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Method for synthesizing magnetic layered composite hydroxide

A composite hydroxide and synthesis method technology, which is applied in the field of synthesis of magnetic layered composite hydroxide, can solve problems such as instability, difficulty in preparation of pure crystalline phase LDH, and limitations on the development and utilization of magnetic LDH, and achieve uniform particle size distribution Effect

Active Publication Date: 2009-12-23
NINGXIA MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, pure crystal phase LDH is not easy to prepare, especially special LDHs containing unstable metal cations such as easily hydrolyzed Fe(III) and easily oxidized Fe(II) are not suitable for hydrothermal synthesis, structural reorganization, double powder synthesis and other methods. Nor can it be made under ordinary co-precipitation conditions
Due to the instability of Fe(III) and Fe(II), iron-containing LDHs are difficult to synthesize, process and store, which severely limits the development and utilization of magnetic LDHs.

Method used

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  • Method for synthesizing magnetic layered composite hydroxide
  • Method for synthesizing magnetic layered composite hydroxide

Examples

Experimental program
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Embodiment 1

[0019] Take a certain amount of ferric salt and ferrous salt, in N 2 Press Fe in the atmosphere glove box 2+ / Fe 3+ A molar ratio of 3 is formulated into a certain volume of mixed salt solution, in which FeCl 2 The concentration is 1.50mol·L -1 , FeCl 3 The concentration is 0.50mol·L -1 , sealed and transferred to the synthesis reaction device; in constant flow N 2 -H 2 Add dropwise 2.0mol·L under the protection of mixed gas -1 NaOH solution to pH 6.0-8.0 at the end point, maintain the reaction temperature at 35-70°C by means of agitator and relay; the co-precipitation slurry is crystallized for 45-60 minutes under the same stirring speed, protective gas flow rate and 35-70°C go to N 2 Atmosphere glove box, centrifuge the slurry, discard the centrifugate, and use twice distilled water for the solid phase in N 2 Wash and centrifuge three times under the action of bubbling, then wash with ethanol in the same way to remove water, and finally treat with ether once; the so...

Embodiment 2

[0022] Press Fe 2+ / Fe 3+ A certain amount of ferric salt and ferrous salt is placed in the reaction device with a molar ratio of 2, and the constant speed N 2 -H 2 Mixed gas to remove the air in the system, add a certain amount of double distilled water under the protection of constant flow of nitrogen and hydrogen, stir and dissolve, then add 2.0mol·L dropwise -1 NaOH solution to pH 6.0-8.0 at the end point, maintain the reaction temperature at 35-70°C by means of agitator and relay; the co-precipitation slurry is crystallized for 45-60 minutes under the same stirring speed, protective gas flow rate and 35-70°C go to N 2 Atmosphere glove box, separate the slurry, discard the centrifugate, use twice distilled water for the solid phase N 2 Gas bubbling washing, centrifugation three times, ethanol rinsing to bring out water, then treated with ether; solid phase at 50-70°CN 2 Put it in an atmosphere oven for 12 to 24 hours, dry it in vacuum and seal it up.

[0023] The fer...

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Abstract

The invention relates to a method for synthesizing magnetic layered composite hydroxide, which is characterized by finishing the preparation of mixed salt solution, coprecipitation by adding a precipitator, primary slurry crystallization, slurry separation, washing and drying treatment under the condition of nitrogen-hydrogen protection. The invention adopts the high purity nitrogen-hydrogen constant flow protection and the forward coprecipitation-primary slurry crystallization technology through the entire process of the preparation of mixed salt solution, addition of precipitators, coprecipitation reaction, crystallization and post treatment aiming at the secondary reactions such as Fe(II) and Fe(OH)2 oxidation, Fe(OH)3 decomposition and the like during dynamics processes of layered composite hydroxide such as precipitation, induced precipitation, compounding, crystallization condensation and the like, thereby avoiding the generation of secondary reactions such as oxidation, decomposition, crystal phase conversion and the like of magnetic LDH and preparing a vector LDH which is combined with magnetism and a layered structure and suitable for the synthesis of magnetic targeting sustained and controlled release preparations. The invention is suitable for the synthesis of magnetic targeting sustained and controlled release drug LDH vector and others specially needing intermediate and high purity LDH crystal phase, and has the advantages of high product purity, high realization rate of target stoichiometric ratio, energy consumption saving, no environment pollution, wide application range and the like.

Description

technical field [0001] The invention relates to the technical field of inorganic material composites, in particular to a method for synthesizing magnetic layered composite hydroxides used in magnetically targeted drug delivery systems. Background technique [0002] The magnetic targeted drug delivery system is a new type of drug delivery system that has attracted much attention at home and abroad in recent years. It is traditionally composed of magnetic materials, carrier materials, drugs and other excipients. How to achieve sustained release and targeting in the magnetic targeted drug delivery system The integration of slow-release carrier and guiding material has always been a technical difficulty in this field, which requires the joint participation of slow-release carrier and guiding material. Combining slow-release carrier and guiding material into one is the simplest solution. [0003] Layered double hydroxides (Layered Double Hydroxides, LDH) is an inorganic compound ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K47/02
Inventor 苟国敬鲍凤娟杨建宏
Owner NINGXIA MEDICAL UNIV
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