CN105502443A - Method of producing magnesium nitrate hyperhydrate with boron mud waste material - Google Patents
Method of producing magnesium nitrate hyperhydrate with boron mud waste material Download PDFInfo
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- CN105502443A CN105502443A CN201410496043.3A CN201410496043A CN105502443A CN 105502443 A CN105502443 A CN 105502443A CN 201410496043 A CN201410496043 A CN 201410496043A CN 105502443 A CN105502443 A CN 105502443A
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- magnesium
- boron mud
- magnesium nitrate
- chloride
- hydroxide
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Abstract
A method of producing a magnesium nitrate hyperhydrate with a boron mud waste material relates to treatment of three wastes and comprehensive utilization in inorganic chemical engineering. The method includes treatment on the boron mud to produce the magnesium nitrate hyperhydrate with combined production of calcium hydroxide and manganese hydroxide. The method particularly includes the following steps: (a) heating the boron mud with steam, and performing liquid-solid separation through a centrifugal spin-drying machine to obtain a filtrate mainly including boric acid, and sending the filtrate to a deep processing unit; (b) in a first anti-corrosion reactor, performing a reaction to magnesium oxide in boron mud filter cake with hydrochloric acid to generate a magnesium chloride hydrate, calcium chloride and very little manganese chloride; (c) performing filtration to obtain silicon dioxide filter cake and sending the silicon dioxide filter cake to a deep processing unit; (d) performing impurity removal and purification to a clear filtrate with a proper amount of magnesium hydroxide, and performing filtration to finally obtain pure magnesium chloride dihydrate clear liquid, calcium hydroxide and manganese hydroxide; (e) in a second anti-corrosion reactor, performing a reaction to the clear magnesium chloride with nitric acid to generate a mixed solution containing magnesium nitrate nonahydrate and hydrochloric acid; and (f) performing distillation and cooling crystallization to obtain magnesium nitrate hexahydrate. The method increases economic benefit of treatment on the boron mud waste material.
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 utilizing boron mud waste material to produce magnesium nitrate hyperhydrate.
Background technology
Boron mud is with szaibelyite (2MgOB
2o
3h
2o) be raw material, by roasting, pulverizing, mix with soda ash, take carbon water law to produce borax (Na
2b
4o
710H
2o), remaining after washing, crystallisation process extract borax solid waste.Produce one ton of borax and can produce 4 tons of boron mud, produce the borax plant of 8000 tons per year for one, can produce boron mud is every year 3.2 ten thousand tons.Because the quantity discharged of boron mud is comparatively large, the multiple comprehensive Utilization Ways of current domestic employing, except production Magnesium Carbonate Light 41-45 and magnesium oxide and plastic and rubber filler, also have produce Peng Mei phosphorus composite fertilizer, to make the coal of honeycomb briquette reinforced and do architectural borax etc.
Magnesium in boron mud is all generally exist with the form of magnesiumcarbonate, sometimes also has difference along with the mineral products difference of szaibelyite.The component of producing Magnesium Carbonate Light 41-45 boron mud is such: magnesium oxide accounts for 38%, and silicon-dioxide accounts for 20%, and carbonic acid gas accounts for 17%, and boron oxide accounts for 3%, and calcium oxide accounts for 3%, and manganese oxide accounts for 0.11%, and other is moisture content.
The value of output object should be improved constantly to the utilization of boron mud, some markets of output in short supply, product that added value is large, to improve the economic benefit that boron mud utilizes.
Therefore, in the technical scheme of process boron mud refuse, the recycling of the compound of boron should be considered, as produced magnesium nitrate hyperhydrate etc. as far as possible.
Summary of the invention
The present invention is intended to utilization for boron mud and the market requirement, provides a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate.
To achieve these goals, a kind of technical scheme utilizing boron mud waste material to produce the method for magnesium nitrate hyperhydrate of the present invention is as follows.
Utilize boron mud waste material to produce a method for magnesium nitrate hyperhydrate, comprise the steps:
By boron mud steam heating to 61 ~ 81 degree of maintenances 1.2 ~ 2.1 hours, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, the filtrate based on boric acid sends to deep processing separately;
By the magnesium oxide in filter cake boron mud and hydrochloric acid by the mass ratio 1: 1.62 ~ 2.04 of pure substance, react in the first corrosion-resistant reactor, stir; React the hydrate, calcium chloride and the Manganous chloride tetrahydrate that generate magnesium chloride; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; The filtrate of clarification does further purifying;
By the appropriate magnesium hydroxide impurity and purification of clear filtrate, filter and finally obtain two pure aqueous magnesium chloride clear liquors; 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, packaging;
The clarification magnesium chloride obtained and nitric acid are reacted in the second corrosion-resistant reactor by the mass ratio 1: 1.12 ~ 1.55 of pure substance; Under agitation generate nine water magnesium nitrate and hydrochloric acid mixed solutions; Filter obtain a small amount of impurity filter cake send to burn or buried, the clear filtrate obtained is sent underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration time, distillate is ejected and have crystallization through cooling, obtain nine water magnesium nitrate crystal products through washing, drying, pulverizing; Nine water magnesium nitrates continue distillation again and evaporate through being cooled to magnesium nitrate hexahydrate after three crystal water, through washing, drying, be ground into magnesium nitrate hexahydrate product; The hydrochloric acid soln of reusable edible is left in twice distillation.
