CN103214011A - Boric sludge comprehensive utilization method for preparing nanometer magnesia and nanocrystalline iron oxide - Google Patents

Boric sludge comprehensive utilization method for preparing nanometer magnesia and nanocrystalline iron oxide Download PDF

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CN103214011A
CN103214011A CN2013101244437A CN201310124443A CN103214011A CN 103214011 A CN103214011 A CN 103214011A CN 2013101244437 A CN2013101244437 A CN 2013101244437A CN 201310124443 A CN201310124443 A CN 201310124443A CN 103214011 A CN103214011 A CN 103214011A
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hydrochloric acid
iron
magnesium chloride
obtains
magnesium
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CN103214011B (en
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张廷安
豆志河
南嘉良
刘燕
范世钢
吕国志
杜承天
赵秋月
杨瑞
赫冀成
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Northeastern University China
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Abstract

The invention belongs to the field of nanometer technology, and particularly relates to a boric sludge comprehensive utilization method for preparing nanometer magnesia and nanocrystalline iron oxide. The boric sludge comprehensive utilization method is carried out according to the following steps of: pressing and leaching boric sludge in a hydrochloric acid system at a low temperature; filtering and separating to obtain magnesium chloride and ferric chloride leachate and borosilicate-rich residue; adding MgO or Fe2O3 to the magnesium chloride and ferric chloride leachate to adjust the pH (Potential Of Hydrogen) of the leachate; adding H2O2 to oxidize bivalent ferrous ions in the leachate into ferric ions during precipitating, in order to precipitate and separate the iron ions in the leachate in a form of ferric hydroxide; filtering and separating to obtain an Fe(OH)3 precipitate and a magnesium chloride solution; roasting the obtained Fe(OH3) precipitate to obtain Fe2O3 powder; and directly pyrolyzing the obtained magnesium chloride solution, thus obtaining the nanometer MgO powder and a hydrochloric acid solution, wherein the hydrochloric acid solution can be returned to be recycled. The boric sludge comprehensive utilization method has high leaching efficiency, enables the leaching time to be reduced, saves the energy, reduces the exhaust emission, realizes non-waste clean production in the whole process, and is a novel typical green and clean production process.

