Manganese dioxide obtaining method

FIELD: metallurgy.

SUBSTANCE: manganese dioxide obtaining method involves dilution of manganese-containing raw material in nitric acid so that solution of manganese nitrates and nitrates of calcium, potassium, magnesium and sodium impurities contained in the ore is obtained. Then, thermal decomposition of nitrates in autoclave is performed. Thermal decomposition is performed at constant pressure drop in autoclave, starting from pressure of 0.6 MPa and reducing it to the end of the process to 0.15 MPa. At that, pulp is constantly mixed at thermal decomposition with the mixer rotating at speed of 1-15 rpm and with superimposition of vibration on it with frequency of 20-50 Hz. Method can be implemented at chemical plants provided with pressure autoclaves.

EFFECT: obtaining manganese dioxide of improved quality.

2 tbl, 2 ex

 

The invention relates to metallurgy and, more specifically, to obtain high quality manganese dioxide, which may find wide application in chemical and metallurgical industries, in particular in the manufacture of electrolytic and electrothermal manganese, medium carbon ferromanganese, low-phosphorus alloys based on it.

From the technical literature there are several ways of obtaining pure manganese dioxide: chemical, hydrometallurgical, pyrohydrolysis and pyro.

The main requirements that apply to chemical methods of obtaining manganese dioxide are:

the efficiency of phosphorus removal and waste rock;

the simplicity of instrumentation;

- high performance;

- the availability and low cost of the reagents.

A method of obtaining pure manganese dioxide sulfuric acid method. The essence of the method consists in the following: through prepared from the ore and solution dithionite calcium suspension (T:W=1:4) is skipped sulfur dioxide containing sulfur (SO2) and sulfur (SO3) anhydrides. The dissolution of these gases in water leads to the formation of sulphurous and sulphuric acids. In sulphurous acid intensively dissolved manganese oxides with the formation of the manganese salt dition is based acid and manganese sulfate according to the reaction: MnO 2+2SO2=MnS2O6; MnO2+SO2=MnSO4.

In the presence of excess dithionite calcium is the precipitation of calcium sulfate and education dithionate manganese: MnSO4+CaS2O6=MnS2O6+CaSO4

Leached pulp is neutralized with lime milk to a pH of 4-5, then it aeronauts for oxidation of ferrous iron and the removal of sulfur dioxide. In the sediment fall: trivalent iron, phosphorus, aluminum, silica. The precipitate is filtered off, washed with hot water and sent to the dump. From the purified solution by adding quicklime precipitated manganese in the form of hydroxide, thus again ditional calcium, which in return process: MnS2O6+CA(Oh)2=MP(OH)2+CaS2O6.

The precipitate of manganese hydroxide is filtered off, washed, dried and calcined. Calcined concentrate contains, %: 92 - MnO2, 1,5 - SiO2, 4,0 - CaO, 0.02 And P2O5and 0.5-3 - SO2(Migosi. Metallurgy manganese. Kyiv: Tekhnika, 1979, p.55-56).

The disadvantages of the known method of producing manganese dioxide are:

- the complexity of the hardware design;

- the product is contaminated by the waste rock (SiO2, CaO and others);

- high concentration of sulfur in the final product (from 0.5 to 3%).

Closest to the proposed to the technical essence and achieved is the reception the effect is a method of producing manganese dioxide by thermal decomposition of manganese nitrate in the presence of nitrates of calcium, magnesium, potassium and sodium, according to which the decomposition is carried out at a pressure of 0.15 to 1.0 MPa (Copyright certificate №1102819, CL C22B 47/00; C01G 45/02, priority from 20.05.83, publ. 15.07.84, bull. No. 26).

According to the method prototype obtaining manganese dioxide in the presence of nitrates of calcium, magnesium, potassium and sodium, the decomposition is carried out at a pressure of 0.15 to 1.0 MPa.

Process parameters and properties of the prototype method:

- decomposition temperature, °C 170-190;

the rate of formation of manganese dioxide, kg/m3h - 500-700;

the degree of decomposition of Mn(NO3)2the % of the original quantity - 78-87;

- conditions of discharge slurry from the reactor by gravity;

the moisture content in the oxides of nitrogen, % - 19-25;

- energy consumption, MJ/kg - 1,7-2,2;

- the content of MnO2in the manganese dioxide, % - 99,5.

The disadvantages of this method are the low rate of decomposition of manganese nitrate, large energy consumption, high amount of water in the resulting oxides of nitrogen.

The present invention is to simplify the technology of production of manganese dioxide, increasing the degradation rate and product yield.

This object is achieved in that the process of thermal decomposition is carried out at a gradual decrease of the pressure in the autoclave, from the pressure of 0.6 MPa and reducing it to the end of the process to 0.15 MPa, while the pulp is continuously processed is t stirrer, rotating with a speed of about 1-15/min; in the process of thermal decomposition on a rotating mixer impose a vibration with a frequency of 20-50 Hz.

The upper pressure value for thermal decomposition of nitrates is determined by the processing conditions of nitrogen oxides in the acid (it is carried out at a pressure not exceeding 0.6 MPa), and the lower limit of practical expediency. Gradual reduction of pressure to 0.15 MPa provides a more complete thermal decomposition of nitrates of manganese.

Reducing the speed of rotation of the agitator below 1 rpm does not provide a homogeneous solution is obtained. The increase in speed above 15 rpm leads to stratification of the slurry and the emergence of areas with a higher concentration of water (due to the difference in densities).

Lower vibration frequency is below 20 Hz, imposed on the mixer, have virtually no effect on the performance of thermal decomposition of manganese nitrate. The increase in the vibration frequency above 50 Hz is not economically justified.

