Preparation method of tetrabutyl titanate-nanodiamond dispersion liquid

Abstract

The application discloses a preparation method of a tetrabutyl titanate-nano diamond dispersion liquid. The tetrabutyl titanate is used as a dispersion stabilizer, and ultrasonic dispersion is adopted to prepare the tetrabutyl titanate-nano diamond dispersion liquid. In the dispersion system, the nano diamond can be stably and uniformly dispersed. The nano diamond dispersion liquid prepared by the method can be widely applied in the fields of grinding and polishing, coating materials, polymer composite materials and lubrication.

Description

Technical Field

[0001] This invention relates to a nanodiamond dispersion and its preparation method, and more particularly to a method for preparing a nanodiamond dispersion using tetrabutyl titanate as a dispersing stabilizer. Background Technology

[0002] Nanodiamonds are diamond powders with an average particle size in the nanometer range. Their preparation methods include detonation, chemical vapor deposition, and high-energy ball milling, with detonation currently being the primary method. Due to their dual properties of diamond and nanomaterials—ultra-high hardness, high thermal conductivity, and excellent chemical stability—nanodiamonds are widely used in grinding and polishing, lubrication, strengthening of polymer composites, and biomedicine.

[0003] However, due to their high surface energy and extremely unstable thermodynamics, nanodiamonds are prone to agglomeration, significantly reducing their effectiveness and posing a major obstacle to their application. Therefore, the dispersion of nanodiamonds has become a key research focus. Good dispersibility is crucial for nanodiamonds to achieve their superior performance. Finding a nanodiamond dispersion technology that offers good dispersibility, uniform dispersion, simple processing, ease of implementation, and environmental friendliness is currently the focus of nanodiamond dispersion research. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing a nanodiamond dispersion that can stably disperse nanodiamonds.

[0005] The technical solution to achieve the purpose of this invention is as follows: a method for preparing a stable and dispersed tetrabutyl titanate-nanodiamond dispersion, using tetrabutyl titanate as a dispersing stabilizer, and utilizing the "cavitation effect" of ultrasound to deagglomerate nanodiamond aggregates, comprising the following steps: First, prepare a solution by mixing 3%-15% tetrabutyl titanate, 5%-25% acetic acid, 50%-80% anhydrous ethanol, and 0%-20% deionized water. All of the above are volume fractions. Sonicate the solution for a period of time until the solution is uniform and transparent. The second step involves adding nanodiamonds to the solution obtained in the first step and sonicating it at room temperature for a period of time to obtain a dispersion. The third step is to centrifuge the dispersion obtained in the second step at a certain speed and take the upper dispersion after centrifugation. Fourth step: If the volume fraction of deionized water in the first step is 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 1-50:1 until homogeneous; if the volume fraction of deionized water in the first step is not 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 0-50:1 until homogeneous to obtain tetrabutyl titanate-nanodiamond dispersion.

[0006] Furthermore, in the first step, detonation nanodiamonds are used.

[0007] Furthermore, in the first step, sonicate for 10-30 minutes until the solution is homogeneous and transparent.

[0008] Furthermore, in the second step, it is sonicated at room temperature for 3-10 days.

[0009] Furthermore, in the second step, the concentration of nanodiamond in the dispersion is 0.05%-2.5wt%.

[0010] Furthermore, in the third step, the dispersion obtained in the second step is centrifuged 1-3 times at 5000-10000 r / min.

[0011] Compared with the prior art, the advantages of this invention are: (1) Tetrabutyl titanate is used as a dispersing stabilizer, which can stably disperse nanodiamonds in a mixed solvent of acetic acid and anhydrous ethanol. (2) The "cavitation effect" of ultrasound can effectively break up the agglomeration of nanodiamonds. (3) The preparation process is simple, easy to implement, and environmentally friendly. (4) The prepared nanodiamond dispersion has good application prospects and can be widely used in polishing, coating materials, lubrication and other fields.

[0012] It should be understood that all combinations of the foregoing concepts and the additional concepts described in more detail below may be considered part of the inventive subject matter of this application, provided that such concepts do not contradict each other. Furthermore, all combinations of the claimed subject matter are considered part of the inventive subject matter of this application.

