CN106517266A - Production method for magnesium nitrate hexahydrate - Google Patents
Production method for magnesium nitrate hexahydrate Download PDFInfo
- Publication number
- CN106517266A CN106517266A CN201611119648.6A CN201611119648A CN106517266A CN 106517266 A CN106517266 A CN 106517266A CN 201611119648 A CN201611119648 A CN 201611119648A CN 106517266 A CN106517266 A CN 106517266A
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- Prior art keywords
- magnesium nitrate
- nitrate hexahydrate
- reaction
- magnesia
- storage tank
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/38—Magnesium nitrates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a production method for magnesium nitrate hexahydrate. The method comprises the following steps: 1) adding magnesium oxide into a reaction vessel filled with dilute nitric acid in proportion for a reaction and controlling temperature and pH value in the reaction vessel; 2) subjecting a reaction solution to solid-liquid separation, filtering out inorganic impurities and allowing a filtrate to directly enter a heat-insulation storage tank; and 3) allowing an aqueous solution of magnesium nitrate in the storage tank to enter a granulation procedure so as to obtain a finished magnesium nitrate product. The production method provided by the invention is simple in process, omits the frequently used process of evaporative concentration, guarantees the quality of the magnesium nitrate product, shortens a production period and reduces energy consumption.
Description
Technical field
The present invention relates to a kind of method for producing magnesium nitrate hexahydrate, belongs to technical field of chemical industry.
Background technology
Magnesium nitrate is a kind of broad-spectrum industrial chemicals, is colourless crystallization, has a water, two water, three water, six water, nine water
Five kinds of hydrates, commercially available are usually six water things, and no anhydride is sold.The magnesium nitrate industrially dehydration as cone nitric acid
The raw material of agent, wheat fogging agent and other magnesium salts and nitrate, is used as chemical reagent in laboratory.
The production method of magnesium nitrate mainly has two kinds, and one kind is with magnesium carbonate and nitric acid as raw material：
MgCO3+2HNO3→Mg(NO3)2+H2O+CO2↑+Q
Another kind is with magnesia and nitric acid as raw material：
MgO+2HNO3→Mg(NO3)2+H2O+Q
The production method of magnesium nitrate is adopted with magnesia and nitric acid as raw material at present.
Chinese patent CN104098115 discloses a kind of side of utilization steel band granulation production full water-soluble sheet magnesium nitrate
Method, detailed process include dust technology with magnesia while feeding to reactor, obtain magnesium nitrate neutralizer into filter press mistake
Filter, filtrate are concentrated by evaporation into flush distillation device, and the magnesium nitrate solution after concentration is transferred to crystallization kettle, plus after dust technology adjusts pH value
Centrifugal filtration obtains nitric acid magnesium crystal, and this crystal is dissolved into molten hopper, and carries out double evaporation-cooling concentrate, and concentrate carries out steel band
Granulation obtains magnesium nitrate finished product.
The method complex operation, needs twice evaporation concentrate process, and long the production cycle, production equipment floor space are big, if
Standby cost input is higher.
The content of the invention
A kind of the problems such as present invention is to solve complex operation in production process, long the production cycle, there is provided simple to operate, equipment
Small investment, the production method of magnesium nitrate hexahydrate with short production cycle.
The technical scheme is that what is be achieved in that：The present invention adopts the following technical scheme that realization：A kind of production
The method of magnesium nitrate hexahydrate, including：
1) magnesia is controlled into temperature of reaction kettle in 90- by being strictly proportionally added in the reactor equipped with dust technology
105 DEG C, the addition of magnesia is controlled, makes the concentration of magnesium nitrate in reactor be maintained at 57.2-57.8%；Above-mentioned reactant liquor exists
90-105 DEG C of insulation reaction 0.5-3h, controls pH value=4-6 in reactor in insulating process.
2) above-mentioned reactant liquor carries out separation of solid and liquid through two-in-one filter, and solid slag of draining, filtrate enter storage tank, control
Magnesium nitrate aqueous solution temperature in storage tank processed is at 90-105 DEG C.
3) above-mentioned magnesium nitrate aqueous solution enters Granulation Equipments, and the granular nitrate magnesium for obtaining directly is packaged to be magnesium nitrate hexahydrate
Finished product.
