阅读说明：本技术 一种二氧化钛纳米材料及其制备方法 (Titanium dioxide nano material and preparation method thereof ) 是由 高锋 张影 程汝舟 刘可 于 2021-01-15 设计创作，主要内容包括：本发明属于二氧化钛纳米材料术领域,特别涉及一种二氧化钛纳米材料,其可采用如下步骤制备而成：S1,向盐酸溶液中加入钛酸异丙酯,超声分散溶解,制得前驱体溶液；S2,向所述前驱体溶液中加入锐钛矿二氧化钛颗粒；S3,接着步骤S2制得的溶液中加入氯化钠,并将溶液转移至高压反应釜中于150～200℃条件下反应,反应生成的白色沉淀即为二氧化钛纳米材料。该制备方法具有制备过程简单、环境友好可控等优点,本发明的产物具有较大的比表面积,为物理化学等领域的发展提供了一种新型的具有仿生结构的纳米材料。(The invention belongs to the technical field of titanium dioxide nano materials, and particularly relates to a titanium dioxide nano material which can be prepared by the following steps: s1, adding isopropyl titanate into the hydrochloric acid solution, and performing ultrasonic dispersion and dissolution to obtain a precursor solution; s2, adding anatase titanium dioxide particles into the precursor solution; s3, adding sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting at the temperature of 150-200 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material. The preparation method has the advantages of simple preparation process, environmental friendliness, controllability and the like, the product of the invention has larger specific surface area, and a novel nano material with a bionic structure is provided for the development of the fields of physical chemistry and the like.)

1. A titanium dioxide nanomaterial characterized by: the titanium dioxide nano material has the appearance of a sea cucumber-shaped bionic structure.

2. The titanium dioxide nanomaterial of claim 1, wherein: the sea cucumber-shaped bionic structure consists of a main body titanium dioxide nanorod and an accessory titanium dioxide nanorod;

the appendage titanium dioxide nano rod is attached to the main body titanium dioxide nano rod;

the diameter of the main titanium dioxide nanorod is 60-100 nm, and the length of the main titanium dioxide nanorod is 300-800 nm;

the diameter of the attached titanium dioxide nano rod is 20-50 nm, and the length of the attached titanium dioxide nano rod is 80-300 nm;

5-80 attached titanium dioxide nanorods are attached to any one of the main titanium dioxide nanorods.

3. The titanium dioxide nanomaterial according to claim 2, characterized in that: the diameter of the main titanium dioxide nanorod is 80-100 nm, and the length of the main titanium dioxide nanorod is 300-600 nm;

the diameter of the attached titanium dioxide nano rod is 30-50 nm, and the length of the attached titanium dioxide nano rod is 80-200 nm;

5-50 attached titanium dioxide nanorods are attached to any one of the main titanium dioxide nanorods.

4. A method for preparing the titanium dioxide nano material as claimed in any one of claims 1 to 3, which comprises the following steps:

s1, adding isopropyl titanate into the hydrochloric acid solution, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

s2, adding anatase titanium dioxide particles into the precursor solution;

s3, adding sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle to react at the temperature of 150-200 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material as claimed in any one of claims 1-3.

5. The method for producing a titanium dioxide nanomaterial according to claim 4, characterized in that: in the step S1, the mass fraction of the hydrochloric acid solution is 20-22%.

6. The method for producing a titanium dioxide nanomaterial according to claim 5, characterized in that: in step S1, 1 to 1.5 parts by volume of isopropyl titanate is added to 80 parts by volume of hydrochloric acid solution.

7. The method for producing a titanium dioxide nanomaterial according to claim 4, characterized in that: in step S2, the particle size of the anatase titanium dioxide particles is 100 to 200 nm.

8. The method for producing a titanium dioxide nanomaterial according to claim 4, characterized in that: in step S2, the anatase titanium dioxide particles are added in an amount of 3-6 mg.

9. The method for producing a titanium dioxide nanomaterial according to claim 4, characterized in that: in step S3, the addition amount of the sodium chloride is 8-12 mg.

10. The method for producing a titanium dioxide nanomaterial according to claim 4, characterized in that: in step S3, the reaction temperature is 160-180 ℃ and the reaction time is 20-50 min.

Technical Field

The invention belongs to the technical field of titanium dioxide nano materials, and particularly relates to a titanium dioxide nano material and a preparation method thereof.

Background

Titanium dioxide is a good inorganic semiconductor material, and is widely applied to the fields of perovskite solar cells, biosensing technology, catalysis technology, energy storage technology and the like at present. The preparation of titanium dioxide and the morphology thereof have been the hot points of scientific research.

In the current scientific research, many stable synthetic methods, such as hydrothermal synthesis method, solvothermal synthesis method, electrospinning synthesis method, etc., have been developed for the microstructure of nano titanium dioxide and its formation mechanism. The titanium dioxide can present different morphologies on the nanometer scale, such as titanium dioxide nanowires, nanospheres, nanoparticles, nanoarrays, and the like. These results indicate that the controllable preparation of the nano titanium dioxide material can be realized by controlling the synthesis conditions.

