CN114057228A - Low-sulfur superfine manganese carbonate and preparation method thereof - Google Patents
Low-sulfur superfine manganese carbonate and preparation method thereof Download PDFInfo
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Abstract
The invention provides low-sulfur superfine manganese carbonate and a preparation method thereof; the preparation raw materials comprise a manganese sulfate solution and an ammonium bicarbonate solution; adding a manganese sulfate solution into an ammonium bicarbonate solution for precipitation reaction; the manganese sulfate solution is added ten to fifty percent of the theoretical amount of precipitation reaction per minute. The chemical reaction formula of the invention is as follows: MnSO4+2NH4HCO3→MnCO3↓+(NH4)2SO4+H2O+CO2×) @. In the reaction process of the precipitation reaction, the rapid feeding mode is adopted, so that the manganese carbonate is rapidly generated in the reaction, the generation of alkaline manganese sulfate precipitation is avoided due to the increase of the reaction PH caused by the ammonium bicarbonate solution, and the content of carbonate in the product is reduced. In addition, since a large amount of manganese ions are put into the ammonium bicarbonate solution, a large amount of seed crystals are generated in a short time, and the particle size of manganese carbonate is reduced. The faster the feed rate, the more manganese ions come into contact with the ammonium bicarbonate at the same time, producing a larger amount of new seed crystals and the finer the particle size.
Description
Technical Field
The invention relates to low-sulfur superfine manganese carbonate and a preparation method thereof, belonging to the technical field of preparation of manganese carbonate.
Background
Manganese carbonates can be classified into high-purity manganese carbonates and industrial manganese carbonates; the industrial manganese carbonate can be used in the fields of agricultural base fertilizer, feed additive, chemical industry, ceramics, printing and dyeing, ore flotation and the like; the high-purity manganese carbonate is an important intermediate for synthesizing a special manganese-related material, and plays an important role in the aspects of special metallurgy and manganese-containing functional materials. Manganese carbonates are generally prepared by reacting manganese sulfate with ammonium bicarbonate. As the pH value is between 6 and 8 during the conventional manganese carbonate precipitation reaction, basic manganese sulfate precipitation is easy to generate, and the sulfate radical content in the product reaches 1 to 2 percent. In addition, the manganese carbonate particles are extremely easy to agglomerate, and the existing product particles are generally at the level of 50-100 mu m and cannot meet the requirements of special manganese-related materials.
Disclosure of Invention
The invention aims to provide low-sulfur superfine manganese carbonate and a preparation method thereof, aiming at least one technical problem in the background technology.
The scheme provided by the invention is as follows:
a method for preparing low-sulfur superfine manganese carbonate comprises preparing raw materials including manganese sulfate solution and ammonium bicarbonate solution; the specific operation is as follows: adding the manganese sulfate solution into an ammonium bicarbonate solution for precipitation reaction; the addition amount of the manganese sulfate solution per minute is ten percent to fifty percent of the theoretical amount of the manganese sulfate solution used in the precipitation reaction.
The chemical reaction formula of the invention is as follows:
MnSO4+2NH4HCO3→MnCO3↓+(NH4)2SO4+H2O+CO2↑
the theoretical amount is the molar ratio of manganese sulfate and ammonium bicarbonate to be matched with the chemical formula in order to complete the precipitation reaction according to the chemical formula. That is, 1 mol of manganese sulfate reacts with 2 mol of ammonium bicarbonate to complete the reaction.
In the reaction process of the precipitation reaction, a rapid feeding mode is adopted, so that manganese carbonate is rapidly generated in the reaction, the generation of basic manganese sulfate precipitation is avoided due to the increase of the reaction PH brought by the ammonium bicarbonate solution, and the content of carbonate in the product is reduced. In addition, since a large amount of manganese ions are put into the ammonium bicarbonate solution, a large amount of seed crystals are generated in a short time, and the particle size of manganese carbonate is reduced. The faster the feed rate, the more manganese ions come into contact with the ammonium bicarbonate at the same time, producing a larger amount of new seed crystals and the finer the particle size. If the charging time is too long, manganese ions grow on the original seed crystal, are agglomerated and become coarse in particle size.
In the present invention, it is preferable that the pH is controlled to 8 to 14 during the precipitation reaction.
As the technology of the present invention, the amount of the ammonium bicarbonate added is preferably 1.05 to 1.2 times the theoretical amount. In the invention, a specific manganese sulfate dosage is determined according to the chemical equation, then the theoretical ammonium bicarbonate dosage is calculated, and then the theoretical ammonium bicarbonate dosage is multiplied by 1.05-1.2 to obtain the final actual ammonium bicarbonate addition. The dosage of the ammonium bicarbonate in the invention is 1.05-1.2 times of the theoretical dosage, so that the manganese ions can be effectively and completely precipitated.
