Method for preparing fluorine-containing carbon black through in-situ fluorination
By directly introducing a fluorine source during the carbon black production process, and using in-situ fluorination method to combine fluorine with carbon black instantly, the problem of uneven bonding between fluorine and carbon black in the prior art is solved, and the product quality is stabilized Reduced sexual and production costs.
Patent Information
- Application Number
- CN202411577650.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-07
- Publication Date
- 2025-02-18
AI Technical Summary
In the prior art, when preparing fluorine-containing carbon black, the post-treatment method leads to uneven bonding between fluorine and carbon black, which increases production costs and is difficult to ensure the stability of product quality.
The fluorine source is directly introduced during the carbon black production process, and the fluorine and carbon black are combined instantly through the in-situ fluorination method to ensure uniform bonding of fluorine and carbon black.
The uniform combination of fluorine and carbon black is achieved, ensuring the stability of product quality, and reducing production costs.
Smart Images
Figure CN119463537A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of carbon black production, and in particular relates to a method for preparing fluorine-containing carbon black by in-situ fluorination. Background Art
[0002] Fluorine-containing carbon black is a product obtained by the reaction of carbon black and fluorine. With the increase of its fluorination degree, its conductivity decreases, its adsorption capacity increases, its hydrophobicity increases, and it has good lubrication performance and thermal stability. It can be used in the field of batteries for pure lithium fluorocarbon primary battery positive electrode materials, lithium manganese battery positive electrode composite materials, and for button-type, soft-pack, cylindrical and special-shaped lithium fluorocarbon primary batteries. It is small and light, has low internal resistance, low self-discharge, and high power specific energy. It can be used in non-battery fields for solid lubricant additives, dry ink additives, etc. Usually, the production methods of fluorine-containing carbon black include high-temperature synthesis method, low-temperature fluorination method, plasma method, and electrolytic synthesis method. These methods belong to carbon black post-treatment, that is, carbon black is used as raw material and then fluorinated. The preparation of fluorine-containing carbon black by post-treatment undoubtedly increases the production cost. At the same time, it is difficult to achieve uniform reaction during the reaction process when using the post-treatment method to prepare fluorine-containing carbon black. The combination of fluorine and carbon black has great randomness and unevenness, and it is difficult to ensure the stability of the quality of the final product. Summary of the invention
[0003] In view of the shortcomings of the above-mentioned prior art, the present invention provides a method for preparing fluorine-containing carbon black by in-situ fluorination, which has more uniform reaction, lower cost and less impurity introduction. The specific technical scheme is as follows:
[0004] A method for preparing fluorine-containing carbon black by in-situ fluorination, wherein a fluorine source is introduced into the carbon black production process, and the fluorine-containing carbon black is prepared by in-situ fluorination.
[0005] The present invention introduces a fluorine source during the carbon black production process and adopts in-situ fluorination to directly produce fluorine-containing carbon black. The carbon black combines with fluorine at the moment of cracking and production. This method can make the fluorine and carbon black combine more evenly, which can effectively guarantee the stability of the product and effectively save costs compared with post-processing methods.
[0006] Furthermore, the method for preparing fluorine-containing carbon black by in-situ fluorination comprises the following steps:
[0007] Step S1: connecting the fluorine source filling equipment to the carbon black production equipment;
[0008] Step S2: introducing a fluorine source into the carbon black production process to prepare a fluorine-containing carbon black product.
[0009] Furthermore, the fluorine source may be introduced into the carbon black production process by one or more of the following methods: introducing the fluorine source into a raw material preheater together with the carbon black raw material oil, introducing the fluorine source into an air preheater together with the air, or introducing the fluorine source into a reactor together with the fuel oil.
[0010] Furthermore, the fluorine source is preferably introduced into the carbon black reactor together with the fuel oil during the carbon black production process.
[0011] Furthermore, the fluorine source includes tetrafluoroethylene, carbon tetrafluoride, nitrogen trifluoride or other fluorine-containing compounds, and the preferred fluorine source is carbon tetrafluoride.
