CN105883864A - Method for producing basic magnesium carbonate from boron mud waste material - Google Patents

Method for producing basic magnesium carbonate from boron mud waste material Download PDF

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Publication number
CN105883864A
CN105883864A CN201410504597.3A CN201410504597A CN105883864A CN 105883864 A CN105883864 A CN 105883864A CN 201410504597 A CN201410504597 A CN 201410504597A CN 105883864 A CN105883864 A CN 105883864A
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China
Prior art keywords
chloride
hydroxide
filtrate
magnesium
boron mud
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CN201410504597.3A
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Chinese (zh)
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邓家国
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CHANGDE YUNGANG BIOTECHNOLOGY Co Ltd
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CHANGDE YUNGANG BIOTECHNOLOGY Co Ltd
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Priority to CN201410504597.3A priority Critical patent/CN105883864A/en
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Abstract

The invention discloses a method for producing basic magnesium carbonate from a boron mud waste material and relates to inorganic chemical three-waste treatment and integrated utilization. The method comprises preparing basic magnesium carbonate through boron mud recovery, purification and synthesis and simultaneously preparing calcium hydroxide and manganese hydroxide. The recovery process comprises that boron mud is subjected to steam heating and then is subjected to liquid-solid separation under action of a spin-drying centrifugal machine so that the filtrate mainly containing boric acid is obtained, the filtrate is processed, ammonium chloride is added into the magnesium oxide-containing filter cake, the mixture undergoes a reaction to produce a magnesium chloride hydrate, ammonium hydroxide, calcium chloride and manganese chloride solution, the solution is filtered and the filter cake is processed. The purification process comprises removing impurities in the recovered filtrate through magnesium hydroxide so that calcium chloride and manganese chloride respectively produce hydroxide precipitates and the precipitates are filtered to form calcium hydroxide and manganese hydroxide. The synthesis process comprises that carbon dioxide is added into the purified filtrate so that magnesium chloride and ammonium hydroxide in the filtrate are carbonized and a basic magnesium carbonate-ammonium chloride mixed solution is obtained, the mixed solution is filtered to form filter cake basic magnesium carbonate and the filtrate ammonium chloride can be recycled. The method improves boron mud waste material economic benefits.

