阅读说明：本技术 一种金属锰制电池级硫酸锰的方法 (Method for preparing battery-grade manganese sulfate from manganese metal ) 是由 陈军 訚硕 邓伟明 于 2019-04-16 设计创作，主要内容包括：本发明公开了一种金属锰制电池级硫酸锰的方法,具体包括以下步骤：步骤一、原料准备；步骤二、预热处理；步骤三、三效蒸发；步骤四、结晶；步骤五、离心干燥和步骤六：冷凝液处理,该金属锰制电池级硫酸锰的方法,保证了随着我国电子化学品(如电解锰、化学二氧化锰、四氧化三锰等一系列高品质、高纯度电子化学品)的迅猛发展,这些电子化学品对硫酸锰更好的使用,越来越受到人们的重视,达到了人们对硫酸锰的质量和数量提出的更高要求,同时,也较大程度的解决了目前硫酸锰的纯度较低的情况,改变了传统对金属锰加工制造的工艺方法,极大的提高了生产的效率和效果,更好的满足了市面上对硫酸锰的需求。(The invention discloses a method for preparing battery-grade manganese sulfate from manganese metal, which specifically comprises the following steps: step one, preparing raw materials; step two, preheating treatment; step three, triple effect evaporation; step four, crystallization; step five, centrifugal drying and step six: the condensate is treated, and the method for preparing the battery-grade manganese sulfate from the metal manganese ensures that along with the rapid development of electronic chemicals (such as electrolytic manganese, chemical manganese dioxide, manganous oxide and other series of high-quality and high-purity electronic chemicals) in China, the electronic chemicals better use the manganese sulfate and are more and more valued by people, so that the higher requirements of people on the quality and the quantity of the manganese sulfate are met, meanwhile, the condition that the purity of the existing manganese sulfate is lower is solved to a greater extent, the traditional process method for processing and manufacturing the metal manganese is changed, the production efficiency and effect are greatly improved, and the requirement on the manganese sulfate on the market is better met.)

1. A method for preparing battery-grade manganese sulfate from metal manganese is characterized by comprising the following steps:

step one, raw material preparation: the worker purchases the manganese metal according to the requirement, and stores the purchased manganese metal in a warehouse for later use;

step two, preheating treatment: conveying the manganese metal purchased in the step one into a preheater through a raw material pump by a flowmeter, and carrying out preheating treatment;

step three, triple effect evaporation: sequentially evaporating the preheated manganese metal through a triple-effect evaporator to reach the concentration meeting the requirement;

step four, crystallization: after reaching a certain concentration in the third step, the manganese sulfate solution enters a crystallizer through a discharge pump, and crystallization is completed in a high-temperature crystallizer;

step five, centrifugal drying: after the crystallization of manganese sulfate in the crystallizer is finished, separating manganese sulfate crystals in a centrifugal machine, returning the separated solution to an evaporator for continuous evaporation and concentration, and packaging the manganese sulfate crystals by a packaging unit after the manganese sulfate crystals reach the water content requirement through drying equipment to obtain each finished product of manganese sulfate;

step six: condensate treatment: the evaporated water and steam pass through the preheater and the condenser and then enter the liquid seal tank, and are discharged by the water pump.

2. The method for preparing battery-grade manganese sulfate from manganese metal according to claim 1, wherein the method comprises the following steps: the materials of the equipment used in the method are all 316L stainless steel materials.

3. The method for preparing battery-grade manganese sulfate from manganese metal according to claim 1, wherein the method comprises the following steps: in the third step, the manganese sulfate solution passes through the preheater and then enters the first-effect heater to be evaporated in the first-effect evaporator, the evaporated secondary steam is supplied to the second-effect heater, due to the vacuum effect, the solution evaporated by the first-effect evaporator enters the second-effect heater to be reheated and enters the second-effect evaporator to be evaporated, in the second-effect evaporation process, partial crystals are considered to be separated out, therefore, a forced circulation pump is additionally arranged at the lower part of the second-effect evaporator, the crystallized material is prevented from being adhered to the inner wall of the heating pipe, the solution reaching a certain concentration enters the third-effect evaporator to be evaporated again, and the third-effect evaporator is also additionally provided with a circulation pump for the same reason.

4. The method for preparing battery-grade manganese sulfate from manganese metal according to claim 1, wherein the method comprises the following steps: in the third step, the technological parameters of the triple-effect evaporator are as follows: the steam pressure of the first-effect heater is 0.4Mpa, the evaporating temperatures of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively 100-110 ℃, 85-95 ℃ and 65-75 ℃, and the vacuum degrees of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively-0.02-0 Mpa, -0.05-0.06 Mpa and-0.08-0.09 Mpa.

Technical Field

The invention relates to the technical field of preparation of battery-grade manganese sulfate, in particular to a method for preparing battery-grade manganese sulfate from manganese metal.

