CN102115104A - Method for co-production of magnesium nitrate anhydride and calcium hydroxide/manganese hydroxide from boron slag - Google Patents
Method for co-production of magnesium nitrate anhydride and calcium hydroxide/manganese hydroxide from boron slag Download PDFInfo
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- CN102115104A CN102115104A CN2010105737054A CN201010573705A CN102115104A CN 102115104 A CN102115104 A CN 102115104A CN 2010105737054 A CN2010105737054 A CN 2010105737054A CN 201010573705 A CN201010573705 A CN 201010573705A CN 102115104 A CN102115104 A CN 102115104A
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Abstract
The invention provides a method for co-production of magnesium nitrate anhydride and calcium hydroxide/manganese hydroxide from boron slag, and relates to the field of treatment and comprehensive utilization of three wastes in the inorganic chemical industry. In the method, the boron slag is subject to acid treatment and recovery procedures and a synthesis and purification procedure to produce magnesium nitrate anhydride as well as calcium hydroxide and manganese hydroxide at the same time. In the acid treatment and recovery procedure, the boron slag is heated with steam, spin-dried and subjected to liquid-solid separation, to produce a filtrate mainly containing boric acid, which is ready for the further deep-processing; magnesium oxide in the boron slag filter cake reacts with hydrochloric acid in a first corrosion-resistant reactor to produce a magnesium chloride hydrate, and other components in the boron slag filter cake reacts with hydrochloric acid to produce calcium chloride and magnesium chloride; and the reaction product is filtered to produce a filter cake of silicon dioxide, which is ready for the further deep-processing. In the synthesis and purification procedure, an appropriate amount of magnesium hydroxide is added to the clear filtrate to remove impurities, the reaction product is filtered to produce a clear solution of magnesium chloride dihydrate, the clear solution of magnesium chloride dihydrate reacts with nitric acid in a second corrosion-resistant reactor, and the reaction product is filtered, distilled under a reduced pressure, crystallized, washed, spin-dried and pulverized to obtain a magnesium nitrate product. By adopting the method, economic benefits obtained from boron slag waste treatment are increased.
Description
Technical field:
The present invention relates 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 nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge.
Technical background:
Boron mud is with szaibelyite (2MgOB
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), remaining solid waste after washing, crystallisation process extract borax.Produce one ton of borax and can produce 4 tons of boron mud, a borax plant that produces 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Because the quantity discharged of boron mud is bigger, the multiple comprehensive Utilization Ways of present domestic employing 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 reinforced and do architectural borax etc.
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 content.
One should improve constantly the value of output object to the utilization of boron mud, and some markets of output product in short supply, that added value is big is to improve the economic benefit that boron mud utilizes.
Its two, well-known, the utilization of boron mud is relevant with magnesium.Magnesium is subjected to people's attention to the effect of industry in recent years, and magnesium is red-letter day fireworks, the essential raw material of salvo; Fireworks often are applied in the business activity, and fireworks are that business activity has increased many colors, and therefore, fireworks are subjected to people's welcome, often use magnesium nitrate in the fireworks.Magnesium nitrate still is applied to dewatering agent, manufacturing explosive, catalyst catalyzer and other magnesium salts and nitrate raw material, the wheat fogging agent etc. of concentrated nitric acid except being used to make the fireworks.
Summary of the invention:
The present invention is intended at the utilization of boron mud and the market requirement, and a kind of method that is equipped with magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge is provided.
To achieve these goals, be equipped with the technical scheme of method of magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge as follows in the present invention.
Be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, boron mud makes the magnesium nitrate anhydride by acid treatment recovery and synthesizing and purifying technology, simultaneously coproduction calcium and manganese oxyhydroxide;
Technology is reclaimed in described acid treatment: boron mud was kept 1～2 hour, and with drying the liquid-solid separation of whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then with steam heating to 60～80 degree.Filter cake boron mud (magnesium oxide meter) reacts in second corrosion-resistant reactor with the pure mass ratio of converting 1: 1.63～2.03 with hydrochloric acid, and stirring issues biochemical reaction blowing slowly.Reaction generates the hydrate of magnesium chloride, and other components generate the Manganous chloride tetrahydrate that calcium chloride also has minute quantity.Filtration obtains filter cake silicon-dioxide and sends to deep processing separately.Clarifying filtrate is done further purifying.
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution, and clarification magnesium chloride that obtains and nitric acid are reacted in second corrosion-resistant reactor with the good mass ratio 1: 1.13～1.53 of pure conversion; Under stirring slowly, generate nine water magnesium nitrate and hydrochloric acid mixed solutions, filtration obtains a spot of impurity filter cake and sends to burning or buried, the clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain nine water magnesium nitrate crystal products; Nine water magnesium nitrates continue distillation again and steam whole crystal water after be cooled to anhydride, after wash, dry, be ground into the anhydrous nitric acid magnesium products; The remaining liquid of distillation is that hydrochloric acid soln returns recycle.
