A hydrothermal pre-carbonization-acid washing purification continuous production device

Abstract

This utility model provides a continuous production device for hydrothermal precarbonization-acid washing and purification, relating to the field of bamboo charcoal processing technology. The device includes two hydrothermal precarbonization reactors, a filtration system, an acid washing reactor, and an intelligent control unit. Each hydrothermal precarbonization reactor is equipped with the filtration system. The outlet of each reactor is connected to a discharge pipe, and the inlet of the acid washing reactor is connected to a feed pipe. The two discharge pipes are respectively connected to the feed pipe, and a slurry pump is installed on the feed pipe. The hydrothermal precarbonization reactor, the filtration system, the slurry pump, and the acid washing reactor are electrically connected to the intelligent control unit. The intelligent control unit uses a PID algorithm module and a timing controller to achieve timing misalignment control when multiple reactors are linked, enabling the device to achieve continuous hydrothermal precarbonization + acid washing and purification, which has the advantages of increasing production capacity, improving product quality, and reducing processing costs.

Description

Technical Field

[0001] This utility model relates to the field of bamboo charcoal processing technology, specifically to a continuous production device for hydrothermal precarbonization-acid washing and purification. Background Technology

[0002] Pre-carbonized bamboo charcoal is an important precursor for bamboo-based hard carbon and bamboo-based porous carbon. Bamboo naturally has a moisture content as high as 30-50% (fresh bamboo). Traditional carbonization processes require drying (45-105℃ / 12-24h) to reduce the moisture content to ≤10% to suit the carbonization process. Hydrothermal pre-carbonization can utilize a liquid-phase environment to achieve deoxygenation and condensation reactions. Bamboo with high moisture content can be directly used for hydrothermal reactions. However, due to the approximately 30% mass loss of bamboo powder and the volume shrinkage rate reaching 60% during the hydrothermal reaction, the liquid-to-solid ratio becomes uncontrollable, causing process fluctuations. Furthermore, it results in low filling rates during acid washing, making it difficult to adapt to continuous production requirements and leading to significant wasted capacity.

[0003] CN201710492244.X discloses a method for preparing carbon fiber from waste bamboo chopsticks using hydrothermal carbonization and its applications. The method involves separate hydrothermal pre-carbonization and acid washing processes to prepare the carbon fiber. However, the separate design of the hydrothermal pre-carbonization and acid washing processes results in a lengthy process and high energy consumption. CN202321087669.X discloses a bamboo strip carbonization treatment device. A lifting component allows a circular tube to slide within the treatment chamber for thorough cooling of the bamboo strips. The support component is detachable for easy cleaning, and a drainage bucket at the lower end of the treatment chamber facilitates the drainage of water. However, it does not solve the problem of integrated acid washing and purification. CN202310507291.2 discloses a plug-flow hydrothermal carbonization reactor. This device uses the wet-heat oxidation of the remaining organic matter from hydrothermal carbonization as the energy source for the hydrothermal carbonization cycle, requiring no external heating except during the initial operation. However, this device cannot achieve continuous hydrothermal carbonization and acid washing. Utility Model Content

[0004] The purpose of this invention is to provide a continuous production device for hydrothermal precarbonization-acid washing and purification, which can realize continuous processing of hydrothermal precarbonization and acid washing and purification, and has the advantages of increasing production capacity, improving product quality and reducing processing costs.

[0005] This utility model is achieved through the following technical solution: A continuous production apparatus for hydrothermal precarbonization-acid washing purification includes two hydrothermal precarbonization reactors, a filtration system, an acid washing reaction tank, and an intelligent control unit. Each hydrothermal precarbonization reactor is equipped with the filtration system. The outlet of each hydrothermal precarbonization reactor is connected to a discharge pipe, and the inlet of each acid washing reaction tank is connected to a feed pipe. The two discharge pipes are respectively connected to the feed pipe. A slurry pump is installed on the feed pipe. The hydrothermal precarbonization reactor, the filtration system, the slurry pump, and the acid washing reaction tank are all electrically connected to the intelligent control unit.

[0006] Furthermore, the lining of the hydrothermal precarbonization reactor is made of Hastelloy C-276 and the inner wall is coated with polytetrafluoroethylene.

[0007] Furthermore, the filtration system includes a belt vacuum filter, which integrates an ultrasonic anti-clogging module.

[0008] Furthermore, the filter screen pore size of the belt vacuum filter is ≤50μm.

[0009] Furthermore, the pickling reaction tank is equipped with a spiral agitator and a porous spray pipe.

[0010] Furthermore, the porous spray pipe is installed on the top of the pickling reaction tank and arranged in a ring, and the porous spray pipe is provided with multiple nozzles.

