Supramolecular glass and method for preparing the same

The preparation of supramolecular glass by reactive hot pressing of cyclodextrin and hydroxybenzoic acid solves the problems of repeatability and preparation cost of traditional glass, and achieves high transmittance and environmentally friendly production, which is suitable for glass handicrafts.

CN117467035BActive Publication Date: 2026-04-07INST OF BAST FIBER CROPS CHINESE ACADEMY OF AGRI SCI +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-03
Publication Date
2026-04-07

AI Technical Summary

Technical Problem

Traditional inorganic and organic glass have drawbacks such as non-reusability, poor compatibility and adaptability, high manufacturing cost, and complex processes.

Method used

Supramolecular glass was prepared by using cyclodextrin as the host molecule and hydroxybenzoic acid as the guest molecule, mixing them and adding an appropriate amount of water, reacting them under specific temperature and pressure, and then hot-pressing and cooling.

Benefits of technology

We have developed a supramolecular glass with high transmittance, reusability, and environmental friendliness. It is suitable for making glass handicrafts and the production process is simple, with readily available, non-toxic, and harmless raw materials.

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Abstract

The application provides a supramolecular glass and a preparation method thereof. The preparation method of the glass comprises the following steps: taking cyclodextrin as a host molecule, taking hydroxybenzoic acid as a guest molecule, mixing the host molecule and the guest molecule, adding a certain amount of water, heating and reacting until a transparent semi-hardened product is obtained; then, the product is hot-pressed and cooled to room temperature to obtain the supramolecular glass; wherein the amount of water added is 5-10 wt% of the mass of the host molecule and the guest molecule. The method can prepare a glass with high transmittance, and the preparation method is simple, raw materials are easy to obtain, the preparation process is non-toxic and harmless, and the method is green and environmentally friendly.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high polymer materials, and more particularly to a supramolecular glass and a preparation method thereof. BACKGROUND

[0002] Glass is a kind of transparent material with a long history and plays an important role in production and life. It is mainly divided into inorganic glass and organic glass. Common inorganic glass mainly includes Na2SiO3, CaSiO3, SiO2 or Na2O·CaO·6SiO2, and the main powder is a silicate complex salt, which is a non-crystalline solid with a random structure and is widely used in buildings for wind insulation and light transmission. In addition, there are colored glass mixed with certain metal oxides or salts to show color, and tempered glass prepared by physical or chemical methods. With the development of science and technology, organic glass is prepared and widely used, and most of the organic glass is a polymer. However, the traditional inorganic glass and organic glass have defects such as non-reusable, poor compatible adaptability, high preparation cost, and complex process. SUMMARY

[0003] Based on the above technical problems existing in the prior art, the present application provides a preparation method of a supramolecular glass, which can prepare a glass with high transmittance, and the preparation method is simple, the raw materials are easy to obtain, the preparation process is non-toxic and harmless, and green and environmentally friendly.

[0004] In order to achieve the above purpose, the technical scheme of the present application is as follows:

[0005] A preparation method of a supramolecular glass, comprising the following steps: taking cyclodextrin as a host molecule and hydroxybenzoic acid as a guest molecule, mixing the host molecule and the guest molecule, adding a certain amount of water, heating and reacting until a transparent semi-hardened product is obtained; then heat pressing the product, cooling to room temperature to obtain the supramolecular glass.

[0006] The amount of water added is 5-10% of the mass (or volume, or molar ratio) of the host molecule and the guest molecule.

[0007] In some embodiments, the molar ratio of the host molecule to the guest molecule is 1:1.

[0008] In some embodiments, the reaction temperature is 80-100℃.

[0009] In some embodiments, the temperature of the heat pressing is 80-100℃; the heat pressing pressure is 5-30MPa; and the heat pressing time is 5-30min.

[0010] In some embodiments, the host molecule is β-cyclodextrin; and the guest molecule is p-hydroxybenzoic acid.

[0011] The present invention also provides supramolecular glasses obtained by the preparation method of any of the above embodiments.

