CN109485099A - A method of it is directly that raw material prepares barium ferrite using low-grade witherite - Google Patents

A method of it is directly that raw material prepares barium ferrite using low-grade witherite Download PDF

Info

Publication number
CN109485099A
CN109485099A CN201811489504.9A CN201811489504A CN109485099A CN 109485099 A CN109485099 A CN 109485099A CN 201811489504 A CN201811489504 A CN 201811489504A CN 109485099 A CN109485099 A CN 109485099A
Authority
CN
China
Prior art keywords
barium ferrite
witherite
barium
temperature
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811489504.9A
Other languages
Chinese (zh)
Inventor
刘仁龙
刘作华
陶长元
杜军
周小霞
刘培乔
刘尚东
曾军辉
唐金晶
范兴
孔令峰
谢昭明
刘艳霞
邓丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CHENGKOU COUNTY PRODUCTIVITY PROMOTION CENTER
Chongqing University
Original Assignee
CHENGKOU COUNTY PRODUCTIVITY PROMOTION CENTER
Chongqing University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CHENGKOU COUNTY PRODUCTIVITY PROMOTION CENTER, Chongqing University filed Critical CHENGKOU COUNTY PRODUCTIVITY PROMOTION CENTER
Priority to CN201811489504.9A priority Critical patent/CN109485099A/en
Publication of CN109485099A publication Critical patent/CN109485099A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/0018Mixed oxides or hydroxides
    • C01G49/0036Mixed oxides or hydroxides containing one alkaline earth metal, magnesium or lead
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Compounds Of Iron (AREA)

Abstract

A method of it is directly that raw material prepares barium ferrite using low-grade witherite, the present invention uses low-grade witherite mineral for raw material, soaks mine by wet process, rationally matches liquid, chemical coprecipitation synthesis, the technological means synthesizing barium ferrite product such as high-temperature calcination.In the present invention, leaching process witherite and hydrochloric acid mass ratio are 1 ︰, 1~1 ︰ 5, and the solid-to-liquid ratio (g/ml) of witherite and water is 1 ︰, 2~1 ︰ 9, and extraction temperature is 30 DEG C~90 DEG C, and extraction time is 1h~6h;Precipitation process pH range is 8~12;Calcination process calcination temperature is 700 DEG C~1400 DEG C, and calcination time is 1h~6h.The present invention makes full use of local low-grade witherite mineral, has good Social benefit and economic benefit while obtained high added value barium ferrite product.With it is existing prepare barium ferrite technology compared with, the advantages of present invention had not only remained its magnetic property, but also overcome its many deficiency, so that preparation totle drilling cost is lower.

