CN101104521A - Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride - Google Patents
Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride Download PDFInfo
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- CN101104521A CN101104521A CNA2007100659324A CN200710065932A CN101104521A CN 101104521 A CN101104521 A CN 101104521A CN A2007100659324 A CNA2007100659324 A CN A2007100659324A CN 200710065932 A CN200710065932 A CN 200710065932A CN 101104521 A CN101104521 A CN 101104521A
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Abstract
The present invention relates to a method for magnesium sulfate liquid waste treatment and active magnesium oxide joint preparation. A certain amount of magnesium sulfate liquid waste is measured to be heated for concentration and crystallization under the mechanical mixing condition, then dried after crystallization and calcined at the temperature between 1130 and 1200 DEG C for 6 to 8 hours to get primary magnesium oxide, while the produced flue gas is reclaimed for sulfuric acid preparation; water is added when the obtained primary magnesium oxide reaches 70 to 95 DEG C for digestion, and then magnesium hydroxide emulsion is achieved through filtering impurity; the magnesium hydroxide emulsion is transferred to a micro-pressure reaction vessel and the pressure will be controlled between 2 to 6 kg; carbon dioxide is charged into the vessel under stirring conditions for carbonizing the emulsion for 1 to 3 hours to obtain magnesium bicarbonate solution through filtering; under the heating and stirring conditions, the magnesium bicarbonate solution is pyrolyzed for 1 to 2 hours to get basic magnesium carbonate sediment; finally, after filtering, washing and drying, the basic magnesium carbonate sediment is calcined at 950 to 1000 DEG C for 4 to 6 hours to get active magnesium oxide. The invention has the advantages of simple technology, high production efficiency, high magnesium yield and low cost, which avoids the problems of large lime consumption and slag amount in lime milk and magnesium sulfate liquid waste and enables reasonable use of magnesium sulfate liquid waste.
Description
Technical field the present invention relates to field of metallurgy, particularly relates to the preparation method of sal epsom treating waste liquid and activated magnesia.
The background technology activated magnesia also claims light calcined magnesia, has been widely used in fields such as chemical industry, papermaking, rubber, medicine, livestock industry, building materials metallurgy and refractory materials.At present, different mutually because of raw material route, known exploitation mainly contains following several preparation method:
Rhombspar-carbonation method: people such as Hu Qingfu " inorganic chemicals industry " 2004 the 36th the 6th phase of volume known the rhombspar carborization method of producing activated magnesia, with rhombspar (xMgCO
3YCaCO
3) or magnesite (MgCO
3) calcine at 1000～1100 ℃, add water digestion and make Mg (OH)
2And Ca (OH)
2, use CO
2Carbonization obtains Magnesium hydrogen carbonate and by-product lime carbonate.Remove mother liquor (heavy magnesium water) behind the lime carbonate,, obtain magnesium basic carbonate, through 500～900 ℃ of calcining 8～10h, can make light magnesium oxide more again through pyrolysis.
These method characteristics are long flow paths, and equipment is huge, but raw material cheaply is easy to get, and production cost is lower.Extensively adopt this method in the industrial production.
Bittern-ammonium carbonate method: with bittern is raw material, utilizes volatile salt or carbonated aqueous ammonia to produce light magnesium oxide.Bittern carries out replacement(metathesis)reaction 1～4h with the carbon ammonium after purifying, generate the magnesiumcarbonate precipitation.Use the deionized water wash post precipitation, magnesiumcarbonate is carried out drying and calcining obtain light magnesium oxide for 800 ℃～900 ℃.This method technology is comparatively simple, easy to operate, the quality product height, and founding the factory is not subjected to the restriction in the places of origin of raw materials, but production cost is higher.
Bittern-ammoniacal liquor method: open closely " chemical engineering .1999 " the 27th the 2nd phase of volume known with MgCl
26H
2O and analytical pure NH
3H
2O is a raw material, adopts the experimentation of direct precipitation method as follows: at first with MgCl
26H
2O is mixed with certain density solution, drips an amount of precipitation agent analytical pure NH under certain temperature and well-beaten condition
3H
2O filters, washs after question response is complete, through the no CI of acidated AgNO3 check
-The time obtain Mg (OH) 2 precipitation, slough planar water through vacuum-drying, make magnesium oxide after the calcining again, product cut size between 20～100nm, median size 62nm, particle shape is based on sphere.
Adopt refined bittern and ammonia react to generate magnesium hydrate precipitate, with reacting rear material filter the magnesium hydroxide reaction mother liquor.Magnesium hydroxide through the washing, the oven dry, calcine light magnesium oxide.
