Method for preparing white carbon black single crystal based on combination of mechanochemical synthesis method and hydrothermal reaction method
Through the method of mechanical chemical synthesis method and water thermal reaction method, the problem of poor decentralization and high energy consumption in traditional white carbon black preparation methods is solved. Production costs and environmental pollution.
Patent Information
- Application Number
- CN202411365890.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-29
- Publication Date
- 2025-01-21
AI Technical Summary
The traditional white carbon black preparation method usually obtains agglomerate or polycrystalline structures, which have poor dispersion and low interfacial activity. The high-temperature calcination or chemical synthesis methods are high in energy consumption and expensive, which may cause environmental pollution.
The mechanochemical synthesis method is combined with the hydrothermal reaction method to achieve low-temperature preparation of silica single crystals by accurately controlling the raw material ratio and reaction conditions, reducing crystal defects and broadening the light absorption range.
It significantly improves the purity and dispersion of silica single crystal, reduces energy consumption and production costs, reduces environmental pollution, and improves the market competitiveness of the product.
Smart Images
Figure CN119332335A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical production, and in particular to a method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method. Background Art
[0002] As an important inorganic nanomaterial, white carbon black has been widely used in many fields such as rubber reinforcement, coatings, medicine, and cosmetics due to its unique physical and chemical properties. However, the traditional preparation method usually obtains white carbon black with agglomerates or polycrystalline structures. These white carbon blacks have problems such as poor dispersibility and low interfacial activity in application, which limits the further development of their performance. In addition, the traditional preparation method of white carbon black single crystals usually involves high-temperature calcination or chemical synthesis, which often have high energy consumption, high cost, and may cause environmental pollution. Therefore, it is of great practical significance to develop an efficient, environmentally friendly, and low-cost preparation method for white carbon black single crystals.
[0003] Silica single crystals (SiO2) are widely used in many fields due to their excellent physical and chemical properties. However, the current output of silica single crystals is low and the impurity content is high, which limits its application in high-end fields. Chemical methods such as chemical vapor deposition (CVD) and hydrothermal method are effective ways to prepare high-purity silica single crystals. The CVD method generates SiO2 thin films in the gas phase through chemical reactions, which can achieve good size and morphology control, but the equipment investment and operating costs are high; in view of this, we proposed a method for preparing silica single crystals based on the combination of mechanochemical synthesis and hydrothermal reaction. Summary of the invention
[0004] The purpose of the present invention is to provide a method for preparing white carbon black single crystals based on the combination of mechanochemical synthesis method and hydrothermal reaction method. The combination of mechanochemical synthesis method and hydrothermal reaction method significantly improves the purity and dispersibility of white carbon black single crystals, while reducing energy consumption and production costs. The present invention realizes a low-temperature preparation process without high-temperature calcination by accurately controlling the raw material ratio and reaction conditions, reduces crystal defects, broadens the light absorption range, and improves the market competitiveness of the product.
[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method, the method comprising the following steps: S1. Raw material preparation: S2, mechanochemical treatment; S3, hydrothermal reaction; S31, adding the dry material to the polytetrafluoroethylene liner; S32, pre-processing; S33, hydrothermal reaction; S34, separation and washing; S4, drying and screening, after drying and screening, pure white carbon black single crystals are obtained.
[0006] Optionally, the raw materials in S1 include a main raw material and auxiliary raw materials, the main raw material includes high-purity powdered silicon dioxide, and the auxiliary raw materials include deionized water, sodium nitrate and phosphorous acid.
[0007] Optionally, in S2, the raw materials are mixed according to the mass ratio of (0.6-0.8): (1.9-2.1): (1.3-1.5): (0.7-0.9), and then the mixture is subjected to mechanochemical synthesis treatment in a ball mill.
[0008] Optionally, S2 further includes: during the ball milling process, controlling the ball milling speed, time and ball-to-material ratio to achieve sufficient mixing and reaction of the raw materials; transferring the mixed ball-milled materials to a freeze dryer and drying them at -40°C for 10 hours.
[0009] Optionally, the S32 further includes: shaking on a shaker at 25° C. for 30 minutes to ensure that the raw materials are fully mixed.
[0010] Optionally, the hydrothermal reaction in S33 further includes: placing the polytetrafluoroethylene liner into a stainless steel kettle, placing it in a box-type reactor with programmed temperature control, setting the temperature to rise from 30°C to 200°C, the heating time is 200 minutes, then setting a constant temperature of 200°C, the constant temperature time is 4200 minutes, and finally setting the temperature to drop from 200°C to 30°C, the cooling time is 2000 minutes.
[0011] Optionally, the S34 further includes: taking out the reactor, opening the liner, pouring the mixture into a centrifuge tube, centrifuging at 7000 rpm, washing with deionized water and ethanol for 3 times respectively, and then separating the precipitate by centrifugation.
[0012] Optionally, S4 further comprises: drying the precipitate at 80° C. for 24 hours, and then screening the complete block crystals under an optical microscope.