[0011] Furthermore, an ultrasonic generator is provided on the outer wall of the pickling reaction vessel.

[0012] Furthermore, each of the aforementioned hydrothermal precarbonization reactors is connected to a nitrogen purging pipe.

[0013] Furthermore, the intelligent control unit includes a PID algorithm module and a timing controller.

[0014] The technical solution of this utility model has at least the following advantages and beneficial effects: By using two hydrothermal precarbonization reactors, one batch of material can be alternately fed into the pickling reactor, overcoming the capacity bottleneck of intermittent production and promoting capacity improvement; the effective operating time of a single reactor has increased from 40% to 85%, and the single-line capacity has reached 2.8t / day (traditional single reactor ≤1.5t / day).

[0015] The liquid-solid ratio (L / S=6:1-10:1) in the hydrothermal precarbonization reactor is dynamically adjusted during the reaction process by using a filtration system, thereby ensuring that the slurry has an acid washing coverage rate of ≥95% in the acid washing reaction tank, guaranteeing the purity of the bamboo charcoal precursor and improving product quality.

[0016] The intelligent control unit controls the two hydrothermal precarbonization reactors and pickling reactors respectively through the PID algorithm module and the timing controller. Through timing misalignment control and material relay transmission, it ensures that the pickling reactor is always in full-load operation: (1) Time allocation: The single-reactor hydrothermal precarbonization cycle (4-6h) is divided into heating period, constant temperature reaction period, and filtration transition period; (2) Phase difference design: The start time interval of the dual-reactor operation is 3 hours (take 50% of the single cycle), so that when one reactor finishes the reaction, the other reactor is in the middle of constant temperature, ensuring continuous feeding of the pickling tank, reducing energy consumption, increasing acid recycling rate, and adapting to the mass production demand of 10,000 tons of bamboo charcoal precursor materials. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of this utility model, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this utility model and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of the structure of the hydrothermal precarbonization-acid washing and purification continuous production device provided in Embodiment 1 of this utility model; Figure 2 This is a schematic diagram of the acid washing reaction vessel provided in Embodiment 1 of this utility model.

[0019] Icons: 1-Hydrothermal precarbonization reactor, 2-Filtering system, 3-Acid washing reaction tank, 4-Intelligent control unit, 5-Discharge pipe, 6-Feed pipe, 7-Slurry pump, 8-Nitrogen purging pipe, 31-Spiral agitator, 32-Porous spray pipe, 33-Spray head, 34-Ultrasonic generator. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. The components of the embodiments of this utility model described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0021] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0022] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0023] In the description of this utility model, it should be noted that if terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" appear to indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product is in use, they are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0024] In the description of this utility model, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0025] Example 1 Reference Figures 1-2 This embodiment provides a continuous hydrothermal precarbonization-acid washing purification production device, including two hydrothermal precarbonization reactors 1, a filtration system 2, an acid washing reaction tank 3, and an intelligent control unit 4. Each hydrothermal precarbonization reactor 1 is equipped with the filtration system 2. The outlet of each hydrothermal precarbonization reactor 1 is connected to a discharge pipe 5, and the inlet of each acid washing reaction tank 3 is connected to a feed pipe 6. The two discharge pipes 5 are respectively connected to the feed pipe 6, and a slurry pump 7 is installed on the feed pipe 6. The hydrothermal precarbonization reactor 1, the filtration system 2, the slurry pump 7, and the acid washing reaction tank 3 are all electrically connected to the intelligent control unit 4. It should be noted that each pipe in this device is equipped with a valve. The intelligent control unit 4 regulates the device temperature (±1℃), pressure (±0.1MPa), and liquid level (ultrasonic sensor ±0.5L accuracy).

[0026] In this embodiment, the lining of the hydrothermal precarbonization reactor 1 is made of Hastelloy C-276, and the inner wall is coated with polytetrafluoroethylene. The lining and coating are designed to resist HCl corrosion.

[0027] In this embodiment, the filtration system 2 includes a belt vacuum filter, which integrates an ultrasonic anti-clogging module. After removing the upper layer of liquid, the remaining liquid-to-solid ratio is adjusted.

[0028] In this embodiment, the filter screen pore size of the belt vacuum filter is ≤50μm.

[0029] In this embodiment, the pickling reaction tank 3 is equipped with a spiral agitator 31 and a porous spray pipe 32. The spiral agitator 31 and the porous spray pipe 32 can improve the pickling efficiency and pickling effect. The spiral agitator 31 is driven by a motor (not shown in the figure) for stirring.

[0030] In this embodiment, the porous spray pipe 32 is installed on the top of the pickling reaction tank 3 and arranged in a ring, and the porous spray pipe 32 is provided with a plurality of nozzles 33.

