CN102701240A - Method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor - Google Patents

Method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor Download PDF

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Publication number
CN102701240A
CN102701240A CN201210142370XA CN201210142370A CN102701240A CN 102701240 A CN102701240 A CN 102701240A CN 201210142370X A CN201210142370X A CN 201210142370XA CN 201210142370 A CN201210142370 A CN 201210142370A CN 102701240 A CN102701240 A CN 102701240A
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sal epsom
waste liquid
magnesium oxide
manganese dioxide
silicon steel
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陈为亮
马力言
宋宁
戴永年
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Priority to CN201210142370XA priority Critical patent/CN102701240A/en
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Abstract

The invention provides a method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor, which comprises the following steps: mixing magnesium sulfate waste liquor and oxydol, regulating the pH value of the mixed liquor, stirring, aging, and filtering, wherein the filtrate is magnesium sulfate purified liquor; adding a precipitant ammonium carbonate solution into the magnesium sulfate purified liquor, stirring, aging, filtering, and drying the filter cake to obtain basic magnesium carbonate; calcining the basic magnesium carbonate, and washing with water at normal temperature to obtain magnesium oxide; and grinding and screening to obtain the silicon-steel-grade magnesium oxide. In the invention, the magnesium sulfate waste liquor generated in the lateritic nickel ore wet-method smelting process is used as the raw material to prepare high-added-value silicon-steel-grade magnesium oxide; the production technique is simple; and the produced silicon-steel-grade magnesium oxide product has the characteristics of high chemical purity, low impurity content and small average particle size. The purity of the silicon-steel-grade magnesium oxide is greater than 98%, the hydration rate is less than 5%, and the average particle size is smaller 5 mu m.

