CN104108732A - Method for utilizing waste forsterite mineral powder to prepare high-purity magnesium oxide - Google Patents
Method for utilizing waste forsterite mineral powder to prepare high-purity magnesium oxide Download PDFInfo
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- CN104108732A CN104108732A CN201310136836.XA CN201310136836A CN104108732A CN 104108732 A CN104108732 A CN 104108732A CN 201310136836 A CN201310136836 A CN 201310136836A CN 104108732 A CN104108732 A CN 104108732A
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Abstract
The invention relates to the field of non-metal mineral processing and environment protection, and provides a method for utilizing a waste forsterite mineral powder to prepare high-purity magnesium oxide, and the method is simple in technology, environment-friendly and high in product purity. The method concretely comprises: mixing the forsterite mineral powder with an inorganic acid, heating and reacting, and filtering to obtain a first mixed filtrate; putting the first mixed filtrate in a constant-temperature water bath, dropwise adding a hydrogen peroxide solution, naturally cooling to room temperature, dropwise adding an alkali solution to adjust pH to 7-8, and then performing standing, ageing and filtering, so as to obtain a second filtrate; dropwise adding an alkali solution into the second filtrate to adjust pH of the solution to 10-12, and then performing standing, ageing and centrifugation, so as to obtain a solid magnesium hydroxide crude product; and finally performing drying and calcining processing on the solid magnesium hydroxide crude product, so as to prepare a high-purity magnesium oxide product. The method is simple in technology, green and environment-friendly, the prepared magnesium oxide has the purity up to 94-98%, and also by-products such as silicon oxide, water glass, ferric oxide and the like can be obtained, the added value is high.
Description
Technical field
The present invention relates to non-metallic minerals processing and field of environment protection, be specifically related to a kind of utilization and discard the preparation method that forsterite breeze is prepared high-purity magnesium oxide.
Background technology
Forsterite belongs to orthosilicate mineral, originates in ultrabasic rocks structural belt, normal and chromite symbiosis.Its chemical equation of forsterite is Mg2SiO4, belongs to the one in olivine mineral, often contains 2FeOSiO
2with a small amount of Na, K and the hopcalite of Al.How many color of forsterite under state of nature presents olive-green, canescence and lividity with its purity height and iron-holder, and proportion is 3.10-3.40g/cm3, and hardness is Mohs 6.5-7 level, not containing free state SiO
2.Pure forsterite crystal is water white transparency body, and when heating, volume change is very little, and refractoriness is greater than 1710 DEG C, can be without calcining directly as refractory aggregate.
MgO content in forsterite is generally 36%-45%, is mainly distributed in Yichang in Henan Xixia Mine, Shangnan County Shaanxi Province and Hubei in mountain range, the Qinling Mountains in China, and total reserves is about 1,000,000,000 tons.The peridotites MgO content generally using now, lower than 40%, can not directly apply in industry, needs through being just applied in metallurgical refractory materials after calcining.Therefore part forsterite raw material can only directly be used as preparing the raw material of keeping out magnesium calcium phosphate fertilizer, resource utilization is not high, in the exploitation process in the ore deposit of forsterite, be about 30% resource and there is no economic worth, can not be fully utilized, can only waste treatment, not only cause the wasting of resources, and environment has also been caused to adverse influence.
The domestic patent of invention (CN200910063283.3) also having for the comprehensive utilization of discarded forsterite ore deposit, its method is after using hydrochloric acid and forsterite breeze to react under certain condition, utilize the method preparing magnesium hydroxide that adds alkaline solution in pickling liquor, reacted solid filter residue reacts and produces water glass with caustic soda, and the iron in system is finally prepared to iron oxide red.But the hydrochloric acid using in this method has the strong irritant gas such as volatility, ammoniacal liquor.All can impact human body and environment, and use the technique of statement completely ironic hydroxide to be separated with magnesium hydroxide, cause final product purity not high.
Therefore, the recycling of discarded forsterite breeze protects two aspects all to have very important value to economy and environment.
Summary of the invention
A kind of the invention provides that technique is simple, environmental protection and the high discarded forsterite breeze of utilization of product purity are prepared high-purity magnesium oxide method.
In order to reach above technique effect, technical scheme of the present invention is as follows:
Utilize discarded forsterite breeze to prepare a method for high-purity magnesium oxide, it is characterized in that: comprise the following steps:
(1) forsterite breeze being mixed with inorganic acid solution, is to carry out reacting by heating 4-10 hour at 60 DEG C-100 DEG C in temperature, has reacted rear filtration, obtains the first filtrate, isolates silicon oxide and uses it for anything else;
(2) the first filtrate is placed in to the water bath with thermostatic control of 60 DEG C-80 DEG C, drips hydrogen peroxide solution, naturally cool to room temperature, drip the first alkaline solution and regulate pH value to 7-8, leave standstill, obtain the second solution after ageing, filtration, isolate solid hydrogen magnesium oxide, for subsequent use;
(3) will in the second solution, drip the second alkaline solution regulate pH value to 10-12, leave standstill, ageing, obtain solid hydrogen magnesium oxide crude product after centrifugal;
(4) the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried respectively, is calcined, make highly purified magnesium oxide product.