Description

A method of it is directly that raw material prepares barium ferrite using low-grade witherite
Technical field
The present invention relates to hydrometallurgys, the preparation field of barium ferrite, in particular to a kind of directly to utilize low-grade poison weight Stone is the method that raw material prepares barium ferrite.
Background technique
Barium ferrite material has a wide range of applications in device elements such as instrument and meter, electroacoustic motor, magnetic separation magnetization.Barium iron Oxysome belongs to research, and a kind of permanent-magnet material, the expression formula of compound can be write as BaFe earlier12O19
People prepare the process of barium ferrite, actually just contain the process of adjustment Ba/Fe ratio.In the prior art, The method for preparing barium ferrite includes mechanical attrition method, chemical coprecipitation, sol-gal process, hydro-thermal method, self propagating high temperature conjunction At method etc..However, raw material used when with these methods to prepare barium ferrite, is chlorate, the oxidation of high-purity Object and molysite etc..
It itself is exactly from Raw Ore by a series of due to the chlorate, oxide and molysite as chemical products What complicated technical process just decomposited, such as barium chloride, barium monoxide, barium hydroxide, be exactly using witherite mineral as raw material and It produces;And the main component of barium ferrite itself but be barium and iron compound in the case where, this is just first passed through at people Then again further through a series of complex technical process a series of complex process separates the barium in witherite mineral with impurity, Allow barium and iron chemical combination.
Not only consume a large amount of resource, the energy in this way, and also create the acid of institute's adapted in two technical process, The waste of great manpower and material resources cost in the reagents such as alkali, salt and finished product forming process.
Summary of the invention
Present invention aim to address in the prior art, prepare barium ferrite not only expend resource, the energy also and can waste it is big The problems such as measuring manpower.
To realize the present invention purpose and the technical solution adopted is that such, a kind of is directly original using low-grade witherite The method that material prepares barium ferrite, which comprises the following steps:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰, 1~1 ︰ 5;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰, 2~1 ︰ 9;
The temperature of the leaching is 30~90 DEG C, and extraction time is 1~6h;
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;
It is total to after pH value adjustment 8~12 in the mixed solution that natrium carbonicum calcinatum and sodium hydroxide is added in mixture A Precipitation reaction;
The molar ratio of metal ion total amount and natrium carbonicum calcinatum in the mixture A is 1 ︰ 1.5;
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 1~5h, and the drying temperature is 60 DEG C~100 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 700 DEG C~1400 DEG C;Calcination time is 1h~6h.
Further, in the whipping process in the step 1.1): stirring rate is 150~350r/min, mixing time 1 ~5h.
Effect of the invention is unquestionable, the invention has the following advantages that
1) present invention is raw materials used to be not the barium chloride of chemical products when preparing barium ferrite, but passes through this Barium chloride solution obtained by inventive method is omitted what the prior art must first separate barium element from witherite mineral The technical process of a series of complex, and directly barium chloride solution is prepared into using natural witherite mineral as primary raw material.Therefore, Compared with existing factory's mature technology, the present invention not only because of the technical process of a series of complex needed for eliminating " separation ", and And save the raw materials such as a large amount of adapted acid, alkali, salt, reagent and a large amount of manpower and material resources time cost.
2) present invention prepares barium ferrite using classical chemical coprecipitation, this illustrates the theoretical base for realizing this technique Plinth and engineering process all have been provided with, it is only necessary to can prepare satisfactory barium iron oxygen using the relatively simple method of technique Body powder.
For example, can be applied on a large scale in the instrument and equipments such as instrument and meter, electroacoustic motor, magnetic separation magnetization.The present invention Method has many advantages, such as that theoretical mature, cost is relatively low, simple process, widely applicable, easy to operate.
The present invention makes full use of local low-grade witherite mineral, tool while obtained high added value barium ferrite product There is good Social benefit and economic benefit.With it is existing prepare barium ferrite technology compared with, the present invention had both remained its magnetic property The advantages of, and overcome its many deficiency, so that preparation totle drilling cost is lower.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used With means, various replacements and change are made, should all include within the scope of the present invention.
Embodiment 1:
A method of it is directly that raw material prepares barium ferrite using low-grade witherite, which is characterized in that including following Step:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰ 1;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰ 2;
The temperature of the leaching is 30 DEG C, extraction time 1h;
In whipping process in the step 1.1): stirring rate 150r/min, mixing time 1h.
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;It will After liquor ferri trichloridi is added in mixture A, under the action of magnetic heating stirrer, 70 DEG C of reaction temperature, adjust while stirring PH to 8 is saved, coprecipitation reaction, reaction time 2h are carried out;
The proportion of the mixture A and ferric trichloride presses barium ferrite (BaFe12O19) chemical formula determines;