[0013] The foregoing and other aspects, embodiments, and features of the teachings of the present invention will be more fully understood from the following description in conjunction with the accompanying drawings. Other additional aspects of the invention, such as features and / or beneficial effects of exemplary embodiments, will become apparent from the following description or may be learned through practice of specific embodiments according to the teachings of the present invention. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the preparation process of a tetrabutyl titanate-nanodiamond dispersion according to the present invention.

[0015] Figure 2 This is a diagram illustrating the mechanism of action of tetrabutyl titanate on the surface of nanodiamonds.

[0016] Figure 3 This is a comparison image of the tetrabutyl titanate-nanodiamond dispersion prepared in Example 1 and the nanodiamond dispersion without tetrabutyl titanate after 7 days. Glass bottle No. 0 contains the nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 1 contains the tetrabutyl titanate-nanodiamond dispersion prepared in Example 1.

[0017] Figure 4 This is a comparison image of the tetrabutyl titanate-nanodiamond dispersion prepared in Example 2 and the nanodiamond dispersion without tetrabutyl titanate after 7 days. Glass bottle No. 0 contains the nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 2 contains the tetrabutyl titanate-nanodiamond dispersion prepared in Example 2.

[0018] Figure 5 This is a comparison image of the tetrabutyl titanate-nanodiamond dispersion prepared in Example 3 and the nanodiamond dispersion without tetrabutyl titanate after 7 days. Glass bottle No. 0 contains the nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 3 contains the tetrabutyl titanate-nanodiamond dispersion prepared in Example 3.

[0019] Figure 6 This is a comparison image of the tetrabutyl titanate-nanodiamond dispersion prepared in Example 4 and the nanodiamond dispersion without tetrabutyl titanate after 7 days. Glass bottle No. 0 contains the nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 4 contains the tetrabutyl titanate-nanodiamond dispersion prepared in Example 1.

[0020] Figure 7 This is a comparison image of the tetrabutyl titanate-nanodiamond dispersion prepared in Example 5 and the nanodiamond dispersion without tetrabutyl titanate after 7 days. Glass bottle No. 0 contains the nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 5 contains the tetrabutyl titanate-nanodiamond dispersion prepared in Example 5. Detailed Implementation

[0021] To better understand the technical content of the present invention, specific embodiments are described below in conjunction with the accompanying drawings.

[0022] In this invention, various aspects of the invention are described with reference to the accompanying drawings, in which numerous illustrative embodiments are shown. The embodiments of the invention are not necessarily intended to encompass all aspects of the invention. It should be understood that the various concepts and embodiments described above, as well as those described in more detail below, can be implemented in any of many ways, because the concepts and embodiments disclosed herein are not limited to any particular implementation. Furthermore, some aspects of the invention disclosed may be used alone or in any suitable combination with other aspects of the invention disclosed.

[0023] Tetrabutyl titanate, as a titanate coupling agent, can form a monolayer on the surface of nanodiamonds, effectively reducing the surface energy of the nanodiamond surface and exhibiting surface modification effects, such as... Figure 2 As shown.

[0024] Combined with appendix Figure 1The present invention discloses a tetrabutyl titanate-nanodiamond dispersion, which is prepared by the following steps: First, prepare a solution by mixing 3%-15% tetrabutyl titanate, 5%-25% acetic acid, 50%-80% anhydrous ethanol, and 0%-20% deionized water. All of the above are volume fractions. Sonicate the solution for 10-30 minutes until the solution is homogeneous and transparent. The second step involves adding the detonated nanodiamond to the solution obtained in the first step and sonicating it at room temperature for 3-10 days to obtain a dispersion with a concentration of 0.05%-2.5wt%. The third step is to centrifuge the dispersion obtained in the second step at 5000-10000 r / min 1-3 times and take the upper dispersion after centrifugation. Fourth step: If the volume fraction of deionized water in the first step is 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 1-50:1 until homogeneous; if the volume fraction of deionized water in the first step is not 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 0-50:1 until homogeneous to obtain tetrabutyl titanate-nanodiamond dispersion.