Description

A kind of method utilizing boric sludge waste to produce basic magnesium carbonate
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly one utilizes boric sludge waste to produce alkali The method of formula magnesium carbonate.
Background technology
Boron mud is with boromagnesite (2MgO B2O3·H2O) it is raw material, is mixed with soda by roasting, pulverizing, take carbon water law Produce Borax (Na2B4O7·10H2O), remaining solid waste after washing, crystallization process extract Borax.Producing one ton of Borax can Producing 4 tons of boron mud, a borax plant producing 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Owing to the discharge capacity of boron mud is relatively big, The current multiple comprehensive Utilization Ways of domestic employing, in addition to producing light magnesium carbonate and magnesium oxide and plastic and rubber filler, also produces boron Mei Lin compound fertilizer, make honeycomb briquette coal charging and do architectural Borax etc..
Magnesium in boron mud is typically all presented in magnesium carbonate, sometimes has difference also with the mineral products difference of boromagnesite. The component of production light magnesium carbonate boron mud is such that magnesium oxide and accounts for 38%, and silicon dioxide accounts for 20%, and carbon dioxide accounts for 17%, Boron oxide accounts for 3%, and calcium oxide accounts for 3%, and manganese oxide accounts for 0.11%, and other is moisture content.
One, should improve constantly the value of output object to the utilization of boron mud, product that some markets of output are in short supply, that added value is big, To improve the economic benefit that boron mud utilizes.
Two, it is known that the utilization of boron mud is relevant with magnesium, and magnesium-containing compound is very extensive in the application of each field, wherein alkali formula Magnesium carbonate can be used as excellent filler and the reinforcing agent of rubber;It also is used as fire-retardant heat-insulation material adiabatic, resistant to elevated temperatures;Stone Cotton light magnesium carbonate is excellent insulant, can be used for shipbuilding and boiler manfacturing;Can be also used for manufacture high glass goods, Magnesium salt, pigment, paint and articles for daily use etc.;Pharmaceutically also acting as antacid;Also can make desiccant, colour fixative, carrier, Anti-caking agent, purposes is quite varied.
Therefore, in the technical scheme processing boron mud refuse, the recycling of the compound of boron should be considered, as produced alkali formula as far as possible Magnesium carbonate.
Summary of the invention
It is contemplated that for the utilization of boron mud and the market demand, it is provided that a kind of method utilizing boric sludge waste to produce basic magnesium carbonate.
For achieving the above object, the technical scheme of a kind of method utilizing boric sludge waste to produce basic magnesium carbonate of the present invention is such as Under:
A kind of method utilizing boric sludge waste to produce basic magnesium carbonate, boron mud, by recovery, purification and synthesis technique, prepares alkali formula Magnesium carbonate, simultaneously co-producing calcium hydroxide and manganous hydroxide:
Described recovery process is: boron mud steam is heated to 59~81 DEG C and maintains 1.2~2.1 hours, then centrifugal with drying Machine solid-liquor separation, obtains the deep processing separately of the filtrate based on boric acid;Magnesium oxide in filter cake boron mud and ammonium chloride are based on pure material Mass ratio 1: 2.45~2.89, add water and react in corrosion-resistant reactor, stirring;Reaction generate magnesium chloride hydrate, Ammonia, calcium chloride and manganese chloride solution;It is filtrated to get the deep processing separately of filter cake silicon dioxide;The filtrate of clarification is done the purest Change;
Described purifying process is: the clear filtrate that recovered technique obtains appropriate magnesium hydroxide impurity and purification, calcium chloride and chlorine Change manganese and generate hydroxide precipitation respectively, through filtration washing, drying and crushing, sizing screening, packaging respectively obtain calcium hydroxide and Manganous hydroxide product;Gained filtrate is magnesium chloride and ammonia clear liquor;
Described synthesis technique is: in the filtrate after purified technique, magnesium chloride and ammonia and the carbon dioxide quality based on pure material Than 1: 0.52~0.954: 0.24~0.68 carbonization in corrosion-resistant asher, stirring;Obtain basic magnesium carbonate and ammonium chloride mixes Close solution;It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be basic carbonate magnesium products;The ammonium chloride of clarification is molten Liquid can recycle in recovery process.
Boron mud used by the present invention be produce light magnesium carbonate boron mud, its component is: magnesium oxide, silicon dioxide, carbon dioxide, Boron oxide, calcium oxide, manganese oxide and moisture.Certainly, other boron mud of similar components also adapt to the one of the present invention and utilize boron Mud waste material produces the method for basic magnesium carbonate.
The chemical equation of the present invention is:
7H2O+MgO+2NH4Cl=MgCl2·6H2O+2NH4OH
H2O+CaO+2NH4Cl=CaCl2+2NH4OH
H2O+MnO+2NH4Cl=MnCl2+2NH4OH
CaCl2+Mg(OH)2=MgCl2+Ca(OH)2
MnCl2+Mg(OH)2=MgCl2+Mn(OH)2
2MgCl2+4NH4OH+CO2=Mg2(OH)2CO3+4NH4Cl+H2O
The beneficial effects of the present invention is: one, it is provided that a kind of method utilizing boric sludge waste to produce basic magnesium carbonate, permissible Effectively process boric sludge waste.Its two, preparation includes basic magnesium carbonate, calcium hydroxide and manganous hydroxide, is respectively provided with multiple use, Remarkable in economical benefits, improves the economic benefit processing boric sludge waste.Its three, prepare ammonium chloride can recycle, investment Few, reduce the cost processing boric sludge waste.Its four, preparation purity is high, and quality is guaranteed.
Detailed description of the invention
Embodiment one
