steps A heat boron mud carry out solid-liquid separation with the drying whizzer, liquid is sent to deep processing;
Step C, separating obtained boron mud solid among the step B is sent into first corrosion-resistant reactor, add hydrochloric acid soln toward first corrosion-resistant reactor simultaneously, stir and make it to react; Described boron mud solid and hydrochloric acid soln react with the pure mass ratio of converting 1: 1.63～2.03; Reaction generates the hydrate of magnesium chloride, and other components generate calcium chloride and also have a small amount of Manganous chloride tetrahydrate.
Step D, gained reaction mixture among the step C is filtered with first strainer, filter cake is sent to deep processing;
Step e, drop into successively with pure mass ratio 1: 0.57～0.97 and carry out stirring reaction in second corrosion-resistant reactor filtering gained filtrate and magnesium hydroxide among the step D;
Step F, gained mixing solutions in the step e is filtered with second strainer;
Step F, the filter cake that filters gained in the step e washed to check the weight after dryings, drying and the pulverizing with first washing and spin-drying machine, first moisture eliminator and first pulverizer successively be packaged to be calcium hydroxide and manganous hydroxide product;
Step G, the filtrate of filtering gained in the step F sent into carry out underpressure distillation in the underpressure distillation device, after steaming six crystal water, distillate discharged send into the cooling tower cooling, the gained crystal washs to check the weight after dryings, drying and the pulverizing with second washing and spin-drying machine, second moisture eliminator and second pulverizer and is packaged to be the anhydrous chlorides of rase magnesium products.
Preferably, the hydrochloric acid soln among the described step C is that volumetric concentration is 30%～60% hydrochloric acid soln.
Magnesium hydroxide in the described step e is that volumetric concentration is 5%～10% dilute solution.
Reaction principle of the present invention is:
MgO+2HCl＝MgCl
2+H
2O
CaO+2HCl＝CaCl
2+H
2O
CaCl
2+Mg(OH)
2＝MgCl
2·6H
2O+Ca(OH)
2
MnO+2HCl＝MnCl
2+H
2O
MnCl
2+Mg(OH)
2＝MgCl
2·6H
2O+Mn(OH)
2
Magnesium in the boron mud generally all is that the form with magnesiumcarbonate exists, and is sometimes also different and difference arranged along with the mineral products of szaibelyite.The component of producing Magnesium Carbonate Light 41-45 boron mud is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3% manganese oxide 0.11%, other are moisture.
The present invention mainly is earlier with boron mud steam heating, separates then, reacts with hydrochloric acid again, after the filtration filtrate and magnesium hydroxide is reacted, and obtains Magnesium Chloride Anhydrous, manganous hydroxide and calcium hydroxide product at last; The present invention can as clean as a pennyly gulp down boron mud waste residue, alleviates the pollution of boron mud waste residue to environment; Can make valuable Magnesium Chloride Anhydrous, manganous hydroxide and calcium hydroxide again, not only have remarkable social benefit and economic benefit, and technology and production unit are simple, be a kind of relatively actual processing and utilize method.
Description of drawings
Fig. 1 is the process flow sheet that is equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate with boric sludge; Wherein:
The 1-reactor, 2-dries whizzer, 3-first corrosion-resistant reactor, 4-first strainer, 5-second corrosion-resistant reactor, 6-second strainer, 7-first washing and spin-drying machine, 8-first moisture eliminator, 9-first pulverizer, 10-two H 2 O calcium sulphates, 11-manganous hydroxide product, 12-underpressure distillation device, the 13-cooling tower, 14-second washing and spin-drying machine, 15-second moisture eliminator, 16-second pulverizer, 17-anhydrous chlorides of rase magnesium products.
Concrete embodiment
Embodiment 1
A kind ofly be equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate, it is characterized in that, comprise being prepared as follows step with boric sludge:
Steps A, boron mud 1000Kg is transferred in the reactor 1, heats, when temperature reaches 60 ℃～80 ℃, be incubated 1～2 hour with steam; Wherein, magnesium oxide 38% (380Kg), silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3% (30Kg) manganese oxide 0.11% (1.1Kg), other are moisture.
Step B, with in the steps A heat boron mud with the drying whizzer 2 carry out solid-liquid separation, liquid is sent to deep processing;
Step C, separating obtained boron mud solid among the step B is sent into first corrosion-resistant reactor 3, add hydrochloric acid solns toward first corrosion-resistant reactor 3 simultaneously, stir and make it to react; Described boron mud solid and hydrochloric acid soln react with the pure mass ratio of converting at 1: 1.63; Reaction generates the hydrate of magnesium chloride, and other components generate calcium chloride and also have a small amount of Manganous chloride tetrahydrate.Wherein said hydrochloric acid soln is that volumetric concentration is 30%～60% hydrochloric acid soln.