Description

A kind of is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid
Technical field
The present invention relates in a kind of sal epsom waste liquid that from the red soil nickel ore wet smelting process, produces the comprehensive method that reclaims magnesium, specifically be a kind of be feedstock production high added value silicon steel level method of magnesium oxide with the sal epsom waste liquid, belong to chemical technology field.
Background technology
Normal association has a large amount of magnesium resources in the red soil nickel ore; Adopt wet method smelting process that red soil nickel ore is carried out often producing a large amount of sal epsom waste liquids after sulfuric acid leaches coprecipitated nickel hydroxide; This sal epsom waste liquid is contaminate environment not only, and makes the higher magnesium resource of potential value not to be utilized effectively, and greatly reduces the comprehensive utilization of resources rate of red soil nickel ore; Therefore, research is a kind of carries out the method that comprehensive resource reclaims to this sal epsom waste liquid and seems particularly important.
Silicon steel level Natural manganese dioxide belongs to extraordinary special-purpose Natural manganese dioxide, is a kind of purity>=98%, suspension is good in water, the aquation rate is low, be insoluble in water, under hot conditions, can form MgSiO with the silicate in the siliconized plate 3The white magnesium oxide powder material of coating, silicon steel level Natural manganese dioxide also plays the effect of separant, dephosphorization, sweetening agent.China is magnesium resource big country, however the silicon steel level Natural manganese dioxide output wretched insufficiency of high added value.Breakthrough along with China's oriented silicon steel production technology; Large-lot producer such as Wuhan Iron and Steel Plant, the Baosteel oriented silicon steel production line that starts one after another; Silicon steel level Natural manganese dioxide demand increases suddenly; Domestic only have the Shanghai minority enterprises such as safe chemical plant of shaking can produce the silicon steel level magnesium oxide product that meets the enterprise-quality standard-required, and silicon steel level Natural manganese dioxide market outlook are wide.
Yet; Produce now that silicon steel level method of magnesium oxide exists also that industrial scale is little, there are the foreign matter content height in unstable product quality, product, robotization, the level that becomes more meticulous are low; Quality product can not satisfy the problems such as requirement of the oriented silicon steel production development of domestic quick growth fully, and from the red soil nickel ore wet smelting process in the sal epsom waste liquid of output preparation high added value silicon steel level method of magnesium oxide do not appear in the newspapers.
Summary of the invention
The invention solves the difficult problem of the comprehensive utilization of resources of the sal epsom waste liquid that produces in the red soil nickel ore wet smelting process,, realize through following technical proposal with the silicon steel level Natural manganese dioxide that this sal epsom waste liquid is the feedstock production high added value.
It is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid that the present invention provides a kind of, following each step of process:
(1) volume by ydrogen peroxide 50 accounts for 3~7% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 10~25g/L is that 30% industrial ydrogen peroxide 50 mixes; Using concentration then is that the pH value that the sodium carbonate solution of 1.5~2.5mol/L is regulated mixed solution is 5~9;, 30~70 ℃, stirring velocity react 10~50min under being the condition of 100~500rpm again; Last ageing 0.5~1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 1.5~2.5mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1~1.4 of theoretical amount; In temperature is that 50~80 ℃, stirring velocity are to react 0.5~1.5h under the condition of 500~1000rpm; Ageing 0.5~1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 1~3h down at 900~1100 ℃, wash 2~5 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain silicon steel level Natural manganese dioxide.
Preferred preparation method of the present invention is:
(1) volume by ydrogen peroxide 50 accounts for 4~6% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 10~25g/L is that 30% industrial ydrogen peroxide 50 mixes; Using concentration then is that the pH value that the sodium carbonate solution of 1.5~2.5mol/L is regulated mixed solution is 6~8;, 40~60 ℃, stirring velocity react 20~40min under being the condition of 300~500rpm again; Last ageing 0.5~1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2~2.5mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.1~1.3 of theoretical amount; In temperature is that 60~80 ℃, stirring velocity are to react 1~1.5h under the condition of 700~1000rpm; Ageing 0.5~1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 2~3h down at 950~1100 ℃, wash 3~5 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain silicon steel level Natural manganese dioxide.
The sal epsom waste liquid of said step (1) is produced the sal epsom waste liquid by industry.
The ydrogen peroxide 50 of said step (1) is industrial ydrogen peroxide 50.
The adjusting pH of mixed value of said step (1) is that to use concentration be that the sodium carbonate solution of 1.5~2.5mol/L is regulated.
The present invention is a raw material with the sal epsom waste liquid that produces in the red soil nickel ore wet smelting process; Adopt the neutralizing hydrolysis method to carry out removal of impurities; Scavenging solution adopts ammonium carbonate method to prepare high-purity magnesium basic carbonate precursor; Precursor prepares Natural manganese dioxide through high-temperature calcination again, and Natural manganese dioxide obtains silicon steel level Natural manganese dioxide through washing, drying, pulverizing, screening.
