CN106517266B - A method of producing magnesium nitrate hexahydrate - Google Patents
A method of producing magnesium nitrate hexahydrate Download PDFInfo
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- CN106517266B CN106517266B CN201611119648.6A CN201611119648A CN106517266B CN 106517266 B CN106517266 B CN 106517266B CN 201611119648 A CN201611119648 A CN 201611119648A CN 106517266 B CN106517266 B CN 106517266B
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- Prior art keywords
- magnesium nitrate
- magnesia
- reaction
- storage tank
- reaction kettle
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 22
- 238000005516 engineering process Methods 0.000 claims abstract description 17
- 239000000428 dust Substances 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000001704 evaporation Methods 0.000 abstract description 4
- 238000004321 preservation Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 9
- 229910017604 nitric acid Inorganic materials 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000009413 insulation Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QDMGKUOANLJICG-UHFFFAOYSA-N [Mg].[N+](=O)(O)[O-] Chemical compound [Mg].[N+](=O)(O)[O-] QDMGKUOANLJICG-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 150000004684 trihydrates Chemical class 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- 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 kind of methods producing magnesium nitrate hexahydrate；Described method includes following steps：1）Magnesia, which is proportionally added into the reaction kettle equipped with dust technology, to be reacted, control temperature of reaction kettle, pH value；2）Reaction solution is separated by solid-liquid separation, and inorganic impurity is filtered out, and filtrate is directly entered the storage tank with heat preservation；3）Magnesium nitrate aqueous solution in storage tank enters granulating working procedure, obtains granular nitrate magnesium finished product.Magnesium nitrate is produced using the present invention, it is simple for process, common evaporating concentration process is eliminated, while ensureing magnesium nitrate product quality, and the production cycle is shortened, reduces energy consumption.
Description
Technical field
The present invention relates to a kind of methods producing magnesium nitrate hexahydrate, belong to technical field of chemical industry.
Background technology
Magnesium nitrate is a kind of widely used industrial chemicals, is colourless crystallization, there is a water, two water, three water, six water, nine water
Five kinds of hydrates, commercially available is usually six water objects, is sold without anhydride.Magnesium nitrate is industrially used as the dehydration of cone nitric acid
Agent, wheat fogging agent and other magnesium salts and nitrate raw material, laboratory be used as chemical reagent.
There are mainly two types of the production methods of magnesium nitrate, and one is using magnesium carbonate and nitric acid as raw material：
MgCO3+2HNO3→Mg(NO3)2+H2O+CO2↑+Q
Another kind is using magnesia and nitric acid as raw material：
MgO+2HNO3→Mg(NO3)2+H2O+Q
The production method of magnesium nitrate is used using magnesia and nitric acid as raw material at present.
Chinese patent CN104098115 discloses a kind of side being granulated production full water-soluble sheet magnesium nitrate using steel band
Method, detailed process include that dust technology feeds to reaction kettle simultaneously with magnesia, obtain magnesium nitrate neutralizer and enter filter press mistake
Filter, filtrate enter flush distillation device evaporation and concentration, and the magnesium nitrate solution after concentration is transferred to crystallization kettle, after adding dust technology tune pH value
Centrifugal filtration obtains nitric acid magnesium crystal, this crystal is dissolved into molten hopper, and carries out double evaporation-cooling concentrate, and concentrate carries out steel band
It is granulated and obtains magnesium nitrate finished product.
This method is complicated for operation, needs twice evaporation concentration process, and the production cycle is long, and production equipment takes up a large area, if
Standby cost input is higher.
Invention content
The problems such as present invention is complicated for operation in solution production process, and the production cycle is long provides a kind of easy to operate, equipment
Small investment, the production method of magnesium nitrate hexahydrate with short production cycle.
The technical proposal of the invention is realized in this way：The present invention adopts the following technical scheme that realization：A kind of production
The method of magnesium nitrate hexahydrate, including：
1) by magnesia by being strictly proportionally added into the reaction kettle equipped with dust technology, control temperature of reaction kettle is in 90-
105 DEG C, the addition of magnesia is controlled, the concentration of magnesium nitrate in reaction kettle is made to be maintained at 57.2-57.8%；Above-mentioned reaction solution exists
90-105 DEG C of insulation reaction 0.5-3h, pH value=4-6 in control reaction kettle in insulating process.
2) above-mentioned reaction solution is separated by solid-liquid separation by two-in-one filter, exhausts solid slag, and filtrate enters 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 obtained granular nitrate magnesium is directly packaged to be magnesium nitrate hexahydrate
Finished product.
For the present invention by magnesia and nitric acid reaction, the molar ratio of reaction raw materials magnesia and dust technology is 1:2, control oxygen
The dosage for changing magnesium, makes after reaction that nitric acid content of magnesium is less than in 57.2-57.8%, this magnesium nitrate solution in temperature in dilute nitric acid solution
Solid precipitation is had at 88 DEG C, material becomes sticky, and causes subsequently to be separated by solid-liquid separation difficulty, cannot be below so to control temperature of reaction kettle
88℃；Magnesia and nitric acid reaction are exothermic reactions, and the charging rate of magnesia will control, and excessive too fast, kettle temperature cannot be added
More than 105 DEG C, magnesium nitrate aqueous solution dehydration, concentration is got higher, and influences 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 in the present invention is industrial light calcined magnesia, and content 87-96%, the inside is contained such as SiO2, CaO, iron and
The impurity such as the oxide of aluminium will directly affect the quality of final products if these impurity cannot be effectively removed.In magnesia
During nitric acid reaction, control system pH value, can be by the SiO in above-mentioned impurity in 4-62It completely removes, iron, aluminium, calcium etc.
