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Preparation method of silicone oil nano iron oxide suspension

A nano-iron oxide and suspension technology, applied in iron oxide, iron oxide/iron hydroxide, nanotechnology, etc., can solve the high pressure resistance requirements of reaction equipment, limit the use of iron oxide suspension, performance and performance stability reduce the problem, achieve good particle size distribution and temperature applicability, wide range of temperature applicability, and increase the effect of reaction temperature

Active Publication Date: 2015-01-07
CHONGQING YUNTIANHUA HIGH END NEW MATERIALS DEV CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of nano-iron oxide by chemical method mainly uses water as a solvent, and is prepared by precipitation method. For example, in the patent CN10092794, it is mentioned that a precipitation method is used to generate nano-iron oxide yellow, and then the nano-iron oxide yellow is calcined to prepare nano-iron oxide. Although it has the characteristics of simple process, low pollution, low energy consumption and short cycle, it is the same as all other methods that require calcination to prepare nano-iron oxide. It cannot avoid and solve the agglomeration phenomenon that occurs during the calcination process. The occurrence of this phenomenon will directly The particle size of nano-iron oxide becomes larger, the particle size distribution becomes wider, and the performance and performance stability are reduced.
At the same time, for other preparation methods that do not use calcination methods, such as the hydrothermal method, there are disadvantages such as high temperature and high pressure required for the production process, high requirements for the pressure resistance of the reaction equipment, and difficulty in achieving industrial scale-up.
Since the reaction system is an aqueous phase, the obtained suspension is also an aqueous phase suspension. Due to the low viscosity of water and the narrow operating temperature range, the use of iron oxide suspension is limited.

Method used

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Examples

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preparation example Construction

[0027] The preparation method of silicone oil nano iron oxide suspension of the present invention comprises the following steps:

[0028] a. Configure the reaction system with modified silicone oil, oil-soluble dispersant and ferric salt;

[0029] b. Add ferric salt to modified silicone oil, add oily dispersant according to the mass fraction of 0.1% to 3%, stir and ultrasonically disperse for more than 2 hours, and prepare a suspension of 0.01 mol / L-0.1 mol / L; Trivalent Iron salt generally adopts ferric chloride or ferric nitrate, etc.;

[0030] c. Under the conditions of 100-180°C and stirring, adjust the pH of the suspension obtained in step b to 8-11, and stir for 2-5 hours; in step b and step c, the stirring is mechanical stirring, and the stirring rate is 100rpm- 3000rpm; the preferred stirring rate is 2000rpm;

[0031] d. The reacted liquid in step c is subjected to static separation, the aqueous phase solution is removed, and the separated silicone oil / nanometer i...

Embodiment 1

[0050] The preparation method of the silicone oil nano iron oxide suspension of the present embodiment comprises the following steps:

[0051] a. Configure the reaction system with modified silicone oil, oil-soluble dispersant and ferric salt; the modified silicone oil in this embodiment is polyether modified silicone oil, the oil-soluble dispersant is oleic acid diacetamide, and the ferric salt is ferric nitrate;

[0052] b. Add the ferric salt to the modified silicone oil, add the oily dispersant according to the mass fraction of 2%, stir and ultrasonically disperse for more than 2 hours, generally stir for 4-5 hours, and prepare a suspension of 0.05 mol / L;

[0053] c. Under the conditions of heating the oil bath to 150°C and stirring, the pH of the suspension obtained in step b was adjusted to 10 by adding sodium hydroxide solution, and the reaction was stirred for 3 hours; in step b and step c, the stirring was mechanical stirring, and the stirring rate was 2000rpm;

...

Embodiment 2

[0057] The preparation method of the silicone oil nano iron oxide suspension of the present embodiment comprises the following steps:

[0058] a. Configure the reaction system with modified silicone oil, oil-soluble dispersant and ferric salt; the modified silicone oil in this example is amino silicone oil, the oil-soluble dispersant is AEO3 or SDBS, fatty alcohol polyoxyethylene ether / dodecylbenzenesulfonate Sodium acid, the ferric salt is ferric chloride;

[0059] b. Add ferric salt to modified silicone oil, add oily dispersant at 0.1% by mass fraction, stir and ultrasonically disperse for more than 2 hours, generally 4-5 hours, and prepare a suspension of 0.01 mol / L;

[0060] c. Under the conditions of heating the oil bath to 100°C and stirring, the pH of the suspension obtained in step b was adjusted to 8 by adding ammonia water, and the reaction was stirred for 5 hours; in step b and step c, the stirring was mechanical stirring, and the stirring rate was 3000rpm;

[0...

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Abstract

The invention discloses a preparation method of silicone oil nanocrystalline iron oxide suspension. Modified silicone oil, oil soluble dispersing agent and trivalent iron salt or divalent iron salt form a reaction system; by taking a modified silicone oil system as a reaction system of ferric oxide, the prepared nano iron oxide is not agglomerated easily; the suspension has good precipitation resistance, good temperature stability and wide temperature application range and does not settle easily; the particle size of the silicone oil nanocrystalline iron oxide suspension is distributed between 20nm and 200nm, and relatively good particle size distribution and temperature adaptability are realized; since the boiling point of the modified silicone oil system is much higher than that of a water-phase system, the reaction temperature can be increased, and the reactant activity can be improved; the reaction does not need to be carried out under a high pressure, and thus high-pressure equipment is not required; and the raw materials of the method are easily available and are low in cost and the preparation technology is simple.

Description

technical field [0001] The invention relates to a preparation method of nano iron oxide suspension, in particular to a preparation method of silicone oil nano iron oxide suspension. Background technique [0002] Nano iron oxide (Fe 2 o 3 ) Different forms of iron oxide, such as α-type iron oxide, δ-type iron oxide, etc., can be prepared by controlling the synthesis process. Due to the advantages of non-toxic, harmless, cheap, and good chemical stability, iron oxide is widely used in fields such as rubber, ceramics, pigments, and building materials. At the same time, due to the advantages of small size effect, surface effect, quantum size effect and macroscopic quantum tunneling effect, nano-iron oxide has great advantages over other materials in terms of tinting strength, transparency and chroma, so it is widely used in printing ink industry and papermaking industry. Industries have a wide range of needs and applications. Furthermore, due to the existence of many potenti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/06B82Y30/00
Inventor 戴曛晔江林叶兴福
Owner CHONGQING YUNTIANHUA HIGH END NEW MATERIALS DEV CO LTD