[0013] Compared with the prior art, the present invention provides a method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method, which has the following beneficial effects: This method for preparing silica single crystals based on the combination of mechanochemical synthesis and hydrothermal reaction uses powdered silicon dioxide, deionized water and sodium nitrate or phosphorous acid as raw materials. By precisely controlling the mass ratio of the raw materials and the reaction conditions, silica single crystals with high purity and good dispersion are successfully prepared. The reaction conditions are mild and no high-temperature calcination is required. The crystals have few defects and a wide light absorption range. The development of a low-temperature calcination-free method for pure silica single crystals has high economic value. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 It is a schematic diagram of the overall process structure of the present invention; Figure 2 This is the XRD pattern of pure silica single crystal in Example 1 of the present invention; Figure 3 This is the DRS image of pure silica single crystal in Example 1 of the present invention; Figure 4 This is the XRD pattern of pure white carbon black single crystal in Example 2 of the present invention; Figure 5 This is the DRS diagram of pure silica single crystal in Example 2 of the present invention. DETAILED DESCRIPTION
[0015] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example 1
[0016] like Figure 1-Figure 3 As shown, this embodiment proposes a method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method, comprising the following steps: Select high-purity nano-scale powdered silicon dioxide as the main raw material, with a purity of not less than 99.9%. Powdered silicon dioxide, deionized water, sodium nitrate and phosphorous acid are added to the ball mill in a mass ratio of 0.7125 g: 2.00 g: 1.3824 g: 0.7977 g for mechanochemical synthesis. The ball milling speed is set to 300 rpm and the ball milling time is 4 hours to ensure that the raw materials are fully mixed and reacted. The mixed material is dried in a freeze dryer at -40°C for 10 hours to remove moisture from the material and prevent the raw materials from agglomerating. After freeze drying, add it to the polytetrafluoroethylene liner; Use a shaker to shake at 25°C for 30 minutes. Put the polytetrafluoroethylene liner into a stainless steel kettle, place it in a program-controlled box-type reactor, set the temperature to rise from 30°C to 200°C, the heating time is 200 minutes, then set the constant temperature to 200°C, the constant temperature time is 4200 minutes, and finally set the temperature to drop from 200°C to 30°C, the cooling time is 2000 minutes. Take out the reactor, open the liner, pour the mixture into a centrifuge tube, centrifuge at 7000 rpm, wash with deionized water and ethanol 3 times respectively, and then separate the precipitate by centrifugation. Dry the precipitate at 80°C for 24 hours, and separate the relatively complete block crystals under an optical microscope, which are pure white carbon black single crystals. Example 2
[0017] like Figure 1 , Figure 4-Figure 5 As shown, this embodiment proposes a method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method, comprising the following steps: Powdered silicon dioxide, deionized water, sodium nitrate and phosphorous acid were added into a ball mill in a mass ratio of 0.7481 g: 2.00 g: 1.4125 g: 0.8428 g for mechanochemical synthesis treatment; After freeze drying, add to the polytetrafluoroethylene liner. Use a shaker to shake at 25°C for 30 minutes. Put the polytetrafluoroethylene liner into a stainless steel kettle and place it in a program-controlled box-type reactor. Set the temperature to rise from 30°C to 200°C for 200 minutes, then set the constant temperature to 200°C for 4200 minutes, and finally set the temperature to drop from 200°C to 30°C for 2000 minutes. Take out the reactor, open the liner, pour the mixture into a centrifuge tube, centrifuge at 7000 rpm, wash with deionized water and ethanol 3 times respectively, and then separate the precipitate by centrifugation. Dry the precipitate at 80°C for 24 hours. Separate the relatively complete block crystals under an optical microscope, which are pure white carbon black single crystals.
[0018] The above generally describes the present invention in detail, but it is obvious to a person skilled in the art that some modifications or improvements can be made to the present invention. Therefore, modifications or improvements that do not depart from the spirit of the present invention are within the scope of protection of the present invention.
Claims
1. A method for preparing white carbon black single crystals based on a combination of a mechanochemical synthesis method and a hydrothermal reaction method, characterized in that: The method comprises the following steps: S1. Raw material preparation: S2, mechanochemical treatment; S3, hydrothermal reaction; S31, adding the dry material to the polytetrafluoroethylene liner; S32, pre-processing; S33, hydrothermal reaction; S34, separation and washing; S4, drying and screening, after drying and screening, pure white carbon black single crystals are obtained.
2. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 1, characterized in that: The raw materials in S1 include main raw materials and auxiliary raw materials. The main raw material includes high-purity powdered silicon dioxide, and the auxiliary raw materials include deionized water, sodium nitrate and phosphorous acid.
3. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 1, characterized in that: In S2, the raw materials are mixed according to the mass ratio of (0.6-0.8): (1.9-2.1): (1.3-1.5): (0.7-0.9), and then subjected to mechanochemical synthesis treatment by a ball mill.
4. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 3, characterized in that: The S2 further comprises: during the ball milling process, controlling the ball milling speed, time and ball-to-material ratio to achieve sufficient mixing and reaction of the raw materials; transferring the mixed ball-milled materials to a freeze dryer and drying them at -40°C for 10 hours.
5. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 1, characterized in that: The S32 further comprises: shaking on a shaker at 25° C. for 30 minutes to ensure that the raw materials are fully mixed.
6. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 5, characterized in that: The hydrothermal reaction in S33 further includes: placing the polytetrafluoroethylene liner into a stainless steel kettle, placing it in a box-type reactor with programmed temperature control, setting the temperature to rise from 30°C to 200°C for 200 minutes, then setting a constant temperature of 200°C for 4200 minutes, and finally setting the temperature to fall from 200°C to 30°C for 2000 minutes.
7. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 6, characterized in that: The S34 further comprises: taking out the reaction kettle, opening the inner liner, pouring the mixture into a centrifuge tube, centrifuging at 7000 rpm, washing with deionized water and ethanol for 3 times respectively, and then separating the precipitate by centrifugation.
8. The method for preparing white carbon black single crystals based on a mechanochemical synthesis method combined with a hydrothermal reaction method according to claim 7, characterized in that: The S4 further comprises: drying the precipitate at 80° C. for 24 hours, and then screening the complete block crystals under an optical microscope.