A kind of method utilizing boric sludge waste to produce basic magnesium carbonate, boron mud, by recovery, purification and synthesis technique, prepares alkali formula Magnesium carbonate, simultaneously co-producing calcium hydroxide and manganous hydroxide, boron mud used by the present invention is the boron mud producing light magnesium carbonate, its component For: magnesium oxide 38%, silicon dioxide 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11 %, other are moisture.
Described recovery process is: takes 500Kg boron mud steam and is heated to 59~81 DEG C of maintenances 1.2~2.1 hours, then with getting rid of Dry centrifuge solid-liquor separation, obtains the deep processing separately of the filtrate based on boric acid;Magnesium oxide (pure quality is 190Kg) in filter cake boron mud With ammonium chloride mass ratio 1: 2.48 based on pure material, add water and react in corrosion-resistant reactor, stirring;Reaction generates chlorination The hydrate of magnesium, ammonia, calcium chloride and manganese chloride solution;It is filtrated to get the deep processing separately of filter cake silicon dioxide;The filtrate of clarification Do further purification;
Described purifying process is: the clear filtrate that recovered technique obtains appropriate magnesium hydroxide impurity and purification, calcium chloride and chlorine Change manganese and generate hydroxide precipitation respectively, through filtration washing, drying and crushing, sizing screening, packaging respectively obtain calcium hydroxide and Manganous hydroxide product;Gained filtrate is magnesium chloride and ammonia clear liquor;
Described synthesis technique is: in the filtrate after purified technique, magnesium chloride (it is 418Kg that previous process generates the pure quality of magnesium chloride) With mass ratio 1: 0.54: 0.26 carbonization based on pure material of ammonia and carbon dioxide in corrosion-resistant asher, stirring;Obtain Basic magnesium carbonate and ammonium chloride mixed solution;It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be basic magnesium carbonate Product 229Kg;The 345Kg ammonium chloride obtained can recycle in recovery process.
Embodiment two
A kind of method utilizing boric sludge waste to produce basic magnesium carbonate, boron mud, by recovery, purification and synthesis technique, prepares alkali formula Magnesium carbonate, simultaneously co-producing calcium hydroxide and manganous hydroxide, boron mud used by the present invention is the boron mud producing light magnesium carbonate, its component For: magnesium oxide 38%, silicon dioxide 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11 %, other are moisture.
Described recovery process is: takes 500Kg boron mud steam and is heated to 59~81 DEG C of maintenances 1.2~2.1 hours, then with getting rid of Dry centrifuge solid-liquor separation, obtains the deep processing separately of the filtrate based on boric acid;Magnesium oxide (pure quality is 190Kg) in filter cake boron mud With ammonium chloride mass ratio 1: 2.68 based on pure material, add water and react in corrosion-resistant reactor, stirring;Reaction generates chlorination The hydrate of magnesium, ammonia, calcium chloride and manganese chloride solution;It is filtrated to get the deep processing separately of filter cake silicon dioxide;The filtrate of clarification Do further purification;
Described purifying process is: the clear filtrate that recovered technique obtains appropriate magnesium hydroxide impurity and purification, calcium chloride and chlorine Change manganese and generate hydroxide precipitation respectively, through filtration washing, drying and crushing, sizing screening, packaging respectively obtain calcium hydroxide and Manganous hydroxide product;Gained filtrate is magnesium chloride and ammonia clear liquor;
Described synthesis technique is: in the filtrate after purified technique, magnesium chloride (it is 452Kg that previous process generates the pure quality of magnesium chloride) With mass ratio 1: 0.74: 0.46 carbonization based on pure material of ammonia and carbon dioxide in corrosion-resistant asher, stirring;Obtain Basic magnesium carbonate and ammonium chloride mixed solution;It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be basic magnesium carbonate Product 339Kg;The 511Kg ammonium chloride obtained can recycle in recovery process.
Embodiment three
A kind of method utilizing boric sludge waste to produce basic magnesium carbonate, boron mud, by recovery, purification and synthesis technique, prepares alkali formula Magnesium carbonate, simultaneously co-producing calcium hydroxide and manganous hydroxide, boron mud used by the present invention is the boron mud producing light magnesium carbonate, its component For: magnesium oxide 38%, silicon dioxide 20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11 %, other are moisture.
Described recovery process is: takes 500Kg boron mud steam and is heated to 59~81 DEG C of maintenances 1.2~2.1 hours, then with getting rid of Dry centrifuge solid-liquor separation, obtains the deep processing separately of the filtrate based on boric acid;Magnesium oxide (pure quality is 190Kg) in filter cake boron mud With ammonium chloride mass ratio 1: 2.88 based on pure material, add water and react in corrosion-resistant reactor, stirring;Reaction generates chlorination The hydrate of magnesium, ammonia, calcium chloride and manganese chloride solution;It is filtrated to get the deep processing separately of filter cake silicon dioxide;The filtrate of clarification Do further purification;
Described purifying process is: the clear filtrate that recovered technique obtains appropriate magnesium hydroxide impurity and purification, calcium chloride and chlorine Change manganese and generate hydroxide precipitation respectively, through filtration washing, drying and crushing, sizing screening, packaging respectively obtain calcium hydroxide and Manganous hydroxide product;Gained filtrate is magnesium chloride and ammonia clear liquor;
Described synthesis technique is: in the filtrate after purified technique, magnesium chloride (it is 486Kg that previous process generates the pure quality of magnesium chloride) With mass ratio 1: 0.94: 0.66 carbonization based on pure material of ammonia and carbon dioxide in corrosion-resistant asher, stirring;Obtain Basic magnesium carbonate and ammonium chloride mixed solution;It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be basic magnesium carbonate Product 463Kg;The 698Kg ammonium chloride obtained can recycle in recovery process.