It is 1 that the present invention passes through magnesia and the mol ratio of nitric acid reaction, reaction raw materials magnesia and dust technology:2, control oxygen
Change the consumption of magnesium, in 57.2-57.8%, this magnesium nitrate solution is less than in temperature to make after reaction nitric acid content of magnesium in dilute nitric acid solution
Solid precipitation is had when 88 DEG C, material becomes sticky, cause follow-up separation of solid and liquid difficult, so temperature of reaction kettle will be controlled cannot be below
88℃；Magnesia and nitric acid reaction are exothermic reactions, and the charging rate of magnesia will be controlled, it is impossible to add excessive too fast, kettle temperature
More than 105 DEG C, magnesium nitrate aqueous solution dehydration, concentration are uprised, affect end product quality, make magnesium nitrate in product a water, two
Water, trihydrate increase.
Reaction raw materials dust technology concentration is in 57.5-58.5%.
Raw material used by the present invention is industrial light calcined magnesia, and content 87-96%, the inside contain such as SiO2, CaO, iron and
The impurity such as the oxide of aluminium, if these impurity effectively can not be removed, will directly affect the quality of final products.In magnesia
During nitric acid reaction, control system pH value, can be by the SiO in above-mentioned impurity in 4-62Remove completely, iron, aluminium, calcium etc.
Impurity residual in the product is less, does not affect product quality.The pH value of reaction system is less than 4, and the impurity such as iron, aluminium is in the product
Content greatly increase, acid stronger, impurity content is bigger, and the color of final products can be partially yellow；The pH value of reaction system is higher than
6, water-insoluble increases, and affects product quality, so wanting strict control system pH value in 4-6.
Because above-mentioned magnesium nitrate aqueous solution has solid precipitation, after reaction terminates, solid-liquid when temperature is less than 88 DEG C
During separation, required heat filtering equipment needs insulation, is used herein as two-in-one filter and solves the problems, such as heat filtering, realizes solid-liquid
Separate, solid slag is drained, filtrate enters the storage tank with insulation.
Beneficial effects of the present invention are：The method of the production magnesium nitrate of the present invention is directly obtained and can be made without the need for being concentrated by evaporation
Grain concentration nitric acid magnesium liquid；Process control operation is stable, and manipulation strength is little, and working condition is gentle, with short production cycle, equipment
Small investment, final magnesium nitrate finished product content is between 99.0-99.9%.
Specific embodiment
With reference to embodiment the present invention will be further explained explanation.
Embodiment 1
To in 50L reactors, add 48.7kg concentration to be 57.6% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning
The common 10kg of 89.1% content magnesia, charging is added to finish rear insulation reaction 1h, pH=4-6 in control kettle, reactant liquor enter two
Unification filter is filtered, and solid slag is discharged, and filtrate is entered in storage tank, and in control storage tank, fluid temperature is made in 95-100 DEG C of entrance
Grain device granulation, obtains magnesium nitrate hexahydrate product 57.6kg, and content 99.0% is up-to-standard；
Embodiment 2
To in 50L reactors, add 48.4kg concentration to be 58% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the common 10kg of magnesia of 89.1% content, charging finishes rear insulation reaction 1h, and pH processed is controlled in 4-6 in control kettle, and reactant liquor enters
Enter two-in-one filter to filter, solid slag is discharged, filtrate is entered in storage tank, in control storage tank, fluid temperature is at 100-105 DEG C
Granulate into prilling granulator, obtain magnesium nitrate hexahydrate product 57.04kg, content 99.5% is up-to-standard.
Embodiment 3
To in 50L reactors, add 48kg concentration to be 58.5% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the common 10kg of magnesia of 89.1% content, charging finishes rear insulation reaction 1h, and pH is controlled in 4-6 in control kettle, and reactant liquor enters
Enter two-in-one filter to filter, solid slag is expelled directly out, filtrate is entered in storage tank, in control storage tank, fluid temperature is in 100-
105 DEG C granulate into prilling granulator, obtain magnesium nitrate 57.04kg, and content 100.2% is up-to-standard.
Comparative example 4
To in 50L reactor A, add 48.4kg concentration to be 58% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the common 10kg of magnesia of 89.1% content, charging finishes rear insulation reaction 1h, and pH value control 6-7 in control kettle, reactant liquor enter
Enter two-in-one filter to filter, solid slag is expelled directly out, filtrate is entered in storage tank, in control storage tank, fluid temperature is in 100-
105 DEG C granulate into prilling granulator, obtain magnesium nitrate 57.04kg, and content 99.5%, water-soluble rear muddiness have White Flocculus to analyse
Go out, it is off quality.