Preferably, described inorganic acid solution is that concentration is one or more in hydrochloric acid, phosphoric acid, sulfuric acid, tetra-sodium and the sulfurous acid of 2-6mol/L.
Preferably, the temperature of described water bath with thermostatic control is 70 DEG C.
Preferably, described the first alkaline solution is that volumetric concentration is one or more in quadrol, triethylamine and the TERTIARY BUTYL AMINE of 85-95%.
Preferably, described the second alkaline solution is that concentration is one or several in potassium hydroxide, sodium hydroxide and the ammoniacal liquor of 2-6mol/L.
Preferably, the proportion of described forsterite breeze is 3.10-3.40g/cm
3, hardness is Mohs 6.5-7 level, and wherein the content of MgO is 36%-45%, and particle diameter is 150-250 order.
Apply technical scheme of the present invention, have following technique effect: (1) the present invention just can make the magnesium oxide product of purity 94-98% by four large processing steps and chemical precipitation method, whole technological process is simple, environmental protection; (2) in technique of the present invention, obtain the by products such as silicon oxide that purity is high and use it for anything else, technique added value is high.
Embodiment
Describe below in conjunction with specific embodiments technical scheme of the present invention in detail, be used for explaining technical scheme of the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
embodiment 1
Utilizing discarded forsterite breeze to prepare purity is 94% magnesium oxide, specifically comprises the following steps:
The first step: by the mixed in hydrochloric acid of 200 object forsterite breezes and 2mol/L, reacting by heating 4 hours at 60 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, drip 85% ethylenediamine solution, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the potassium hydroxide solution that drips 2mol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is carried out, after the calcination processing of 120 DEG C dry and 600 DEG C, make high-purity magnesium oxide product.
The magnesian purity making by this method is 94%, and recovery rate is calculated as 30% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 71.4%.
embodiment 2
Utilizing discarded forsterite breeze to prepare purity is 96% magnesium oxide, specifically comprises the following steps:
The first step: 200 object forsterite breezes are mixed with the phosphoric acid of 3mol/L, reacting by heating 6 hours at 80 DEG C, reaction finishes rear filtration, obtains the first mixing solutions and the solid oxidation silicon of magnesium, iron inorganic salt, and silicon oxide solid uses it for anything else;
Second step: the first mixing solutions is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the triethylamine solution that dropping volumetric concentration is 90%, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the sodium hydroxide solution that drips 3mol/L in the second solution, the pH to 10-12 of regulator solution, through leaving standstill, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The prepared magnesian purity of this method is 96%, and recovery rate is calculated as 30.7% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 73.1%.
embodiment 3
Utilizing discarded forsterite breeze to prepare purity is 98% magnesium oxide, specifically comprises the following steps:
The first step: 200 object forsterite breezes are mixed with the sulfuric acid of 4mol/L, and reacting by heating 6 hours at 100 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the uncle that dropping volumetric concentration is 95% determines amine aqueous solution, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the potassium hydroxide solution that drips 4mol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The magnesian purity that this method makes is 98%, and recovery rate is calculated as 34% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 80.9%.
embodiment 4
Utilizing discarded forsterite breeze to prepare purity is 98% magnesium oxide, specifically comprises the following steps:
The first step: 200 object forsterite breezes are mixed with the sulfurous acid of 5mol/L, and reacting by heating 8 hours at 100 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the ethylenediamine solution that dropping volumetric concentration is 95%, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the ammonia soln that drips 5mol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The magnesian purity that this method makes is 96%, and recovery rate is calculated as 31.8% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 75.7%.
embodiment 5
Utilizing discarded forsterite breeze to prepare purity is 95% magnesium oxide, specifically comprises the following steps:
The first step: 200 object forsterite breezes are mixed with the sub-tetra-sodium of 6mol/L, and reacting by heating 10 hours at 90 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the triethylamine solution that dropping volumetric concentration is 90%, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the sodium hydroxide solution that drips 6ol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The magnesian purity that this method makes is 95%, and recovery rate is calculated as 32.7% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 77.9%.
embodiment 6
Utilizing discarded forsterite breeze to prepare purity is 96% magnesium oxide, specifically comprises the following steps:
The first step: 200 object forsterite breezes are mixed with the sulfuric acid of 6mol/L, and reacting by heating 6 hours at 80 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the triethylamine solution that dropping volumetric concentration is 95%, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the ammonia soln that drips 4mol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The magnesian purity that this method makes is 96%, and recovery rate is calculated as 33.6% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 80%.
embodiment 7
Utilizing discarded forsterite breeze to prepare purity is 97% magnesium oxide, specifically comprises the following steps:
The first step: by the mixed in hydrochloric acid of 200 object forsterite breezes and 4mol/L, reacting by heating 8 hours at 100 DEG C, filters, obtains first of magnesium, iron inorganic salt and mixes filtrate and solid oxidation silicon, and silicon oxide solid uses it for anything else;
Second step: the first solution is placed in to 70 DEG C of waters bath with thermostatic control, drip hydrogen peroxide solution, naturally cool to room temperature, the triethylamine solution that dropping volumetric concentration is 80%, the pH to 7-8 of regulator solution, through standing, ageing, filtration, obtain the second filtrate and solid hydrogen magnesium oxide containing magnesium ion again, solid hydrogen magnesium oxide is for subsequent use;
The 3rd step: to the potassium hydroxide solution that drips 4mol/L in the second solution, the pH to 10-12 of regulator solution, then leaves standstill mixing solutions, ageing, centrifugally operated, obtains solid hydrogen magnesium oxide crude product;
The 4th step: the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried and the calcination processing of 600 DEG C after, make high-purity magnesium oxide product.
