Method for continuously preparing soft agglomerated nano manganese carbonate

A manganese carbonate and nanotechnology, which is applied in the field of nanomaterials, can solve the problems that nanomanganese carbonate cannot be reached, is not a nanomaterial, and is unfavorable for large-scale production, and achieves the effect of improving production efficiency.

Active Publication Date: 2016-10-12
烟台佳隆纳米产业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Liquid phase precipitation method prepares monodisperse submicron spherical manganese carbonate (inorganic salt industry, the 8th phase of volume 41 in 2009, Su Haifeng) discloses a kind of manganese sulfate as manganese source, ammonium bicarbonate as precipitant, twelve Alkyl sodium sulfate is used as the particle size control agent, and two solutions of manganese sulfate and ammonium bicarbonate are quickly added at the same time. By controlling the appropriate reaction and crystallization conditions, submicron-sized monodisperse spherical manganese carbonate particles are prepared, with an average particle size of about 540nm, the disadvantage of this method is intermittent feeding, which is not conducive to large-scale production, and the product particle size is 540nm, which belongs to the submicron range, and is not strictly a nanomaterial
[0007] (2) The nano-manganese carbonate prepared by several methods described in (2) is rod-shaped, fibrous or spherical, and the agglomeration is hard agglomeration, but the hard agglomeration is difficult to disperse to obtain the primary particle size during use, and the spherical manganese carbonate particle size It is also only sub-micron, with a particle size of more than 500 nanometers, which cannot meet the requirements of nano-manganese carbonate particle size of 1-100nm

Method used

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Experimental program
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Effect test

Embodiment 1

[0022] A method for continuously preparing soft agglomerated nano manganese carbonate, the steps are as follows:

[0023] (1) Preparation concentration is 1L of manganese sulfate solution of 1mol / L, adds 1g cetyltrimethylammonium bromide, obtains the manganese sulfate solution containing 0.1wt% crystal form control agent; Preparation concentration is the carbonic acid of 1mol / L Ammonium hydrogen solution 2L;

[0024] (2) the manganese sulfate solution containing the crystal form control agent and the ammonium bicarbonate solution of step (1) are added in the reactor in the mode of adding, the feed rate of the manganese sulfate solution containing the crystal form control agent is 100L / h, The feed rate of the ammonium bicarbonate solution is 200L / h, stirred evenly at a speed of 200r / min, and the pH is controlled to be 7.0;

[0025] (3) The reaction in step (2) is carried out at a temperature of 25° C. and a pressure of 101 kPa. The reaction discharge is filtered through a memb...

Embodiment 2

[0028] A method for continuously preparing soft agglomerated nano manganese carbonate, the steps are as follows:

[0029] (1) preparation concentration is 1L of manganese sulfate solution of 1.5mol / L, adds 2g ammonium citrate, obtains the manganese sulfate solution containing 0.2wt% crystal form control agent; preparation concentration is 2L of ammonium bicarbonate solution of 1.5mol / L;

[0030] (2) the manganese sulfate solution containing the crystal form control agent and the ammonium bicarbonate solution of step (1) are added in the reactor in the mode of adding, the feed rate of the manganese sulfate solution containing the crystal form control agent is 200L / h, The feed rate of the ammonium bicarbonate solution is 400L / h, stirred evenly at a speed of 250r / min, and the pH is controlled to be 7.5;

[0031] (3) The reaction in step (2) is carried out at a temperature of 25° C. and a pressure of 101 kPa. The reaction discharge is filtered through a membrane and washed 3 times...

Embodiment 3

[0034] A method for continuously preparing soft agglomerated nano manganese carbonate, the steps are as follows:

[0035] (1) preparation concentration is 1L of manganese sulfate solution of 2mol / L, adds 3g formic acid, obtains the manganese sulfate solution containing 0.3wt% crystal form control agent; Preparation concentration is 1L of ammonium carbonate solution of 2mol / L;

[0036] (2) the manganese sulfate solution containing the crystal form control agent and the ammonium carbonate solution of step (1) are added in the reactor in the mode of adding, the feed rate of the manganese sulfate solution containing the crystal form control agent is 150L / h, the carbonic acid The feed rate of the ammonium solution is 150L / h, stirred evenly at a speed of 300r / min, and the pH is controlled to be 8.0;

[0037] (3) The reaction in step (2) is carried out at a temperature of 25° C. and a pressure of 101 kPa. The reaction discharge is filtered through a membrane and washed 3 times with p...

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Abstract

The invention belongs to the technical field of nano materials and particularly relates to a method for continuously preparing soft agglomerated nano magnesium carbonate. Reagent-grade manganese sulfate and a precipitant are used as materials, preventing the reduction in the quality of finished manganese carbonate due to the introduction of impurities to the materials. A continuous feeding mode is used in the synthetic process, so that reaction is continuously carried out and production efficiency is improved. The manganese carbonate prepared herein is less than 30 nm in particle size and is strictly a nano material, the prepared manganese carbonate is spherical and is softly agglomerated, and soft agglomeration is advantageous in that agglomeration easily turns to disagglomeration in use to obtain nanoparticles of primary particle size.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a method for continuously preparing soft agglomerated nanometer manganese carbonate. Background technique [0002] Manganese carbonate is the raw material for the production of electrolytic manganese metal. It can be used to manufacture magnetically permeable materials. It is one of the main components of soft ferrite. It can also be used in desulfurization catalysts, enamel pigments, varnish driers and fertilizer additives. [0003] With the development of new energy technology, the application of manganese carbonate in the field of battery materials is becoming more and more extensive, especially the good development trend of lithium manganate battery and nickel-cobalt-manganese ternary battery, which further enhances the application value of manganese carbonate. While the application value of manganese carbonate increases, the quality requirements for the product a...

Claims

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Application Information

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IPC IPC(8): C01G45/00B82Y40/00
CPCC01G45/00C01P2004/64
Inventor 岳都元欧阳俊施建军
Owner 烟台佳隆纳米产业有限公司
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