Comparative example 5
To in 50L reactors, add 48.4kg concentration to be 58% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the common 10kg of magnesia of 89.1% content, charging finishes rear insulation reaction 1h, and pH value control 2-3 in control kettle, reactant liquor enter
Enter two-in-one filter to filter, solid slag is expelled directly out, filtrate is entered in storage tank, in control storage tank, fluid temperature is in 100-
105 DEG C granulate into prilling granulator, obtain magnesium nitrate 57.04kg, content 99.5%, and off quality, outward appearance is faint yellow, water-soluble
Muddiness has brown floccule to separate out afterwards.
Comparative example 6
To in 50L reactors, add 49.3kg concentration to be 57% dust technology, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the common 10kg of magnesia of 89.1% content, charging finishes rear insulation reaction 1h, and pH is controlled in 4-5 in control kettle, and reactant liquor enters
Enter two-in-one filter to filter, solid slag is expelled directly out, filtrate is entered in storage tank, in control storage tank, fluid temperature is in 100-
105 DEG C granulate into prilling granulator, obtain magnesium nitrate 58.2kg, and content 98.10% is off quality.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.
Claims (5)
1. a kind of method for producing magnesium nitrate hexahydrate, is with magnesia and dust technology as raw material, it is characterised in that include successively with
Lower step：
1）By magnesia by being added in the reactor equipped with dust technology, 90-105 DEG C of temperature of reaction kettle is controlled, reacts 0.5-3h,
PH value=4-6 in control reactor；
2）Heat filtering is carried out with filter, solid slag of draining, filtrate enter storage tank, control the magnesium nitrate solution temperature in storage tank
At 90-105 DEG C；
3）Above-mentioned magnesium nitrate solution is granulated, granular magnesium nitrate hexahydrate is obtained.
2. it is according to claim 1 production magnesium nitrate hexahydrate method, it is characterised in that concentration 57.5- of dust technology
58.5%。
3. it is according to claim 1 production magnesium nitrate hexahydrate method, it is characterised in that reaction raw materials magnesia and dilute nitre
The mol ratio of acid is 1:2.
4. it is according to claim 1 production magnesium nitrate hexahydrate method, it is characterised in that magnesium nitrate in kettle is answered after reaction
Concentration is maintained at 57.2-57.8%.
5. it is according to claim 1 production magnesium nitrate hexahydrate method, it is characterised in that the magnesia be light-burned oxidation
Magnesium, content is in 87-96%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611119648.6A CN106517266B (en) | 2016-12-08 | 2016-12-08 | A method of producing magnesium nitrate hexahydrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611119648.6A CN106517266B (en) | 2016-12-08 | 2016-12-08 | A method of producing magnesium nitrate hexahydrate |
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| CN106517266A true CN106517266A (en) | 2017-03-22 |
| CN106517266B CN106517266B (en) | 2018-11-02 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086235A (en) * | 2014-07-22 | 2014-10-08 | 路永宽 | Method for producing full-water-soluble magnesium ammonium nitrate by using steel belt granulator |
| CN104098115A (en) * | 2014-07-22 | 2014-10-15 | 路永宽 | Method for producing full-water-soluble flaky magnesium nitrate through steel belt granulator |
| CN105502443A (en) * | 2014-09-17 | 2016-04-20 | 常德云港生物科技有限公司 | Method of producing magnesium nitrate hyperhydrate with boron mud waste material |
| CN105621461A (en) * | 2015-12-28 | 2016-06-01 | 大连百傲化学股份有限公司 | Continuous magnesium nitrate production device and technological method |
-
2016
- 2016-12-08 CN CN201611119648.6A patent/CN106517266B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086235A (en) * | 2014-07-22 | 2014-10-08 | 路永宽 | Method for producing full-water-soluble magnesium ammonium nitrate by using steel belt granulator |
| CN104098115A (en) * | 2014-07-22 | 2014-10-15 | 路永宽 | Method for producing full-water-soluble flaky magnesium nitrate through steel belt granulator |
| CN105502443A (en) * | 2014-09-17 | 2016-04-20 | 常德云港生物科技有限公司 | Method of producing magnesium nitrate hyperhydrate with boron mud waste material |
| CN105621461A (en) * | 2015-12-28 | 2016-06-01 | 大连百傲化学股份有限公司 | Continuous magnesium nitrate production device and technological method |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究院等: "《无机盐工业手册 上册》", 31 October 1979, 化学工业出版社 * |
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