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Zirconium carbonate specially used for synthesizing ammonium zirconium carbonate anti-water crosslinking agent and preparation method thereof

A technology of ammonium zirconium carbonate and zirconium carbonate, which is applied in the field of zirconium carbonate and its preparation, can solve problems such as difficulty in control, reduced product activity, and cross-linking failure, and achieve the goal of reducing the amount of acid, reducing waste water discharge, and reducing salt content Effect

Active Publication Date: 2019-11-01
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 ammonium zirconium carbonate produced from it, and crosslinking failure within the storage period
It is even difficult to produce clear and stable ammonium zirconium carbonate products;
[0011] 2. In the process of preparing ammonium zirconium carbonate, the mass ratio range of zirconium carbonate: ammonium bicarbonate that can be adapted 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 ammonium zirconium carbonate 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

Method used

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  • Zirconium carbonate specially used for synthesizing ammonium zirconium carbonate anti-water crosslinking agent and preparation method thereof
  • Zirconium carbonate specially used for synthesizing ammonium zirconium carbonate anti-water crosslinking agent and preparation method thereof
  • Zirconium carbonate specially used for synthesizing ammonium zirconium carbonate anti-water crosslinking agent and preparation method thereof

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Experimental program
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Embodiment 1

[0113]A preparation method of zirconium carbonate specially used for synthesizing ammonium zirconium carbonate water-resistant crosslinking agent of the present invention. It includes the following steps:

[0114] ①. Preparation of basic zirconium sulfate

[0115] a. Preparation of zirconium oxychloride solution

[0116] In the stirring reaction kettle, put into deionized water and zirconium oxychloride, stir and dissolve, and prepare a 110g / l zirconium oxychloride aqueous solution;

[0117] b. Preparation of basic zirconium sulfate

[0118] Under stirring, in the aqueous solution of zirconium oxychloride prepared in item a, add concentrated sulfuric acid dropwise or add anhydrous sodium sulfate to control SO 4 2- : ZrO 2 The molar ratio is 0.7, the heating rate is controlled at 1°C / min, the temperature is raised to 90°C, and at a temperature of 90°C, the reaction is incubated for 1 to 1.5 hours, ready for filtration;

[0119] c. Filtration, washing, pulping

[0120] Th...

Embodiment 2

[0140] A preparation method of zirconium carbonate specially used for synthesizing ammonium zirconium carbonate water-resistant crosslinking agent of the present invention. It includes the following steps:

[0141] ①. Preparation of basic zirconium sulfate

[0142] a. Preparation of zirconium oxychloride solution

[0143] In the stirring reaction kettle, put into deionized water and zirconium oxychloride, stir and dissolve, and prepare a 90g / l zirconium oxychloride aqueous solution;

[0144] b. Preparation of basic zirconium sulfate

[0145] Under stirring, in the aqueous solution of zirconium oxychloride prepared in item a, add concentrated sulfuric acid dropwise or add anhydrous sodium sulfate to control SO 4 2- : ZrO 2 The molar ratio is 0.6, the heating rate is controlled at 1°C / min, the temperature is raised to 90°C, and at a temperature of 90°C, the reaction is incubated for 1 to 1.5 hours, ready for filtration;

[0146] c. Filtration, washing, pulping

[0147] Th...

Embodiment 3

[0168] ①. Preparation of basic zirconium sulfate

[0169] a. Preparation of zirconium oxychloride solution

[0170] In the stirring reaction kettle, put into deionized water and zirconium oxychloride, stir and dissolve, and prepare a 100g / l zirconium oxychloride aqueous solution;

[0171] b. Preparation of basic zirconium sulfate

[0172] Under stirring, in the aqueous solution of zirconium oxychloride prepared in item a, add concentrated sulfuric acid dropwise or add anhydrous sodium sulfate to control SO 4 2- : ZrO 2 The molar ratio is 0.65, the heating rate is controlled at 1 °C / min, the temperature is raised to 90 °C, and at a temperature of 90 °C, the reaction is incubated for 1 to 1.5 hours, ready for filtration;

[0173] c. Filtration, washing, pulping

[0174] The basic zirconium sulfate feed solution prepared in step 1 is filtered by a belt vacuum filtration washing machine, and the filter cake is continuously washed with deionized water under vacuum until the pH...

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Abstract

The invention discloses a zirconium carbonate product specially used for synthesis of ammonium zirconium carbonate water-resistant cross-linking agent, and preparation method thereof, and belongs to the field of zirconium compound preparation. The particle size D50 of the zirconium carbonate ranges from 35 to 40<mu>m, ZrO2wt% is equal to or larger than 40, activity retention time is 24 months or longer; the weight ratio of zirconium carbonate to ammonium bicarbonate is controlled to be 1:0.8-2.8:1; the synthesized water-resistant cross-linking agent reaction time is 30min or shorter. The zirconium carbonate is long in active retention time, wide in zirconium carbonate to ammonium bicarbonate mass ratio range, and short in reaction time; zirconium carbonate particle size is relatively large; filtration operation is convenient; product ZrO2 content is high. Production cost is reduced, waste water discharge amount and salt content in waste water are reduced, raw materials are saved, and the zirconium carbonate and the preparation method are beneficial for environment protection.

Description

technical field [0001] The invention relates to a special zirconium carbonate for synthesizing ammonium zirconium carbonate water-resistant crosslinking agent and a preparation method thereof. A method for preparing a compound of 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 purification catalyst, papermaking water-resistant crosslinking agent, paint and ink drier, and also an economical raw material for the production of ultrafine silica. [0003] The application of zirconium carbonate in water-based coatings and adhesives cross-linking agent is to convert it into ammonium zirconium carbonate cross-linking agent. Ammonium zirconium carbonate is easily soluble in water, unstable in air, and soluble in dilute acid and alkali. The aqueous solution decomposes rapidly at 60°C and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00
CPCC01G25/00C01P2004/61C01P2006/80
Inventor 郝本清
Owner 山东广通新材料有限公司
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