[0012] Conventional methods do not use other fluorine-containing substances instead of fluorine gas as a fluorine source. The main reason is that, on the one hand, the fluorine atom ratio of other fluorides is mostly low, which will result in more raw materials being required to provide sufficient fluorine atoms. On the other hand, other fluorides need to be cracked at a relatively high temperature to provide fluorine atoms. At the same time, the entire cracking process will cause the final fluorine-containing carbon black to be doped with some impurities from the raw materials that may affect the performance of the final fluorine-containing carbon black, which has an adverse effect on production energy consumption and product quality.
[0013] The present invention directly introduces the fluorine source during the generation process of carbon black, which can well avoid the above-mentioned problems. As for the fluorine source, carbon tetrafluoride, tetrafluoroethylene, and nitrogen trifluoride are all fluorides with a high proportion of fluorine atoms, and the generation of carbon black itself is carried out at high temperature. The above-mentioned fluorine source is directly introduced during the generation process, and there is no need to use additional energy consumption for the cracking of the fluorine source material to provide fluorine atoms. At the same time, in comparison, carbon tetrafluoride itself is only composed of fluorine atoms and carbon atoms, which greatly reduces the possibility of impurity introduction. At the same time, carbon tetrafluoride is a non-toxic gas, which avoids the risks of using fluorine gas or other toxic fluorides as fluorination during transportation and storage. Based on the above reasons, directly introducing a fluorine source to produce fluorine-containing carbon black (i.e., in-situ fluorination to prepare fluorine-containing carbon black) during the generation process of carbon black is significantly better than post-processing carbon black to produce fluorine-containing carbon black.
[0014] Furthermore, the amount of the fluorine source added is 0.1%-2% of the mass of the carbon black raw oil, and the preferred amount is 1% of the mass of the carbon black raw oil.
[0015] The beneficial effects of the present invention are:
[0016] The present invention introduces a fluorine source in the process of carbon black production by in-situ fluorination to directly produce fluorine-containing carbon black. The carbon black combines with fluorine at the moment of cracking and generation. This method can make the fluorine and carbon black combine more evenly, and can effectively guarantee the stability of the product. At the same time, compared with the post-treatment method, it can effectively save costs. The present invention can use other fluorine-containing substances instead of fluorine gas as the fluorine source, and there is no need to use additional energy for the cracking of the fluorine source substance to provide fluorine atoms, and less impurities are introduced. The fluorine content of the final fluorine-containing carbon black product is controlled by adjusting the fluorine source filling amount. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1The present invention is a simplified production process diagram of the in-situ fluorination process for preparing fluorine-containing carbon black. DETAILED DESCRIPTION
[0018] The principles and features of the present invention are described below in conjunction with embodiments. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.
[0019] The following examples are all based on the production process of carbon black:
[0020] After the raw material oil is preheated in the raw material preheater at a preheating temperature of 100°C-300°C, it enters the reaction furnace and generates carbon black at 1200°C-1700°C. After rapid cooling and heat exchange, it is collected. The temperature of the air preheater is 500°C-900°C, and the temperature of the fuel oil is 80°C-130°C. The raw material oil is selected from at least one of coal tar, anthracene oil, ethylene tar, petrochemical residue oil or catalytic oil slurry, and the fuel oil is selected from one of the raw material oils. Natural gas can also be used as fuel.
[0021] In the following examples, the preheating temperature of the raw material preheater is 200° C., the temperature of the reaction furnace is 1500° C., the temperature of the air preheater is 700° C., and the temperature of the fuel oil is 110° C. The raw material oil is coal tar, and the fuel oil is natural gas.
[0022] According to the above-mentioned production process of carbon black, the method for preparing fluorine-containing carbon black by in-situ fluorination of the present invention is as follows: Figure 1 As shown, the filling points of the fluorine source include Figure 1 M1-enters the raw material preheater together with the carbon black raw material oil, M2-enters the air preheater together with the air, and M3-enters the carbon black reactor together with the fuel oil and is added simultaneously at one or more points.
[0023] Embodiment 1:
[0024] A method for preparing fluorine-containing carbon black by in-situ fluorination comprises the following steps:
[0025] Step S1: Fill the fluorine source into the equipment such as Figure 1 The M1 shown is connected to a carbon black production device;
[0026] Step S2: using carbon tetrafluoride as a fluorine source, entering the raw material preheater together with the raw material oil at M1, and entering the carbon black production process; controlling the amount of carbon tetrafluoride added to be 1% of the mass of the carbon black raw material oil.
