阅读说明：本技术 不同颜色凹土颜料的水热合成方法 (Hydrothermal synthesis method of attapulgite pigments with different colors ) 是由 蒋睿雯 王训芝 夏正旺 芮国峰 高晓燕 倪伶俐 陈静 于 2019-11-20 设计创作，主要内容包括：本发明涉及无机非金属材料领域,公开了一种不同颜色凹土颜料的水热合成方法,将凹凸棒石黏土加入到含有一定金属离子的水溶液中,打浆混合均匀后转入聚四氟乙烯衬底的高压反应釜中,150-200℃反应72-288h,反应结束之后,自然冷却到室温后,用去离子水洗涤至滤液中检测不到相应的金属离子(ICP检测),再于80℃烘箱中烘干后,置于马弗炉中280℃煅烧3h,得到不同颜色凹土颜料。本发明的制备方法操作方便,节能环保,制备的不同颜色的凹土颜料可应用到不同的水性高分子乳液中,其涂层产品具有耐水性好、耐候性高、色彩艳丽等优点,具有广阔的市场前景。(The invention relates to the field of inorganic non-metallic materials, and discloses a hydrothermal synthesis method of attapulgite pigments with different colors, which comprises the steps of adding attapulgite clay into an aqueous solution containing certain metal ions, pulping, mixing uniformly, transferring into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, reacting for 72-288h at the temperature of 150-. The preparation method is convenient to operate, energy-saving and environment-friendly, the prepared attapulgite pigments with different colors can be applied to different water-based polymer emulsions, and the coating product has the advantages of good water resistance, high weather resistance, bright color and the like, and has wide market prospect.)

1. A hydro-thermal synthesis method of attapulgite pigments with different colors is characterized in that: taking the following raw materials in percentage by weight: 5% of attapulgite clay, 2-10% of metal ion aqueous solution and the balance of water;

the synthesis steps are as follows:

(1) preparing a metal ion aqueous solution with the concentration of 0.1-0.5 g/mL;

(2) adding attapulgite clay into the metal ion aqueous solution, pulping, mixing uniformly, transferring into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, reacting for 72-288h at the temperature of 150-;

(3) washing the obtained sample with deionized water until no corresponding metal ion can be detected in the filtrate, and drying in an oven at 80 ℃;

(4) and (3) calcining the dried sample in a muffle furnace at 280 ℃ for 3h to obtain the attapulgite pigments with different colors.

2. The hydrothermal synthesis method of attapulgite pigments with different colors according to claim 1, characterized in that the aqueous solution of metal ions is any one of the following:

FeCl₃·6H₂O、CuCl₂·2H₂O、Ce(NO₃)₃·6H₂O。

3. the hydrothermal synthesis method of attapulgite pigments with different colors according to claim 1, wherein the attapulgite clay is attapulgite clay purified.

4. The hydrothermal synthesis method of attapulgite pigments with different colors according to claim 1, characterized in that in step (3), the metal ions are detected using ICP.

Technical Field

The invention relates to the field of inorganic non-metallic materials, in particular to a hydrothermal synthesis method of attapulgite pigments with different colors.

Background

The traditional inorganic pigment generally has higher weather resistance, but also has the defects of incomplete color spectrum, monotonous products and the like which are difficult to overcome, and most of the inorganic pigments contain heavy metals and have certain toxicity, so the application depth and the application range of the inorganic pigments are limited from the side. At present, small molecule dyes are commonly used for obtaining colored waterborne polyurethane products. Since the common small molecule dye is usually fixed on the aqueous polyurethane through ionic bond, hydrogen bond, van der waals force and the like, the small molecule dye has weak bonding force with the polyurethane, and is easy to migrate to the surface of the material during the processes of placing, washing, dry cleaning, using and the like, thereby causing continuous falling and fading.

The natural attapulgite clay mineral is partially caused by Mg in the process of mineralization²⁺Resulting in partial position in its octahedral structure being Fe³⁺And replacing to make the formed attapulgite clay brick red. The brick color of the attapulgite clay is very stable, and the attapulgite clay has good acid and alkali resistance and weather resistance. But the color is single, the purity is low, and the industrial utilization is difficult.

Disclosure of Invention

The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a hydrothermal synthesis method of attapulgite pigments with different colors, the synthesized attapulgite pigment has good weather resistance, strong tinting strength and simple preparation process, the prepared attapulgite pigments with different colors can be applied to different water-based polymer emulsions, and the coating product has the advantages of good water resistance, high weather resistance, bright color and the like, and has wide market prospect.

The technical scheme is as follows: the invention provides a hydrothermal synthesis method of attapulgite pigments with different colors, which is characterized by comprising the following steps: taking the following raw materials in percentage by weight: 5% of attapulgite clay, 2-10% of metal ion aqueous solution and the balance of water;

the synthesis steps are as follows:

(1) preparing a metal ion aqueous solution with the concentration of 0.1-0.5 g/mL;

(2) adding attapulgite clay into the metal ion aqueous solution, pulping, mixing uniformly, transferring into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, reacting for 72-288h at the temperature of 150-;

(3) washing the obtained sample with deionized water until no corresponding metal ion can be detected by ICP in the filtrate, and drying in an oven at 80 ℃;

(4) and (3) calcining the dried sample in a muffle furnace at 280 ℃ for 3h to obtain the attapulgite pigments with different colors. (rich in different metal elements, such as Fe element in red, Cu element in blue, Ce element in earthy yellow).

Preferably, the aqueous solution of metal ions is any one of: FeCl₃·6H₂O、CuCl₂·2H₂O、Ce(NO₃)₃·6H₂O。

Preferably, the attapulgite clay is attapulgite clay subjected to impurity removal and purification.

Preferably, in step (3), the metal ions are detected using ICP.

Has the advantages that: the invention simulates the mineralization condition of attapulgite clay by a hydrothermal method, adds specific metal ions to replace octahedral Mg in attapulgite clay crystals²⁺Thereby obtaining the attapulgite clay pigment with high purity and different colors (for example, Fe element is red, Cu element is blue, Ce element is earthy yellow). The method is convenient to operate, the prepared attapulgite pigments with different colors can be applied to different water-based polymer emulsions, the polymer materials can be effectively reinforced due to the fibrous morphology of the attapulgite clay, and the obtained coating product has the advantages of good water resistance, high weather resistance, bright color and the like, and has wide market prospect.

Compared with the prior art, the invention has the following advantages:

1. the attapulgite pigment prepared by the method has good weather resistance, strong tinting strength and simple preparation process, and is suitable for industrial production;

2. the attapulgite pigment prepared by the method can be applied to different aqueous polymer emulsions, and the coating product has the advantages of good water resistance, high weather resistance, bright color and the like, and has wide market prospect.

Drawings

FIG. 1 shows Fe in example 1³⁺Scanning electron micrographs of substituted red attapulgite clay.

Detailed Description

The present invention will be described in detail with reference to the accompanying drawings.