The used boron mud of the present invention is for producing Magnesium Carbonate Light 41-45 boron mud, and its component is such: magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide, other are moisture content.Certainly, other boron mud of similar components also can be suitable for the present invention's the method for preparing magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide.
Chemical equation of the present invention is:
MgO+2HCl＝＝＝＝MgCl
2+H
2O
CaO+2HCl＝＝＝＝CaCl
2+H
2O
CaCl
2+Mg(OH)
2＝＝＝＝MgCl
2+Ca(OH)
2
MnO+2HCl＝＝＝＝MnCl
2+H
2O
MnCl
2+Mg(OH)
2＝＝＝＝MgCl
2+Mn(OH)
2
MgCl
2+2HNO
3+9H
2O＝＝＝＝Mg(NO
3)
2·9H
2O+2HCl
Beneficial effect of the present invention is: one, and provide a kind of and be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, open up an approach for effectively handling boron mud waste material.Its two, preparation comprises magnesium nitrate, calcium hydroxide and manganous hydroxide, wherein magnesium nitrate is the bigger best-selling product of a kind of economic worth, has improved the economic benefit of handling boron mud waste material.Its three, less investment, particularly suitable to the boron mud of used boron mud of process for producing Magnesium Carbonate Light 41-45 and similar components, we can say and opened up a new road.Its four, the purity height of preparation, quality is guaranteed.
Embodiment
Embodiment one
Be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, boron mud makes the magnesium nitrate anhydride by acid treatment recovery and synthesizing and purifying technology, simultaneously coproduction calcium and manganese oxyhydroxide;
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1～2 hour, and with drying the liquid-solid separation of whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then with steam heating to 60～80 degree.Filter cake boron mud (magnesium oxide meter) reacts in first corrosion-resistant reactor with the pure mass ratio of converting with hydrochloric acid at 1: 1.83, and stirring issues biochemical reaction blowing slowly.Reaction generates the hydrate of 454 kilograms of magnesium chlorides, and other components generate the Manganous chloride tetrahydrate that calcium chloride also has minute quantity.Filtration obtains filter cake silicon-dioxide and sends to deep processing separately.Clarifying filtrate is done further purifying.
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution, clarifies magnesium chloride to 454 kilograms that obtain and nitric acid reacts in second corrosion-resistant reactor with the good mass ratio of pure conversion at 1: 1.33; Under stirring slowly, generate nine water magnesium nitrate and hydrochloric acid mixed solutions, filtration obtains a spot of impurity filter cake and sends to burning or buried, the clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 1188.47 kilogram of nine water magnesium nitrate crystal product; Nine water magnesium nitrates continue distillation again and steam whole crystal water after be cooled to anhydride, after washing, dry, pulverize and obtain 412.13 kilograms of anhydrous nitric acid magnesium products; The remaining liquid of distillation is that hydrochloric acid soln returns recycle.
The used boron mud of the present invention is for producing Magnesium Carbonate Light 41-45 boron mud, and its component 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 content.
Embodiment two
Be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, boron mud makes the magnesium nitrate anhydride by acid treatment recovery and synthesizing and purifying technology, simultaneously coproduction calcium and manganese oxyhydroxide;
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1～2 hour, and with drying the liquid-solid separation of whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then with steam heating to 60～80 degree.Filter cake boron mud (magnesium oxide meter) reacts in first corrosion-resistant reactor with the pure mass ratio of converting with hydrochloric acid at 1: 2.03, and stirring issues biochemical reaction blowing slowly.Reaction generates the hydrate of 504 kilograms of magnesium chlorides, and other components generate the Manganous chloride tetrahydrate that calcium chloride also has minute quantity.Filtration obtains filter cake silicon-dioxide and sends to deep processing separately.Clarifying filtrate is done further purifying.
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution, clarifies magnesium chloride to 504 kilograms that obtain and nitric acid reacts in second corrosion-resistant reactor with the good mass ratio of pure conversion at 1: 1.53; Under stirring slowly, generate nine water magnesium nitrate and hydrochloric acid mixed solutions, filtration obtains a spot of impurity filter cake and sends to burning or buried, the clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 1517.76 kilogram of nine water magnesium nitrate crystal product; Nine water magnesium nitrates continue distillation again and steam whole crystal water after be cooled to anhydride, after washing, dry, pulverize and obtain 526.32 kilograms of anhydrous nitric acid magnesium products; The remaining liquid of distillation is that hydrochloric acid soln returns recycle.