Although the synthesis method of titanium dioxide is mature day by day, a new report of novel titanium dioxide with a bionic morphology is provided, and the synthesis of nano titanium dioxide with a certain bionic structure becomes a challenge of the current research.

Disclosure of Invention

In order to solve the problems, the invention provides a titanium dioxide nano material, breaks through the single appearance of the traditional titanium dioxide, has larger specific surface area, and provides a novel nano material with a bionic structure for the development of the fields of physical chemistry and the like; the invention also provides a preparation method of the titanium dioxide nano material, which has the characteristics of simplicity, environmental friendliness, controllability and the like.

The invention is realized by adopting the following technical scheme:

a titanium dioxide nano material has the appearance of a sea cucumber-shaped bionic structure.

As further description, the sea cucumber-like bionic structure consists of a main body titanium dioxide nanorod and an appendage titanium dioxide nanorod;

as a further description, the appendage titanium dioxide nanorods are attached to the host titanium dioxide nanorods;

as further description, the diameter of the main titanium dioxide nanorod is 60-100 nm;

as a further description, the diameter of the main titanium dioxide nanorod is 80-100 nm;

as further description, the length of the main titanium dioxide nanorod is 300-800 nm;

as a further description, the length of the main titanium dioxide nanorod is 300-600 nm;

as further description, the diameter of the attached titanium dioxide nano-rod is 20-50 nm;

as a further description, the diameter of the attached titanium dioxide nano-rod is 30-50 nm;

as further description, the length of the attached titanium dioxide nanorod is 80-300 nm;

as a further description, the length of the attached titanium dioxide nanorod is 80-200 nm;

as a further description and a preferred protection scheme, 5-80 attached titanium dioxide nanorods are attached to any one of the main titanium dioxide nanorods;

as a further description and a preferred protection scheme, in the sea cucumber-like bionic structure, 5-50 attached titanium dioxide nanorods are attached to any one main titanium dioxide nanorod;

as a further description and a preferred protection scheme, in the sea cucumber-like bionic structure, 10-30 attached titanium dioxide nanorods are attached to any one main titanium dioxide nanorod;

as a further description and a preferred protection scheme, in the sea cucumber-shaped bionic structure, 15-20 attached titanium dioxide nanorods are attached to any one main titanium dioxide nanorod.

A preparation method for preparing the titanium dioxide nano material comprises the following steps:

s1, adding isopropyl titanate into the hydrochloric acid solution, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

preferably, in the step S1, the mass fraction of the hydrochloric acid solution is 20-22%;

in a further preferable scheme, the hydrochloric acid solution is prepared from 1 part by volume of distilled water and 1-1.2 parts by volume of concentrated hydrochloric acid with a mass percent concentration of 36-37%;

in a further preferable scheme, in the step S1, 1 to 1.5 parts by volume of isopropyl titanate is added to 80 parts by volume of hydrochloric acid solution;

s2, adding anatase titanium dioxide particles into the precursor solution;

preferably, in step S2, the particle size of the anatase titanium dioxide particles is 100 to 200 nm;

preferably, in step S2, the addition amount of the anatase titanium dioxide particles is 3 to 6 mg;

s3, adding sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting at the temperature of 150-200 ℃, wherein white precipitates generated by the reaction are the titanium dioxide nano material;

preferably, the purity of the sodium chloride is AR, and after the sodium chloride solution is added into the solution, the released chloride ions have strong electronegativity and can induce the titanium dioxide to grow in a multi-stage structure form at high temperature;

preferably, in the step S3, the adding amount of the sodium chloride is 8-12 mg; when the content of sodium chloride is too high, a salt effect is generated to accelerate the dissolution of isopropyl titanate, so that the reaction process is not easy to control;

in a preferable scheme, in the step S3, the reaction temperature in the high-pressure reaction kettle is 160-180 ℃;

preferably, in the step S3, the reaction time in the high-pressure reaction kettle is 20-50 min.

The invention has the beneficial effects that:

1. the invention provides a novel titanium dioxide nano material with a novel material bionic morphology for the fields of physical chemistry and the like, breaks through the traditional single morphology of titanium dioxide, has a larger specific surface area, and provides a novel nano material with a bionic structure for the development of the fields of physical chemistry and the like.

2. The preparation method of the titanium dioxide nano material has the advantages of simple preparation process, environmental friendliness, controllability and the like.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.

FIG. 1 is a scanning electron microscope image of a titania nanomaterial of example 1 of the present invention.

FIG. 2 is a scanning electron microscope image of the titanium dioxide nanomaterial of example 2 of the present invention.

FIG. 3 is an X-ray diffraction pattern of the titanium dioxide nanomaterial of example 2.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.

Example 1

A preparation method of titanium dioxide nano material comprises the following steps:

s1, adding 1.5mL of isopropyl titanate into 80mL of prepared hydrochloric acid solution in parts by volume, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

preferably, the hydrochloric acid solution is prepared from 1 part by volume of distilled water and 1.1 part by volume of concentrated hydrochloric acid with the mass percent concentration of 37%;

s2, adding 5mg of anatase titanium dioxide particles with the particle size of 100-200 nm into the precursor solution;

s3, adding 10mg of sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting for 30min at 180 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material.