This method advantage is that technology is comparatively simple.Shortcoming is that energy consumption and production cost are higher, founds the factory to be subjected to places of origin of raw materials restriction.
Sal epsom-ammonia process: it is raw material that people such as Hu Zhangwen disclosed with the serpentine in " Anhui University of Engineering Science ﹠ Technology's journal " 2004 the 19th the 4th phases of volume, obtain purified sal epsom by acidleach, purification, adopt the ammonia precipitation process legal system to be equipped with magnesium hydroxide, through calcine high-purity magnesium oxide.Orthogonal experiment has been determined precipitin reaction and incinerating optimum process condition: 50 ℃ of temperature of reaction, reaction times 40min, POV magnesium solution concentration 1.5mol/L, calcination time 3h.With this understanding, the magnesian purity of reaction final product reaches more than 99%, has satisfied the requirement of high-purity magnesium oxide.This method technical process is simple, and constant product quality is adapted to suitability for industrialized production, and very big development prospect is arranged.
Bittern-lime method: Wang Luming has reported with bittern to be raw material in the 30th the 1st phase of volume of " sea lake salt and chemical industry " calendar year 2001, is precipitation agent with lime or rhombspar, generates magnesium hydrate precipitate.The precipitation after filtration, wash, dry and calcine light magnesium oxide.Promptly utilize purified bittern and milk of lime to do raw material,, carry out precipitin reaction four different reaction times sections by strictness control reaction pH value and reaction times.Drip flocculation agent and make Mg (OH)
2The slip rapid subsidence is through washing, filtration.(800 ℃) calcining is fallen forward under lower temperature, and the MgO particle that finally makes meets the requirement of ultra-fine grain between 60nm-80nm.
Brucite is produced magnesium oxide method: Guo Ruxin and has been set forth brucite production method of magnesium oxide in " sea lake salt and chemical industry " 2000 the 29th the 2nd phases of volume, promptly gets 200 order brucite powder 30g, sizes mixing with 1L water.Under 15 ℃ of conditions with the pressure carbonization 1h of 1.25MPa.By brucite effective ingredient 62%MgO, transformation efficiency is 78%.Carry out pyrolysis then under 98 ℃, form magnesium basic carbonate, yield is more than 99%.And then carry out drying and calcining, and slough crystal water at 215 ℃ when dry, further be warming up to 532 ℃ and remove CO
2, when temperature reaches 590 ℃, the CO in the magnesium basic carbonate
2And H
2O all removes, and forms light magnesium oxide.
Sal epsom-carbon ammonium: people such as Li Junmei have sketched with small fertilizer plant's carbonating mother liquor and sal epsom in " chemical industry metallurgical " 1998 the 19th the 1st phases of volume to be raw material, to carry out precipitin reaction, prepare highly purified light magnesium oxide that the application uniform design has been investigated V
1/ V
2(volume ratio of the hydrochloric acid that consumes when titration carbonization mother liquor to the first point of equivalent and second point of equivalent), precipitation agent consumption, temperature of reaction, reaction times ageing temperature and time are to the influence of productive rate, obtain regression equation by regression analysis, this equation asks extreme value to obtain optimum process condition, experimental result under top condition shows: the productive rate of magnesium basic carbonate is optional 95.5%, and the purity of light magnesium oxide reaches more than 99.5%.
Magnesite-carborization: people such as Wang Yafang disclosed in " mineral products comprehensive utilization " the 6th phase in 2005: with magnesite calcining system must magnesia unslacked be raw material, make magnesium bicarbonate solution through digestion, carbonating, adopting gac is that sorbent material removes impurity such as calcium, iron, and pyrolysis again, calcining make high-purity magnesium oxide.Studied of the influence of factors such as adsorption temp and duration of contact, and sour consumption and time are to the influence of regeneration of activated carbon to the charcoal absorption deironing.The result shows: under 20 ℃, and absorption reaction 80min, MgO content is greater than 995% in the final magnesium oxide product, and CaO content is less than 0.09%%, and Fe content is less than 0.05%; Time is very little to the regeneration effect influence, and regeneration of activated carbon is respond well, can reuse, and provides a new way for preparing various high-purity magnesium oxides.