[0025] Example 1: The preparation method of the tetrabutyl titanate-nanodiamond dispersion of the present invention includes the following steps: The first step is the preparation of the tetrabutyl titanate dispersion. Take 1.5 ml of tetrabutyl titanate, 9.5 ml of acetic acid, 34 ml of anhydrous ethanol, and 5 ml of deionized water, and sonicate for 20 min. The solution is uniform and transparent.

[0026] In the second step, 0.0218g of detonated nanodiamond (commercially available) was added to the tetrabutyl titanate dispersion prepared in the first step, and sonicated at room temperature for 7 days. After 7 days, the nanodiamond was stably and uniformly dispersed in the tetrabutyl titanate dispersion.

[0027] The third step is to centrifuge the nanodiamond dispersion obtained in the second step at 9000 r / min for 5 min. Take the upper dispersion after centrifugation.

[0028] Step four: Take 10 ml of the supernatant dispersion from step four after centrifugation, without adding acetic acid. This yields the tetrabutyl titanate-nanodiamond dispersion. The prepared tetrabutyl titanate-nanodiamond dispersion remained stable after 7 days. In the nanodiamond dispersion without tetrabutyl titanate, the nanodiamonds were almost completely precipitated. Figure 3 As shown, glass bottle 0 contains nanodiamond dispersion without tetrabutyl titanate, and glass bottle 1 contains the prepared tetrabutyl titanate-nanodiamond dispersion.

[0029] Example 2: The preparation method of the tetrabutyl titanate-nanodiamond dispersion of the present invention includes the following steps: Step 1: Preparation of tetrabutyl titanate dispersion. Take 2.5 ml tetrabutyl titanate, 12.5 ml acetic acid, 25 ml anhydrous ethanol, and 10 ml deionized water, and sonicate for 20 min. The solution is homogeneous and transparent.

[0030] In the second step, 1.1630g of detonated nanodiamond (commercially available) was added to the tetrabutyl titanate dispersion prepared in the first step, and sonicated at room temperature for 7 days. After 7 days, the nanodiamond was stably and uniformly dispersed in the tetrabutyl titanate dispersion.

[0031] The third step is to centrifuge the nanodiamond dispersion obtained in the second step at 9000 r / min for 5 min. Take the upper dispersion after centrifugation.

[0032] Fourth step: Take 10 ml of the supernatant dispersion from the centrifuged solution in step four, add 10 ml of acetic acid, and mix thoroughly. This yields the tetrabutyl titanate-nanodiamond dispersion. The prepared tetrabutyl titanate-nanodiamond dispersion remained stably dispersed even after 7 days, while the nanodiamonds in the nanodiamond dispersion without added tetrabutyl titanate had almost completely precipitated. Figure 4 As shown, glass bottle No. 0 contains nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 2 contains the prepared tetrabutyl titanate-nanodiamond dispersion.

[0033] Example 3: The preparation method of the tetrabutyl titanate-nanodiamond dispersion of the present invention includes the following steps: The first step is the same as step one in Example 2.

[0034] The second step is the same as step two in Example 2.

[0035] The third step is the same as step three in Example 2.

[0036] Fourth step: Take 10ml of the supernatant dispersion from the centrifuged mixture in step four, add 20ml of acetic acid, and mix thoroughly. This yields the tetrabutyl titanate-nanodiamond dispersion. The prepared tetrabutyl titanate-nanodiamond dispersion remained stably dispersed even after 7 days, while the nanodiamonds in the nanodiamond dispersion without added tetrabutyl titanate had almost completely precipitated. Figure 5 As shown, glass bottle No. 0 contains nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 3 contains the prepared tetrabutyl titanate-nanodiamond dispersion.

[0037] Example 4: The preparation method of the tetrabutyl titanate-nanodiamond dispersion of the present invention includes the following steps: The first step is the preparation of the tetrabutyl titanate dispersion. Take 7.5 ml of tetrabutyl titanate, 2.5 ml of acetic acid, and 40 ml of anhydrous ethanol, and sonicate for 20 min. The solution is homogeneous and transparent.

[0038] In the second step, 0.5064g of detonated nanodiamond (commercially available) was added to the tetrabutyl titanate dispersion prepared in the first step, and sonicated at room temperature for 7 days. After 7 days, the nanodiamond was stably and uniformly dispersed in the tetrabutyl titanate dispersion.

