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Ammonium dichromate and sodium sulfate mixed crystal as well as preparation method and application thereof

A technology for mixing crystals, sodium dichromate, applied in chemical instruments and methods, chromate/dichromate, chromium oxide/hydrate, etc., can solve feeding difficulties, combustion, explosion, unrealized components Proportion and particle size, etc., to achieve the effect of ensuring the yield and particle size uniformity

Active Publication Date: 2020-12-29
GANSU JINSHI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the production methods of chromium oxide green pigment mainly include chromic anhydride thermal decomposition method and sodium dichromate-ammonium sulfate thermal decomposition method. The former preparation method is simple, but there are The problem of high cost and serious environmental pollution, the latter method produces less harmful gas, and the product color parameters are easy to control, but its product performance still needs to be improved, such as water granulation or wet mixing measures
US 4067747A discloses that sodium dichromate solution and ammonium sulfate solution are mixed and reacted, and excess water is removed by evaporation to obtain a mixture of ammonium dichromate and sodium sulfate, which is heated and roasted in the presence of water to obtain a pigment product, but the method The mixture of ammonium dichromate and sodium sulfate obtained in the method has a relatively high viscosity, and in order to ensure continuous feeding during roasting, the feeding needs to be dispersed and non-bonding, so there is a problem of feeding difficulties, although spray drying to a certain extent This problem can be solved, but the energy consumption is high and the control is difficult
[0004] In order to obtain a dispersed mixture, it is a method to directly mix ammonium dichromate and sodium sulfate raw materials. However, ammonium dichromate and organic matter contact friction, The impact can cause combustion and explosion, and it will start to decompose at 170-185°C, which is not conducive to transportation; at the same time, in industrial production, ammonium dichromate is obtained by the double decomposition reaction of sodium dichromate and ammonium chloride, and sulfuric acid can also be used Ammonium is used instead of ammonium chloride to produce ammonium dichromate. It can be seen that it is more appropriate to use sodium dichromate and ammonium sulfate as raw materials to prepare a dispersed, non-bonding mixture of ammonium dichromate and sodium sulfate.
[0005]CN 108675353A discloses a production method of high-end pigment chromium oxide green, using sodium dichromate and ammonium sulfate or ammonium carbonate as raw materials, and first producing Mixed crystals of ammonium dichromate and sodium sulfate or ammonium dichromate and sodium carbonate, then add roasting additives and roast at high temperature in a rotary kiln, and finally wash and remove impurities, dry, and pulverize to obtain chromium oxide green products, but this method does not The control of the component ratio and particle size in the mixed crystal has not been realized, and the performance of the chromium oxide green pigment cannot be guaranteed

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  • Ammonium dichromate and sodium sulfate mixed crystal as well as preparation method and application thereof
  • Ammonium dichromate and sodium sulfate mixed crystal as well as preparation method and application thereof
  • Ammonium dichromate and sodium sulfate mixed crystal as well as preparation method and application thereof

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preparation example Construction

[0063] The specific embodiment part of the present invention provides a kind of ammonium dichromate and sodium sulfate mixed crystal and its preparation method and application, and described preparation method comprises:

[0064] (1) Cool and crystallize after the mixed solution of sodium dichromate and ammonium sulfate is heated up, obtain saturated saline solution;

[0065] (2) Add ammonium sulfate first after the saturated salt solution obtained in step (1) is heated up, then add sodium dichromate, wherein the mol ratio of sodium dichromate and ammonium sulfate is 1:(0.9~1.1), after stirring reaction Cool and crystallize to obtain mixed crystals and crystallization mother liquor, and the crystallization mother liquor returns to step (1).

[0066] Described mixed crystal is used for preparing chromium oxide green pigment, and preparation method comprises:

[0067] The mixed crystals of ammonium dichromate and sodium sulfate are calcined, washed and dried to obtain chromium ...