It is raw material that 2006 the 40th the 4th phases of volume of magnesite-calcination method: Li Huanzai " refractory materials " have set forth with magnesite, calcine 2h down at 850 ℃ earlier and obtain light calcined magnesia, aquation becomes magnesium hydroxide then, dry back is light-burned down in differing temps (being respectively 450 ℃, 500 ℃, 550 ℃, 600 ℃) and soaking time (being respectively 1h, 1.5h, 2h), has prepared extra light calcined magnesia by decomposing magnesium hydroxide.The result shows: magnesium hydroxide resolves into magnesium oxide fully in the time of 500 ℃; Light roasting temperature and soaking time have bigger influence to magnesium oxide activity (characterizing with iodine absorption value), and along with the rising of temperature, the magnesium oxide activity reduces gradually, and under uniform temp, along with holding time prolonging, magnesian active the reduction; In Heating temperature is 500 ℃, and soaking time is a light-burned decomposition magnesium hydroxide under the condition of 1h, can obtain the activated magnesia that iodine absorption value reaches 191.42mgg.
In sum, utilizing operations such as sal epsom waste liquid condensing crystal, calcining, digestion, filtration, carbonization, pyrolysis to prepare activated magnesia does not appear in the newspapers as yet.Task of the present invention is to make full use of the sal epsom waste liquid, and decontamination is turned waste into wealth, and has realized effective improvement of sal epsom on the one hand, has realized effective utilization of magnesium on the other hand.
Summary of the invention the purpose of this invention is to provide a kind of sal epsom treating waste liquid and coproduction activated magnesia method, have that technology is simple, production efficiency is high, magnesium yield height, low cost and other advantages, can make the sal epsom waste liquid reach the purpose of administering and rationally utilizing, administering for sal epsom simultaneously provides a kind of novel method.
1. the present invention finishes according to the following steps: measure a certain amount of sal epsom waste liquid, heat condensing crystal under the mechanical stirring condition, the crystallization after drying at 1130～1200 ℃ of calcining 6～8h, just obtains primary oxidation magnesium, and the flue gas of generation reclaims, and uses as system sulfuric acid; The primary oxidation magnesium that obtains is added water digestion at 70～95 ℃, filtering and impurity removing, obtain magnesium hydroxide emulsion, emulsion is moved in the minute-pressure reactor, control pressure is at 2～6kg, logical carbonic acid gas carbonization under agitation condition, carbonization time is 1～3h, after filtration, obtain magnesium bicarbonate solution, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, pyrolysis time is 1～2h, filter at last, wash, dry,, obtain activated magnesia at 950～1000 ℃ of calcining 4～6h.
2. the technico-economical comparison that reaches:
1. content of magnesia is greater than 95%;
2. the magnesium yield is greater than 92%.
The advantage that has compared with prior art:
With other method of handling the sal epsom waste liquid relatively, its technical process of the technology of the present invention is short, simple to operate, production efficiency is high, magnesium yield height, low, the environmental friendliness of cost.The sal epsom waste liquid obtains activated magnesia through operations such as condensing crystal, drying, calcining, digestion, carbonization, pyrolysis.This technology has realized effective improvement of sal epsom, but while output activated magnesia reaches the improvement of sal epsom waste liquid and effectively utilization.Present method has been avoided ammoniacal liquor directly to precipitate producing the sad filter of magnesium hydroxide, yellow soda ash or volatile salt directly precipitating, produce in follow-up pollution and the lime and consume amount of lime big, produce problems such as the quantity of slag is big.In addition, this method energy consumption is low, requiredly concentrates, calcining, pyrolysis, carbonizing apparatus is made easily and process, process is simple, is convenient to operation and produces, and is suitable for large-scale processing, thereby the present invention provides a kind of novel method for handling a large amount of sal epsom waste liquids, has potential and uses and promotional value.Patent of the present invention has that technology is simple, production efficiency is high, magnesium yield height, low cost and other advantages, problems such as milk of lime neutralisation of sulphuric acid magnesium waste liquid lime consumption is big, the quantity of slag have been avoided, can make the sal epsom waste liquid reach reasonable utilization, administer for sal epsom simultaneously and utilization provides a kind of novel method.