The magnesian purity that this method makes is 97%, and recovery rate is calculated as 33.2% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 79%.
The present invention utilizes discarded forsterite breeze, generate iron ion and magnesium ion through acid solution reaction, then according to different elements different precipitation rule (element precipitates pH value in Different Alkali solution) in alkaline solution, magnesium in forsterite in forsterite can be separated completely, can be obtained again by product silicon oxide, water glass and ferric oxide.The inventive method technique is simple, environmental protection, and the magnesium oxide purity 94%-98% of preparation, recovery rate is calculated as 30-34% with forsterite powdered ore quality, taking the cubage of magnesium in forsterite breeze as 71.4-80.9%, can also obtain the value-added products such as silicon oxide, water glass and ferric oxide.
Silicon oxide in the inventive method can be used for reacting with sodium hydroxide water glass that can obtain high purity, high-module etc.
The highly purified magnesium oxide that adopts the inventive method to make can widespread use in the field such as magneticsubstance, electronic product.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (6)
1. utilize discarded forsterite breeze to prepare a method for high-purity magnesium oxide, it is characterized in that: comprise the following steps:
(1) forsterite breeze being mixed with inorganic acid solution, is to carry out reacting by heating 4-10 hour at 60 DEG C-100 DEG C in temperature, has reacted rear filtration, obtains the first mixing filtrate, isolates silicon oxide and uses it for anything else;
(2) the first mixing filtrate is placed in to the water bath with thermostatic control of 60 DEG C-80 DEG C, drips hydrogen peroxide solution, naturally cool to room temperature, drip the first alkaline solution and regulate pH value to 7-8, leave standstill, obtain the second solution after ageing, filtration, isolate solid hydrogen magnesium oxide for subsequent use;
(3) will in the second solution, drip the second alkaline solution regulate pH value to 10-12, leave standstill, ageing, obtain solid hydrogen magnesium oxide crude product after centrifugal;
(4) the solid hydrogen magnesium oxide in solid hydrogen magnesium oxide crude product and step (2) is dried, is calcined, make high-purity magnesium oxide product.
2. the discarded forsterite breeze of utilization according to claim 1 is prepared the method for high-purity magnesium oxide, it is characterized in that: described inorganic acid solution is that concentration is one or more in hydrochloric acid, phosphoric acid, sulfuric acid, tetra-sodium and the sulfurous acid of 2-6mol/L.
3. the discarded forsterite breeze of utilization according to claim 1 is prepared the method for high-purity magnesium oxide, it is characterized in that: the temperature of described water bath with thermostatic control is 70 DEG C.
4. the discarded forsterite breeze of utilization according to claim 1 is prepared the method for high-purity magnesium oxide, it is characterized in that: described the first alkaline solution is that volumetric concentration is one or more in quadrol, triethylamine and the TERTIARY BUTYL AMINE of 85-95%.
5. the discarded forsterite breeze of utilization according to claim 1 is prepared the method for high-purity magnesium oxide, it is characterized in that: described the second alkaline solution is that concentration is one or several in potassium hydroxide, sodium hydroxide and the ammoniacal liquor of 2-6mol/L.
6. the discarded forsterite breeze of utilization according to claim 1 is prepared the method for high-purity magnesium oxide, it is characterized in that: the proportion of described forsterite breeze is 3.10-3.40g/cm
3, hardness is Mohs 6.5-7 level, and wherein the content of MgO is 36%-45%, and particle diameter is 150-250 order.
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Cited By (3)
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| CN108439440A (en) * | 2018-06-05 | 2018-08-24 | 张勤福 | The technique for producing magnesia using peridotite ore |
| CN110844925A (en) * | 2019-12-07 | 2020-02-28 | 商南金石工贸有限公司 | Process for preparing magnesium sulfate and white carbon black by using forsterite tailings |
| CN114162826A (en) * | 2022-01-17 | 2022-03-11 | 商南金石工贸有限公司 | Process and equipment for producing magnesium fluosilicate by using forsterite tailing |
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| CN110844925A (en) * | 2019-12-07 | 2020-02-28 | 商南金石工贸有限公司 | Process for preparing magnesium sulfate and white carbon black by using forsterite tailings |
| CN114162826A (en) * | 2022-01-17 | 2022-03-11 | 商南金石工贸有限公司 | Process and equipment for producing magnesium fluosilicate by using forsterite tailing |
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Application publication date: 20141022 |