Zirconium carbonate specially used for synthesis of ammonium zirconium carbonate water-resistant cross-linking 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 product activity reduction, difficulty in control, and cross-linking failure, and achieve the goal of reducing waste water discharge, acid consumption, and salt content Effect

Active Publication Date: 2018-04-20
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

Method used

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  • Zirconium carbonate specially used for synthesis of ammonium zirconium carbonate water-resistant cross-linking agent, and preparation method thereof
  • Zirconium carbonate specially used for synthesis of ammonium zirconium carbonate water-resistant cross-linking agent, and preparation method thereof
  • Zirconium carbonate specially used for synthesis of ammonium zirconium carbonate water-resistant cross-linking agent, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0114] ①. Preparation of basic zirconium sulfate

[0115] a. Preparation of zirconium oxychloride solution

[0116] 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;

[0117] b. Preparation of basic zirconium sulfate

[0118] 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;

[0119] c. Filtration, washing, pulping

[0120] Step 1. The basic zirconium s...

Embodiment 2

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

[0141] ①. Preparation of basic zirconium sulfate

[0142] a. Preparation of zirconium oxychloride solution

[0143] In the stirred reactor, drop 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, 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;

[0146] c. Filtration, washing, pulping

[0147] Step 1. The basic zirconium sulfate feed ...

Embodiment 3

[0168] ①. Preparation of basic zirconium sulfate

[0169] a. Preparation of zirconium oxychloride solution

[0170] In the stirred reactor, drop 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, 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;

[0173] c. Filtration, washing, pulping

[0174] 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 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 zirconium carbonate specially used for synthesizing ammonium zirconium carbonate anti-water crosslinking agent 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 ammonium zirconium carbonate crosslinking agent. Ammonium zirconium carbonate is easily soluble in water, unstable in air, and soluble in dilute acids and alkalis. The aqueous solu...

Claims

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Application Information

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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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