Description of drawings Fig. 1 is a process flow sheet of the present invention
Embodiment
Embodiment 1:
1, the chemical ingredients of sal epsom waste liquid is as follows:
Fe
2+2.42~2.49g/L；Mg
2+12.78~13.01g/L；Na
+3.97~4.26g/L；Ni
2+0.044~0.047g/L
2. processing condition: measure the sal epsom waste liquid of 5000ml, heat condensing crystal under the mechanical stirring condition, the crystallization after drying at 1130 ℃ of calcining 8h, just obtains primary oxidation magnesium, and the flue gas of generation reclaims, and uses as system sulfuric acid; The primary oxidation magnesium that obtains is added water digestion at 80 ℃, and filtering and impurity removing obtains magnesium hydroxide emulsion, emulsion is moved in the minute-pressure reactor, and control pressure leads to the carbonic acid gas carbonization at 4kg under agitation condition, carbonization time is 2h, after filtration, obtain magnesium bicarbonate solution, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, pyrolysis time is 1.5h, filter at last, wash, dry,, obtain activated magnesia at 950 ℃ of calcining 6h.Under these processing condition, content of magnesia 97.71%; The magnesium yield reaches 93.04%.
Embodiment 2:
1. the chemical ingredients of sal epsom waste liquid is as follows:
Fe
2+2.85~2.96g/L；Mg
2+14.76~14.90g/L；Na
+4.57~4.66g/L；Ni
2+0.031~0.040g/L
2. processing condition: measure the sal epsom waste liquid of 10000ml, heat condensing crystal under the mechanical stirring condition, the crystallization after drying at 1150 ℃ of calcining 7h, just obtains primary oxidation magnesium, and the flue gas of generation reclaims, and uses as system sulfuric acid; The primary oxidation magnesium that obtains is added water digestion at 90 ℃, and filtering and impurity removing obtains magnesium hydroxide emulsion, emulsion is moved in the minute-pressure reactor, and control pressure leads to the carbonic acid gas carbonization at 5kg under agitation condition, carbonization time is 1.5h, after filtration, obtain magnesium bicarbonate solution, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, pyrolysis time is 2.0h, filter at last, wash, dry,, obtain activated magnesia at 970 ℃ of calcining 5h.Under these processing condition, content of magnesia 96.44%; The magnesium yield reaches 93.59%.
Embodiment 3:
1. the chemical ingredients of sal epsom waste liquid is as follows:
Fe
2+2.71~2.87g/L；Mg
2+16.98~17.24g/L；Na
+4.72~4.93g/L；Ni
2+.056~0.059g/L
2. processing condition: measure the sal epsom waste liquid of 8000ml, heat condensing crystal under the mechanical stirring condition, the crystallization after drying at 1200 ℃ of calcining 6h, just obtains primary oxidation magnesium, and the flue gas of generation reclaims, and uses as system sulfuric acid; The primary oxidation magnesium that obtains is added water digestion at 95 ℃, and filtering and impurity removing obtains magnesium hydroxide emulsion, emulsion is moved in the minute-pressure reactor, and control pressure leads to the carbonic acid gas carbonization at 6kg under agitation condition, carbonization time is 2.0h, after filtration, obtain magnesium bicarbonate solution, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, pyrolysis time is 1.0h, filter at last, wash, dry,, obtain activated magnesia at 100 ℃ of calcining 4h.Under these processing condition, content of magnesia 98.01%; The magnesium yield reaches 94.27%.
Claims (3)
1. the method for sal epsom treating waste liquid and coproduction activated magnesia, it is characterized in that finishing according to the following steps: measure a certain amount of sal epsom waste liquid, under the mechanical stirring condition, heat condensing crystal, the crystallization after drying, calcining, the primary oxidation magnesium of acquisition, the flue gas that produces reclaims, and uses as system sulfuric acid; The primary oxidation magnesium that obtains is added water digestion, filtering and impurity removing, obtain magnesium hydroxide emulsion, move into emulsion in the minute-pressure reactor and control pressure, logical carbonic acid gas carbonization under agitation condition, after filtration, obtain magnesium bicarbonate solution, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, filter at last, wash, dry and calcine, obtain activated magnesia.
2. according to the method for claims 1 described sal epsom treating waste liquid and coproduction activated magnesia, it is characterized in that calcining temperature is 1130 ~ 1200 ℃ after the described crystallization, calcination time is 6 ~ 8h.
3. according to the method for claims 1 described sal epsom treating waste liquid and coproduction activated magnesia, it is characterized in that, the described temperature that adds water digestion is 70 ~ 95 ℃, control pressure is at 2 ~ 6kg, carbonization time is 1 ~ 3h, pyrolysis time is 1 ~ 2h, filters at last, washs, dries, at 950 ~ 1000 ℃ of calcining 4 ~ 6h.