[0039] The third step is to centrifuge the nanodiamond dispersion obtained in the second step at 9000 r / min for 5 min. Take the upper dispersion after centrifugation.

[0040] Fourth step: Take 10 ml of the supernatant dispersion from the centrifuged solution in step four, add 10 ml of acetic acid, and mix thoroughly. This yields the tetrabutyl titanate-nanodiamond dispersion. The prepared tetrabutyl titanate-nanodiamond dispersion remained stably dispersed even after 7 days, while the nanodiamonds in the nanodiamond dispersion without added tetrabutyl titanate had almost completely precipitated. Figure 6 As shown, glass bottle No. 0 contains nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 4 contains the prepared tetrabutyl titanate-nanodiamond dispersion.

[0041] Example 5: A method for preparing the tetrabutyl titanate-nanodiamond dispersion of the present invention includes the following steps: Step 1: Preparation of tetrabutyl titanate dispersion. Take 3.4 ml of tetrabutyl titanate, 10 ml of acetic acid, and 36 ml of anhydrous ethanol, and sonicate for 20 min. The solution becomes uniform and transparent.

[0042] In the second step, 0.3289 g of detonated nanodiamonds were added to the tetrabutyl titanate dispersion prepared in the first step, and sonicated at room temperature for 7 days. After 7 days, the nanodiamonds were stably and uniformly dispersed in the tetrabutyl titanate dispersion.

[0043] The third step is to centrifuge the nanodiamond dispersion obtained in the second step at 9000 r / min for 5 min. Take the upper dispersion after centrifugation.

[0044] Fourth step: Take 10ml of the supernatant dispersion from the centrifuged mixture in step four, add 20ml of acetic acid, and mix thoroughly. This yields the tetrabutyl titanate-nanodiamond dispersion. The prepared tetrabutyl titanate-nanodiamond dispersion remained stably dispersed even after 7 days, while the nanodiamonds in the nanodiamond dispersion without added tetrabutyl titanate had almost completely precipitated. Figure 7 As shown, glass bottle No. 0 contains nanodiamond dispersion without tetrabutyl titanate, and glass bottle No. 5 contains the prepared tetrabutyl titanate-nanodiamond dispersion.

Claims

1. A method for preparing a stable and dispersed tetrabutyl titanate-nanodiamond dispersion, characterized in that, Using tetrabutyl titanate as a dispersant and stabilizer, the nanodiamond aggregates are depolymerized through the "hole effect" of ultrasound, including the following steps: First, prepare a solution by mixing 3%-15% tetrabutyl titanate, 5%-25% acetic acid, 50%-80% anhydrous ethanol, and 0%-20% deionized water. All of the above are volume fractions. Sonicate the solution for a period of time until the solution is uniform and transparent. The second step involves adding nanodiamonds to the solution obtained in the first step and sonicating it at room temperature for a period of time to obtain a dispersion. The nanodiamonds used are detonated nanodiamonds. The third step is to centrifuge the dispersion obtained in the second step at a certain speed and take the upper dispersion after centrifugation. Fourth step: If the volume fraction of deionized water in the first step is 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 1-50:1 until homogeneous; if the volume fraction of deionized water in the first step is not 0, mix acetic acid and the upper dispersion obtained in the third step at a volume ratio of 0-50:1 until homogeneous to obtain tetrabutyl titanate-nanodiamond dispersion.

2. The method as described in claim 1, characterized in that, In the first step, sonicate for 10-30 minutes until the solution is homogeneous and transparent.

3. The method as described in claim 1, characterized in that, In the second step, it is sonicated at room temperature for 3-10 days.

4. The method as described in claim 1, characterized in that, In the second step, the concentration of nanodiamonds in the dispersion is 0.05%-2.5wt%.

5. The method as described in claim 1, characterized in that, In the third step, the dispersion obtained in the second step is centrifuged 1-3 times at 5000-10000 r / min.

6. The stable dispersion of tetrabutyl titanate-nanodiamond prepared by the method according to any one of claims 1-5.

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