CN111085165A

CN111085165A - Preparation method of surface mineralized diatom biomineralized silicon

Info

Publication number: CN111085165A
Application number: CN201811234357.0A
Authority: CN
Inventors: 冯超; 穆愈之; 陈西广
Original assignee: Ocean University of China
Current assignee: Ocean University of China
Priority date: 2018-10-23
Filing date: 2018-10-23
Publication date: 2020-05-01

Abstract

The invention discloses a preparation method of surface mineralized diatom biomineralized silicon, namely a preparation method of metal ion modified diatom biomineralized silicon constructed through hydrothermal reaction. Can be used for medical biomaterials and drug carriers, and has good research and development application prospects.

Description

Preparation method of surface mineralized diatom biomineralized silicon

Technical Field

The invention belongs to a preparation method of surface mineralized diatom biomineralized silicon in the chemical field.

Background

Diatoms, a unicellular photosynthetic algae, of the marine diatom type over 10 million, have cell walls composed of silica, are called frustules, and are also called biomineralization. The frustules have a highly ordered pore structure and a layered pore organization, have unique mechanical properties, molecular transport characteristics and optical properties, and are high-quality resources which have high activity, can be cultured in a large scale and are environment-friendly. The diatom biomineralization silicon has great application potential in the aspects of hemostasis, bone tissue repair and the like as a biological material. In various reactions of organisms, different ions can generate various promotion reactions such as calcium ions promoting blood coagulation and bone tissue generation, strontium ions promoting angiogenesis and the like. The diatom biomineralization silicon mainly comprises silicon dioxide, and the diatom biomineralization silicon is stable in chemical property, so that chemical modification of the diatom biomineralization silicon has certain difficulty. At present, the diatom biomineralization silicon mainly has two types of loading modes to metal ions: 1. physical adsorption, namely adsorbing the metal ion salt solution through a porous structure on the surface of the diatom biomineralization silicon. 2. Biomineralization, diatoms can replace silicon with certain metal ions such as titanium in a culture environment to construct cell walls, and therefore diatom biomineralization silicon containing other metal elements is obtained. The two modes have certain defects, and ions adsorbed physically have weak binding force, so that rapid local large-amount release is easily caused, and certain biological toxicity is caused; the biomineralization mode has low efficiency and high cost, and has more limitation on the types of metal ions. According to the invention, the diatom biomineralization silicon is loaded with metal ions in a chemical modification mode through a hydrothermal reaction, the loading capacity of the metal ions on the diatom biomineralization silicon can be increased on the premise of not influencing the self structure of the diatom biomineralization silicon, the metal ions can be slowly released from the diatom biomineralization silicon, a large amount of surface mineralized diatom biomineralization silicon loaded with various metal ions can be constructed, and the diatom biomineralization silicon has very important theoretical significance and clinical application value.

Disclosure of Invention

The invention aims to provide a preparation method of biomineralized silicon with surface mineralized diatoms to make up for the defects of the prior art.

The invention takes diatom biomineralization silicon and various water-soluble metal salts as raw materials, prepares the surface biomineralization silicon by hydrothermal reaction, and comprises the following steps:

the diatom biomineralization silicon is uniformly dispersed in a reaction solution, and then a metal salt solution and an alkaline compound are added, wherein the metal salt added per milligram of diatom biomineralization silicon is 0.1 mu M-0.1 mM, and the mass volume ratio of the added alkaline compound in the system is 0.01% -40%. And (3) uniformly stirring the mixture, putting the mixture into a hydrothermal reaction kettle, and reacting at the temperature of 90-220 ℃ for 1-48 hours. And washing and drying the product after the reaction for multiple times by using deionized water to obtain the surface mineralized diatom biomineralization silicon.

The method has the advantages of simple and convenient operation, simple preparation technology process, low manufacturing cost and the like, the mineralization degree can be adjusted by changing the feed ratio and the reaction time so as to adjust the loading capacity of metal ions, and the formed surface mineralized diatom biomineralization silicon has complete appearance and clear surface aperture structure. The invention has the important significance that the formed surface mineralized diatom biomineralized silicon can increase the loading capacity of metal ions on the surface of the diatom biomineralized silicon, avoids the metal ions from being released from the diatom biomineralized silicon too fast, can construct a large amount of diatom biomineralized silicon loaded with various metal ions, and has good development and application potentials. The invention is further explained below with reference to the figures and examples.

Drawings

FIG. 1 is a scanning electron microscope image of the surface copper mineralized diatom biomineralized silicon.

FIG. 2 is an element energy spectrum of the surface copper mineralized diatom biomineralized silicon.

Example 1

30 mg of purified diatom biomineralization silicon is weighed and dispersed in 3 mL of deionized water. 0.563 mg of copper nitrate and 0.3 mg of sodium hydroxide were added thereto, and mixed well at room temperature. And adding the reaction solution into a hydrothermal reaction kettle, reacting for 12 hours at 180 ℃, fully washing a product by using deionized water, and drying at 70 ℃ to obtain the surface copper element mineralized diatom biomineralized silicon.

Example 2

100 mg of purified diatom biomineralization silicon is weighed and dispersed in 20 mL of 1: 1 mixture of deionized water and ethanol. 1.11 g of calcium chloride and 5 ml of ammonia water were added thereto, and mixed at room temperature. And adding the reaction solution into a hydrothermal reaction kettle, reacting for 48 hours at 90 ℃, fully washing a product by using deionized water, and drying at 70 ℃ to obtain the surface calcium mineralized diatom biomineralized silicon.

Example 3

70 mg of purified diatomic biomineralization silicon was weighed out and dispersed in 15 mL of deionized water. 56.7mg of calcium chloride and 6mg of sodium hydroxide were added thereto, and mixed well at room temperature. And adding the reaction solution into a hydrothermal reaction kettle, reacting for 1 hour at 200 ℃, fully washing a product by using deionized water, and drying at 70 ℃ to obtain the surface calcium mineralized diatom biomineralized silicon.

Claims

1. a preparation method of surface mineralized diatom biomineralized silicon, it is characterized in that utilizing hydrothermal method to make diatom biomineralized silicon surface react with metal ions under alkaline conditions, make diatom biomineralized silicon Various metal silicates are formed on the surface to obtain surface mineralized diatom biomineralized silicon. The specific steps are as follows: uniformly disperse the diatom biomineralized silicon in the reaction solution, and then add a metal salt solution and an alkaline compound, wherein The metal salt put in per milligram of diatom biomineralized silicon is 0.1 μM ~ 0.1 mM, the mass volume ratio of the added basic compound in the system is 0.01% ~ 40%, the mixture is stirred evenly, and placed in a hydrothermal reactor , the reaction is carried out at 90 ~ 220 ° C for 1 ~ 48 hours, and the product after the reaction is washed with deionized water for several times and dried to obtain the surface mineralized diatom biomineralized silicon.

2. the preparation method of surface mineralized diatom biomineralized silicon according to claim 1, is characterized in that used diatom biomineralized silicon source can be the diatom and Diatomaceous earth; the reaction solution can be deionized water or a mixture of deionized water and ethanol; basic compounds include ammonia water, sodium hydroxide, etc.; metal salts used include copper salts, calcium salts, magnesium salts, strontium salts, etc. .

3. The application of the surface mineralized diatom biomineralized silicon according to claim 1 includes the following aspects: fields such as food processing, biomedicine, cosmetics, textile processing, health care products and the like.