Advantage that the present invention possesses and effect:
The present invention is a raw material with the sal epsom waste liquid that produces in the red soil nickel ore wet smelting process, to the comprehensive utilization of resources of this sal epsom waste liquid a kind of method of supply using for reference is provided.Prepare the silicon steel level Natural manganese dioxide of high added value with the sal epsom waste liquid, can either obtain remarkable economic efficiency, also have important environmental benefit and social benefit.Production technique of the present invention silicon steel level magnesium oxide product simple, that produce has chemical purity height, foreign matter content is low, median size is little characteristics.The silicon steel level Natural manganese dioxide purity that obtains greater than 98%, the aquation rate less than 5%, median size is less than 5 μ m.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
(1) volume by ydrogen peroxide 50 accounts for 4% of sal epsom waste liquid volume, with Mg 2+Concentration by the industry of 14.5g/L product sal epsom waste liquid and mass concentration be that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 2mol/L then is 7;, 50 ℃, stirring velocity react 20min under being the condition of 300rpm again; Last ageing 1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.1 of theoretical amount; In temperature is that 50 ℃, stirring velocity are to react 1h under the condition of 600rpm; Ageing 1h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 2h down at 950 ℃, wash 3 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, carry out 300 mesh sieve branches then, promptly obtain purity and be 98.51%, aquation rate 4.2%, median size be the silicon steel level Natural manganese dioxide of 3.92 μ m.
Embodiment 2
(1) volume by ydrogen peroxide 50 accounts for 5% of sal epsom waste liquid volume, with Mg 2+Concentration by the industry of 18.3g/L product sal epsom waste liquid and mass concentration be that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 2mol/L then is 8;, 70 ℃, stirring velocity react 25min under being the condition of 400rpm again; Last ageing 1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.2 of theoretical amount; In temperature is that 60 ℃, stirring velocity are to react 0.5h under the condition of 700rpm; Ageing 1h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 1.5h down at 1000 ℃, wash 4 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain purity and be 99.33%, aquation rate 3.7%, median size be the silicon steel level Natural manganese dioxide of 3.73 μ m.
Embodiment 3
(1) volume by ydrogen peroxide 50 accounts for 7% of sal epsom waste liquid volume, with Mg 2+Concentration by the industry of 22.5g/L product sal epsom waste liquid and mass concentration be that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 2mol/L then is 7;, 60 ℃, stirring velocity react 30min under being the condition of 500rpm again; Last ageing 1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.2 of theoretical amount; In temperature is that 70 ℃, stirring velocity are to react 1h under the condition of 800rpm; Ageing 1h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 1.5h down at 1100 ℃, wash 5 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain purity and be 98.73%, aquation rate 3.2%, median size be the silicon steel level Natural manganese dioxide of 4.05 μ m.
Embodiment 4
(1) volume by ydrogen peroxide 50 accounts for 3% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 25g/L is that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 2.5mol/L then is 5;, 40 ℃, stirring velocity react 50min under being the condition of 100rpm again; Last ageing 0.8h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2.5mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.4 of theoretical amount; In temperature is that 80 ℃, stirring velocity are to react 1.5h under the condition of 500rpm; Ageing 0.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 3h down at 900 ℃, wash 2 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain purity and be 98.37%, aquation rate 4.6%, median size be the silicon steel level Natural manganese dioxide of 4.37 μ m.
Embodiment 5
(1) volume by ydrogen peroxide 50 accounts for 6% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 10g/L is that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 1.5mol/L then is 6;, 60 ℃, stirring velocity react 40min under being the condition of 400rpm again; Last ageing 0.5h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1.3 of theoretical amount; In temperature is that 80 ℃, stirring velocity are to react 1.5h under the condition of 1000rpm; Ageing 1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 2h down at 1100 ℃, wash 4 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain purity and be 98.78%, aquation rate 3.9%, median size be the silicon steel level Natural manganese dioxide of 4.13 μ m.
Embodiment 6
(1) volume by ydrogen peroxide 50 accounts for 7% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 15g/L is that 30% industrial ydrogen peroxide 50 mixes; The pH value of using concentration to regulate mixed solution as the sodium carbonate solution of 2.5mol/L then is 9;, 30 ℃, stirring velocity react 10min under being the condition of 300rpm again; Last ageing 1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 1.5mol/L is a precipitation agent with concentration; Its consumption adds in the resulting sal epsom scavenging solution of step (1) by theoretical amount; In temperature is that 70 ℃, stirring velocity are to react 1.5h under the condition of 900rpm; Ageing 1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 1h down at 1100 ℃, wash 5 times to remove CaO wherein, after be drying to obtain Natural manganese dioxide with normal temperature again;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain purity and be 98.81%, aquation rate 4.7%, median size be the silicon steel level Natural manganese dioxide of 3.91 μ m.