[0031] In this embodiment, an ultrasonic generator 34 is installed on the outer wall of the pickling reaction tank 3. The ultrasonic generator 34 includes a transducer and a vibrating plate. The transducer is fixedly connected to the outer wall of the tank, and an acoustic coupling layer is provided between the vibrating plate and the outer wall of the tank to transmit ultrasonic vibrations into the pickling solution inside the tank, thereby enhancing the peeling effect of the pickling solution on the oxide layer on the workpiece surface. The acoustic coupling layer is an acid-resistant silicone layer or a metal weld layer. The ultrasonic generator 34 is electrically connected to the intelligent control unit 4. The ultrasonic generator 34 assists in pickling, improving the pickling purification effect. The intelligent control unit 4 includes a PID algorithm module and a timing controller.

[0032] In this embodiment, each of the hydrothermal precarbonization reactors 1 is connected to a nitrogen purging pipe 8. The nitrogen purging pipe 8 facilitates cleaning of the reactor body.

[0033] The working process of a hydrothermal precarbonization-acid washing and purification continuous production unit is as follows: Step 1: Hydrothermal precarbonization: 40-mesh bamboo powder (moisture content ≤10%) and deionized water are added to hydrothermal precarbonization reactor 1 at a ratio of L / S=6:1, and the temperature is raised to 200℃ / 2.5MPa for 5 hours. Step 2: Vacuum filtration adjustment: Turn on the belt vacuum filter and remove the upper layer of liquid until the remaining L / S ratio is ≤3:1 (0.8kg of solid mass corresponds to ≤2.4L of liquid). Step 3: The intelligent control unit 4 implements timing misalignment control and material relay transfer through the PID algorithm module and timing controller. The materials from the two reactors are alternately injected into the pickling reaction tank 3, and 1.5MHCl is added to make L / S=3:1. The pickling is carried out for 3 hours with stirring (50rpm) and ultrasonic assistance (30kHz). The specific alternation process is shown in Table 1. Table 1

[0034] Step 4: Product: Bamboo charcoal precursor, SSA=8.5m 2 / g, Fe content <30ppm, initial efficiency 88.3% (half-cell test, 1C rate).

[0035] The following is a comparison between traditional split-type equipment and this device: Production capacity: Traditional split-type equipment: 1.2t / day; This unit: 2.8t / day. Acid consumption: Traditional split equipment consumes 1.3 tons / ton of product, while this unit consumes 0.9 tons / ton of product; Energy consumption: 1450 kWh / t for traditional split-type equipment, 850 kWh / t for this unit.

[0036] The above are merely preferred embodiments of this utility model and are not intended to limit the scope of this utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A continuous production apparatus for hydrothermal precarbonization-acid washing and purification, characterized in that: The device includes two hydrothermal precarbonization reactors, a filtration system, an acid washing reactor, and an intelligent control unit. Each hydrothermal precarbonization reactor is equipped with the filtration system. The outlet of each hydrothermal precarbonization reactor is connected to a discharge pipe, and the inlet of each acid washing reactor is connected to a feed pipe. The two discharge pipes are respectively connected to the feed pipe, and a slurry pump is installed on the feed pipe. The hydrothermal precarbonization reactor, the filtration system, the slurry pump, and the acid washing reactor are all electrically connected to the intelligent control unit.

2. The apparatus for continuous production of hydrothermal pre-carbonization and acid pickling purification according to claim 1, characterized in that, The lining of the hydrothermal precarbonization reactor is made of Hastelloy C-276, and the inner wall is coated with polytetrafluoroethylene.

3. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 1, characterized in that, The filtration system includes a belt vacuum filter, which integrates an ultrasonic anti-clogging module.

4. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 3, characterized in that, The filter screen pore size of the belt vacuum filter is ≤50μm.

5. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 1, characterized in that, The pickling reaction tank is equipped with a spiral agitator and a porous spray pipe.

6. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 5, characterized in that, The porous spray pipe is installed on the top of the pickling reaction tank and is arranged in a ring. The porous spray pipe is equipped with multiple nozzles.

7. The apparatus for continuous production of purified activated carbon black by hydrothermal pre-carbonization and acid washing according to claim 5, wherein An ultrasonic generator is installed on the outer wall of the pickling reaction tank.

8. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 1, characterized in that, Each of the aforementioned hydrothermal precarbonization reactors is connected to a nitrogen purging pipeline.

9. The apparatus for continuous production of purified pre-carbonized hydrothermal according to claim 1, characterized in that, The intelligent control unit includes a PID algorithm module and a timing controller.

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