CN111333912A - Preparation method of functional filler - Google Patents

Abstract

The invention provides a preparation method of a functional filler, which comprises the following steps: dissolving attapulgite in a certain amount of water for ultrasonic treatment, adding a dispersing agent, stirring, adjusting the pH value of the system, settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite; dissolving the purified attapulgite in a certain amount of water, and adding a surfactant for reaction; and after the reaction is finished, carrying out suction filtration, washing, drying and sieving on the product to obtain the functional filler. The functional filler prepared by the method has the advantages of obviously improved dispersity, increased thermal weight loss rate, improved compatibility with organic polymer resin, certain flame retardance and wide application in reinforcement or synergistic flame retardant modification of polymer materials.

Description

Preparation method of functional filler

Technical Field

The invention provides a preparation method of a functional filler, belonging to the field of preparation of inorganic reinforced materials.

Technical Field

Attapulgite is an aqueous magnesium-rich aluminosilicate mineral with a special layer chain-like molecular structure, and the microstructure of the attapulgite comprises 3 layers: (1) the basic structural unit is a rod-shaped or fibrous monocrystal, the diameter of the rod-shaped monocrystal is 0.01 mu m in order of magnitude, and the length of the rod-shaped monocrystal can reach 0.1-1 mu m; (2) a rod crystal bundle formed by parallelly gathering single crystals; (3) the particle size of each aggregate formed by stacking bundles of crystals (including rod crystals) together is usually in the order of 0.01 to 0.1 mm. The rod crystal is a natural one-dimensional inorganic nano material, and because the attapulgite has large specific surface area, high surface activity and easy agglomeration, and the surface contains a large amount of silicon hydroxyl, the affinity of the rod crystal with organic high polymers is poor.

Disclosure of Invention

The invention aims to overcome the defects, and aims to purify and organically modify the surface of the attapulgite before use, so that the functional filler is provided, the product has good dispersibility, the thermal weight loss rate is increased, the compatibility with organic polymer resin is improved, and the functional filler has certain flame retardance and can be widely applied to the reinforcement or synergistic flame retardant modification of polymer materials.

Another object of the present invention is to provide a method for preparing the above functional filler.

The technical solution for realizing the purpose of the invention is as follows: firstly, purifying attapulgite, and then organically modifying the purified attapulgite to obtain a product, wherein the method comprises the following steps:

(1) dissolving attapulgite in a certain amount of water, performing ultrasonic treatment, adding dispersant, stirring, and regulating body

Is pH; and then settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain the purified attapulgite.

(2) Dissolving the purified attapulgite in a certain amount of water, and adding a surfactant for reaction; and after the reaction is finished, carrying out suction filtration, washing, drying and sieving on the product to obtain the functional filler.

In the invention, the dispersant is any one of sodium hexametaphosphate, sodium pyrophosphate or polyethylene glycol 200, and the dosage of the dispersant is 1-5% of the mass of the attapulgite;

in the invention, the pH value is 3-7;

in the invention, the surfactant is any one of sodium stearate, octadecyl trimethyl ammonium chloride or titanate coupling agent NDZ-311, and the amount of the coupling agent is 1-5% of the mass of the purified attapulgite;

compared with the prior art, the invention has the advantages that: the functional filler has the advantages of obviously improved dispersibility, increased thermal weight loss rate, improved compatibility with organic polymer resin and certain flame retardance.

Detailed Description

The invention relates to a preparation method of a functional filler, which comprises the following specific steps:

(1) weighing a certain amount of attapulgite, dissolving the attapulgite in a proper amount of water, carrying out ultrasonic treatment for 8-20 minutes, adding a dispersing agent with the mass of 1-5% of an inorganic filler, fully and uniformly stirring at 60-90 ℃ for 0.5-2.5 hours, adjusting the pH of a system to 3-7 by using 0.5 mol/L hydrochloric acid, then settling the solution, decanting an upper suspension, centrifuging, washing and drying to obtain the purified attapulgite.