Description

A kind of boron mud method of comprehensive utilization for preparing nano magnesia, nano-sized iron oxide
Technical field
The invention belongs to field of nanometer technology, particularly a kind of boron mud method of comprehensive utilization for preparing nano magnesia, nano-sized iron oxide.
Background technology
Boron mud is the solid slag that industrial use boron magnesium mineral or ferro-boron mineral are produced boron product process dischargings such as boric acid and borax, and color is light brown or canescence.In recent years, along with a large amount of uses of boron compounds such as boric acid, borax, boron alloy, the output of China's boron product is with the speed increase in every year 6% ~ 7%, and the grade in boron magnesium ore deposit descends year by year, causes average boron product per ton (with B 2O 3Meter) the boron mud of output does not wait for being increased to 4 ~ 5 tons from 3 ~ 4 tons, causes boron mud quantity discharged and day to increase progressively.By the end of the year ends 2011, China's boron mud stacking amount has always surpassed the forty-two million ton, and only Liaoning Province just surpasses 2,600 ten thousand tons, and sharply increases with annual quantity more than 1,500,000 tons.The boron dust is long-pending not only to take a large amount of farmlands, and environmental pollution is serious.Because its alkalescence is strong, severe contamination farmland, soil and underground water, make and stack ground not even a blade of grass grows for many years.The boron argillization consists of: MgO23.0% ~ 43.4%, SiO 222.6% ~ 32.7%, FeO2.4% ~ 14.6%, B 2O 30.7% ~ 5.6%, Al 2O 30.1% ~ 5.0%.Boron mud is mainly used in flocculation agent, refractory materials, devitrified glass, steel-making additive, the filler for plastic of material of construction, wastewater treatment and contains boron fertilizer.Above purposes all is the magnesium elements that is based on effectively utilizing in the boron mud basically, and the iron in the boron mud, silicon, boron etc. have the valency constituent element to fail to realize comprehensive utilization.If have the valency constituent element to extract effectively these, not only produce huge economic benefit, alleviate China's industrial raw material in short supply, can also solve serious environmental and pollute, have very high social benefit.
At present, boron mud utilizes method mainly to comprise: acid hydrolyzation, alkaline hydrolysis method and carborization etc.Wherein, acid hydrolyzation is at first with the preroasting under 600 ℃ ~ 800 ℃ condition of boron mud; Then with the boron mud after sulfuric acid or the salt acid treatment roasting, make magnesium, iron, major metal such as aluminium, calcium element enters in the liquid solution and exists with ionic species, and the oxide solid or the siliceous colloid form flocculation sediment that make boron form boric acid colloidal form, silicon formation silicon separate with leach liquor with the solid form.The alkaline hydrolysis method at first reclaims the magnet mineral by physical methods such as magnetic separation, to hang down the boron sludge of iron and the solid mixture that caustic soda high-temperature roasting reaction obtains alkaline hydrolysis again, make soluble silicate enter solution after water embathes and be present in the liquid phase, magnesium enters solid with the precipitation forms of oxyhydroxide.After the solid-liquid filtering separation, handle magnesium respectively, the thick product of silicon obtains products such as silicon-dioxide, water glass, magnesium oxide.Carborization is at first with boron mud solid and unslaked lime or rhombspar mixture slaking (can add a certain amount of solubility calcium, magnesium salts as catalyzer), obtain magnesium hydroxide and other solid mixtures, add carbonic acid gas carbonization utilization, obtain Magnesium hydrogen carbonate soluble in water and indissoluble solid mixture, separate after the super-dry calcining obtains Magnesium Carbonate Light 41-45 and magnesium oxide product.Above method all exists complex process, energy consumption height, pollutes defective workmanships such as big, does not meet the requirement of greatly developing recycling economy that national medium-term and long-term development program proposes.
Summary of the invention
At the problems referred to above, the object of the present invention is to provide the green production flow process of a kind of save energy, minimizing environmental pollution, a kind of boron mud method of comprehensive utilization for preparing nano magnesia, nano-sized iron oxide of the present invention, carry out according to following steps:
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:(5 ~ 20) L, extraction temperature is 50 ~ 120 ℃, concentration of hydrochloric acid is 2 ~ 8mol/L, and extraction time is 30 ~ 120min, and magnesium, iron leaching yield are all greater than 95%; Principal reaction in the leaching process:
Mg 2SiO 4+4HCl=2MgCl 2+SiO 2 +2H 2O
Fe 2O 3+6HCl =2FeCl 3+3H 2O
MgCO 3+2HCl =MgCl 2+H 2O+CO 2
2Fe 2SiO 3+O 2+12HCl=4FeCl 3+2SiO 2+6H 2O ；
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.0 ~ 3.8, for effective precipitate and separate iron, adds excessive H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution; Principal reaction in the precipitate and separate process: MgO+2HCl=MgCl 2+ H 2O
Fe 2O 3+6HCl=2FeCl 3+3H 2O
4Fe 2++O 2+2H 2O=4Fe 3++4OH -
Fe 3++3OH -=Fe(OH) 3↓；
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcining temperature are 200 ~ 500 ℃, and calcination time is 30 ~ 120min; Principal reaction in the calcination process: Fe (OH) 3=Fe 2O 3+ 3H 2O;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 400 ~ 700 ℃, and pyrolysis time is 30 ~ 120min; Principal reaction in the pyrolytic process: MgCl 2+ H 2O=MgO+2HCl.