Background

Manganese sulfate is reddish orthorhombic crystal, has relative density of 3.50 and melting point of 700 ℃, is easily soluble in water and insoluble in ethanol. It exists in the form of various hydrates. Manganese sulfate begins to decompose at 850 ℃, and due to different heating degrees, SO3, SO2 or oxygen can be released, and manganese dioxide or manganomanganic oxide is remained. When the crystalline hydrate of manganese sulfate is heated to 280 ℃, the crystalline water of the manganese sulfate is lost and the manganese sulfate becomes anhydrous. Manganese sulfate is a trace element needed by crops for synthesizing fatty acid, so that the manganese sulfate can be applied to soil as a fertilizer, and the yield can be increased. Manganese sulfate is added into animal feed, and has fattening effect. Manganese sulfate is also a raw material and analytical reagent for preparing other manganese salts. Manganese sulfate is also used in the industrial production of electrolytic manganese, dye, paper making, ceramics and the like.

Manganese sulfate is an important microelement fertilizer, can make crops grow well, is also an important feed additive, and can make livestock and poultry develop well by supplementing it into feed, and has the effect of increasing weight. In addition, manganese sulfate is widely used in medicine, paint driers, paper making, ceramics, printing and dyeing, production of electrolytic manganese, manufacture of other manganese salts, and the like. In recent years, along with the rapid development of electronic chemicals (such as electrolytic manganese, chemical manganese dioxide, trimanganese tetroxide and other series of high-quality and high-purity electronic chemicals) in China, manganese sulfate is increasingly regarded as a main raw material for producing the electronic chemicals. But at the same time, people also put higher requirements on the quality and quantity of manganese sulfate, and particularly, the requirements on high-purity manganese sulfate are quite strict, and the content of heavy metal impurities in the manganese sulfate reaches trace levels. The traditional method is difficult to meet the requirements, the production efficiency and the effect are relatively low, and the requirement of the market on manganese sulfate cannot be met.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a method for preparing battery-grade manganese sulfate from manganese metal, which solves the problems that the traditional method is difficult to meet the requirements, the production efficiency and the effect are relatively low, and the requirements on manganese sulfate in the market cannot be met.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: a method for preparing battery-grade manganese sulfate from metal manganese specifically comprises the following steps:

step one, raw material preparation: the worker purchases the manganese metal according to the requirement, and stores the purchased manganese metal in a warehouse for later use;

step two, preheating treatment: conveying the manganese metal purchased in the step one into a preheater through a raw material pump by a flowmeter, and carrying out preheating treatment;

step three, triple effect evaporation: sequentially evaporating the preheated manganese metal through a triple-effect evaporator to reach the concentration meeting the requirement;

step four, crystallization: after reaching a certain concentration in the third step, the manganese sulfate solution enters a crystallizer through a discharge pump, and crystallization is completed in a high-temperature crystallizer;

step five, centrifugal drying: after the crystallization of manganese sulfate in the crystallizer is finished, separating manganese sulfate crystals in a centrifugal machine, returning the separated solution to an evaporator for continuous evaporation and concentration, and packaging the manganese sulfate crystals by a packaging unit after the manganese sulfate crystals reach the water content requirement through drying equipment to obtain each finished product of manganese sulfate;

step six: condensate treatment: the evaporated water and steam pass through the preheater and the condenser and then enter the liquid seal tank, and are discharged by the water pump.

Preferably, the materials of the equipment used in the method are 316L stainless steel materials.

Preferably, in the third step, the manganese sulfate solution passes through the preheater and then enters the first-effect heater to be evaporated in the first-effect evaporator, the evaporated secondary steam is supplied to the second-effect heater, the solution evaporated by the first-effect evaporator enters the second-effect heater to be reheated and then enters the second-effect evaporator to be evaporated under the action of vacuum, and in the process of second-effect evaporation, partial crystal precipitation is considered, so that a forced circulation pump is additionally arranged at the lower part of the second-effect evaporator to prevent the crystallized material from being adhered to the inner wall of the heating pipe, the solution reaching a certain concentration enters the third-effect evaporator to be evaporated again, and the third-effect evaporator is additionally provided with a circulation pump for the same reason.

Preferably, in the third step, the process parameters of the triple-effect evaporator are as follows: the steam pressure of the first-effect heater is 0.4Mpa, the evaporating temperatures of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively 100-110 ℃, 85-95 ℃ and 65-75 ℃, and the vacuum degrees of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively-0.02-0 Mpa, -0.05-0.06 Mpa and-0.08-0.09 Mpa.

