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Method for preparing diantimony trioxide nano-particles by mechanochemical modification technology

A technology of antimony trioxide and mechanochemistry, applied in chemical instruments and methods, inorganic chemistry, antimony oxide/antimony hydroxide/antimony oxyacid, etc., can solve the problem of high cost, difficult industrial application, and many factors affecting the preparation process and other issues, to achieve the effect of increasing product added value, easy industrial production, and simple process

Pending Publication Date: 2020-04-07
LANZHOU UNIVERSITY OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Regardless of gas phase method or liquid phase method, or conventional chemical methods such as solid phase method, in the preparation of nano Sb 2 o 3 All flame retardants are difficult to be applied industrially due to complex preparation process, high cost and low output.
⑴ Due to nano-Sb 2 o 3 The special effect of particles, it is difficult to disperse in the composite material, especially when the addition amount exceeds 5%, it is difficult to obtain a uniformly dispersed PBT composite material, which greatly limits the comprehensive performance of the composite material and solves the problem of nano-Sb 2 o 3 The dispersion of particles in the PBT matrix material is the main technical problem
⑵Comprehensive performance-to-price ratio is the restriction of nano-Sb 2 o 3 The key to the industrial application of particles, the preparation of nano-Sb by ball milling technology 2 o 3 Although particles have the advantages of simple process and large output, there are many factors affecting the preparation process. Find the best method for preparing multi-size nano-Sb 2 o 3 Particle process conditions, the preparation of size-controllable nanoparticles is also a technical difficulty

Method used

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  • Method for preparing diantimony trioxide nano-particles by mechanochemical modification technology
  • Method for preparing diantimony trioxide nano-particles by mechanochemical modification technology
  • Method for preparing diantimony trioxide nano-particles by mechanochemical modification technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Example 1 A method for preparing nano antimony trioxide particles by a mechanochemical modification method, comprising the following steps:

[0067] (1) Put 10g of micron antimony trioxide, 395g of hard alloy small steel balls and 14mL of distilled water into the stainless steel ball milling tank of a planetary high-energy ball mill, and ball mill for 30 hours at a speed of 300 r / min to obtain nano-Sb 2 o 3 Particles (such as Figure 5 shown).

[0068] ⑵nano-Sb 2 o 3 The particles are often washed with warm deionized water, dried at 90°C for 12 hours, and passed through a 100-mesh metal mesh sieve to obtain nano-Sb 2 o 3 samples (such as Figure 6 (b)).

[0069] (3) Add 5g nano-Sb 2 o 3 Put the sample, 195g of hard alloy small steel balls and 9mL of distilled water into the stainless steel ball milling tank of the planetary high-energy ball mill, and adjust the concentration of the solution in the ball milling tank with hydrochloric acid with a concentration of...

Embodiment 2

[0072] Example 2 A method for preparing nano antimony trioxide particles by a mechanochemical modification method, comprising the following steps:

[0073] ⑴Put 10g of micron antimony trioxide, 405g of hard alloy small steel balls and 16mL of distilled water into the stainless steel ball mill tank of planetary high-energy ball mill, and ball mill for 18 hours at a speed of 500 r / min to obtain nano-Sb 2 o 3 Particles (such as Figure 5 shown).

[0074] ⑵nano-Sb 2 o 3 The particles are often washed with warm deionized water, dried at 110°C for 8 hours, and passed through a 100-mesh metal mesh sieve to obtain nano-Sb 2 o 3 samples (such as Figure 6 (b)).

[0075] (3) Add 5g nano-Sb 2 o 3Put the sample, 205g of hard alloy small steel balls and 11mL of distilled water into the stainless steel ball milling tank of the planetary high-energy ball mill, and adjust the concentration of the solution in the ball milling tank with hydrochloric acid with a concentration of 0.01N o...

Embodiment 3

[0078] Example 3 A method for preparing nanometer antimony trioxide particles by mechanochemical modification, comprising the following steps:

[0079] ⑴Put 10g of micron antimony trioxide, 400g of hard alloy small steel balls and 15mL of distilled water into a stainless steel ball mill tank of a planetary high-energy ball mill, and ball mill for 24 hours at a speed of 400 r / min to obtain nano-Sb 2 o 3 Particles (such as Figure 5 shown).

[0080] ⑵nano-Sb 2 o 3 The particles are often washed with warm deionized water, dried at 100°C for 10 hours, and passed through a 100-mesh metal mesh sieve to obtain nano-Sb 2 o 3 samples (such as Figure 6 (b)).

[0081] (3) Add 5g nano-Sb 2 o 3 Put the sample, 200g of hard alloy small steel balls and 10mL of distilled water into the stainless steel ball milling jar of planetary high-energy ball mill, and adjust the concentration of the solution in the ball milling jar with hydrochloric acid with a concentration of 0.01N or sodium...

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Abstract

The invention relates to a method for preparing diantimony trioxide nano-particles by a mechanochemical modification technology. The method comprises the following steps: (1) mixing and ball-milling micrometer diantimony trioxide, small hard alloy steel balls and distilled water to obtain nano-Sb2O3 particles; (2) washing, drying and sieving the nano-Sb2O3 particles to obtain a nano-Sb2O3 sample;(3) mixing the nano-Sb2O3 sample, small hard alloy steel balls and distilled water, adjusting the pH value, adding hexadecyltrimethylammonium bromide, carrying out ball milling, and cleaning, filtering and drying the obtained mixture to obtain cationic surfactant CTAB modified nano-Sb2O3 particles; (4) adding the cationic surfactant CTAB modified nano-Sb2O3 particles into an ethanol-water solution, and carrying out ultrasonic dispersion so as to obtain cationic surfactant CTAB modified nano-Sb2O3 particles; and (5) mixing and ball-milling the cationic surfactant CTAB modified nano-Sb2O3 particles, a silane coupling agent KH580, small hard alloy steel balls and anhydrous ethanol, and cleaning, filtering and drying the obtained mixture to obtain CTAB and KH580 compounded modified nano-Sb2O3.The method has the advantages of simple process, high yield, high operability, and easiness in realization of industrial production.

Description

technical field [0001] The invention relates to the technical field of nanometer metal oxides, in particular to a method for preparing nanometer antimony trioxide particles by a mechanochemical modification method. Background technique [0002] High efficiency, low toxicity and environmental protection are the research and development directions of flame retardants. Compared with micron flame retardants, nano flame retardants have the characteristics of quantum size effect, small size effect and surface effect. Due to the small particle size (less than 100nm ), easy to disperse, when used as a flame retardant for polymer materials, it has less filling amount and good compatibility, which can enhance the flame retardancy and mechanical properties of materials, and has ideal effects in the use of polymer materials. Therefore, the development and application of new nano-flame retardants has gradually become an important development direction in the field of flame retardants. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00B02C17/08B02C17/10
CPCB02C17/08B02C17/10C01G30/005C01P2002/72C01P2002/82C01P2004/51C01P2004/62C01P2004/64
Inventor 牛磊王书涛苏加强刘烨
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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