A kind of preparation method of high-purity fecl2·4h2o

A fecl2·4h2o, high-purity technology, applied in iron halide and other directions, can solve the problems of polluting tap water, complicated treatment methods, and complicated treatment processes, and achieves the effect of improving the scope of industrial applications, increasing economic benefits, and low equipment investment.

Active Publication Date: 2019-05-07
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

[0003] In the prior art, there is a resource recovery method for hot-dip galvanizing acidic waste liquid, which mainly uses the diffusion dialysis method to treat the hot-dip galvanizing waste liquid, and obtains the waste water containing HCl and a small amount of Zn respectively. 2+ and the recovery liquid of its complexes and containing Fe 2+ , Zn 2+ Residual liquid, the method equipment requirements are high, the treatment process is complicated, and a large amount of waste liquid is still by-produced; and FeCl 2 4H 2 O is the preparation of FeCl 3 The main raw material, FeCl 3 Widely used in the tap water industry, residues in FeCl 2 4H 2 O Zn 2+ Belongs to heavy metal ions, will pollute tap water
In addition, the treatment method of galvanizing waste acid is to prepare superparamagnetic ferroferric oxide nanoparticles by co-precipitation method, using superparamagnetic ferroferric oxide as the core, and coating the surface of ferroferric oxide by hydrolysis One or more layers of silica shell, using the principle of coupling reaction, to modify the core coated with silica, using 3-aminopropyltrimethoxysilane as the modifying agent, on the core-shell structure Carry out modification to connect amino groups, and then use it to adsorb zinc in waste galvanizing acid, which contains Zn in waste galvanizing acid 2+ , Fe 2+ and hydrochloric acid, selective adsorption of Zn at room temperature 2+ ions to separate zinc, but there are also problems such as complex processing methods

Method used

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  • A kind of preparation method of high-purity fecl2·4h2o

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preparation example Construction

[0020] Such as figure 1 High-purity FeCl shown 2 4H 2 The preparation method of O, with hot-dip galvanizing waste acid as raw material, comprises the following operations:

[0021] 1) Filter the waste hot-dip galvanizing acid to remove suspended matter and solid floating matter;

[0022] 2) Add a reducing agent to the spent acid after step (1) to make Fe 3+ Convert to Fe 2+ ;

[0023] 3) Vacuum distillation of the reduced waste acid to obtain FeCl 2 4H 2 O crystallization and FeCl 2 Mother liquor;

[0024] 4) FeCl obtained in step (3) 2 4H 2 O crystallization and FeCl 2 The first grade FeCl is obtained after the mother liquor is filtered 2 4H 2 O crystallization and mother liquor, and then the mother liquor is thoroughly distilled to obtain secondary FeCl 2 4H 2 O product, the secondary FeCl 2 4H 2 O product as a by-product; the secondary FeCl 2 4H 2 O products can be directly used for sewage and wastewater treatment;

[0025] 5) The primary FeCl 2 4H 2 O...

Embodiment 1

[0038] The chemical analysis of the waste acid of the sample hot-dip galvanizing is as follows: FeCl 2 : 40%, FeCl 3 : 5%, HCl: 0.4%, impurity: 0.3%, and the balance is water.

[0039] Experimental steps:

[0040] (1) Filter the waste acid with a plate and frame filter to remove suspended solids, solid floating solids, etc.

[0041] (2) Add a certain amount of reducing agent (the reducing agent is iron slag) to the waste acid filtered by the plate and frame filter to make Fe 3+ Convert to Fe 2+ . The weight ratio of reducing agent to waste acid is 1:40.

[0042] (3) Low-temperature vacuum distillation of the obtained waste acid to obtain FeCl 2 solution. The distillation temperature is 95°C, the vacuum degree is 500Pa, and the distillation time is 90min. The water in the spent acid evaporates 84% ​​of the total water to obtain FeCl 2 4H 2 O crystallization and FeCl 2 mother liquor. Get FeCl 2 The content is 98.396%.

[0043] (4) FeCl 2 4H 2 O crystallization an...

Embodiment 2

[0049] The chemical analysis of the waste acid of the sample hot-dip galvanizing is as follows: FeCl 2 : 8%, FeCl 3 : 0.1%, HCl: 0.2%, impurity: 0.3%, and the balance is water.

[0050] Experimental steps:

[0051] (1) Filter the waste acid to remove suspended matter, solid floating matter, etc.

[0052] (2) Add a certain amount of reducing agent (the reducing agent is iron powder) to the waste acid filtered by the plate and frame filter to make Fe 3+ Convert to Fe 2+ . The weight ratio of reducing agent to waste acid is 1:100.

[0053] (3) Put the obtained waste acid into a vacuum distillation furnace and perform low-temperature vacuum evaporation to obtain FeCl 2 solution. The temperature in the vacuum furnace is 60° C., the vacuum degree is 10 Pa, and the evaporation time is 30 minutes. The water in the waste acid evaporates 40% of the total water to obtain FeCl 2 4H 2 O crystallization and FeCl 2 mother liquor. Get FeCl 2 The content is 98.558%.

[0054] (4) ...

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Abstract

The invention discloses a preparation method of high-purity FeCl2.4H2O. The preparation method comprises the following processes for preparing the high-purity FeCl2.4H2O: by taking hot galvanizing waste acid as a raw material, filtering, reducing, performing vacuum distillation, recycling mother liquor, and the like. According to the embodiment of the invention, the problem of influence of Zn<2+> on the FeCl2.4H2O purity and FeCl2 use scope can be solved, the comprehensive utilization rate of FeCl2 is increased and the problems of high cost, single product and secondary pollution of extraction of high purity FeCl2.4H2O from waste acid can be solved. The invention provides a new method for recycling hot galvanizing waste acid. The waste acid is subjected to simple and low-consumption process, so that the purpose of increasing the additional value of products is achieved, the environment pressure is effectively reduced and the economic benefit of the enterprise is increased.

Description

technical field [0001] The invention belongs to the technical field of high-purity material preparation, in particular to a high-purity FeCl 2 4H 2 O preparation method. Background technique [0002] Hot-dip galvanizing is the most widely used steel surface treatment method with the best cost performance in the world today. Hot-dip galvanized products play an irreplaceable role in corrosion reduction and life extension of steel, energy saving and material saving. At the same time, coated steel is also a high value-added short-term product supported and prioritized by the state. However, a large amount of waste acid produced in the hot-dip galvanizing process is difficult deal with. If these waste acids are discharged directly, it will not only cause serious environmental pollution, but also reduce the economic benefits of enterprises. In order to realize the resource treatment of waste acid, protect the environment, save and rationally utilize resources, domestic and for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/10
CPCC01G49/10C01P2006/80
Inventor 李世伟李浩宇张利波彭金辉尹少华夏洪应周俊文郭胜惠胡途杨黎王仕兴
Owner KUNMING UNIV OF SCI & TECH
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