RU2645007C1 - Method of obtaining composite material - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: use to produce a composite material containing a polymer based on acrylamide or methacrylamide and carbon nanotubes. Essence of invention lies in that the method for producing a composite material based on a polymer and carbon nanotubes includes the following steps: treatment in ultrasound of a solution containing acrylamide or methacrylamide, water or acid, dimethylsulfoxide with fluorinated carbon nanotubes dissolved therein; dilution of the treated solution with water, followed by centrifugation of the diluted solution; deposition of a composite material based on a polymer and carbon nanotubes from a solution in ampoules; dilution of the composite material based on a polymer and carbon nanotubes followed by treatment of the aqueous solution in an ultrasonic bath; filtration of a treated aqueous solution of the composite material based on a polymer and carbon nanotubes, washing and drying.

EFFECT: reduced energy costs and time of producing a composite material with a high yield of the composite material.

5 cl, 1 tbl

Description

FIELD OF TECHNOLOGY

The invention relates to a method for producing a composite material containing a polymer based on acrylamide or methacrylamide and carbon nanotubes, designed to enhance the mechanical properties of composite materials based on epoxy resins, modification of various adhesive compositions to obtain supercapacitors, etc.

BACKGROUND

A known method of producing a nanocomposite material based on polyolefins and carbon nanotubes dispersed by ultrasonic treatment, characterized in that the carbon nanotubes are mechanically triturated in water for 0.5-1 hours with the addition of a water-soluble polymer with a concentration of 0.01-0.1 wt. %, after which the resulting suspension is dispersed by ultrasound for 30 min at a maximum medium temperature of not higher than 70 ° C, followed by applying it to the surface of the polyolefin granules and drying the obtained nanocomposite granules containing up to 0.5 wt. % carbon tubes (RU 2490204 C1, publ. 08/20/2013).

A disadvantage of the known composite material is the high energy consumption and the duration of obtaining the composite material, the inability to obtain carpets of the composite material.

The closest analogue of the claimed invention is a method for replacing fluorine in fluorinated carbon nanotubes by chemical reactions with various reagents, such as amines, amides, amino acids, amino alcohols, etc. (V. N. Habashesku. Covalent functionalization of carbon nanotubes: synthesis, properties and application of fluorinated Derivatives, Review: Advances in Chemistry 80 (8), 2011, pp. 739-760).

The disadvantage of the closest analogue is the high energy consumption and the duration of obtaining the composite material, the stitching of the pipes with polymer chains, for example, when using urea.

SUMMARY OF THE INVENTION

The objective of the claimed group of inventions is to develop a method for producing a composite material based on acrylamide or methacrylamide and carbon nanotubes (AA or MAA) -carbon nanotubes.

The technical result of the claimed group of inventions is to reduce energy consumption and time to obtain a composite material with a high yield of composite material.

The specified technical result is achieved due to the fact that the method of producing a composite material based on a polymer and carbon nanotubes includes the following steps:

a) sonication of a solution containing acrylamide or methacrylamide, water or acid, dimethyl sulfoxide with fluorinated carbon nanotubes dissolved in it;

b) diluting with water the treated solution, followed by centrifugation of the diluted solution;

c) the deposition of a composite material based on a polymer and carbon nanotubes from a solution in ampoules;

d) dilution of the composite material based on polymer and carbon nanotubes, followed by treatment of the aqueous solution in ultrasound;

e) filtering the treated aqueous solution of a composite material based on a polymer and carbon nanotubes, washing and drying.

Single or multilayer fluorinated carbon nanotubes are used.

The concentration of fluorinated carbon nanotubes is 1-2 mg / g.

Additionally, after step d), a composite material based on a polymer and carbon nanotubes is heated at a temperature of 75-80 ° С in the presence of concentrated mineral acids, such as sulfuric, nitric, etc.

Additionally, after step d), a polymer-based composite material and carbon nanotubes are reacted in the presence of alkali and sodium hypochlorite. Apply alkalis containing metals of the first and second groups of the periodic table, such as KOH, NaOH, Ba (OH) ₂ , etc.

DETAILED DESCRIPTION OF THE INVENTION

A method of obtaining a composite material based on a polymer and carbon nanotubes (CNTs) is as follows.