(2) Dissolving the purified attapulgite in a certain amount of water, adding 1-5% of surfactant based on the mass of the purified attapulgite, reacting for 1-3 hours, and after the reaction is finished, performing suction filtration, washing, drying, grinding and sieving (200 meshes and 1000 meshes) on the product to obtain the functional filler;

example 1

(1) Weighing 80 g of attapulgite, dissolving the attapulgite in 300 ml of water, carrying out ultrasonic treatment for 8 minutes, adding 4.0 g of sodium pyrophosphate, fully and uniformly stirring at 90 ℃ for 0.5 hour, adjusting the pH of the system to 6-7 by using 0.5 mol/L hydrochloric acid, then settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite;

(2) dissolving 60 g of purified attapulgite in 300 ml of water, adding 3.0 g of octadecyl trimethyl ammonium chloride, reacting for 3 hours, and performing suction filtration, washing, drying, grinding and sieving (200 meshes) on a product to obtain a functional filler;

example 2

(1) Weighing 80 g of attapulgite, dissolving the attapulgite in 300 ml of water, carrying out ultrasonic treatment for 20 minutes, adding 0.8 g of sodium pyrophosphate, fully and uniformly stirring at 60 ℃ for 1 hour, adjusting the pH of the system to 4-5 by using 0.5 mol/L hydrochloric acid, settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite;

(2) dissolving 60 g of purified attapulgite in 300 ml of water, adding 0.6 g of sodium stearate, reacting for 2 hours, and performing suction filtration, washing, drying, grinding and sieving (400 meshes) on a product to obtain a functional filler;

example 3

(1) Weighing 80 g of attapulgite, dissolving the attapulgite in 300 ml of water, carrying out ultrasonic treatment for 15 minutes, adding 1.6 g of sodium hexametaphosphate, fully and uniformly stirring at 80 ℃ for 2.5 hours, adjusting the pH of a system to 3-4 by using 0.5 mol/L hydrochloric acid, then settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite;

(2) dissolving 60 g of purified attapulgite in 300 ml of water, adding 1.8 g of octadecyl trimethyl ammonium chloride, reacting for 3 hours, and performing suction filtration, washing, drying, grinding and sieving (1000 meshes) on a product to obtain a functional filler;

example 4

(1) Weighing 80 g of attapulgite, dissolving the attapulgite in 300 ml of water, carrying out ultrasonic treatment for 15 minutes, adding 2.4 g of polyethylene glycol 200, fully and uniformly stirring at 70 ℃ for 0.5 hour, adjusting the pH of the system to 5-6 by using 0.5 mol/L hydrochloric acid, then settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite;

(2) dissolving 60 g of purified attapulgite in 300 ml of water, adding 1.2 g of titanate coupling agent NDZ-311, reacting for 2 hours, and performing suction filtration, washing, drying, grinding and sieving (600 meshes) on a product to obtain a functional filler;

although the present invention has been described in detail with reference to the preferred embodiments, it is not to be construed as limiting the invention thereto. Various modifications and alterations may be made by those skilled in the art without departing from the spirit and scope of the invention. The scope of the invention should therefore be seen as that defined by the appended claims.

Claims (2)

1. A process for preparing functional filler features that the novel clay has high dispersity, high thermal weight loss rate, high compatibility with organic high-molecular resin and flame-retarding nature.

2. The method for preparing the functional filler according to claim 1, wherein the preparation process comprises the following steps:

(1) dissolving attapulgite in a certain amount of water for ultrasonic treatment, adding a dispersant, stirring, and adjusting the pH value of the system; then settling the solution, decanting the upper suspension, centrifuging, washing and drying to obtain purified attapulgite;

(2) dissolving the purified attapulgite in a certain amount of water, and adding a surfactant for reaction; and after the reaction is finished, carrying out suction filtration, washing, drying and sieving on the product to obtain the functional filler.