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
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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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