Step D, gained reaction mixture among the step C is filtered with first strainer 4, filter cake is sent to deep processing;
Step e, successively drop into second corrosion-resistant reactor at 1: 0.57 with pure mass ratio and carry out stirring reaction for 5 li filtering gained filtrate and magnesium hydroxide among the step D; Wherein said magnesium hydroxide is that volumetric concentration is 5%～10% dilute solution.
Step F, gained mixing solutions in the step e is filtered with second strainer 6;
Step F, the filter cake that filters gained in the step e washed to check the weight after dryings, drying and the pulverizing with first washing and spin-drying machine 7, first moisture eliminator 8 and first pulverizer 9 successively be packaged to be 13.09Kg calcium hydroxide 10 and 0.95Kg manganous hydroxide product 11;
Step G, the filtrate of filtering gained in the step F sent into carry out underpressure distillation in the underpressure distillation device 12, after steaming six crystal water, distillate discharged send into cooling tower 13 coolings, the gained crystal washs to check the weight after dryings, drying and the pulverizing with second washing and spin-drying machine 14, second moisture eliminator 15 and second pulverizer 16 and is packaged to be 430.12Kg anhydrous chlorides of rase magnesium products 17.
Embodiment 2
A kind ofly be equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate, it is characterized in that, comprise being prepared as follows step with boric sludge:
Steps A, boron mud 1000Kg is transferred in the reactor 1, heats, when temperature reaches 60 ℃～80 ℃, be incubated 1～2 hour with steam; Wherein, magnesium oxide 38% (380Kg), silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3% (30Kg) manganese oxide 0.11% (1.1Kg), other are moisture.
Step B, with in the steps A heat boron mud with the drying whizzer 2 carry out solid-liquid separation, liquid is sent to deep processing;
Step C, separating obtained boron mud solid among the step B is sent into first corrosion-resistant reactor 3, add hydrochloric acid solns toward first corrosion-resistant reactor 3 simultaneously, stir and make it to react; Described boron mud solid and hydrochloric acid soln react with the pure mass ratio of converting at 1: 1.93; Reaction generates the hydrate of magnesium chloride, and other components generate calcium chloride and also have a small amount of Manganous chloride tetrahydrate.Wherein said hydrochloric acid soln is that volumetric concentration is 30%～60% hydrochloric acid soln.
Step D, gained reaction mixture among the step C is filtered with first strainer 4, filter cake is sent to deep processing;
Step e, successively drop into second corrosion-resistant reactor at 1: 0.77 with pure mass ratio and carry out stirring reaction for 5 li filtering gained filtrate and magnesium hydroxide among the step D; Wherein said magnesium hydroxide is that volumetric concentration is 5%～10% dilute solution.
Step F, gained mixing solutions in the step e is filtered with second strainer 6;
Step F, the filter cake that filters gained in the step e washed to check the weight after dryings, drying and the pulverizing with first washing and spin-drying machine 7, first moisture eliminator 8 and first pulverizer 9 successively be packaged to be 20.03Kg calcium hydroxide 10 and 1.05Kg manganous hydroxide product 11;
Step G, the filtrate of filtering gained in the step F sent into carry out underpressure distillation in the underpressure distillation device 12, after steaming six crystal water, distillate discharged send into cooling tower 13 coolings, the gained crystal washs to check the weight after dryings, drying and the pulverizing with second washing and spin-drying machine 14, second moisture eliminator 15 and second pulverizer 16 and is packaged to be 530.67Kg anhydrous chlorides of rase magnesium products 17.
Embodiment 3
A kind ofly be equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate, it is characterized in that, comprise being prepared as follows step with boric sludge:
Steps A, boron mud 1000Kg is transferred in the reactor 1, heats, when temperature reaches 60 ℃～80 ℃, be incubated 1～2 hour with steam; Wherein, magnesium oxide 38% (380Kg), silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3% (30Kg) manganese oxide 0.11% (1.1Kg), other are moisture.