When these conditions increases not only the rate of decomposition of manganese nitrate, but the process as a whole becomes more technological. It is established that in the proposed process the output of the pulp is not strongly dependent on its physical properties, which greatly simplifies the process of unloading from the reactor, the nitrogen oxides content is t a lower concentration of water and can be easily recycled back into the acid. Table 1 presents comparative data of process parameters for obtaining manganese dioxide on known and proposed methods. Indicators (average) on the proposed method of obtaining manganese dioxide are presented in table 1, taken on the basis of the results of experiments (example 1).

Table 1
Process parameters and propertiesMethod
KnownOffer
Decomposition temperature, °C170-190170-190
Pressure, MPa0,15-1,0A gradual reduction in pressure from 0.6 to 0.15
The rate of formation of manganese dioxide, kg/m3h500-700750-865
The time required for the formation of 200 kg of manganese dioxide, h0,30,25
The degree of decomposition of Mn(NO3)2in % of the original quantity 78-8790-92*
Conditions of discharge of the pulp from the digesterGravityGravity
The moisture content in the oxides of nitrogen, wt.%19-25Less than 10
Energy consumption, MJ/kg MnO21.7 to 2.21,3-1,5
The content of MnO2product99,599,6
The rotation speed of the stirrer, vol./minutes-8*

when thermal decomposition on a rotating mixer superimposed vibration frequency of 30 Hz is the degree of decomposition of Mn(NO3)2increases by 2-3,5%.

Physico-chemical properties of the powder:

- density of 5.10 g/cm3;

- the content of MnO2- a 99.6 wt.%;

the Fe content is less than 3×10-4wt.%,

- the content of P is not more than 5×10-3wt.%;

- N2O - not more than 3×10-2wt.%.

Below are examples, not excluding others, in the scope of the claims.

Example 1

In the autoclave was loaded with 1.5 kg of a solution of the nitrates of the following composition, wt.%: 40,15 Mn(NO3)2; 25,7 Ca(NO3)2 ; 7,3 Mg(NO3)2; 9,2 KNO3; 5,7 NaNO3; 15,0 H2O.

The weight is dropped by thermal decomposition of water was determined by the difference between its weight in the initial solution and in the liquid phase of the pulp. The amount of released nitrogen oxides were determined by the stoichiometry of the reaction of thermal decomposition of manganese nitrate in accordance with the received amount of MnO2. The main results of the experiments are presented in table 2.

Table 2
OptionsExamples of specific performance
The known methodThe proposed method
1234
Decomposition temperature,°C180-190180-190180-190180-190180-190
Pressure, MPa*1,0to 0.6-0.15to 0.6-0.15to 0.6-0.15to 0.6-0.15
The rotation speed of the stirrer, rpm-1815-
Vibration frequency, Hz--205010
Time decay, min1511,5108,015
The rate of formation of MnO2kg/m3h700750810865650
The content of water vapor in the oxides of nitrogen, wt.%10-25,68,5-9,0the 8.6 and 7.16,5-7,016
The amount of released gases, m31 kg MnO21,20,80,60,41,0
The yield of dry dioxide Marg the NCA, %7884889280
- the upper limit pressure for thermal decomposition of nitrates is determined by the processing conditions of nitrogen oxides in acid

The obtained manganese dioxide of the following composition, wt.%: MnO2- 99,6; P<0,005; S<0,05; SiO2<0,1; (K, Mg, Na, Ca)<0,1.

Thus, the proposed method provides not only a more rapid decomposition of manganese nitrate, but also greatly simplifies the production technology MnO2as at the unloading stage and at the stage of regeneration of nitrogen oxides; this significantly reduces the costs of redistribution. The output of dry manganese dioxide is 84-92% versus 78% (by known means) from theoretically possible.

Example 2

The obtained manganese dioxide used for smelting metal manganese secondary process.

The mixture had a composition, kg:

- MnO2- 10;

- Al - 4,9;

- CaO - 0,6.

Only 15.5 kg

The mixture was mixed, loaded into a melting mine and using the fuse burned. The melting duration was 2.4 minutes Received 5.25 kg manganese metal composition. % MP 98,9; Al To 0.96; P - traces (less than 0,005%) and 9.3 kg of slag composition, wt.%: IGOs 14,6; Al2About368,3; Cao and 1.0.

Extraction of manganese in the alloy amounted to 85.0 per cent.

The slag from the smelting of manganese metal can be used as raw materials (instead of bauxite) upon receipt of aluminum.

The application of the present invention will solve the problem of using large stockpiles of poor manganese ore, in particular carbonate ores Usinsk Deposit or ferromanganese nodules, enrichment which all other methods currently unprofitable.

The obtained manganese alloys have a high concentration of a driving element (manganese) and low content of harmful impurities (phosphorus and carbon).

The use of manganese ferroalloys in the smelting of high quality steels leads to the decrease of metal structures, simplifies the process of alloying and provides a significant economic effect.

Production of manganese concentrate chemical methods will significantly reduce the deficit in the country in manganese ferroalloys, and its production can be organized in chemical plants.

The proposed method of producing manganese dioxide can be arranged at the enterprises with the opportunity to dispose of the oxides of nitrogen.

A method of producing manganese dioxide by thermal decomposition, including the dissolution of mn containing raw materials in nitric key is the item with the receipt of a solution of nitrates of manganese and nitrates, present in the ore impurities of calcium, potassium, magnesium, sodium, and subsequent thermal decomposition of the nitrates in the autoclave, wherein thermal decomposition is carried out at constant pressure drop in the autoclave, from the pressure of 0.6 MPa and reducing it to the end of the process to 0.15 MPa, while the pulp is continuously treated with a stirrer rotating at a speed of about 1-15/min and overlaid with vibration with a frequency of 20-50 Hz.



 

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