The adjusting pH process: it is first adjusted using excessive Carbon Dioxide sodium solution (1.5 times of metal ion mol times); It is adjusted again with the NaOH solution of 6mol/L to required pH, the purpose for the arrangement is that barium ions is made to firstly generate barium carbonate sediment, In subsequent high-temperature burning process, it is more conducive to be converted into barium monoxide and iron oxide further generates barium ferrite crystal, meanwhile, also It can save and directly adjust a large amount of NaOH reagents, save the cost consumed by pH with NaOH solution.
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 1h, and the drying temperature is 60 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 700 DEG C;Calcination time is 1h.
Barium ferrite product obtained in the present embodiment is measured: experiment is using national standard " barium in celestite ore The measurement of content-barium chromate volumetric method " content of barium in (GB9018.2-1988) measurement experiment, using EDTA volumetric determination The content of strontium and calcium in leachate, using the content of the molten middle iron ion of spectrophotometric determination o-phenanthroline leachate.Meanwhile Obtained barium ferrite powder is tested for the property, to illustrate its characteristic performance with magnetic material, it was demonstrated that obtain Barium ferrite material belongs to permanent-magnet material, is to be detected by 7410 vibrating specimen magnetometer of Lake Shore, to obtain it Magnetic parameter.
Measurement result are as follows: the saturation magnetization of barium ferrite product obtained is 25emu/g, coercivity in the present embodiment For 3180Oe.
Embodiment 2:
A method of it is directly that raw material prepares barium ferrite using low-grade witherite, which is characterized in that including following Step:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰ 2;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰ 4;
The temperature of the leaching is 50 DEG C, extraction time 2h;
In whipping process in the step 1.1): stirring rate 200r/min, mixing time 2h.
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;It will After liquor ferri trichloridi is added in mixture A, under the action of magnetic heating stirrer, 70 DEG C of reaction temperature, adjust while stirring PH to 9 is saved, coprecipitation reaction, reaction time 2h are carried out;
The proportion of the mixture A and ferric trichloride presses barium ferrite (BaFe12O19) chemical formula determines;
The adjusting pH process: it is first adjusted using excessive Carbon Dioxide sodium solution (1.5 times of metal ion mol times); It is adjusted again with the NaOH solution of 6mol/L to required pH, the purpose for the arrangement is that barium ions is made to firstly generate barium carbonate sediment, In subsequent high-temperature burning process, it is more conducive to be converted into barium monoxide and iron oxide further generates barium ferrite crystal, meanwhile, also It can save and directly adjust a large amount of NaOH reagents, save the cost consumed by pH with NaOH solution.
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 2h, and the drying temperature is 70 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 900 DEG C;Calcination time is 2h.
Barium ferrite product obtained in the present embodiment is measured: experiment is using national standard " barium in celestite ore The measurement of content-barium chromate volumetric method " content of barium in (GB9018.2-1988) measurement experiment, using EDTA volumetric determination The content of strontium and calcium in leachate, using the content of the molten middle iron ion of spectrophotometric determination o-phenanthroline leachate.Meanwhile Obtained barium ferrite powder is tested for the property, to illustrate its characteristic performance with magnetic material, it was demonstrated that obtain Barium ferrite material belongs to permanent-magnet material, is to be detected by 7410 vibrating specimen magnetometer of Lake Shore, to obtain it Magnetic parameter.
Measurement result are as follows: the saturation magnetization of barium ferrite product obtained is 40.5emu/g, coercive in the present embodiment Power is 4500Oe.
Embodiment 3:
A method of it is directly that raw material prepares barium ferrite using low-grade witherite, which is characterized in that including following Step:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰ 3;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰ 6;
The temperature of the leaching is 70 DEG C, extraction time 3h;
In whipping process in the step 1.1): stirring rate 250r/min, mixing time 3h.
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;It will After liquor ferri trichloridi is added in mixture A, under the action of magnetic heating stirrer, 70 DEG C of reaction temperature, adjust while stirring PH to 10 is saved, coprecipitation reaction, reaction time 2h are carried out;
The proportion of the mixture A and ferric trichloride presses barium ferrite (BaFe12O19) chemical formula determines;
The adjusting pH process: it is first adjusted using excessive Carbon Dioxide sodium solution (1.5 times of metal ion mol times); It is adjusted again with the NaOH solution of 6mol/L to required pH, the purpose for the arrangement is that barium ions is made to firstly generate barium carbonate sediment, In subsequent high-temperature burning process, it is more conducive to be converted into barium monoxide and iron oxide further generates barium ferrite crystal, meanwhile, also It can save and directly adjust a large amount of NaOH reagents, save the cost consumed by pH with NaOH solution.
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 3h, and the drying temperature is 80 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 1100 DEG C;Calcination time is 3h.
Barium ferrite product obtained in the present embodiment is measured: experiment is using national standard " barium in celestite ore The measurement of content-barium chromate volumetric method " content of barium in (GB9018.2-1988) measurement experiment, using EDTA volumetric determination The content of strontium and calcium in leachate, using the content of the molten middle iron ion of spectrophotometric determination o-phenanthroline leachate.Meanwhile Obtained barium ferrite powder is tested for the property, to illustrate its characteristic performance with magnetic material, it was demonstrated that obtain Barium ferrite material belongs to permanent-magnet material, is to be detected by 7410 vibrating specimen magnetometer of Lake Shore, to obtain it Magnetic parameter.
