Red rare-earth lanthanum cerium sulfide dye and preparation method thereof

A lanthanum sulfide and rare earth technology, applied in chemical instruments and methods, inorganic pigment treatment, fibrous fillers, etc., can solve the problems of poor stability and color performance of sulfur oxides, poor β-type structure, and sulfur deficiency, and achieve rich Effects of color and tint, lower synthesis temperature, and improved stability

Inactive Publication Date: 2008-01-16

CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI

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AI-Extracted Technical Summary

Problems solved by technology

In the above method, if S is used as the sulfur source, sulfur actually boils at about 400 degrees, so the reaction at high temperature is prone to sulfur deficiency, so that the product is easily mixed with sulfur oxides, and the stability of sulfur oxides and c...

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Abstract

The invention relates to a rare earth lanthanum and cerium sulfate which can be used as a red paint and a preparation method of the rare earth lanthanum and cerium. The chemical formula of the paint is: AxLayCe1-yS(3+x)/2, wherein, A stands for one of alkali metals lithium, sodium and potassium, x is equal to or bigger tan 0 and is equal to or smaller than 1, and y is equal to or bigger tan 0 and is equal to or smaller than 1. The alkali metal elements are doped into the rare earth lanthanum and cerium sulfate matrix to prepare rare earth sulfide paints in different red color systems through adjusting the doped amount of the alkali metal elements and different proportions of the lanthanum and cerium in high temperature solid-state reaction with mixed sulfate source gas produced by ammonium thiocyanate being heated and melted as reaction gas under the conditions of unoxidizing atmosphere with inert gas being input and the heating temperature of 400 to 1000 DEG C. The structure of a series of rare earth lanthanum and cerium sulfate doped with the alkali metal elements is NaC1type or Th3P4 type of gamma type in single cubic crystal system. The preparation method is safer and more environment protecting, the paint is non-toxic, so that the paint can be used for coloring for plastic, oil paint, coating, rubber, leather, ceramic, ink, paper, cosmetic and construction material like cement.

Application Domain

Inorganic pigment treatment

Technology Topic

ChemistryLanthanum +21

Image

Examples

Experimental program(12)

Example Embodiment

[0038] Example 1

[0039] According to the chemical structure of the product is Na 0.2 CeS 1.6 The molar content of the various metal raw materials and the total amount of raw materials are 500 grams. Weigh the raw materials, mix the raw materials sodium bicarbonate, rare earth lanthanum oxide and rare earth cerium oxide, and then put them into the reaction boat, and then put them into the tube furnace Inside, the reactor is closed, the inert gas is high-purity nitrogen, and the gas flow rate is 0.1 liter/min. After 10 minutes, the sulfur source gas produced by the heating and melting decomposition of ammonium thiocyanate is introduced, and then the heating rate is 10℃/min. , Raise the high temperature tubular reactor to 700℃ and keep it at this temperature for 3h. Continue to pass sulfur source gas and inert gas, and then continue to heat up to 900°C at a rate of 10°C/min, and keep it at this temperature for 2h. Then stop heating and supply sulfur source gas, cool naturally, and continue to supply inert gas. The temperature drops to 150°C, stop passing inert gas, take it out, grind the product evenly, wash and dry (less than 100°C) to obtain a red product, whose structure is Th in the cubic γ-type structure 3 P 4 Crystalline phase. The CIE color coordinate is: L * =50.082, a * = 23.379, b * = 14.492.

[0040] For the tail gas (the remaining unreacted sulfur source gas) during the reaction process, copper sulfate (CuSO 4 ) And zinc sulfate (ZnSO 4 ) (Their purity ≥98%) saturated aqueous solution to absorb, so that the by-products copper sulfide (CuS) and zinc sulfide (ZnS) appear in the form of precipitation, and then filtered, dried and ground to obtain by-products.

[0041] Method for heating and melting and decomposing ammonium thiocyanate to produce sulfur source gas

[0042] Raw material ammonium thiocyanate NH 4 SCN (industrial purity, purity ≥98%) is added into the glass tube of the vertical tubular resistance furnace at a time of 700g, and then sealed, heated to 180℃, keeping this temperature unchanged, you can get the mixed sulfur source gas, using a hose It is connected to the high-temperature tube furnace and sent to the high-temperature tube furnace.

[0043] When no inert gas is required, the vertical tubular resistance furnace is closed 15-30 minutes in advance.

Example Embodiment

[0044] Example 2

[0045] The rare earth raw material is cerium carbonate, and the others are the same as in Example 1. A red product is obtained. Its structure is Th in cubic γ-type structure 3 P 4 Crystalline phase. The CIE color coordinate is: L * =50.082, a * = 23.379, b * = 14.492.

Example Embodiment

[0046] Example 3

[0047] Anhydrous sodium carbonate is used as the alkali metal raw material, and the inert gas is high-purity argon. The others are the same as in Example 1, to obtain a red product. Its structure is Th in cubic γ-type structure 3 P 4 Crystalline phase. The CIE color coordinate is: L * =50.082, a * = 23.379, b * = 14.492.

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Description & Claims & Application Information

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

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