Described boron mud, containing magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide and moisture content in its component.
Chemical equation of the present invention is:
MgO+2HCl＝MgCl
2+H
20
CaO+2HCl＝CaCl
2+H
2O
CaCl
2+Mg(OH)
2＝MgCl
2+Ca(OH)
2
MnO+2HCl＝MnCl
2+H
2O
MnC1
2+Mg(OH)
2＝MgCl
2+Mn(OH)
2
MgC1
2+2HNO
3+9H
2O＝Mg(NO3)
2·9H
2O+2HC1
Beneficial effect of the present invention is: one, providing a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate, opening up an approach for effectively processing boron mud waste material.Its two, preparation comprises magnesium nitrate, calcium hydroxide and manganous hydroxide, and wherein magnesium nitrate is the best-selling product that a kind of economic worth is larger, improves the economic benefit of process boron mud waste material.Its three, less investment, particularly applicable to the boron mud of process for producing lightweight magnesium nitrate boron used mud and similar components, open a Tiao Xin road.Its four, the purity of preparation is high, and quality is guaranteed.
Embodiment
Embodiment one, a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate, comprises the steps:
Get 500 kilograms, boron mud (wherein containing magnesium oxide 38%) by steam heating to 61 ~ 81 degree of maintenances 1.2 ~ 2.1 hours, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, the filtrate based on boric acid sends to deep processing separately;
By the magnesium oxide in filter cake boron mud and hydrochloric acid by the mass ratio 1: 1.63 of pure substance, react in the first corrosion-resistant reactor, stirring issues biochemical reaction slowly; The hydrate of reaction generation 404 kilograms of magnesium chlorides, other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; The filtrate of clarification does further purifying;
By the appropriate magnesium hydroxide impurity and purification of clear filtrate, filter and finally obtain two pure aqueous magnesium chloride clear liquors; 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, packaging; The magnesium chloride generated improves the concentration of original solution;
The 404 kilograms of clarification magnesium chlorides obtained and nitric acid are reacted in the second corrosion-resistant reactor by the mass ratio 1: 1.13 of pure substance; Nine water magnesium nitrate and hydrochloric acid mixed solutions are generated under slowly stirring; Filter obtain a small amount of impurity filter cake send to burn or buried, the clear filtrate obtained is sent underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration time, distillate is ejected and have crystallization through cooling, through washing, drying, pulverize the nine water magnesium nitrate crystal products obtaining 1123 kilograms; Nine water magnesium nitrates continue to distill the magnesium nitrate hexahydrate evaporated through being cooled to 927.4 kilograms after three crystal water again, through washing, drying, be ground into magnesium nitrate hexahydrate product; The hydrochloric acid soln of reusable edible is left in twice distillation.
Containing magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11% in the present invention's its component of boron mud used, other is moisture content.
Embodiment two, a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate, comprises the steps:
Get 500 kilograms, boron mud (wherein containing magnesium oxide 38%) by steam heating to 61 ~ 81 degree of maintenances 1.2 ~ 2.1 hours, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, the filtrate based on boric acid sends to deep processing separately;
By the magnesium oxide in filter cake boron mud and hydrochloric acid by the mass ratio 1: 1.83 of pure substance, react in the first corrosion-resistant reactor, stirring issues biochemical reaction slowly; The hydrate of reaction generation 453.8 kilograms of magnesium chlorides, other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; The filtrate of clarification does further purifying;
By the appropriate magnesium hydroxide impurity and purification of clear filtrate, filter and finally obtain two pure aqueous magnesium chloride clear liquors; 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, packaging; The magnesium chloride generated improves the concentration of original solution;
The 453.8 kilograms of clarification magnesium chlorides obtained and nitric acid are reacted in the second corrosion-resistant reactor by the mass ratio 1: 1.33 of pure substance; Nine water magnesium nitrate and hydrochloric acid mixed solutions are generated under slowly stirring; Filter obtain a small amount of impurity filter cake send to burn or buried, the clear filtrate obtained is sent underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration time, distillate is ejected and have crystallization through cooling, through washing, drying, pulverize the nine water magnesium nitrate crystal products obtaining 1485 kilograms; Nine water magnesium nitrates continue to distill the magnesium nitrate hexahydrate evaporated through being cooled to 1226.3 kilograms after three crystal water again, through washing, drying, be ground into magnesium nitrate hexahydrate product; The hydrochloric acid soln of reusable edible is left in twice distillation.