Measurement result are as follows: the saturation magnetization of barium ferrite product obtained is 39.6emu/g, coercive in the present embodiment Power is 1033Oe.
Embodiment 4:
A method of it is directly that raw material prepares barium ferrite using low-grade witherite, which is characterized in that including following Step:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰ 4;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰ 7;
The temperature of the leaching is 80 DEG C, extraction time 4h;
In whipping process in the step 1.1): stirring rate 300r/min, mixing time 4h.
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;It will After liquor ferri trichloridi is added in mixture A, under the action of magnetic heating stirrer, 70 DEG C of reaction temperature, adjust while stirring PH to 11 is saved, coprecipitation reaction, reaction time 2h are carried out;
The proportion of the mixture A and ferric trichloride presses barium ferrite (BaFe12O19) chemical formula determines;
The adjusting pH process: it is first adjusted using excessive Carbon Dioxide sodium solution (1.5 times of metal ion mol times); It is adjusted again with the NaOH solution of 6mol/L to required pH, the purpose for the arrangement is that barium ions is made to firstly generate barium carbonate sediment, In subsequent high-temperature burning process, it is more conducive to be converted into barium monoxide and iron oxide further generates barium ferrite crystal, meanwhile, also It can save and directly adjust a large amount of NaOH reagents, save the cost consumed by pH with NaOH solution.
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 4h, and the drying temperature is 90 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 1200 DEG C;Calcination time is 4h.
Barium ferrite product obtained in the present embodiment is measured: experiment is using national standard " barium in celestite ore The measurement of content-barium chromate volumetric method " content of barium in (GB9018.2-1988) measurement experiment, using EDTA volumetric determination The content of strontium and calcium in leachate, using the content of the molten middle iron ion of spectrophotometric determination o-phenanthroline leachate.Meanwhile Obtained barium ferrite powder is tested for the property, to illustrate its characteristic performance with magnetic material, it was demonstrated that obtain Barium ferrite material belongs to permanent-magnet material, is to be detected by 7410 vibrating specimen magnetometer of Lake Shore, to obtain it Magnetic parameter.
Measurement result are as follows: the saturation magnetization of barium ferrite product obtained is 35.5emu/g, coercive in the present embodiment Power is 3880Oe.
Embodiment 5:
A method of it is directly that raw material prepares barium ferrite using low-grade witherite, which is characterized in that including following Step:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰ 5;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰ 9;
The temperature of the leaching is 90 DEG C, extraction time 6h;
In whipping process in the step 1.1): stirring rate 350r/min, mixing time 5h.
1.2) liquid after leaching obtained in step 1.1) is filtered, isolated solid phase and liquid phase will be consolidated It is mutually washed, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;It will After liquor ferri trichloridi is added in mixture A, under the action of magnetic heating stirrer, 70 DEG C of reaction temperature, adjust while stirring PH to 12 is saved, coprecipitation reaction, reaction time 2h are carried out;
The proportion of the mixture A and ferric trichloride presses barium ferrite (BaFe12O19) chemical formula determines;
The adjusting pH process: it is first adjusted using excessive Carbon Dioxide sodium solution (1.5 times of metal ion mol times); It is adjusted again with the NaOH solution of 6mol/L to required pH, the purpose for the arrangement is that barium ions is made to firstly generate barium carbonate sediment, In subsequent high-temperature burning process, it is more conducive to be converted into barium monoxide and iron oxide further generates barium ferrite crystal, meanwhile, also It can save and directly adjust a large amount of NaOH reagents, save the cost consumed by pH with NaOH solution.
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, used Distilled water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 5h, and the drying temperature is 100 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, Obtain barium ferrite product;
The calcination temperature is 1400 DEG C;Calcination time is 6h.
Barium ferrite product obtained in the present embodiment is measured: experiment is using national standard " barium in celestite ore The measurement of content-barium chromate volumetric method " content of barium in (GB9018.2-1988) measurement experiment, using EDTA volumetric determination The content of strontium and calcium in leachate, using the content of the molten middle iron ion of spectrophotometric determination o-phenanthroline leachate.Meanwhile Obtained barium ferrite powder is tested for the property, to illustrate its characteristic performance with magnetic material, it was demonstrated that obtain Barium ferrite material belongs to permanent-magnet material, is to be detected by 7410 vibrating specimen magnetometer of Lake Shore, to obtain it Magnetic parameter.
Measurement result are as follows: the saturation magnetization of barium ferrite product obtained is 36.8emu/g, coercive in the present embodiment Power is 3690Oe.
From the various embodiments described above as can be seen that barium ferrite powder obtained by the present invention to meet permanent-magnet ferrite height full With the intensity of magnetization (Ms), the feature of high-coercive force (Hc), and the maximum saturation intensity of magnetization (MS) are 40.5emu/g, maximum coercive Power (HC) is M.M.Rashad pure material FeCl under 4500Oe, with equal conditions3、BaCl2The BaFe of preparation12O19Magnetic property (MS=61.8emu/g, HC=3646Oe) comparison, coercivity have advantage, and saturation magnetization is to be improved.

