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Preparation method of zirconium acetate solution with low free acetic acid

A zirconium acetate, low-free technology, applied in carboxylate preparation, organic chemistry, etc., can solve the problems of unrecovered acetic acid, large amount of acetic acid used, and strong odor of acetic acid, so as to shorten the production cycle, save consumption, and reduce the environment the effect of the influence

Inactive Publication Date: 2019-06-28
QUANNAN JINGXIN ENVIRONMENTAL PROTECTION MATERIALCO LTD
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Problems solved by technology

At present, zirconium acetate products on the market have a strong smell of acetic acid. The main reason for this is that there is more free acetic acid in the zirconium acetate solution. This zirconium acetate solution has a greater impact on the environment during production and use.
Such as Chinese patent (publication number: CN 108752189 A) provides a kind of preparation method of zirconium acetate, and this method adds acetic acid in the zirconium carbonate and heats up to dissolve and then filters, and then evaporates and crystallizes in a water bath to obtain zirconium acetate, and this method can obtain purer zirconium acetate. Good zirconium acetate, but zirconium carbonate is not selected in the production process, resulting in excessive use of acetic acid (zirconium carbonate: acetic acid is 1:0.75), and it needs to be filtered three times before it can be clear. Acetic acid has not been recovered, which has a certain impact on the environment

Method used

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  • Preparation method of zirconium acetate solution with low free acetic acid
  • Preparation method of zirconium acetate solution with low free acetic acid

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preparation example Construction

[0022] A kind of zirconium acetate solution preparation method of low free acetic acid, see figure 1 , the steps are as follows:

[0023] 1) Preferentially choose zirconium carbonate with good activity, that is: one part of zirconium carbonate consumes less than 0.6 parts of acetic acid;

[0024] 2) Put acetic acid into the electric heating enamel reaction kettle, and the amount of acetic acid put in is 20% to 60% of the volume of the container;

[0025] 3) According to the weight ratio of zirconium carbonate and acetic acid in the enamel reaction kettle in step 2) of 1:0.35~0.6, gradually add zirconium carbonate, stir, heat up and dissolve, control the temperature range from 20 ℃ to 80 ℃, and react until the solution is clear ( That is: 0.1 g of zirconium carbonate is put into the solution and dissolved until it becomes clear for more than 30 minutes), and a high-concentration zirconium acetate solution is obtained, and the content of zirconia in this solution is 28% to 31%;...

Embodiment 1

[0034] A kind of zirconium acetate solution preparation method of low free acetic acid is as follows (as figure 1 shown):

[0035] 1) Preferentially select one part of zirconium carbonate to consume less than 0.6 parts of active zirconium carbonate by weight of acetic acid;

[0036] 2) Put acetic acid into the electric heating enamel reaction kettle, and the amount of acetic acid put in is 30% of the volume of the container;

[0037] 3) Add zirconium carbonate gradually to the enamel reaction kettle in step 2) according to the weight ratio of zirconium carbonate to acetic acid of 1:0.4, stir, heat up and dissolve, control the temperature range to 50 °C ± 5 °C, and react until the solution is clear (ie: 0.1 g of zirconium carbonate is put into the solution and dissolved until it becomes clear for more than 30 minutes), and a high-concentration zirconium acetate solution is obtained, and the content of zirconium oxide in this solution is 30%;

[0038] 4) Dilute the high-concen...

Embodiment 2

[0040] The zirconium acetate solution preparation method of another kind of low free acetic acid is as follows (as figure 2 shown):

[0041] 1) to 3) steps are the same as steps 1) to 3) in Example 1;

[0042] 4) Using double-cone vacuum drying equipment, vacuum-dry the high-concentration zirconium acetate solution in step 3) to obtain zirconium acetate grains / powder, the zirconium oxide content in the zirconium acetate grains / powder is 48%, and recover acetic acid;

[0043] 5) Use step 4) to dilute the zirconium acetate grains / powder with water to prepare a zirconium acetate solution with 5% zirconia content and low free acetic acid.

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Abstract

The invention discloses a preparation method of a zirconium acetate solution with low free acetic acid, which comprises the following steps of: preferentially selecting zirconium carbonate with good activity; adding acetic acid into an electric heating enamel reaction kettle; gradually adding the zirconium carbonate, stirring, heating, dissolving and reacting until the solution is clear to obtaina high-concentration zirconium acetate solution with the zirconium oxide content of 28-31%; and diluting the high-concentration zirconium acetate solution with water to prepare the zirconium acetate solution with low free acetic acid, wherein the zirconium oxide content is 5-30%. In addition, the high-concentration zirconium acetate solution is vacuum-dried by a double-cone vacuum drying device toobtain zirconium acetate crystal grains / powder, and acetic acid is recovered; and the zirconium acetate crystal grains / powder is diluted by adding water to prepare the zirconium acetate solution withlow free acetic acid, wherein the zirconium oxide content is 5-30%. The method saves the consumption of acetic acid resources, greatly shortens the production period, reduces the production cost andreduces the influence on the environment.

Description

technical field [0001] The invention belongs to the technology for preparing zirconium acetate in the field of fine chemicals, and in particular relates to a method for preparing a zirconium acetate solution with low free acetic acid. Background technique [0002] Zirconium acetate is mainly used as drier of paint, surface treatment of fiber and paper, waterproofing agent of building materials, adhesive in precision casting industry, etc. At present, zirconium acetate products on the market have a strong smell of acetic acid, which is mainly caused by the presence of more free acetic acid in the zirconium acetate solution, which has a greater impact on the environment during production and use. Such as Chinese patent (publication number: CN 108752189 A) provides a kind of preparation method of zirconium acetate, and this method adds acetic acid in the zirconium carbonate and heats up to dissolve and then filters, and then evaporates and crystallizes in a water bath to obtain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/10C07C51/41
Inventor 董雪平郭树军
Owner QUANNAN JINGXIN ENVIRONMENTAL PROTECTION MATERIALCO LTD
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