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A new process for preparing fully water-soluble titanyl sulfate powder

A titanium oxysulfate powder, titanium oxysulfate technology, applied in the direction of titanium and titanyl sulfate, titanium compounds, inorganic chemistry, etc., can solve the problems affecting product purity, high equipment maintenance cost, high energy consumption, etc., to simplify production Process flow, reducing anti-corrosion sealing requirements, reducing the effect of sulfuric acid usage

Active Publication Date: 2022-06-17
SHANDONG JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this technical solution, it is necessary to add acidifying additives, which will introduce impurities and affect the purity of the product, and the mass ratio of metatitanic acid to the sulfuric acid after dehydration is 1:3-6, the more sulfuric acid added, the The selection of preparation equipment materials, protective facilities and parameter control all have high technical index requirements, and there are technical problems of high energy consumption and high equipment maintenance costs
The titanyl sulfate solution prepared by the traditional titanyl sulfate production process contains a large amount of excess sulfuric acid, so the simple crystallization method obtained by distilling the titanyl sulfate solution is a viscous paste instead of a titanyl sulfate solid; Complicated operations of adding seed crystals, heating crystallization, filtering, and rinsing with organic solvents

Method used

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  • A new process for preparing fully water-soluble titanyl sulfate powder
  • A new process for preparing fully water-soluble titanyl sulfate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A new process for preparing fully water-soluble titanium oxysulfate powder, comprising the following steps:

[0025] (1) Take 1000 g of industrial metatitanic acid solid, dry it at 120 °C for 2 hours, and sieve it with a 100-mesh stainless steel sieve after crushing;

[0026] (2) Mix and granulate the sieved metatitanic acid powder with 98% sulfuric acid and distilled water, and the material ratio of metatitanic acid, sulfuric acid and water is 1:0.5:1;

[0027] (3) Homogenize the material ball at 120 °C for 1 hour, then heat it up to 260 °C for 8 hours, and the conversion rate of this step is about 70.5%;

[0028] (4) Cool and pulverize the calcined material balls, and sieve them with a 100-mesh stainless steel sieve;

[0029] (5) Use 1 times the mass of 0.4% dilute sulfuric acid to dissolve the sieved powder, and continue leaching for 6 hours at a temperature of 50 °C and an ultrasonic frequency of 40 kHz;

[0030] (6) Filter the leached slurry, and the clear and tr...

Embodiment 2

[0034] A new process for preparing fully water-soluble titanium oxysulfate powder, comprising the following steps:

[0035] (1) Take 1000 g of industrial metatitanic acid solid, dry it at 120 °C for 2 hours, and sieve it with a 100-mesh stainless steel sieve after crushing;

[0036] (2) Mix and granulate the sieved metatitanic acid powder with 98% sulfuric acid and distilled water, and the material ratio of metatitanic acid, sulfuric acid and water is 1:1.25:0.2;

[0037] (3) The material balls were homogenized at 120 °C for 1 hour, and then heated to 260 °C and calcined for 8 hours. The conversion rate of this step was 98.7%;

[0038] (4) Cool and pulverize the calcined material balls, and sieve them with a 100-mesh stainless steel sieve;

[0039] (5) Use 0.4% dilute sulfuric acid with twice the mass of the solid material to dissolve the sieved powder, and continue leaching for 6 hours at a temperature of 50 °C and an ultrasonic frequency of 40 kHz;

[0040] (6) Filter the ...

Embodiment 3

[0045] A new process for preparing fully water-soluble titanium oxysulfate powder, comprising the following steps:

[0046] (1) Take 1000 g of industrial metatitanic acid solid, dry it at 120 °C for 2 hours, and sieve it with a 100-mesh stainless steel sieve after crushing;

[0047] (2) Mix and granulate the sieved metatitanic acid powder with 98% sulfuric acid and distilled water, and the material ratio of metatitanic acid, sulfuric acid and water is 1:3:0.2;

[0048] (3) The material balls were homogenized at 120 °C for 1 hour, and then heated to 260 °C and calcined for 8 hours. The conversion rate of this step was 99.5%;

[0049] (4) Cool and pulverize the calcined material balls, and sieve them with a 100-mesh stainless steel sieve;

[0050] (5) Use 0.4% dilute sulfuric acid with twice the mass of the solid material to dissolve the sieved powder, and continue leaching for 6 hours at a temperature of 50 °C and an ultrasonic frequency of 40 kHz;

[0051] (6) Filter the lea...

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Abstract

The invention discloses a new process for preparing fully water-soluble titanyl sulfate powder. The metatitanic acid powder and sulfuric acid are mixed and granulated, and the crude product of titanyl sulfate is obtained through low-temperature calcination, and then leached and dissolved by dilute sulfuric acid, and the solution is filtered. Then the titanyl sulfate solution is vacuum concentrated, heated and dried to obtain high-quality fully water-soluble titanyl sulfate powder. This method adopts a new calcination process in the preparation of crude titanyl sulfate, and replaces the reaction kettle in the acid-dissolving section with a calciner, which reduces the residue of sulfuric acid in the system, so a new crystallization process can be adopted without adding additional titanyl sulfate seeds , filtration operations and the use of organic solvent flushing agents such as ethanol simplify the production process of titanyl sulfate.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to the technical field of titanium oxysulfate preparation, and in particular to a new process for preparing fully water-soluble titanium oxysulfate powder. Background technique [0002] Titanium oxysulfate is white powder, light yellow when carrying a small amount of impurities, deliquescence, soluble in cold water. Titanium oxysulfate industrial products are generally double salts or mixtures of titanyl sulfate-sulfuric acid-water. Due to differences in production processes, acid content and water content, its molecular formula can be considered as TiOSO 4 ·xH 2 SO 4 ·yH 2 O. Titanium oxysulfate is used in industries such as fibers in industrial textiles, mordants for fabrics, chromium-free passivation processes for industrial electroplating, and industrial catalysts, especially as a source or raw material for titanium fertilizers for agricultural crops. Chlorophyll...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00
CPCC01G23/008
Inventor 朱丽丽李硕董庆凯
Owner SHANDONG JIAOTONG UNIV
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