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

A technology of potassium zirconium carbonate and zirconium carbonate, which is applied in the field of zirconium carbonate and its preparation, can solve the problems of reduced product activity, difficulty in control, and low product content, and achieve the goals of reducing salt content, reducing waste water discharge, and reducing the amount of acid used Effect

Active Publication Date: 2019-09-24
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

[0008] 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 potassium zirconium carbonate produced from it, and crosslinking failure within the storage period
It is even difficult to produce clear and stable potassium zirconium carbonate products;
[0009] 2. In the process of preparing potassium zirconium carbonate, the mass ratio range of zirconium carbonate:potassium carbonate 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 potassium zirconium carbonate anti-water crosslinking agent
[0011] 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 potassium zirconium carbonate anti-water crosslinking agent and preparation method thereof
  • Zirconium carbonate specially used for synthesizing potassium zirconium carbonate anti-water crosslinking agent and preparation method thereof
  • Zirconium carbonate specially used for synthesizing potassium zirconium carbonate anti-water crosslinking agent and preparation method thereof

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Experimental program
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Embodiment 1

[0112] A method for preparing zirconium carbonate specially used for synthesizing potassium zirconium carbonate water-resistant crosslinking agent of the present invention. Including the following steps:

[0113] ①. Preparation of basic zirconium sulfate

[0114]a. Preparation of zirconium oxychloride solution

[0115] 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;

[0116] b. Preparation of basic zirconium sulfate

[0117] 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;

[0118] c. Filtration, washing, pulping

[0119] Step 1. The basic zirconium ...

Embodiment 2

[0140] A method for preparing zirconium carbonate specially used for synthesizing potassium 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 relates to zirconium carbonate special for synthesis of potassium zirconium carbonate water-resistant crosslinker and a preparation method thereof and belongs to preparation methods of zirconium compounds. The zirconium carbonate special for synthesis of potassium zirconium carbonate water-resistant crosslinker is characterized in that finished zirconium carbonate has particle size of D5035-40 mu m, ZrO2 of > / -40% by weight and activity retention time of > / =24 months, the ratio of zirconium carbonate to potassium carbonate for synthesis of the water-resistant crosslinker is 1:0.8to 2:1, and reaction time for the synthesis of the water-resistant crosslinker is < / =30 min. Finished potassium carbonate having long activity retention time, wide range of zirconium-potassium mass ratio, short reaction time and good applicability as a raw material for synthesis of potassium zirconium carbonate water-resistant crosslinker is provided. A preparation method of zirconium carbonate special for synthesis of potassium zirconium carbonate water-resistant crosslinker, by which zirconium carbonate of large particle size is synthesized, which facilitates filtering and by which high content is achieved, is provided. The production cost is lowered. Wastewater emission and salt content in wastewater are decreased, raw materials are saved, and environmental protection is benefited.

Description

technical field [0001] The invention relates to zirconium carbonate specially used for synthesizing potassium zirconium carbonate water-resistant 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] Potassium zirconium carbonate anti-water crosslinking agent, does not contain harmful substances such as aldehydes, and is easy to cross-link and solidify; the finished paper coated with zirconium carbonate water-resistant agent coating has higher Excellent gloss (75%), whiteness and napping...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00C09D11/03C09D7/61
Inventor 扬美洁
Owner 山东广通新材料有限公司
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