Characteristics of the present invention and beneficial effect are:
(1) utilizes low temperature and pressure to soak, have the leaching efficiency height, shorten extraction time; Having cancelled the high-temperature roasting pre-treatment step of existing method simultaneously, saved the energy, reduced exhaust gas emission, is typical green cleaner production new technological process;
(2) realized that magnesium, iron, silicon, boron etc. in the boron mud have the comprehensive utilization of valency constituent element, improved resource utilization, met the recycling economy development requirement that country proposes;
(3) adopt the solution pyrolytic technique, obtained the MgO product, hydrochloric acid obtains recycle simultaneously, has realized that whole process do not have useless cleaner production;
(4) present technique has obtained high-quality iron product, nano magnesia and rich borosilicate slag simultaneously, has improved value-added content of product.
Description of drawings
The boron mud former state XRD figure spectrum that Fig. 1 uses for the embodiment of the invention;
The SEM photo (200nm) of the nano magnesia that Fig. 2 makes for the embodiment of the invention 1;
The SEM photo (400nm) of the nano-sized iron oxide that Fig. 3 makes for the embodiment of the invention 1;
The XRD figure spectrum of the nano magnesia that Fig. 4 makes for the embodiment of the invention 1;
The XRD figure spectrum of the nano-sized iron oxide that Fig. 5 makes for the embodiment of the invention 1.
Embodiment
The present invention will be further described below in conjunction with embodiment.
The test set that the embodiment of the invention is used is scanning electron microscope SU8020 of Hitachi and German Brooker A8 type x-ray diffractometer.
Embodiment 1
The XRD of used boron mud as shown in Figure 1, mainly by thing phase composites such as magnesiumcarbonate, Magnesium Silicate q-agent, ferric metasilicate, ferric oxide, its chemical constitution is as shown in table 1.
Table 1 boron argillization composition/mass%
Form B 2O 3 MgO CaO SiO 2 Fe 2O 3 Al 2O 3
Content 2.5 35 5 18 25 2
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:5L, extraction temperature is 120 ℃, concentration of hydrochloric acid is 8mol/L, and extraction time is 30min, and the leaching yield of magnesium and iron is respectively 95.5%, 95.2%;
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.8, for effective precipitate and separate iron, adds H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution;
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcination condition: calcining temperature is 200 ℃, calcination time is 120min;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 400 ℃, and pyrolysis time is 120min.
The SEM photo of the nano magnesia that makes, nano-sized iron oxide is found out by figure that respectively as Fig. 2, shown in Figure 3 the average particulate diameter of magnesium oxide powder is less than 200nm, and the average particulate diameter of croci is less than 400nm; The nano magnesia that makes, the XRD figure of nano-sized iron oxide are composed respectively as Fig. 4, shown in Figure 5, are found out that by figure magnesium oxide powder is single magnesium oxide phase, and ferric oxide is single Fe 2O 3Phase composite.
Embodiment 2
Used boron mud is with embodiment 1.
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:10L, extraction temperature is 100 ℃, concentration of hydrochloric acid is 5mol/L, and extraction time is 90min, and the leaching yield of magnesium and iron is respectively 96.5%, 95.5%;
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.2, for effective precipitate and separate iron, adds H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution;
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcination condition: calcining temperature is 300 ℃, calcination time is 90min;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 500 ℃, and pyrolysis time is 90min.
After testing, the magnesium oxide and the ferric oxide that make are Nano grade.
Embodiment 3
Used boron mud is with embodiment 1.
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:15L, extraction temperature is 80 ℃, concentration of hydrochloric acid is 3mol/L, and extraction time is 60min, and the leaching yield of magnesium and iron is respectively 97.5%, 96.2%;
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.5, for effective precipitate and separate iron, adds H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution;
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcination condition: calcining temperature is 400 ℃, calcination time is 60min;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 600 ℃, and pyrolysis time is 60min.
After testing, the magnesium oxide and the ferric oxide that make are Nano grade.
Embodiment 4
Used boron mud is with embodiment 1.
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:20L, extraction temperature is 50 ℃, concentration of hydrochloric acid is 2mol/L, and extraction time is 120min, and the leaching yield of magnesium and iron is respectively 98.5%, 97.2%;
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.0, for effective precipitate and separate iron, adds H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution;
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcination condition: calcining temperature is 500 ℃, calcination time is 30min;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 700 ℃, and pyrolysis time is 30min.
After testing, the magnesium oxide and the ferric oxide that make are Nano grade.