(III) advantageous effects

The invention provides a method for preparing battery-grade manganese sulfate from manganese metal. The method has the following beneficial effects: the method for preparing battery-grade manganese sulfate from metal manganese comprises the following steps of firstly, preparing raw materials; step two, preheating treatment; step three, triple effect evaporation; step four, crystallization; step five, centrifugal drying and step six: the condensate liquid treatment ensures that along with the rapid development of electronic chemicals (such as electrolytic manganese, chemical manganese dioxide, trimanganese tetroxide and other series of high-quality and high-purity electronic chemicals) in China, the electronic chemicals are better used for manganese sulfate and are more and more emphasized by people, higher requirements of people on the quality and the quantity of the manganese sulfate are met, meanwhile, the condition that the purity of the existing manganese sulfate is lower is solved to a greater extent, the traditional process method for processing and manufacturing the metal manganese is changed, the production efficiency and effect are greatly improved, and the requirement of the manganese sulfate on the market is better met.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Based on the technical problems existing in the background technology, the invention provides a technical scheme that: a method for preparing battery-grade manganese sulfate from metal manganese specifically comprises the following steps:

step one, raw material preparation: the worker purchases the manganese metal according to the requirement, and stores the purchased manganese metal in a warehouse for later use;

step two, preheating treatment: conveying the manganese metal purchased in the step one into a preheater through a raw material pump by a flowmeter, and carrying out preheating treatment;

step three, triple effect evaporation: sequentially evaporating the preheated manganese metal through a triple-effect evaporator to reach the concentration meeting the requirement;

step four, crystallization: after reaching a certain concentration in the third step, the manganese sulfate solution enters a crystallizer through a discharge pump, and crystallization is completed in a high-temperature crystallizer;

step five, centrifugal drying: after the crystallization of manganese sulfate in the crystallizer is finished, separating manganese sulfate crystals in a centrifugal machine, returning the separated solution to an evaporator for continuous evaporation and concentration, and packaging the manganese sulfate crystals by a packaging unit after the manganese sulfate crystals reach the water content requirement through drying equipment to obtain each finished product of manganese sulfate;

step six: condensate treatment: the evaporated water and steam pass through the preheater and the condenser and then enter the liquid seal tank, and are discharged by the water pump.

In the invention, the materials of the equipment used in the method are all 316L stainless steel materials.

In the third step, manganese sulfate solution passes through the preheater and then enters the first-effect heater to be evaporated in the first-effect evaporator, evaporated secondary steam is used by the second-effect heater, the solution evaporated by the first-effect evaporator enters the second-effect heater to be reheated and then enters the second-effect evaporator to be evaporated under the action of vacuum, and in the process of the second-effect evaporation, partial crystal precipitation is considered, so that a forced circulation pump is additionally arranged at the lower part of the second-effect evaporator to prevent crystallized materials from being adhered to the inner wall of a heating pipe, the solution reaching a certain concentration enters the third-effect evaporator to be evaporated again, and the third-effect evaporator is also additionally provided with a circulation pump due to the same reason.

In the third step, the technological parameters of the triple-effect evaporator are as follows: the steam pressure of the first-effect heater is 0.4Mpa, the evaporating temperatures of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively 100-110 ℃, 85-95 ℃ and 65-75 ℃, and the vacuum degrees of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively-0.02-0 Mpa, -0.05-0.06 Mpa and-0.08-0.09 Mpa.

Description of the apparatus

(1) And an evaporator: the evaporator is made of 316L stainless steel carbon steel material and is provided with a manhole, a sight hole, a thermometer, a vacuum gauge and other devices.

(2) And a preheater: the preheater is shell and tube preheater, and the heating pipe specification is phi 38, and the tube side and the tube sheet material of preheater adopt to choose for use 316L stainless steel, the shell side material of preheater: 316L stainless steel material;

(3) and a feeding pump: a pump made of 316L stainless steel is used as a feeding pump.

(4) Circulating pump, discharge pump: the circulating pump and the discharging pump are required to be well sealed and temperature resistant, and can ensure that high-concentration materials or crystallized materials can be discharged continuously to work in a negative pressure state, and the material is 316L stainless steel material.

(5) And a condenser: the condenser is a shell-and-tube condenser, the specification of a condenser tube is phi 38, and the materials of a condenser tube pass and a tube plate adopt 316L stainless steel and shell pass materials: carbon steel material.

(6) And liquid seal tank: 316L stainless steel material is adopted, and the volume is 2000L.

(7) And a vacuum unit: the adopted water ring vacuum pump.

(8) And process accessories: the process pipeline is made of materials such as 316L and the like.

(9) And an instrument: all pressure, temperature and vacuum are detected by sensors, and the number is displayed in a centralized way.

(10) And a high-temperature crystallizer is adopted, and the material is 316L stainless steel material.

Complete set of instructions

The feed inlet, the power supply and the circulating water are connected to corresponding parts of corresponding equipment, the feed inlet is DN65, the circulating water inlet is DN200, the capacitance is matched according to 150KW, and the feed pump, the discharge pump, the circulating pump, the water pump and the like are controlled on site and the temperature, the pressure and the vacuum degree operation chambers are controlled in a centralized way.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.