The residual of impurity in the product is less, does not influence product quality.The pH value of reaction system is less than 4, and the impurity such as iron, aluminium are 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 influences product quality, so wanting stringent control system pH value in 4-6.
Because above-mentioned magnesium nitrate aqueous solution has solid when temperature is less than 88 DEG C and is precipitated, after reaction, solid-liquid
When separation, required heat filtering equipment needs heat preservation, is used herein as two-in-one filter and solves the problems, such as heat filtering, realizes solid-liquid
Separation, solid slag exhaust, and filtrate enters the storage tank with heat preservation.
Beneficial effects of the present invention are：Without being concentrated by evaporation, directly obtaining can make the method for the production magnesium nitrate of the present invention
Grain concentration nitric acid magnesium liquid；Process control operation is stablized, and manipulation strength is small, and working condition is mild, with short production cycle, equipment
Small investment, final magnesium nitrate finished product content is between 99.0-99.9%.
Specific implementation mode
With reference to embodiment the present invention will be further explained explanation.
Embodiment 1
A concentration of 57.6% dust technologies of 48.7kg are added into 50L reaction kettles, control 90-95 DEG C of temperature of reaction kettle, portioning
The 89.1% total 10kg of content magnesia, insulation reaction 1h after charging is added, controls pH=4-6 in kettle, reaction solution enters two
Unify filter filtering, solid slag discharge, filtrate enters in storage tank, controls fluid temperature in storage tank and is made in 95-100 DEG C of entrance
Grain device is granulated, and obtains magnesium nitrate hexahydrate product 57.6kg, content 99.0% is up-to-standard；
Embodiment 2
A concentration of 58% dust technologies of 48.4kg are added into 50L reaction kettles, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the total 10kg of magnesia of 89.1% content, insulation reaction 1h after charging, control in kettle pH controls processed in 4-6, reaction solution into
Enter two-in-one filter filtering, solid slag discharge, filtrate enters in storage tank, and fluid temperature is at 100-105 DEG C in control storage tank
It is granulated into prilling granulator, obtains magnesium nitrate hexahydrate product 57.04kg, content 99.5% is up-to-standard.
Embodiment 3
A concentration of 58.5% dust technologies of 48kg are added into 50L reaction kettles, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the total 10kg of magnesia of 89.1% content, insulation reaction 1h after charging, control in kettle pH controls in 4-6, reaction solution into
Enter two-in-one filter filtering, solid slag is expelled directly out, and filtrate enters in storage tank, and fluid temperature is in 100- in control storage tank
105 DEG C enter prilling granulator and are granulated, and obtain magnesium nitrate 57.04kg, content 100.2% is up-to-standard.
Comparative example 4
A concentration of 58% dust technologies of 48.4kg are added into 50L reaction kettles A, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the total 10kg of magnesia of 89.1% content, insulation reaction 1h after charging, control pH value in kettle and control 6-7, reaction solution into
Enter two-in-one filter filtering, solid slag is expelled directly out, and filtrate enters in storage tank, and fluid temperature is in 100- in control storage tank
105 DEG C enter prilling granulator and are granulated, and obtain magnesium nitrate 57.04kg, content 99.5%, and water-soluble rear muddiness has White Flocculus analysis
Go out, it is off quality.
Comparative example 5
A concentration of 58% dust technologies of 48.4kg are added into 50L reaction kettles, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the total 10kg of magnesia of 89.1% content, insulation reaction 1h after charging, control pH value in kettle and control 2-3, reaction solution into
Enter two-in-one filter filtering, solid slag is expelled directly out, and filtrate enters in storage tank, and fluid temperature is in 100- in control storage tank
105 DEG C enter prilling granulator and are granulated, and obtain magnesium nitrate 57.04kg, content 99.5%, off quality, appearance is faint yellow, water-soluble
Muddiness has the precipitation of brown floccule afterwards.
Comparative example 6
A concentration of 57% dust technologies of 49.3kg are added into 50L reaction kettles, control 90-95 DEG C of temperature of reaction kettle, portioning adds
Enter the total 10kg of magnesia of 89.1% content, insulation reaction 1h after charging, control in kettle pH controls in 4-5, reaction solution into
Enter two-in-one filter filtering, solid slag is expelled directly out, and filtrate enters in storage tank, and fluid temperature is in 100- in control storage tank
105 DEG C enter prilling granulator and are granulated, and obtain magnesium nitrate 58.2kg, content 98.10% is off quality.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope of present disclosure, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (1)
1. a kind of method producing magnesium nitrate hexahydrate is using magnesia and dust technology as raw material, which is characterized in that include successively with
Lower step：
1）By magnesia by being added in the reaction kettle equipped with dust technology, 90-105 DEG C of temperature of reaction kettle is controlled, 0.5-3h is reacted,
Control pH value=4-6 in reaction kettle；
2）Heat filtering is carried out with filter, exhausts solid slag, filtrate enters storage tank, controls 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；
The concentration 57.5-58.5% of dust technology；
The molar ratio of reaction raw materials magnesia and dust technology is 1:2；
The concentration of magnesium nitrate in kettle is answered to be maintained at 57.2-57.8% after reaction., the magnesia is light calcined magnesia, and content exists
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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| Publication Number | Publication Date |
|---|---|
| CN106517266A CN106517266A (en) | 2017-03-22 |
| CN106517266B true 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 |
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|---|---|
| CN106517266A (en) | 2017-03-22 |
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