Claims (1)

1. boron mud method of comprehensive utilization for preparing nano magnesia, nano-sized iron oxide is characterized in that carrying out according to following steps:
(1) boron mud being hanged down temperature and pressure under hydrochloric acid system soaks, filtering separation obtains magnesium chloride, iron(ic) chloride leach liquor and rich borosilicate slag then, wherein, the low temperature and pressure condition of soaking is: the solid-to-liquid ratio of boron mud and hydrochloric acid is 1kg:(5 ~ 20) L, extraction temperature is 50 ~ 120 ℃, concentration of hydrochloric acid is 2 ~ 8mol/L, and extraction time is 30 ~ 120min, and magnesium, iron leaching yield are all greater than 95%;
(2) add MgO or Fe in the magnesium chloride that in step (1), obtains, the iron(ic) chloride leach liquor 2O 3The pH value of regulating leach liquor is 3.0 ~ 3.8, for effective precipitate and separate iron, adds H in precipitation process 2O 2Make the divalence ferrous ion in the leach liquor be oxidized to ferric ion, iron ion is wherein separated out with ironic hydroxide form precipitation, filtering separation obtains Fe (OH) then 3Precipitation and magnesium chloride solution;
(3) with the Fe (OH) that obtains in the step (2) 3Precipitation is calcined and is obtained Fe 2O 3Powder, calcination condition: calcining temperature is 200 ~ 500 ℃, calcination time is 30 ~ 120min;
(4) the magnesium chloride solution direct heat that obtains in the step (2) is separated obtain nano-MgO powder and hydrochloric acid soln, wherein hydrochloric acid soln returns and realizes recycle in the step (1), and pyrolysis temperature is 400 ~ 700 ℃, and pyrolysis time is 30 ~ 120min.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106214011A (en) * 2016-09-30 2016-12-14 广东美的厨房电器制造有限公司 Cooking appliance
CN112456523A (en) * 2020-12-08 2021-03-09 山东理工大学 Method for preparing high-purity magnesium chloride hexahydrate product by directly leaching magnesium element in magnesite
CN116143177A (en) * 2023-01-18 2023-05-23 贵州大学 Method for producing iron oxide red from gangue leachate

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Publication number Priority date Publication date Assignee Title
GB1572053A (en) * 1976-04-07 1980-07-23 Veitscher Magnesitwerke Ag Method for the production of pure magnesium oxide
CN101549876A (en) * 2009-05-15 2009-10-07 东北大学 Method for producing boric acid and co-produce magnesium hydrate and calcium sulphate by utilizing boron-rich slag

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GB1572053A (en) * 1976-04-07 1980-07-23 Veitscher Magnesitwerke Ag Method for the production of pure magnesium oxide
CN101549876A (en) * 2009-05-15 2009-10-07 东北大学 Method for producing boric acid and co-produce magnesium hydrate and calcium sulphate by utilizing boron-rich slag

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106214011A (en) * 2016-09-30 2016-12-14 广东美的厨房电器制造有限公司 Cooking appliance
CN112456523A (en) * 2020-12-08 2021-03-09 山东理工大学 Method for preparing high-purity magnesium chloride hexahydrate product by directly leaching magnesium element in magnesite
CN112456523B (en) * 2020-12-08 2022-06-17 山东理工大学 Method for preparing high-purity magnesium chloride hexahydrate product by directly leaching magnesium element in magnesite
CN116143177A (en) * 2023-01-18 2023-05-23 贵州大学 Method for producing iron oxide red from gangue leachate

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