[0027] The fluorine-containing carbon black produced in the above steps was analyzed and its fluorine content was 0.7%.
[0028] Embodiment 2:
[0029] Compared with Example 1, the filling position of the fluorine source carbon tetrafluoride is changed from M1 where it enters the raw material preheater together with the raw material oil to M2 where it enters the air preheater together with the air, and other steps and conditions remain unchanged.
[0030] The fluorine-containing carbon black produced in the above steps was analyzed and its fluorine content was 0.7%.
[0031] Embodiment 3:
[0032] Compared with Example 1, the filling position of the fluorine source carbon tetrafluoride is changed from M1 where it enters the raw material preheater together with the raw material coal tar to M3 where it enters the reactor together with the fuel oil, and other steps and conditions remain unchanged.
[0033] The fluorine-containing carbon black produced in the above steps was analyzed and found to have a fluorine content of 0.8%.
[0034] Embodiment 4:
[0035] Compared with Example 1, the addition amount of the fluorine source carbon tetrafluoride is controlled to 0.5% of the mass of the carbon black feedstock oil, and the other steps and conditions remain unchanged.
[0036] The fluorine-containing carbon black produced in the above steps was analyzed and the fluorine content was 0.5%.
[0037] Embodiment 5:
[0038] A method for preparing fluorine-containing carbon black by in-situ fluorination comprises the following steps:
[0039] Step S1: Fill the fluorine source into the equipment such as Figure 1 M1 and M3 are shown connected everywhere to the carbon black production equipment;
[0040] Step S2: using carbon tetrafluoride as a fluorine source, entering the raw material preheater together with the raw material oil at M3 and entering the raw material preheater together with the raw material oil and coal tar at M1, and adding them simultaneously, entering the carbon black production process; controlling the amount of carbon tetrafluoride added into the raw material preheater together with the raw material oil at M3 and the amount of carbon tetrafluoride added into the raw material preheater together with the raw material oil at M1 to be 0.5% of the mass of the carbon black raw material oil.
[0041] The fluorine-containing carbon black produced in the above steps was analyzed and its fluorine content was 0.7%.
[0042] According to the fluorine content of the final fluorine-containing carbon black, it can be determined that using M3 as the addition point of carbon tetrafluoride can enable more fluorine atoms produced by the cracking of carbon tetrafluoride to combine with carbon black, thereby producing fluorine-containing carbon black with a higher fluorine content. At the same time, compared with the post-treatment fluorination production of fluorine-containing carbon black, the in-situ fluorination method omits the post-treatment process and can effectively reduce costs.
[0043] The above are only preferred embodiments of the present invention and their comparative examples, and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing fluorine-containing carbon black by in-situ fluorination, characterized in that: A fluorine source is introduced into the carbon black production process, and fluorine-containing carbon black is prepared by in-situ fluorination.
2. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 1, characterized in that: The steps include: Step S1: connecting the fluorine source filling equipment to the carbon black production equipment; Step S2: introducing a fluorine source into the carbon black production process to prepare a fluorine-containing carbon black product.
3. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 1 or 2, characterized in that: The methods of introducing the fluorine source in the carbon black production process include one or more of simultaneously introducing the fluorine source into the raw material preheater together with the carbon black raw material oil, introducing the fluorine source into the air preheater together with the air, and introducing the fluorine source into the reaction furnace together with the fuel oil.
4. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 3, characterized in that: The way to introduce the fluorine source in the carbon black production process is to enter the carbon black reactor together with the fuel oil.
5. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 1, characterized in that: The fluorine source includes tetrafluoroethylene, carbon tetrafluoride, nitrogen trifluoride or other fluorine-containing compounds.
6. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 5, characterized in that: The fluorine source is carbon tetrafluoride.
7. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 1, characterized in that: The amount of the fluorine source added is 0.1%-2% of the mass of the carbon black raw material oil.
8. The method for preparing fluorine-containing carbon black by in-situ fluorination according to claim 7, characterized in that: The amount of the fluorine source added is 1% of the mass of the carbon black raw material oil.