Claims (2)

1. one kind utilizes the method that boric sludge waste produces basic magnesium carbonate, it is characterised in that: boron mud is by recovery, purification and synthesis Technique, prepares basic magnesium carbonate, co-producing calcium hydroxide and manganous hydroxide simultaneously: described recovery process is: added by boron mud steam Heat to 59~81 DEG C maintains 1.2~2.1 hours, then with drying centrifuge solid-liquor separation, obtains the filtrate based on boric acid another Row deep processing;Magnesium oxide in filter cake boron mud and the ammonium chloride mass ratio 1: 2.45~2.89 based on pure material, adds water and reacts on In corrosion-resistant reactor, stirring;Reaction generates the hydrate of magnesium chloride, ammonia, calcium chloride and manganese chloride solution;It is filtrated to get The deep processing separately of filter cake silicon dioxide;The filtrate of clarification does further purification;Described purifying process is: recovered technique obtains Clear filtrate with appropriate magnesium hydroxide impurity and purification, calcium chloride and manganese chloride generate hydroxide precipitation respectively, through diafiltration Wash, drying and crushing, sizing screening, packaging respectively obtain calcium hydroxide and manganous hydroxide product;Gained filtrate is magnesium chloride and ammonia Clarification of water liquid;Described synthesis technique is: in the filtrate after purified technique, magnesium chloride and ammonia with carbon dioxide based on pure material Mass ratio 1: 0.52~0.954: 0.24~0.68 carbonization in corrosion-resistant asher, stirring;Obtain basic magnesium carbonate and chlorine Change ammonium mixed solution;It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be basic carbonate magnesium products;The chlorine of clarification Change ammonium salt solution can recycle in recovery process.
A kind of method utilizing boric sludge waste to produce basic magnesium carbonate the most according to claim 1, it is characterised in that: described Boron mud, containing magnesium oxide, silicon dioxide, carbon dioxide, boron oxide, calcium oxide, manganese oxide and moisture in its component.
CN201410504597.3A 2014-09-16 2014-09-16 Method for producing basic magnesium carbonate from boron mud waste material Pending CN105883864A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107915241A (en) * 2017-05-30 2018-04-17 张旭 Boric sludge is for method of magnesium oxide
CN108358223A (en) * 2018-05-02 2018-08-03 淄博美盛化工有限公司 A kind of processing method of boracic magnesium slag
CN108408747A (en) * 2018-05-02 2018-08-17 淄博美盛化工有限公司 A kind of calcination method puies forward the processing method of magnesium slag obtained by lithium

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107915241A (en) * 2017-05-30 2018-04-17 张旭 Boric sludge is for method of magnesium oxide
CN108358223A (en) * 2018-05-02 2018-08-03 淄博美盛化工有限公司 A kind of processing method of boracic magnesium slag
CN108408747A (en) * 2018-05-02 2018-08-17 淄博美盛化工有限公司 A kind of calcination method puies forward the processing method of magnesium slag obtained by lithium

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Application publication date: 20160824