Claims (2)

1. a kind of method for directly preparing barium ferrite using low-grade witherite for raw material, which is characterized in that including following step It is rapid:
1) barium chloride solution is prepared
1.1) witherite after ball milling being sieved is added in hydrochloric acid solution, stirring, wet-leaching;
The weight ratio of the witherite and hydrochloric acid solution is 1 ︰, 1~1 ︰ 5;
The witherite and the w/v (g ︰ mL) of water stated is 1 ︰, 2~1 ︰ 9;
The temperature of the leaching is 30~90 DEG C, and extraction time is 1~6h;
1.2) by obtained in step 1.1) leach after liquid filter, isolated solid phase and liquid phase, by solid phase into Row washing, the liquid after collecting washing;
1.3) after mixing the liquid after liquid phase and washing after separating obtained in step 1.2), mixture A is obtained;
The mixed solution of natrium carbonicum calcinatum and sodium hydroxide is added in mixture A, after pH value adjustment to 8~12, carries out coprecipitated It forms sediment and reacts;
The molar ratio of metal ion total amount and natrium carbonicum calcinatum in the mixture A is 1 ︰ 1.5;
2) barium ferrite powder is prepared
2.1) mixture after progress coprecipitation reaction in step 1.3) is filtered, obtains filtrate and filter cake, uses distillation Water is by Washing of Filter Cake to neutrality, then filter cake is placed in drying box and is dried, and obtains barium ferrite precursor powder;
The drying time is 1~5h, and the drying temperature is 60 DEG C~100 DEG C;
2.2) barium ferrite precursor powder obtained in step 2.1) is placed in temperature programming Muffle furnace and is calcined, obtained Barium ferrite product;
The calcination temperature is 700 DEG C~1400 DEG C;Calcination time is 1h~6h.
2. a kind of method for directly preparing barium ferrite using low-grade witherite for raw material according to claim 1, Be characterized in that: in the whipping process in the step 1.1): stirring rate is 150~350r/min, and mixing time is 1~5h.
CN201811489504.9A 2018-12-06 2018-12-06 A method of it is directly that raw material prepares barium ferrite using low-grade witherite Pending CN109485099A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811489504.9A CN109485099A (en) 2018-12-06 2018-12-06 A method of it is directly that raw material prepares barium ferrite using low-grade witherite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811489504.9A CN109485099A (en) 2018-12-06 2018-12-06 A method of it is directly that raw material prepares barium ferrite using low-grade witherite

Publications (1)

Publication Number Publication Date
CN109485099A true CN109485099A (en) 2019-03-19

Family

ID=65698291

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811489504.9A Pending CN109485099A (en) 2018-12-06 2018-12-06 A method of it is directly that raw material prepares barium ferrite using low-grade witherite

Country Status (1)

Country Link
CN (1) CN109485099A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111762817A (en) * 2020-04-24 2020-10-13 重庆大学 Method for preparing strontium barium ferrite from strontium slag
CN114735754A (en) * 2022-05-24 2022-07-12 沈阳理工大学 Barium ferrite and preparation method thereof
CN115772032A (en) * 2022-12-14 2023-03-10 宁波合荣磁业有限公司 Preparation method of permanent magnetic ferrite material for calendering