Step B, with in the steps A heat boron mud with the drying whizzer 2 carry out solid-liquid separation, liquid is sent to deep processing;
Step C, separating obtained boron mud solid among the step B is sent into first corrosion-resistant reactor 3, add hydrochloric acid solns toward first corrosion-resistant reactor 3 simultaneously, stir and make it to react; Described boron mud solid and hydrochloric acid soln react with the pure mass ratio of converting at 1: 2.03; Reaction generates the hydrate of magnesium chloride, and other components generate calcium chloride and also have a small amount of Manganous chloride tetrahydrate.Wherein said hydrochloric acid soln is that volumetric concentration is 30%～60% hydrochloric acid soln.
Step D, gained reaction mixture among the step C is filtered with first strainer 4, filter cake is sent to deep processing;
Step e, successively drop into second corrosion-resistant reactor at 1: 0.97 with pure mass ratio and carry out stirring reaction for 5 li filtering gained filtrate and magnesium hydroxide among the step D; Wherein said magnesium hydroxide is that volumetric concentration is 5%～10% dilute solution.
Step F, gained mixing solutions in the step e is filtered with second strainer 6;
Step F, the filter cake that filters gained in the step e washed to check the weight after dryings, drying and the pulverizing with first washing and spin-drying machine 7, first moisture eliminator 8 and first pulverizer 9 successively be packaged to be 33.78Kg calcium hydroxide 10 and 1.33Kg manganous hydroxide product 11;
Step G, the filtrate of filtering gained in the step F sent into carry out underpressure distillation in the underpressure distillation device 12, after steaming six crystal water, distillate discharged send into cooling tower 13 coolings, the gained crystal washs to check the weight after dryings, drying and the pulverizing with second washing and spin-drying machine 14, second moisture eliminator 15 and second pulverizer 16 and is packaged to be 942.38Kg anhydrous chlorides of rase magnesium products 17.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (3)
1. be equipped with the method for Magnesium Chloride Anhydrous coproduction manganous hydroxide and calcium hydroxide with boric sludge, it is characterized in that, comprise being prepared as follows step:
Steps A, boron mud is transferred in the reactor (1), heats, when temperature reaches 60 ℃～80 ℃, be incubated 1～2 hour with steam;
Step B, with in the steps A heat boron mud with the drying whizzer (2) carry out solid-liquid separation, liquid is sent to deep processing;
Step C, separating obtained boron mud solid among the step B is sent into first corrosion-resistant reactor (3), add hydrochloric acid soln toward first corrosion-resistant reactor (3) simultaneously, stir and make it to react; Described boron mud solid and hydrochloric acid soln react with the pure mass ratio of converting 1: 1.63～2.03; Reaction generates the hydrate of magnesium chloride, and other components generate calcium chloride and also have a small amount of Manganous chloride tetrahydrate.
Step D, gained reaction mixture among the step C is filtered with first strainer (4), filter cake is sent to deep processing;
Step e, drop into second corrosion-resistant reactor (5) lining successively with pure mass ratio 1: 0.57～0.97 and carry out stirring reaction filtering gained filtrate and magnesium hydroxide among the step D;
Step F, gained mixing solutions in the step e is filtered with second strainer (6);
Step F, the filter cake that filters gained in the step e used first washing and spin-drying machine (7), first moisture eliminator (8) and first pulverizer (9) to wash to check the weight after dryings, drying and the pulverizing successively be packaged to be calcium hydroxide (10) and manganous hydroxide product (11);
Step G, the filtrate of filtering gained in the step F sent in the underpressure distillation device (12) carry out underpressure distillation, after steaming six crystal water, distillate discharged send into cooling tower (13) cooling, the gained crystal washs to check the weight after drying, drying and the pulverizing with second washing and spin-drying machine (14), second moisture eliminator (15) and second pulverizer (16) and is packaged to be anhydrous chlorides of rase magnesium products (17).
2. according to claim 1ly be equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate, it is characterized in that the hydrochloric acid soln among the described step C is that volumetric concentration is 30%～60% hydrochloric acid soln with boric sludge.
3. according to claim 1ly be equipped with the method for seven aqueous magnesium chloride co-producing sulfuric acid manganese and calcium sulfate, it is characterized in that the magnesium hydroxide in the described step e is that volumetric concentration is 5%～10% dilute solution with boric sludge.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105616651A CN102167370A (en) | 2010-11-25 | 2010-11-25 | Method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105616651A CN102167370A (en) | 2010-11-25 | 2010-11-25 | Method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge |
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| CN2010105616651A Pending CN102167370A (en) | 2010-11-25 | 2010-11-25 | Method for preparing anhydrous magnesium chloride and coproducing manganic hydroxide and calcium hydroxide by utilizing boric sludge |
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Application publication date: 20110831 |