Embodiment 1

[0070] The present embodiment provides a kind of preparation method of ammonium dichromate and sodium sulfate mixed crystal and the purposes of preparing chromium oxide green pigment by mixed crystal, specifically comprise the following steps:

[0071] (1) heating sodium dichromate, ammonium sulfate and sodium sulfate saturated solution at room temperature to 40°C, cooling and crystallizing to room temperature, and separating solid and liquid to obtain a saturated salt solution;

[0072] (2) ammonium sulfate is dissolved in the saturated salt solution that step (1) obtains, and its mass fraction reaches 10wt%, obtains ammonium sulfate solution; Sodium dichromate is dissolved in the saturated salt solution that step (1) obtains, Make its mass fraction reach 30wt%, obtain sodium dichromate solution;

[0073] (3) at 40 DEG C, under stirring state, the sodium dichromate solution that step (2) obtains is joined in the ammonium sulfate solution that step (2) obtains, and wherein the...

Embodiment 2

[0079] The present embodiment provides a kind of preparation method of ammonium dichromate and sodium sulfate mixed crystal and the purposes of preparing chromium oxide green pigment by mixed crystal, specifically comprise the following steps:

[0080] (1) heating sodium dichromate, ammonium sulfate and sodium sulfate saturated solution at room temperature to 90°C, cooling and crystallizing to room temperature, and separating solid and liquid to obtain saturated salt solution;

[0081](2) ammonium sulfate is dissolved in the saturated salt solution that step (1) obtains, and its mass fraction reaches 12wt%, obtains ammonium sulfate solution; Sodium dichromate is dissolved in the saturated salt solution that step (1) obtains, Make its mass fraction reach 20wt%, obtain sodium dichromate solution;

[0082] (3) at 90 DEG C, under stirring state, the sodium dichromate solution that step (2) obtains is joined in the ammonium sulfate solution that step (2) obtains, and wherein the mo...

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Abstract

The invention provides an ammonium dichromate and sodium sulfate mixed crystal as well as a preparation method and application thereof. The preparation method comprises the following steps: heating amixed solution of sodium dichromate, ammonium sulfate and sodium sulfate, and conducting cooling and crystallizing to obtain a saturated salt solution; and heating the obtained saturated salt solution, then adding ammonium sulfate, then adding sodium dichromate, conducting stirring for reaction, and then conducting cooling for crystallization to obtain mixed crystals and crystallization mother liquor. According to the invention, the saturated salt solution is used as a reaction base solution, and then the mixed crystal with uniform, dispersed and non-sticky particle size is prepared by controlling the reactant adding mode and proportion, reaction and post-treatment process, so that the generation of double salt is avoided, and the composition of the mixed crystal is ensured to meet the requirements; meanwhile, due to the use of the reaction base solution, evaporation and concentration steps can be omitted, and the crystallization yield is increased; and a chromium oxide green pigment is prepared from the obtained mixed crystal, so that the problem of difficult feeding in industrial production can be effectively solved, and the obtained product has better chromaticity parameters andexcellent performance.

Description

technical field [0001] The invention belongs to the technical field of mixed crystal preparation, and relates to a mixed crystal of ammonium dichromate and sodium sulfate and its preparation method and application, in particular to a mixed crystal of ammonium dichromate and sodium sulfate, its preparation method and its use in the preparation of oxidized The use of chrome green pigment. Background technique [0002] Chromium oxide green is a commonly used pigment with good stability, acid and alkali resistance, high temperature resistance, light and weather resistance, etc. It can be used in paints, coatings, inks, plastics, rubber, chemical fibers, textiles, ceramics, glass, cement and other industries Among them, chromium oxide green has a color similar to plant chlorophyll, and has great advantages as a camouflage material; in addition, chromium oxide green is also used in cosmetics, tapes, food, adhesives, electrostatic copying and other fields . When used as a pigment...

Claims

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Application Information

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IPC IPC(8): C01G37/14C01D5/00C01G37/02B01D9/02
CPCC01G37/14C01D5/00C01G37/02B01D9/0004C01P2006/62C01P2006/63C01P2006/64
Inventor 张红玲张忠元张笛陈荣雒敏婷谢希智庆朋辉孔红霞裴丽丽徐红彬张懿
Owner GANSU JINSHI CHEM
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