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101092243A (en) * 2006-06-20 2007-12-26 河北盛华化工有限公司 Method for producing liquid of barium chloride by using mineral powder of Duyingshi in low grade
RO121812B1 (en) * 2003-03-20 2008-05-30 Ionel Augustin Stoica Process for preparing precipitated barium sulphate
CN102485692A (en) * 2010-12-06 2012-06-06 沈阳理工大学 Preparation method of two-dimensional sheet-shaped barium ferrite
CN104891549A (en) * 2015-05-06 2015-09-09 四川理工学院 Technology for producing barium chloride by taking witherite as raw material
CN106517289A (en) * 2017-01-05 2017-03-22 四川理工学院 Method of using low-grade witherite to produce high-purity barium chloride

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RO121812B1 (en) * 2003-03-20 2008-05-30 Ionel Augustin Stoica Process for preparing precipitated barium sulphate
CN101092243A (en) * 2006-06-20 2007-12-26 河北盛华化工有限公司 Method for producing liquid of barium chloride by using mineral powder of Duyingshi in low grade
CN102485692A (en) * 2010-12-06 2012-06-06 沈阳理工大学 Preparation method of two-dimensional sheet-shaped barium ferrite
CN104891549A (en) * 2015-05-06 2015-09-09 四川理工学院 Technology for producing barium chloride by taking witherite as raw material
CN106517289A (en) * 2017-01-05 2017-03-22 四川理工学院 Method of using low-grade witherite to produce high-purity barium chloride

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王冰青: "毒重石的浸取及钡铁氧体的制备实验研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111762817A (en) * 2020-04-24 2020-10-13 重庆大学 Method for preparing strontium barium ferrite from strontium slag
CN114735754A (en) * 2022-05-24 2022-07-12 沈阳理工大学 Barium ferrite and preparation method thereof
CN114735754B (en) * 2022-05-24 2023-06-16 沈阳理工大学 Barium ferrite and preparation method thereof
CN115772032A (en) * 2022-12-14 2023-03-10 宁波合荣磁业有限公司 Preparation method of permanent magnetic ferrite material for calendering

Similar Documents

Publication Publication Date Title
CN109485099A (en) A method of it is directly that raw material prepares barium ferrite using low-grade witherite
CN103101935B (en) Method for preparing lithium carbonate from coal ash
CN104150576B (en) A kind of coal ash for manufacturing is for the method for PAFC
CN101913853B (en) Method for preparing bismuth titanate-barium titanate powder by hydrothermal method
CN101508471B (en) Process for producing cobaltic-cobaltous oxide
CN101475367A (en) Preparation of nanometer-level barium ferrite magnetic material
CN105110382A (en) Method for preparing high-purity gamma-Fe2O3 iron oxide red pigment
CN105293555B (en) A kind of method that utilization strontium slag prepares high-purity strontium chloride
CN102786095B (en) Method for preparing manganous manganic oxide
CN108840343A (en) A method of silica solution is prepared using gangue
CN106745124B (en) A kind of technique that aluminium hydroxide and concrete admixture are produced from Coaseries kaolin
CN107793180A (en) Improve the method for magnesium leaching efficiency and application in phosphorus ore
CN102703982A (en) Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine
CN101786670A (en) Method for synthesizing iron oxide black through liquid phase oxidation with oxygen
CN111268743B (en) Method for preparing ferroferric oxide by using copperas
CN102219493A (en) Method for preparing MnZn ferrite material powder from acid washing waste liquid and galvanized zinc slag
CN103303955B (en) Production method of calcium carbonate whisker
CN102070332A (en) Nano-crystal Mn-Zn ferrite magnetic material with high initial permeability and high thermal-magnetic sensitivity and preparation method of nano-crystal Mn-Zn ferrite magnetic material
CN107697893A (en) Improve the method for calcium leaching efficiency and its product and application in phosphorus ore
CN106868321B (en) A method of processing scheelite extracts tungsten
CN103833061B (en) A kind of flyash dissolution fluid combination method deferrization process
CN102627304A (en) Method for preparing magnesium-aluminum hydrotalcite
CN109384263A (en) A method of iron oxide yellow is prepared using the waste acid liquor of chloride containing iron
CN112194189B (en) Process for preparing iron-based pigment from sulfur-chlorine coupling waste liquid
CN105347399A (en) Chromium leaching method by ammonium sulfate roasting decomposition of chromite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190319