Prepare at room temperature a solution containing 5-7 wt. % acryamide (AA) or methacrylamide (MAA), 1-5 wt. water or 0.1-1 wt. % acid and the rest is dimethyl sulfoxide (DMSO) with fluorinated carbon nanotubes (F-CNTs) dissolved in it, while the concentration of fluorinated carbon nanotubes is 1-2 mg / g. As the acid in the preparation of the above solution, concentrated mineral acids, such as hydrochloric, sulfuric, nitric, etc., are used.

Then, the prepared solution is placed in an ultrasonic concentrator, in which the solution was subjected to sound processing at a frequency of 10 KHz for 20 min, as a result of which fluorine is replaced by AA or MAA to obtain a solution of a composite material polymer (AA or MAA) -NTNT.

Next, the resulting solution of the composite material at room temperature is diluted with water 10 times and subjected to centrifugation at 6000 rpm for 15 minutes As a result of centrifugation, the polymer-CNT is deposited in ampoules.

Then the composite material is diluted with water, the aqueous solution is subjected to treatment in an ultrasonic bath at a frequency of 50 Hz for 10-15 minutes to remove the remaining AA or MAA as well as their polymers and DMSO residues. After that, the treated aqueous solution of the composite material is passed through a 1 micron filter, where the composite material (AA or MAA) - CNTs is filtered off from water (acid to neutral reaction), then washed with acetone and dried in a cabinet at a temperature of 125 ° C. The result is a solid final product in the form of a composite material polymer (AA or MAA) -UNCT.

Then, if necessary, after treatment in an ultrasonic bath, the solution of the MAA-CNT composite material is heated at a temperature of 75-80 ° C in the presence of concentrated mineral acids (sulfuric, perchloric, nitric, etc.) to obtain a composite material polyacrylic acid (PAA) -CNT or interaction with alkali and sodium hypochlorite to obtain a composite material polyvinylamine (PVAM) -CNT.

To obtain the PAK-CNT composite material, the MAA-CNT composite material solution is heated in 100-fold excess of the mass of the composite material with concentrated HCl for 12 hours at 80 ° C. Then the excess acid is washed with water until the solution is neutral. PAK-CNT composite material is precipitated from an aqueous solution by centrifugation at 6 thousand rpm. The resulting precipitate contains about 98% water, then it is filled with anhydrous isopropyl alcohol, in about a 10-fold excess, and water is removed due to the formation of an azeotrope, washing with excess alcohol on a 1 micron filter.

To obtain a PVAM-CNT composite material, an MAA-CNT composite material solution is reacted with a large excess of alkali (100-fold with respect to the composite material) and a small excess of sodium hypochlorite. After that, the excess alkali is washed with water until the solution is neutral, then it is filled with anhydrous isopropyl alcohol in about a 10-fold excess and water is removed due to the formation of an azeotrope, washing with excess alcohol on a 1 micron filter.

Table 1 presents the experimental results of the claimed method.

Thus, the present invention allows to reduce the energy consumption and time of obtaining a composite material with a high yield of composite material, by performing the method at room temperature, in comparison with the closest analogue in which ultrasound treatment is carried out at a temperature above 130 ° C, for example, when using urea .

The invention has been disclosed above with reference to a specific embodiment. Other specialists may be obvious to other embodiments of the invention, without changing its essence, as it is disclosed in the present description. Accordingly, the invention should be considered limited in scope only by the following claims.

Claims (10)

1. A method of producing a composite material based on a polymer and carbon nanotubes, comprising the following steps: a) sonication of a solution containing acrylamide or methacrylamide, water or acid, dimethyl sulfoxide with fluorinated carbon nanotubes dissolved in it; b) diluting with water the treated solution, followed by centrifugation of the diluted solution; c) the deposition of a composite material based on a polymer and carbon nanotubes from a solution in ampoules; d) diluting the composite material based on polymer and carbon nanotubes, followed by treating the aqueous solution in an ultrasonic bath; e) filtering the treated aqueous solution of a composite material based on a polymer and carbon nanotubes, washing and drying. 2. The method according to p. 1, characterized in that apply single-layer or multilayer fluorinated carbon nanotubes. 3. The method according to p. 1, characterized in that the concentration of fluorinated carbon nanotubes is 1-2 mg / g 4. The method according to p. 1, characterized in that in addition, after step d), a composite material based on a polymer and carbon nanotubes is heated at a temperature of 75-80 ° C in the presence of concentrated mineral acids. 5. The method according to p. 1, characterized in that additionally, after step d), the composite material based on the polymer and carbon nanotubes interacts with alkali and sodium hypochlorite.