Industrial zirconium carbonate with high purity, high activity and good storage stability and preparation method thereof

A high-purity technology of zirconium carbonate, applied in chemical instruments and methods, zirconium compounds, pharmaceutical formulations, etc., can solve problems such as difficult control, narrow range of ammonium bicarbonate mass ratio, cross-linking failure, etc., and achieve the goal of reducing the amount of acid Effect

Active Publication Date: 2018-06-08
山东广通新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. The activity retention time of zirconium carbonate products is relatively short, and after storage for 3 to 5 months, the activity of the product is significantly reduced, resulting in poor storage stability of zirconium carbonate salts produced with it as raw materials, and cross-linking failure within the storage period
It is even difficult to produce clear and stable zirconium carbonate products;
[0011] 2. In the process of preparing zirconium carbonate salt, the range of suitable zirconium carbonate: ammonium bicarbonate mass ratio is relatively narrow, and can only be used between 1:0.8 and 1:1. The production process conditions are harsh and difficult to control
Detrimental effect on the subsequent centrifugation process, resulting in lower product content
Not suitable for use as a raw material for zirconium carbonate salt water-resistant crosslinking agent
[0013] 4. When the zirconium carbonate product of the prior art is used for the synthesis process of the water-resistant crosslinking agent, the reaction time is long, more than 1 hour
[0014] 5. In coatings and adhesives, especially when used as a crosslinking agent in the preparation of emulsion polyurethane adhesives, emulsion acrylic adhesives, styrene-acrylic emulsion adhesives, and styrene-butadiene rubber emulsions, Commercially available zirconium carbonate cannot meet user needs
Commercially available zirconium carbonate is difficult to meet these demands

Method used

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  • Industrial zirconium carbonate with high purity, high activity and good storage stability and preparation method thereof
  • Industrial zirconium carbonate with high purity, high activity and good storage stability and preparation method thereof
  • Industrial zirconium carbonate with high purity, high activity and good storage stability and preparation method thereof

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Experimental program
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Embodiment 1

[0118] The invention relates to a method for preparing industrial zirconium carbonate with high purity, high activity and good storage stability. Including the following steps:

[0119] ①. Preparation of basic zirconium sulfate

[0120] a. Preparation of zirconium oxychloride solution

[0121] In the stirring reaction kettle, drop into deionized water and zirconium oxychloride, stir and dissolve, and prepare a zirconium oxychloride aqueous solution of 110g / l;

[0122] b. Preparation of basic zirconium sulfate

[0123] Under stirring, add concentrated sulfuric acid or anhydrous sodium sulfate dropwise to the zirconium oxychloride aqueous solution prepared in item a to control SO 4 2- : ZrO 2 The molar ratio is 0.7, the heating rate is controlled at 1°C / min, the temperature rises to 90°C, and at 90°C, the reaction is kept for 1 to 1.5 hours, and the filter is prepared;

[0124] c. Filtration, washing, pulping

[0125] Step 1. The basic zirconium sulfate feed solution prep...

Embodiment 2

[0143] The invention relates to a method for preparing industrial zirconium carbonate with high purity, high activity and good storage stability. Including the following steps:

[0144] ①. Preparation of basic zirconium sulfate

[0145] a. Preparation of zirconium oxychloride solution

[0146] In the stirred reactor, drop into deionized water and zirconium oxychloride, stir and dissolve, and prepare a 90g / l zirconium oxychloride aqueous solution;

[0147] b. Preparation of basic zirconium sulfate

[0148] Under stirring, add concentrated sulfuric acid or anhydrous sodium sulfate dropwise to the zirconium oxychloride aqueous solution prepared in item a to control SO 4 2- : ZrO 2 The molar ratio is 0.6, the heating rate is controlled at 1°C / min, the temperature rises to 90°C, and at 90°C, the reaction is kept for 1 to 1.5 hours, and the filter is prepared;

[0149] c. Filtration, washing, pulping

[0150] Step 1. The basic zirconium sulfate feed solution prepared in step ...

Embodiment 3

[0169] ①. Preparation of basic zirconium sulfate

[0170] a. Preparation of zirconium oxychloride solution

[0171] In the stirred reactor, drop into deionized water and zirconium oxychloride, stir and dissolve, and prepare a 100g / l zirconium oxychloride aqueous solution;

[0172] b. Preparation of basic zirconium sulfate

[0173] Under stirring, add concentrated sulfuric acid or anhydrous sodium sulfate dropwise to the zirconium oxychloride aqueous solution prepared in item a to control SO 4 2- : ZrO 2 The molar ratio is 0.65, the heating rate is controlled at 1°C / min, the temperature rises to 90°C, and at 90°C, the reaction is kept for 1 to 1.5 hours, and the filter is prepared;

[0174] c. Filtration, washing, pulping

[0175] Step 1. The basic zirconium sulfate feed solution prepared in step 1 is filtered by a belt-type vacuum filter washing machine, and the filter cake is continuously washed with deionized water under vacuum until the pH is qualified, and an appropri...

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Abstract

The invention discloses industrial zirconium carbonate with high purity, good activity and good storage stability, and a preparation method thereof, and belongs to preparation methods of zirconium compounds. The product quality of the industrial zirconium carbonate with high purity, good activity and good storage stability reaches the following standards: the particle size D50 ([mu]m) is 35-40, the activity retention time is larger than or equal to 24 months, the ZrO2 content is larger than or equal to 42 wt%, and the impurity content is lower than a current national standard. The invention provides the zirconium carbonate product, which has a high ZrO2 content, a long activity retention time, and a wide range of the mass ratio of zirconium carbonate to ammonium bicarbonate, is applicableas a raw material with a short reaction time for synthesizing a zirconium carbonate water-repelling crosslinking agent, and can also meet demands for preparation of the zirconium carbonate crosslinking agent required for automobile exhaust ternary catalysis purifier carrier materials and aqueous coating adhesives. The invention provides the preparation method for the industrial zirconium carbonatewith high purity, good activity and good storage stability, wherein the preparation method is easy for filtering operation, and the product content is high. According to the technical scheme, the production cost is reduced, raw materials are saved and environmental protection is facilitated.

Description

technical field [0001] The invention relates to an industrial zirconium carbonate with high purity, high activity and good storage stability and a preparation method thereof. A method for the preparation of compounds belonging to zirconium. Background technique [0002] Zirconium carbonate Zr 2 O(CO 3 ).nH 2 O, also known as basic zirconium carbonate ZrO 2 CO 2 .nH 2 O. It is an important zirconium compound, mainly used in cosmetic antiperspirant, automobile exhaust gas purification catalyst, papermaking water-resistant crosslinking agent, paint and ink drier, and is also a relatively economical raw material for the production of ultrafine silica. [0003] The application of zirconium carbonate in water-based coatings and adhesive crosslinking agents is to convert it into zirconium carbonate salt crosslinking agent. Zirconium carbonate salt is easily soluble in water, unstable in air, and soluble in dilute acid and alkali. The aqueous solution decomposes rapidly at 6...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00C09D7/61C09J11/04B01J27/232A61K8/28A61Q15/00C01B33/18
CPCA61K8/28A61Q15/00B01J27/232C01B33/18C01G25/00C01P2004/61C01P2006/80C09J11/04
Inventor 郝本清
Owner 山东广通新材料有限公司
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