Method for preparing nano iron oxide red

A technology of iron oxide red and nanometer, which is applied in the direction of fibrous fillers, can solve the problems of difficult control of particle size and shape, complex process, long production cycle, etc., and achieve easy control of process parameters, simple preparation process and good dispersion performance Effect

Inactive Publication Date: 2004-06-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
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Problems solved by technology

[0006] The purpose of the present invention is to solve the existing problems in the existing preparation method that the particle size and shape of the particles are difficult to control, and the dispersion of the particles is not good, and the particles are easy to agglomerate, as well as the existing preparation methods have complex processes and low yields. , high cost and long production cycle, thus providing a monodisperse nanometer α-Fe with a particle size of 10-100nm 2 o 3 Granular iron oxide red particle preparation method

Method used

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  • Method for preparing nano iron oxide red
  • Method for preparing nano iron oxide red
  • Method for preparing nano iron oxide red

Examples

Experimental program
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Embodiment 1

[0032] The preparation process of this embodiment is as follows Figure 7 shown. 31.8g anhydrous Na 2 CO 3 Dissolve in 300ml of deionized water to make lye, add 0.05ml of ethyl acetate under vigorous stirring (600 rpm) to make the solution evenly mixed, then add 300ml of FeCl with a concentration of 0.1mol / l under continuous stirring 3 ·6H 2 O solution to form a gel, then add 30ml to a concentration of 1×10 -4 mol / l sodium dihydrogen phosphate solution, the PH value of the mixed solution is 9; aging at 85°C for 5 minutes to obtain a red suspension, which is then centrifuged with a centrifugal pump, washed 3 times with deionized water, and heated at 25°C After drying for 1.5 hours, the spherical α-Fe with an average particle size of 60nm was obtained after grinding. 2 o 3 Particles, the grain size is close to monodisperse, and its TEM picture is shown in image 3 .

Embodiment 2

[0034] The preparation process of this embodiment is as follows Figure 7 shown. 95g anhydrous NaHCO 3 Dissolve in 300ml of deionized water to make lye, then add 0.3g of citric acid under stirring condition (1000 rpm) to make the solution fully mixed. FeSO 4 ·7H 2 O (0.3mol / l) solution 1000ml was oxidized in the air for 0.5 hours, and the oxidized product was added to the above mixture to form a gel under continuous stirring, and then 3000ml was added to a concentration of 1×10 -3 mol / l sodium dihydrogen phosphate solution, the PH value of the mixed solution is 8; aged at 110°C for 20 minutes to obtain a red suspension, which was centrifuged with a centrifugal pump and washed 5 times with deionized water. Cubic α-Fe with an average particle size of 42 nm was obtained after drying at ℃ for 3 hours. 2 o 3 Particles, the grain size is close to monodisperse, and its TEM picture is shown in Figure 4 .

Embodiment 3

[0036] The preparation process of this embodiment is as follows Figure 7 shown. 45mlNH 3 ·H 2 O (25%, mass ratio) and 11ml of acetic anhydride are fully stirred (1100 rpm) and mixed, and 300ml of Fe(NO 3 ) 3 9H 2 O solution to form a gel, then add 60ml to a concentration of 1×10 -4 mol / l sodium dihydrogen phosphate solution, the pH value of the mixed solution is 10; aged at 105°C for 20 minutes, a red suspension was obtained, which was centrifuged with a centrifugal pump, and then washed 3 times with deionized water. Cubic α-Fe with an average particle size of 35 nm was obtained after drying at ℃ for 1.5 hours. 2 o 3 Particles, the grain size is close to monodisperse, and its TEM picture is shown in Figure 5 .

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Abstract

The invention relates to a nano iron oxide red preparing method, fully mixing crystal converting agent and lye under normal temperature and pressure, then stirring and adding the product obtained by oxidizing soluble trivalent or bivalent ferric salt solution at the same time to form gelatin, then adding in buffer solution, maintaining the pH value of the mixed liquid within 8-12, heating and maintaining the reaction temperature within 85-110 deg.C aging for 5-20minutes, centrifugating turbid liquid by centrifugal pump, washing for 3-5times, drying for 1.5-3hours under 25-50 deg.C, and grinding to obtain single disperse nano alpha-Fe2O3 particles. The particle size can be regulated and controlled within 10-100nm, the distribution even.

Description

technical field [0001] The invention relates to the field of production methods of iron oxide red, in particular to a monodisperse nano-iron oxide red particle α-Fe 2 o 3 method of preparation. Background technique [0002] α-Fe 2 o 3 It is an iron oxide with a stable crystal phase structure. Due to its many excellent properties, it is widely used in the fields of pigments and coatings, catalysts, functional ceramics, magnetic materials, gas sensors, photosensitive materials, cosmetics and biomedicine. α-Fe 2 o 3 After the particle size is nanometerized, many specific physical and chemical properties are produced, such as strong absorption of ultraviolet rays and infrared rays. Since the specific physical and chemical properties of nanoparticles are closely related to the size, shape and internal structure of the particles, how to control the size and shape of nanoparticles has become the focus of preparing nano-iron red particles. [0003] In the reports of scientif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/24
Inventor 樊红雷宋宝珍刘菊花仰振求李巧霞
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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