Example 2

A preparation method of titanium dioxide nano material comprises the following steps:

s1, adding 1.3mL of isopropyl titanate into 80mL of prepared hydrochloric acid solution in parts by volume, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

preferably, the hydrochloric acid solution is prepared from 1 part by volume of distilled water and 1.1 part by volume of concentrated hydrochloric acid with the mass percent concentration of 37%;

s2, adding 3mg of anatase titanium dioxide particles with the particle size of 100-200 nm into the precursor solution;

s3, adding 11mg of sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting for 45min at 160 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material.

Example 3

A preparation method of titanium dioxide nano material comprises the following steps:

s1, adding 1.2mL of isopropyl titanate into 80mL of hydrochloric acid solution with the mass fraction of 21% in parts by volume, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

s2, adding 4mg of anatase titanium dioxide particles with the particle size of 100-200 nm into the precursor solution;

s3, adding 12mg of sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting for 50min at 150 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material.

Example 4

A preparation method of titanium dioxide nano material comprises the following steps:

s1, adding 1.4mL of isopropyl titanate into 80mL of hydrochloric acid solution with the mass fraction of 22% in parts by volume, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

preferably, the hydrochloric acid solution is prepared from 1 part by volume of distilled water and 1-1.1 parts by volume of concentrated hydrochloric acid with the mass percentage concentration of 37%;

s2, adding 5mg of anatase titanium dioxide particles with the particle size of 100-200 nm into the precursor solution;

s3, adding 10mg of sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting for 20min at 180 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material.

Example 5

A preparation method of titanium dioxide nano material comprises the following steps:

s1, adding 1mL of isopropyl titanate into 80mL of hydrochloric acid solution with the mass fraction of 20% in parts by volume, and performing ultrasonic dispersion and dissolution to obtain a precursor solution;

s2, adding 4mg of anatase titanium dioxide particles with the particle size of 100-200 nm into the precursor solution;

s3, adding 12mg of sodium chloride into the solution prepared in the step S2, transferring the solution into a high-pressure reaction kettle, and reacting for 30min at 200 ℃, wherein the white precipitate generated by the reaction is the titanium dioxide nano material.

The titanium dioxide nano material prepared in the embodiment 1-5 has the appearance of a sea cucumber-like bionic structure.

Fig. 1 is a scanning electron microscope image of a titania nanomaterial of example 1 of the present invention, and fig. 2 is a scanning electron microscope image of a titania nanomaterial of example 2 of the present invention.

As can be seen from fig. 1 to 2, the titanium dioxide nanomaterials prepared in examples 1 to 2 have sea cucumber-like biomimetic structures with substantially the same shapes and are composed of two types of titanium dioxide nanorods, for convenience of description, a titanium dioxide nanorod with a long length in the sea cucumber-like biomimetic structure is defined as a main titanium dioxide nanorod, and a titanium dioxide nanorod with a short length in the sea cucumber-like biomimetic structure is defined as an appendage titanium dioxide nanorod.

FIG. 1 shows a titanium dioxide nanomaterial prepared in example 1, which has a sea cucumber-like bionic structure; the diameter of the main titanium dioxide nanorod is 80-100 nm; the length of the main titanium dioxide nanorod is 300-800 nm; the diameter of the attached titanium dioxide nano-rod is 30-50 nm; the length of the attached titanium dioxide nano-rod is 100-300 nm;

in the titanium dioxide nanomaterial prepared in the embodiment 1, in the sea cucumber-shaped bionic structure, 5-50 attached titanium dioxide nanorods are attached to one main titanium dioxide nanorod; or 10-30 attached titanium dioxide nanorods are attached to one main titanium dioxide nanorod; or 15-20 attached titanium dioxide nanorods are attached to one main titanium dioxide nanorod.

FIG. 2 is a titanium dioxide nanomaterial prepared in example 2, which has a sea cucumber-like bionic structure; the diameter of the main titanium dioxide nanorod is 60-100 nm; the length of the main titanium dioxide nanorod is 300-600 nm; the diameter of the attached titanium dioxide nano-rod is 20-50 nm; the length of the attached titanium dioxide nano-rod is 80-200 nm;

in the titanium dioxide nanomaterial prepared in the embodiment 2, in the sea cucumber-shaped bionic structure, 10-30 attached titanium dioxide nanorods are attached to one main titanium dioxide nanorod; or 15-20 attached titanium dioxide nanorods are attached to one main titanium dioxide nanorod.

FIG. 3 is an X-ray diffraction pattern of the titanium dioxide nanomaterial prepared in example 2 of the present invention, and the result shows that the obtained titanium dioxide is in a rutile phase and has good crystallinity.

The invention is not limited to the above-described examples, and various modifications or alterations without inventive work may be made by those skilled in the art within the scope of the invention defined by the claims appended hereto.