The used boron mud of the present invention is for producing Magnesium Carbonate Light 41-45 boron mud, and its component 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 content.
Embodiment three
Be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, boron mud makes the magnesium nitrate anhydride by acid treatment recovery and synthesizing and purifying technology, simultaneously coproduction calcium and manganese oxyhydroxide;
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1～2 hour, and with drying the liquid-solid separation of whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then with steam heating to 60～80 degree.Filter cake boron mud (magnesium oxide meter) reacts in first corrosion-resistant reactor with the pure mass ratio of converting with hydrochloric acid at 1: 1.63, and stirring issues biochemical reaction blowing slowly.Reaction generates the hydrate of 404 kilograms of magnesium chlorides, and other components generate the Manganous chloride tetrahydrate that calcium chloride also has minute quantity.Filtration obtains filter cake silicon-dioxide and sends to deep processing separately.Clarifying filtrate is done further purifying.
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution, clarifies magnesium chloride to 454 kilograms that obtain and nitric acid reacts in second corrosion-resistant reactor with the good mass ratio of pure conversion at 1: 1.13; Under stirring slowly, generate nine water magnesium nitrate and hydrochloric acid mixed solutions, filtration obtains a spot of impurity filter cake and sends to burning or buried, the clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 898.55 kilogram of nine water magnesium nitrate crystal product; Nine water magnesium nitrates continue distillation again and steam whole crystal water after be cooled to anhydride, after washing, dry, pulverize and obtain 311.59 kilograms of anhydrous nitric acid magnesium products; The remaining liquid of distillation is that hydrochloric acid soln returns recycle.
The used boron mud of the present invention is for producing Magnesium Carbonate Light 41-45 boron mud, and its component 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 content.
Claims (2)
1. be equipped with the method for magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge, it is characterized in that: boron mud makes the magnesium nitrate anhydride by acid treatment recovery and synthesizing and purifying technology, simultaneously coproduction calcium and manganese oxyhydroxide;
Technology is reclaimed in described acid treatment: boron mud was kept 1～2 hour, and with drying the liquid-solid separation of whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then with steam heating to 60～80 degree; Filter cake boron mud (magnesium oxide meter) reacts in first corrosion-resistant reactor with the pure mass ratio of converting 1: 1.63～2.03 with hydrochloric acid, stirring issues biochemical reaction blowing slowly, reaction generates the hydrate of magnesium chloride, and other components generate the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution, and clarification magnesium chloride that obtains and nitric acid are reacted in second corrosion-resistant reactor with the good mass ratio 1: 1.13～1.53 of pure conversion; Under stirring slowly, generate nine water magnesium nitrate and hydrochloric acid mixed solutions, filtration obtains a spot of impurity filter cake and sends to burning or buried, the clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain nine water magnesium nitrate crystal products; Nine water magnesium nitrates continue distillation again and steam whole crystal water after be cooled to anhydride, after wash, dry, be ground into the anhydrous nitric acid magnesium products; The remaining liquid of distillation is that hydrochloric acid soln returns recycle.
2. the method that is equipped with magnesium nitrate anhydride coproduction calcium and manganese oxyhydroxide with boric sludge according to claim 1, it is characterized in that: described boron mud, contain magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide, other are moisture content in its component.
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|---|---|---|---|
| CN2010105737054A CN102115104A (en) | 2010-12-03 | 2010-12-03 | Method for co-production of magnesium nitrate anhydride and calcium hydroxide/manganese hydroxide from boron slag |
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|---|---|---|---|
| CN2010105737054A CN102115104A (en) | 2010-12-03 | 2010-12-03 | Method for co-production of magnesium nitrate anhydride and calcium hydroxide/manganese hydroxide from boron slag |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830021A (en) * | 2017-03-20 | 2017-06-13 | 青海盐湖工业股份有限公司 | A kind of preparation technology of magnesium nitrate hexahydrate |
| CN116140325A (en) * | 2023-01-03 | 2023-05-23 | 重庆交通大学 | Formula, treatment method and finished product of stable solidified electrolytic manganese slag |
-
2010
- 2010-12-03 CN CN2010105737054A patent/CN102115104A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830021A (en) * | 2017-03-20 | 2017-06-13 | 青海盐湖工业股份有限公司 | A kind of preparation technology of magnesium nitrate hexahydrate |
| CN116140325A (en) * | 2023-01-03 | 2023-05-23 | 重庆交通大学 | Formula, treatment method and finished product of stable solidified electrolytic manganese slag |
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Application publication date: 20110706 |