[0012] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0013] This invention uses cyclodextrin as the main component and hydroxybenzoic acid as the guest component. After adding a certain amount of water, the mixture is reacted under specific reaction conditions, followed by hot pressing and finally cooling and hardening to obtain supramolecular glass. It has the advantages of simple preparation, readily available raw materials, and non-toxic and harmless production process. Moreover, the obtained glass has high transmittance and strong thermoplasticity at 80-100℃. It can be used to prepare glass handicrafts (such as glass ornaments, glass pendants, etc.) and is reusable, making it green and environmentally friendly. Attached Figure Description

[0014] Figure 1 This is a photograph of the supramolecular glass prepared in Example 1.

[0015] Figure 2 The images show the 1H NMR spectra of the supramolecular glass, host molecule, and guest molecule prepared in Example 1.

[0016] Figure 3 The infrared spectra of the supramolecular glass, host molecule, and guest molecule prepared in Example 1 are shown below.

[0017] Figure 4 The transmittance is that of the supramolecular glass prepared in Example 1;

[0018] Figure 5 The refractive index is that of the supramolecular glass prepared in Example 1;

[0019] Figure 6 The transmittance of the supramolecular glass prepared in Example 1 under 800 nm light after different cycles is shown. Detailed Implementation

[0020] Numerous specific details are set forth in the following description to provide a full understanding of the invention. However, the invention can be practiced in many other ways different from those described herein, and similar modifications can be made by those skilled in the art without departing from the spirit of the invention. Therefore, the invention is not limited to the specific embodiments disclosed below.

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0022] Example 1

[0023] A supramolecular glass, the preparation method of which is as follows:

[0024] Methyl-β-cyclodextrin and p-hydroxybenzoic acid were mixed at a molar ratio of 1:1, and then water was added at a mass of 10% of the total mass of methyl-β-cyclodextrin and p-hydroxybenzoic acid. The mixture was heated to 80°C and reacted until all the unreacted water evaporated, yielding a transparent, semi-cured product. The product was then hot-pressed at 80°C at a pressure of 10 MPa for 10 minutes. After hot pressing, the product was allowed to cool naturally to room temperature to obtain a supramolecular glass with a thickness of 1 mm.

[0025] The obtained supramolecular glass was cut into sheets of equal length and width. A photograph of the resulting supramolecular glass is shown below. Figure 1 As shown.

[0026] The supramolecular glass was tested using 1H NMR and Fourier transform infrared spectroscopy, and the test results are as follows: Figure 2 and Figure 3 As shown.

[0027] The transmittance and refractive index of supramolecular glass were tested, and the test results are as follows: Figure 4 and Figure 5 As shown.

[0028] The supramolecular glass obtained in Example 1 was added to an excess of water, heated to 80°C until completely dissolved, and then the water was evaporated to dryness. The glass was then hot-pressed at 80°C, and the cyclic transmittance of the glass was tested. The test results are as follows: Figure 6 As shown.

[0029] Comparative Example 1

[0030] Methyl-β-cyclodextrin and p-hydroxybenzoic acid were mixed at a molar ratio of 1:1 and heated to 80°C for reaction. The product was then hot-pressed at 80°C for 10 min at a pressure of 10 MPa. After hot pressing, the product was cooled to room temperature to obtain a transparent viscous product.

[0031] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0032] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A method for preparing supramolecular glass, characterized in that, The process includes the following steps: using cyclodextrin as the host molecule and hydroxybenzoic acid as the guest molecule, mixing the host molecule and the guest molecule, adding a certain amount of water, heating to carry out the reaction until a transparent semi-hardened product is obtained; then hot-pressing the product and cooling it to room temperature to obtain the supramolecular glass. The amount of water added is 5-10% of the total mass of the host molecules and guest molecules; The molar ratio of the host molecule to the guest molecule is 1:1; The reaction temperature is 80-100℃.

2. The method for preparing supramolecular glass according to claim 1, characterized in that, The hot pressing temperature is 80-100℃; the hot pressing pressure is 5-30MPa.

3. The method for preparing supramolecular glass according to claim 1, characterized in that, The host molecule is β-cyclodextrin; the guest molecule is p-hydroxybenzoic acid.

4. The supramolecular glass obtained by the method for preparing supramolecular glass according to any one of claims 1-3.