As the technique of the invention, the concentration of the manganese sulfate solution is preferably 240g/L-375 g/L. The higher the manganese sulfate concentration is, the larger the capacity is, the unnecessary water waste is reduced, and meanwhile, the higher the manganese ion concentration in the solution is, the easier the new seed crystal is produced, and the finer the manganese carbonate particle size is.
In the present invention, it is preferable that ammonia water is further added to the precipitation reaction.
The reaction equation when adding ammonia is:
MnSO4+NH4HCO3+NH3·H2O→MnCO3↓+(NH4)2SO4+H2O
the ammonia water is added into the ammonium bicarbonate solution, so that the generation of carbon dioxide can be effectively reduced, and the reaction kettle is prevented from overflowing when the manganese carbonate is rapidly synthesized; the stable reaction is ensured.
In the technique of the present invention, the ammonia water is preferably added in an amount of 0 to 50% by mole based on the total ammonium content. The ammonia water exceeds 50 percent of the total ammonia content, and can generate manganese hydroxide in the precipitation process, and the manganese hydroxide is easy to oxidize, thereby influencing the quality of the manganese carbonate.
In the present invention, the precipitation reaction is preferably carried out at room temperature. The reaction is carried out at normal temperature, heating is not needed, and energy and time are saved.
Preferably, the manganese carbonate precipitate obtained by the precipitation reaction is dried for 12-18h at the temperature of 60-120 ℃. Because the prepared manganese carbonate precipitate has different water content and decomposition degree, superfine manganese carbonate products with different granularities can be obtained by adopting different drying temperatures and drying times, and the granularity D50 is between 1 and 40 mu m, thus the requirements of various industries can be well met.
Based on the same technical concept, the application also provides low-sulfur superfine manganese carbonate prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the industrial manganese sulfate or high-purity manganese sulfate is subjected to precipitation reaction in the ammonium bicarbonate solution, and the manganese sulfate solution is quickly added into the ammonium bicarbonate solution by controlling the adding time of the manganese sulfate solution, so that a large amount of seed crystals can be generated, and the granularity of the manganese carbonate is thinned. And because the pH value of the ammonium bicarbonate is easy to increase for the reaction environment, the generation of alkaline manganese sulfate precipitation is avoided, and the content of carbonate in the product is reduced. Therefore, the sulfate radical content in the manganese carbonate precipitate prepared by the method is less than 500ppm, the granularity D50 can be controlled to be between 1 and 40um according to different drying temperatures and drying times, and the requirements of various industries can be well met.
Drawings
FIG. 1 is a particle size diagram of a low sulfur ultra fine manganese carbonate product in example 1 of the present invention;
FIG. 2 is a particle size diagram of a low sulfur ultra fine manganese carbonate product in example 2 of the present invention;
FIG. 3 is a particle size diagram of a low sulfur ultra fine manganese carbonate product in example 3 of the present invention;
FIG. 4 is a particle size diagram of a low sulfur ultra fine manganese carbonate product in example 4 of the present invention;
FIG. 5 is a particle size diagram of a low sulfur ultra fine manganese carbonate product according to example 5 of the present invention;
FIG. 6 is a particle size diagram of a low sulfur ultra fine manganese carbonate product according to example 6 of the present invention;
FIG. 7 is a particle size diagram of a low sulfur ultra fine manganese carbonate product according to example 7 of the present invention;
FIG. 8 is a graph of the particle size of the manganese carbonate product of comparative example 1 of the present invention;
FIG. 9 is a graph of the particle size of the manganese carbonate product of comparative example 2 of the present invention;
FIG. 10 is a particle size diagram of a manganese carbonate product of comparative example 3 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention is described more fully and in detail below, but the scope of the invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate, putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L of solution, weighing 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, adding the solution into the ammonium bicarbonate solution at a constant speed of 2.4L per minute, and stirring for five minutes after pouring. The pH value was controlled at 8.0 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in figure 1.
Example 2
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.0 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 2.
Example 3
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 5 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.0 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 3.
Example 4
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 4.
Example 5
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 950g of ammonium bicarbonate and 736g of 28% ammonia water solution to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 5.
Example 6
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 80 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 6.
Example 7
A method for preparing low-sulfur superfine manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 18 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 7.