Containing magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11% in the present invention's its component of boron mud used, other is moisture content.
Embodiment three, a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate, comprises the steps:
Get 500 kilograms, boron mud (wherein containing magnesium oxide 38%) by steam heating to 61 ~ 81 degree of maintenances 1.2 ~ 2.1 hours, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, the filtrate based on boric acid sends to deep processing separately;
By the magnesium oxide in filter cake boron mud and hydrochloric acid by the mass ratio 1: 2.03 of pure substance, react in the first corrosion-resistant reactor, stirring issues biochemical reaction slowly; The hydrate of reaction generation 503.6 kilograms of magnesium chlorides, other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; The filtrate of clarification does further purifying;
By the appropriate magnesium hydroxide impurity and purification of clear filtrate, filter and finally obtain two pure aqueous magnesium chloride clear liquors; 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, packaging; The magnesium chloride generated improves the concentration of original solution;
The 503.6 kilograms of clarification magnesium chlorides obtained and nitric acid are reacted in the second corrosion-resistant reactor by the mass ratio 1: 1.53 of pure substance; Nine water magnesium nitrate and hydrochloric acid mixed solutions are generated under slowly stirring; Filter obtain a small amount of impurity filter cake send to burn or buried, the clear filtrate obtained is sent underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration time, distillate is ejected and have crystallization through cooling, through washing, drying, pulverize the nine water magnesium nitrate crystal products obtaining 1895.7 kilograms; Nine water magnesium nitrates continue to distill the magnesium nitrate hexahydrate evaporated through being cooled to 1565.5 kilograms after three crystal water again, through washing, drying, be ground into magnesium nitrate hexahydrate product; The hydrochloric acid soln of reusable edible is left in twice distillation.
Containing magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11% in the present invention's its component of boron mud used, other is moisture content.
Claims (2)
1. the method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate, it is characterized in that comprising the steps: boron mud steam heating to 61 ~ 81 degree of maintenances 1.2 ~ 2.1 hours, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, the filtrate based on boric acid sends to deep processing separately; By the magnesium oxide in filter cake boron mud and hydrochloric acid by the mass ratio 1: 1.62 ~ 2.04 of pure substance, react in the first corrosion-resistant reactor, stir; React the hydrate, calcium chloride and the Manganous chloride tetrahydrate that generate magnesium chloride; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; The filtrate of clarification does further purifying; By the appropriate magnesium hydroxide impurity and purification of clear filtrate, filter and finally obtain two pure aqueous magnesium chloride clear liquors; 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, packaging; The clarification magnesium chloride obtained and nitric acid are reacted in the second corrosion-resistant reactor by the mass ratio 1: 1.12 ~ 1.55 of pure substance; Under agitation generate nine water magnesium nitrate and hydrochloric acid mixed solutions; Filter obtain a small amount of impurity filter cake send to burn or buried, the clear filtrate obtained is sent underpressure distillation device to and is carried out underpressure distillation, when solution reaches capacity concentration time, distillate is ejected and have crystallization through cooling, obtain nine water magnesium nitrate crystal products through washing, drying, pulverizing; Nine water magnesium nitrates continue distillation again and evaporate through being cooled to magnesium nitrate hexahydrate after three crystal water, through washing, drying, be ground into magnesium nitrate hexahydrate product; The hydrochloric acid soln of reusable edible is left in twice distillation.
2. a kind of method utilizing boron mud waste material to produce magnesium nitrate hyperhydrate according to claim 1, is characterized in that: described boron mud, containing magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide and moisture content in its component.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517266A (en) * | 2016-12-08 | 2017-03-22 | 大连百傲化学股份有限公司 | Production method for magnesium nitrate hexahydrate |
| 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 |
-
2014
- 2014-09-17 CN CN201410496043.3A patent/CN105502443A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517266A (en) * | 2016-12-08 | 2017-03-22 | 大连百傲化学股份有限公司 | Production method for magnesium nitrate hexahydrate |
| CN106517266B (en) * | 2016-12-08 | 2018-11-02 | 大连百傲化学股份有限公司 | A method of producing magnesium nitrate hexahydrate |
| 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 |
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Application publication date: 20160420 |
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