A kind of direct production method of sulfate monohydrate

A production method and sulfate technology, which is applied in the production of sulfate preparations and bulk chemicals, can solve the problems of low product pH, high operating cost, and long production cycle, and achieve satisfactory product pH, low follow-up operating costs, and The effect of simple equipment

Active Publication Date: 2019-07-23
GUANGDONG JIANA ENERGY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Two-step method, that is, first prepare polyhydrate sulfate by evaporation concentration-cooling crystallization, and then perform high temperature treatment on polyhydrate sulfate to remove crystal water. This method has the following disadvantages: (1) The process is complicated, the production cycle is long, and the production efficiency (2) The process of removing crystal water at high temperature requires high energy consumption and high cost
One-step method, that is, direct production of sulfate monohydrate through evaporation and crystallization under high pressure and high temperature conditions. This method needs to be carried out in a high-pressure environment in an autoclave, and the equipment investment is large and the operating cost is high.
[0004] Patent CN104291367A discloses the dehydration of magnesium sulfate monohydrate by acid analysis method. This method is simple and feasible, but because high-concentration acid solution is used as forced dehydrating agent, the requirements for equipment are too high, so it is not suitable for industrial production, and it is worth explaining Yes, the entrained sulfuric acid in the product produced by this method leads to a low pH of the product, which cannot meet the market demand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Will Co 2+ The 130g / L cobalt sulfate solution is pumped into the evaporating kettle, the stirring is started, the heater is heated, and then ethylene glycol is pumped in as a water-soluble organic solvent; when the volume of ethylene glycol added is 10% of the volume of the cobalt sulfate mother liquor, stop adding ethylene glycol. Monitor the temperature in the feed liquid at any time, keep heating and boiling to evaporate and concentrate. When the slurry in the evaporating kettle has a constant boiling point, use a centrifuge to separate the solid and liquid while it is hot; the obtained solid is the cobalt sulfate monohydrate product, and the obtained mother liquor is directly returned to the evaporation The concentration process acts as a water-soluble organic solvent. The crystallization rate of this evaporative concentration is 99.0%, and the ethylene glycol content in the mother liquor is 95.0% (v / v) and returned to the evaporator.

Embodiment 2

[0026] 1000mlNi 2+ Pour 80g / L nickel sulfate solution into a beaker, start stirring and heating, then add 1000mL glycerol (glycerin) as a water-soluble organic solvent. Keep heating and boiling to evaporate and concentrate, monitor the density in the feed liquid at any time, and carry out suction filtration while the feed liquid is hot when the density of the feed liquid reaches 1.3g / ml. The obtained filter cake is nickel sulfate monohydrate product. The crystallization rate of this evaporation concentration was 95.0%. The glycerol content in the mother liquor is 90.0% (v / v) and returned to the evaporator.

Embodiment 3

[0028] 1000mlMg 2+ Pour 20g / L magnesium sulfate solution into a beaker, start stirring and heating, then add 550mL propionic acid as a water-soluble organic solvent. Keep heating and boiling to evaporate and concentrate, monitor the density in the feed liquid at any time, and carry out suction filtration while the feed liquid is hot when the density of the feed liquid reaches 1.45g / ml. The obtained filter cake is the magnesium sulfate monohydrate product. The crystallization rate of this evaporation concentration was 90.0%. The content of propionic acid in the mother liquor is 92.0% (v / v) and returned to the evaporator.

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Abstract

The invention discloses a direct production method of sulfate monohydrate. The method is characterized by comprising the following steps: (1) adding a water soluble organic solvent into an evaporation kettle filled with a sulfate solution and uniformly stirring and mixing the mixture; (2) stopping adding the organic solvent, heating the evaporating kettle, and performing solid-liquid separation while being still hot after being evaporated and concentrated to the slurry terminal point density of 1.2-1.6g / ml; and (3) obtaining the solid after solid-liquid separation, that is a sulfate monohydrate product, and returning mother liquor to the evaporating kettle. The crystallizing rate is 98% above, the sulfate monohydrate product can be produced directly by a one-step method, the mother liquor can be recycled, the production process is short, and the method is simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of preparation of metal sulfate compounds, in particular to a method for directly producing sulfate monohydrate through evaporation and concentration in a water-soluble organic solvent environment. [0002] technical background [0003] Compared with sulfate monohydrate, sulfate polyhydrate has sulfur content, lower metal content, lower price, and limited market. The production of sulfate monohydrate can further increase the added value of sulfate products. It has become an important research topic to prepare high value-added monohydrate sulfate by using the existing polyhydrate sulfate. The monohydrate sulfate in the current industrial production usually adopts two-step method and one-step method. Two-step method, that is, first prepare polyhydrate sulfate by evaporation concentration-cooling crystallization, and then perform high temperature treatment on polyhydrate sulfate to remove crystal water. This method has th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/96
CPCC01B17/96Y02P20/54
Inventor 李文津付海阔吴理觉陈耀柴志华
Owner GUANGDONG JIANA ENERGY TECH CO LTD
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