Comparative example 1
A method for preparing manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 1 liter per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 8.
Comparative example 2
A method for preparing manganese carbonate.
Weighing 1.9kg of ammonium bicarbonate and putting the ammonium bicarbonate into a 15L plastic barrel to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 7.5 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 9.
Comparative example 3
A method for preparing manganese carbonate.
Weighing 950g of ammonium bicarbonate and 883g of 28% ammonia water solution to prepare 12L solution; measuring 5L of 346g/L industrial manganese sulfate solution under the condition of stirring, and pouring the solution into ammonium bicarbonate solution at a constant speed according to the rate of adding 2.4 liters per minute; after pouring, the mixture is stirred for five minutes. The pH value was controlled at 8.4 during the reaction.
Separating the product, washing the solid with 60 deg.C warm water at a liquid-solid ratio of 5 for 3 times, and oven drying at 60 deg.C for 12 h. The obtained detection data of the manganese carbonate product are shown in table 1. The particle size diagram is shown in fig. 10.
Table 1:
the foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (9)
1. The preparation method of the low-sulfur superfine manganese carbonate is characterized in that the preparation raw materials comprise a manganese sulfate solution and an ammonium bicarbonate solution; the specific operation is as follows: adding the manganese sulfate solution into an ammonium bicarbonate solution for precipitation reaction;
the addition amount of the manganese sulfate solution per minute is ten percent to fifty percent of the theoretical amount of the manganese sulfate solution used in the precipitation reaction.
2. The method according to claim 1, wherein the pH is controlled to 8 to 14 during the precipitation reaction.
3. The method according to claim 1, wherein the amount of ammonium bicarbonate added is 1.05 to 1.2 times the theoretical amount.
4. The method according to claim 1, wherein the concentration of the manganese sulfate solution is 240g/L to 375 g/L.
5. The production method according to any one of claims 1 to 4, wherein ammonia is further added to the precipitation reaction.
6. The method according to claim 5, wherein the aqueous ammonia is added in an amount of 0 to 50% by mole based on the total ammonium content.
7. The production method according to claim 1, wherein the precipitation reaction is carried out at normal temperature.
8. The preparation method of claim 1, wherein the manganese carbonate precipitate obtained by the precipitation reaction is dried at 60-120 ℃ for 12-18 h.
9. A low-sulfur ultrafine manganese carbonate produced by the production method according to any one of claims 1 to 8.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121049A (en) * | 1994-10-18 | 1996-04-24 | 冶金工业部长沙矿冶研究院 | Method for producing high-purity manganese carbonate by using pyrolusite |
| JP3032975B1 (en) * | 1998-12-25 | 2000-04-17 | 株式会社ジャパンエナジー | Manganese carbonate production method |
| CN104891576A (en) * | 2015-05-06 | 2015-09-09 | 陕西省紫阳县湘贵锰业有限公司 | Preparation method of manganese sulfate monohydrate |
| CN107082452A (en) * | 2017-04-28 | 2017-08-22 | 潍坊泰兴生物化工有限责任公司 | A kind of production technology for preparing manganese carbonate |
| CN109095503A (en) * | 2018-07-18 | 2018-12-28 | 重庆上甲电子股份有限公司 | A method of manganese carbonate is produced using hydroquinone reduction electrolytic manganese anode mud |
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- 2021-12-01 CN CN202111455065.1A patent/CN114057228A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121049A (en) * | 1994-10-18 | 1996-04-24 | 冶金工业部长沙矿冶研究院 | Method for producing high-purity manganese carbonate by using pyrolusite |
| JP3032975B1 (en) * | 1998-12-25 | 2000-04-17 | 株式会社ジャパンエナジー | Manganese carbonate production method |
| CN104891576A (en) * | 2015-05-06 | 2015-09-09 | 陕西省紫阳县湘贵锰业有限公司 | Preparation method of manganese sulfate monohydrate |
| CN107082452A (en) * | 2017-04-28 | 2017-08-22 | 潍坊泰兴生物化工有限责任公司 | A kind of production technology for preparing manganese carbonate |
| CN109095503A (en) * | 2018-07-18 | 2018-12-28 | 重庆上甲电子股份有限公司 | A method of manganese carbonate is produced using hydroquinone reduction electrolytic manganese anode mud |
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| 王博知等: "用软锰矿矿浆脱硫吸收液制备碳酸锰", 《湿法冶金》, pages 148 - 151 * |
| 甘永兰等: "一种重质二氧化锰的制备方法", 《河南化工》, pages 17 - 20 * |
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