CN110844913A - Hydrothermal synthesis method of attapulgite pigments with different colors - Google Patents
Hydrothermal synthesis method of attapulgite pigments with different colors Download PDFInfo
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- CN110844913A CN110844913A CN201911140989.5A CN201911140989A CN110844913A CN 110844913 A CN110844913 A CN 110844913A CN 201911140989 A CN201911140989 A CN 201911140989A CN 110844913 A CN110844913 A CN 110844913A
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- attapulgite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
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.
Description
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.
Embodiment 1:
the embodiment provides a hydrothermal synthesis method for preparing a red attapulgite pigment, which comprises the following raw materials in percentage by weight: attapulgite clay 5%, FeCl3·6H2O2 percent and the balance of water.
The synthesis steps are as follows:
s1: weighing 2g FeCl3·6H2O was dissolved in 93g of water for further use.
S2: adding 5g of attapulgite clay into the prepared FeCl3Pulping and mixing the mixture in the aqueous solution, transferring the mixture into a high-pressure reaction kettle with a tetrafluoroethylene substrate, reacting the mixture for 72 hours at 180 ℃, and naturally cooling the mixture to room temperature after the reaction is finished.
S3: washing the obtained sample with deionized water until no Fe can be detected in the filtrate3+(ICP detection), and then dried in an oven at 80 ℃.
S4: and (3) calcining the dried sample in a muffle furnace at 280 ℃ for 3h to obtain the red attapulgite pigment rich in the iron element.
FIG. 1 shows that Fe is formed by hydrothermal treatment at 180 ℃ for 72 hours and calcination at 280 ℃ for 3 hours3+The fibrous morphology of the substituted red attapulgite clay is not destroyed, and the water resistance, solvent resistance and weather resistance data are shown in table 1.
Embodiment 2:
the embodiment provides a hydrothermal synthesis method for preparing a blue attapulgite pigment, which comprises the following raw materials in percentage by weight: attapulgite clay 5%, CuCl2·2H2O5% and the balance of water.
The synthesis steps are as follows:
s1: 5g of CuCl are weighed2·2H2O was dissolved in 90g of water for use.
S2: adding 5g of attapulgite clay into the prepared CuCl2Pulping and mixing the mixture in the aqueous solution, transferring the mixture into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, reacting the mixture for 144 hours at 180 ℃, and naturally cooling the mixture to room temperature after the reaction is finished.
S3: the obtained sample is washed by deionized water until no Cu can be detected in the filtrate2+(ICP detection), and then dried in an oven at 80 ℃.
S4: and (3) calcining the dried sample in a muffle furnace at 280 ℃ for 3h to obtain the blue attapulgite pigment rich in copper element.
The water resistance, solvent resistance and weather resistance data are shown in the table 1.
Embodiment 3:
the embodiment provides a hydrothermal synthesis method for preparing yellow attapulgite pigment, which comprises the following raw materials in percentage by weight: attapulgite Clay 5%, Ce (NO)3)3·6H2O10% and the balance of water.
The synthesis steps are as follows:
s1: weighing 10g Ce (NO)3)3·6H2O was dissolved in 85g of water for use.
S2: adding 5g of attapulgite clay into the prepared Ce (NO)3)3Pulping and mixing the mixture in the aqueous solution, transferring the mixture into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, reacting for 288 hours at 200 ℃, and naturally cooling to room temperature after the reaction is finished.
S3: washing the obtained sample with deionized water until no Ce can be detected in the filtrate3+(ICP detection), and then dried in an oven at 80 ℃.
S4: and (3) calcining the dried sample in a muffle furnace at 280 ℃ for 3h to obtain the yellow attapulgite pigment rich in cerium.
The water resistance, solvent resistance and weather resistance data are shown in the table 1.
The weathering resistance and solvent resistance of the attapulgite pigments of different colors prepared by the methods of the above embodiments were respectively tested by the following methods:
weather resistance: after the prepared pigment powder is sprayed to form a film, detection is carried out according to GB/T1865-2009 color paint and varnish-artificial weathering and artificial radiation exposure (filtered xenon arc radiation), and after 1000 hours, judgment and measurement are carried out on the color change of the pigment coating according to GB/T250-2008.
Water resistance and solvent resistance: the samples were tested according to the method of GB/T5211.5-2008 pigment resistance test.
The fluorescent waterborne polyurethanes obtained in examples 1, 2 and 3 were tested for weather resistance, water resistance and solvent resistance, and the results are shown in Table 1 below:
TABLE 1
| Weather resistance | Water resistance | Solvent resistance | |
| Example 1 | Grade 5 | Grade 5 | Grade 5 |
| Example 2 | Grade 5 | Grade 5 | Grade 5 |
| Example 3 | Grade 5 | Grade 5 | Grade 5 |
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
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.
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Citations (5)
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| RU2169041C1 (en) * | 2000-02-08 | 2001-06-20 | Государственное унитарное предприятие Электростальское научно-производственное объединение "Неорганика" | Catalyst preparation method |
| CN105694539A (en) * | 2016-02-29 | 2016-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing iron oxide red hybridization pigment by means of clay minerals |
| CN105802282A (en) * | 2016-02-29 | 2016-07-27 | 中国科学院兰州化学物理研究所 | Method for preparing red hybridized pigment from red attapulgite clay |
| CN108102433A (en) * | 2017-12-28 | 2018-06-01 | 中国科学院兰州化学物理研究所 | The method that high heat stability type clay mineral-iron oxide red hybrid pigment is prepared using chemical coprecipitation technique |
| CN109181369A (en) * | 2018-10-15 | 2019-01-11 | 中国科学院兰州化学物理研究所 | Microwave hydrothermal auxiliary prepares high chroma cobalt blue/clay mineral hybrid pigment method |
-
2019
- 2019-11-20 CN CN201911140989.5A patent/CN110844913B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2169041C1 (en) * | 2000-02-08 | 2001-06-20 | Государственное унитарное предприятие Электростальское научно-производственное объединение "Неорганика" | Catalyst preparation method |
| CN105694539A (en) * | 2016-02-29 | 2016-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing iron oxide red hybridization pigment by means of clay minerals |
| CN105802282A (en) * | 2016-02-29 | 2016-07-27 | 中国科学院兰州化学物理研究所 | Method for preparing red hybridized pigment from red attapulgite clay |
| CN108102433A (en) * | 2017-12-28 | 2018-06-01 | 中国科学院兰州化学物理研究所 | The method that high heat stability type clay mineral-iron oxide red hybrid pigment is prepared using chemical coprecipitation technique |
| CN109181369A (en) * | 2018-10-15 | 2019-01-11 | 中国科学院兰州化学物理研究所 | Microwave hydrothermal auxiliary prepares high chroma cobalt blue/clay mineral hybrid pigment method |
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Application publication date: 20200228 Assignee: Jiangsu Huaxia Yunjin Weaving Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2021980010936 Denomination of invention: Hydrothermal synthesis of concave soil pigments with different colors Granted publication date: 20210101 License type: Common License Record date: 20211020 |