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Cited By (14)
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| CN101880772A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recycling magnesium from magnesium-containing waste solution |
| CN101880771A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recovering magnesium from magnesium-contained waste liquid |
| CN102390848A (en) * | 2011-08-08 | 2012-03-28 | 河北科技大学 | Comprehensive utilization process for magnesium sulfate |
| WO2014067403A1 (en) * | 2012-10-30 | 2014-05-08 | 甘肃科特光电科技材料有限责任公司 | Method for preparing ultrapure magnesia powder |
| CN104843748A (en) * | 2014-02-14 | 2015-08-19 | 中国科学院过程工程研究所 | Low-grade magnesite and low-grade magnesite tailing comprehensive recycling use method |
| 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 |
| CN106976895A (en) * | 2017-05-11 | 2017-07-25 | 广州峰华化工科技有限公司 | A kind of manufacture method of activated magnesia |
| CN107364879A (en) * | 2017-06-29 | 2017-11-21 | 中国恩菲工程技术有限公司 | The method that magnesium elements and calcium constituent are reclaimed from Adlerika |
| CN109179484A (en) * | 2018-11-13 | 2019-01-11 | 常宁市华兴冶化实业有限责任公司 | A kind of method that carbonizatin method prepares activated zinc oxide |
| CN111041204A (en) * | 2018-10-11 | 2020-04-21 | 有研稀土新材料股份有限公司 | Comprehensive utilization method of magnesium and/or calcium-containing waste liquid in rare earth smelting separation process |
| CN112661178A (en) * | 2020-12-25 | 2021-04-16 | 山东信能达工程科技有限公司 | Preparation and production process of high-purity magnesium oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1025180C (en) * | 1992-02-24 | 1994-06-29 | 西安地质学院科技开发公司 | Method for extracting magnesium oxide from serpentine |
| CN1302993C (en) * | 2004-04-07 | 2007-03-07 | 田玉海 | Production of light magnesium carbonate or light magnesium oxide |
-
2007
- 2007-06-05 CN CN200710065932A patent/CN100579906C/en not_active Expired - Fee Related
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| CN101880772A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recycling magnesium from magnesium-containing waste solution |
| CN101880771A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recovering magnesium from magnesium-contained waste liquid |
| CN101880772B (en) * | 2010-06-07 | 2012-07-04 | 中国恩菲工程技术有限公司 | Method for recycling magnesium from magnesium-containing waste solution |
| CN102390848A (en) * | 2011-08-08 | 2012-03-28 | 河北科技大学 | Comprehensive utilization process for magnesium sulfate |
| WO2014067403A1 (en) * | 2012-10-30 | 2014-05-08 | 甘肃科特光电科技材料有限责任公司 | Method for preparing ultrapure magnesia powder |
| 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 |
| CN104843748A (en) * | 2014-02-14 | 2015-08-19 | 中国科学院过程工程研究所 | Low-grade magnesite and low-grade magnesite tailing comprehensive recycling use method |
| 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 |
| CN106976895A (en) * | 2017-05-11 | 2017-07-25 | 广州峰华化工科技有限公司 | A kind of manufacture method of activated magnesia |
| CN107364879A (en) * | 2017-06-29 | 2017-11-21 | 中国恩菲工程技术有限公司 | The method that magnesium elements and calcium constituent are reclaimed from Adlerika |
| CN107364879B (en) * | 2017-06-29 | 2019-11-15 | 中国恩菲工程技术有限公司 | The method of magnesium elements and calcium constituent is recycled from Adlerika |
| CN111041204A (en) * | 2018-10-11 | 2020-04-21 | 有研稀土新材料股份有限公司 | Comprehensive utilization method of magnesium and/or calcium-containing waste liquid in rare earth smelting separation process |
| CN109179484A (en) * | 2018-11-13 | 2019-01-11 | 常宁市华兴冶化实业有限责任公司 | A kind of method that carbonizatin method prepares activated zinc oxide |
| CN114180603A (en) * | 2020-12-11 | 2022-03-15 | 安徽金禾实业股份有限公司 | Method for producing active magnesium oxide from waste residues of spices |
| CN112661178A (en) * | 2020-12-25 | 2021-04-16 | 山东信能达工程科技有限公司 | Preparation and production process of high-purity magnesium oxide |
| CN115072812A (en) * | 2021-03-16 | 2022-09-20 | 宝山钢铁股份有限公司 | Silicon steel magnesium oxide wastewater recycling treatment method and treatment system |
| CN115536192A (en) * | 2021-06-29 | 2022-12-30 | 宝山钢铁股份有限公司 | Silicon steel magnesium oxide wastewater recycling treatment and sludge recycling process |
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