Claims (5)

1. one kind is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid, it is characterized in that through following each step:
(1) volume by ydrogen peroxide 50 accounts for 3~7% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 10~25g/L is that 30% ydrogen peroxide 50 mixes; The pH value of regulating mixed solution then is 5~9;, 30~70 ℃, stirring velocity react 10~50min under being the condition of 100~500rpm again; Last ageing 0.5~1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 1.5~2.5mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1~1.4 of theoretical amount; In temperature is that 50~80 ℃, stirring velocity are to react 0.5~1.5h under the condition of 500~1000rpm; Ageing 0.5~1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 1~3h down at 900~1100 ℃, again with normal temperature washing 2~5 times, after be drying to obtain Natural manganese dioxide;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain silicon steel level Natural manganese dioxide.
2. according to claim 1 is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid, it is characterized in that said preferred manufacturing procedure is:
(1) volume by ydrogen peroxide 50 accounts for 4~6% of sal epsom waste liquid volume, with Mg 2+Concentration is that sal epsom waste liquid and the mass concentration of 10~25g/L is that 30% ydrogen peroxide 50 mixes; The pH value of regulating mixed solution then is 6~8;, 40~60 ℃, stirring velocity react 20~40min under being the condition of 300~500rpm again; Last ageing 0.5~1h, through filtering, filtrating is the sal epsom scavenging solution again;
(2) be that the sal volatile of 2~2.5mol/L is a precipitation agent with concentration; Its consumption is extraordinarily gone in the resulting sal epsom scavenging solution of step (1) by 1~1.4 of theoretical amount; In temperature is that 60~80 ℃, stirring velocity are to react 1~1.5h under the condition of 700~1000rpm; Ageing 0.5~1.5h then, through filtering, filter cake is drying to obtain magnesium basic carbonate again;
(3) step (2) gained magnesium basic carbonate is calcined 2~3h down at 950~1100 ℃, again with normal temperature washing 3~5 times, after be drying to obtain Natural manganese dioxide;
(4) adopt airflow milling that the Natural manganese dioxide that step (3) obtains is ground, sieve then, promptly obtain silicon steel level Natural manganese dioxide.
3. according to claim 1 and 2 is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid, it is characterized in that: the sal epsom waste liquid of said step (1) is produced the sal epsom waste liquid by industry.
4. according to claim 1 and 2 is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid, and it is characterized in that: the ydrogen peroxide 50 of said step (1) is industrial ydrogen peroxide 50.
5. according to claim 1 and 2 is feedstock production silicon steel level method of magnesium oxide with the sal epsom waste liquid, it is characterized in that: the adjusting pH of mixed value of said step (1) is that to use concentration be that the sodium carbonate solution of 1.5~2.5mol/L is regulated.
CN201210142370XA 2012-05-10 2012-05-10 Method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor Pending CN102701240A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923738A (en) * 2012-11-15 2013-02-13 吉首大学 Method for recovering water soluble manganese and magnesium from electrolytic manganese residue
CN103787376A (en) * 2012-10-30 2014-05-14 甘肃科特光电科技材料有限责任公司 Preparation method of ultrapure magnesium oxide powder
CN105540622A (en) * 2015-12-31 2016-05-04 上海应用技术学院 Recycling and re-preparation method of silicon-steel level magnesium oxide
CN106745106A (en) * 2016-12-21 2017-05-31 武汉工程大学 A kind of method that nanometric magnesium hydroxide is prepared by phosphorus ore de-magging waste liquid
CN110775993A (en) * 2019-12-18 2020-02-11 上栗县上栗镇中心小学 Process for preparing basic magnesium carbonate by liquid-phase crystal method
CN112320825A (en) * 2020-10-26 2021-02-05 安徽景成新材料有限公司 Method for preparing nano magnesium oxide by solid phase method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101456564A (en) * 2009-01-09 2009-06-17 昆明理工大学 Method for preparing magnesium oxide powder by magnesium sulphate demanganization

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101456564A (en) * 2009-01-09 2009-06-17 昆明理工大学 Method for preparing magnesium oxide powder by magnesium sulphate demanganization

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787376A (en) * 2012-10-30 2014-05-14 甘肃科特光电科技材料有限责任公司 Preparation method of ultrapure magnesium oxide powder
CN103787376B (en) * 2012-10-30 2016-04-27 甘肃科特光电科技材料有限责任公司 A kind of preparation method of ultra pure magnesium oxide powder
CN102923738A (en) * 2012-11-15 2013-02-13 吉首大学 Method for recovering water soluble manganese and magnesium from electrolytic manganese residue
CN105540622A (en) * 2015-12-31 2016-05-04 上海应用技术学院 Recycling and re-preparation method of silicon-steel level magnesium oxide
CN106745106A (en) * 2016-12-21 2017-05-31 武汉工程大学 A kind of method that nanometric magnesium hydroxide is prepared by phosphorus ore de-magging waste liquid
CN106745106B (en) * 2016-12-21 2018-07-17 武汉工程大学 A method of nanometric magnesium hydroxide is prepared by phosphorus ore de-magging waste liquid
CN110775993A (en) * 2019-12-18 2020-02-11 上栗县上栗镇中心小学 Process for preparing basic magnesium carbonate by liquid-phase crystal method
CN112320825A (en) * 2020-10-26 2021-02-05 安徽景成新材料有限公司 Method for preparing nano magnesium oxide by solid phase method

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Application publication date: 20121003