Device and method for continuously preparing graphite oxide
阅读说明：本技术 一种连续制备氧化石墨的装置及其方法 (Device and method for continuously preparing graphite oxide ) 是由 陈成猛 孔庆强 孙国华 苏方远 李晓明 刘卓 黄显虹 李树珍 李正杰 康文杰 于 2019-12-06 设计创作，主要内容包括：本发明涉及一种连续制备氧化石墨的装置及其方法,属于氧化石墨制备技术领域,包括以下步骤：将石墨粉、硝酸钠、硫酸和氧化剂加入到低温反应器内,充分混合后,进入中温管式反应器中,进行氧化反应；物料流至溶剂管式混合器时加入溶剂,进入高温管式反应器中进行反应,之后在冷却管式反应器中冷却至室温；物料流至还原剂管式混合器时加入还原剂,再经后处理得到氧化石墨。本发明通过管道及管道混合器控制物料的混合及反应方式,克服了单纯的釜式反应器不能连续生产和单纯管道反应器的混料不均匀的弊端,生产过程安全、高效,产品质量稳定,既保证了反应过程中物料混合均匀度,又确保了连续性,利于工业化生产。(The invention relates to a device and a method for continuously preparing graphite oxide, belonging to the technical field of graphite oxide preparation and comprising the following steps: adding graphite powder, sodium nitrate, sulfuric acid and an oxidant into a low-temperature reactor, fully mixing, and then entering a medium-temperature tubular reactor for oxidation reaction; adding a solvent when the material flows to a solvent tubular mixer, reacting in a high-temperature tubular reactor, and cooling to room temperature in a cooling tubular reactor; adding a reducing agent when the material flows to the reducing agent tubular mixer, and carrying out post-treatment to obtain the graphite oxide. The invention controls the mixing and reaction modes of materials through the pipeline and the pipeline mixer, overcomes the defects that a pure kettle type reactor cannot continuously produce materials and the mixing of the pure pipeline reactor is not uniform, has safe and high-efficiency production process and stable product quality, ensures the mixing uniformity of the materials in the reaction process, ensures the continuity and is beneficial to industrial production.)
1. An apparatus for continuously preparing graphite oxide, which is characterized in that: comprises a low-temperature reactor, a medium-temperature reactor (17), a solvent mixer (18), a high-temperature reactor (19), a cooling reactor (20), a reducing agent mixer (21), a buffer tank (22) and a post-treatment system (37) which are connected in sequence;
the low-temperature reactor is a low-temperature tubular reactor (16), one end of the low-temperature tubular reactor (16) is provided with a feed inlet, the other end of the low-temperature tubular reactor (16) is provided with a discharge outlet, the first feeder (2) and the second feeder (3) are communicated with the feed inlet of the low-temperature tubular reactor (16) through pipelines, the sulfuric acid storage tank (1) is communicated with the feed inlet of the low-temperature tubular reactor (16) through a pipeline, and a delivery pump (13), an adjusting valve (6) and a flow meter (10) are sequentially arranged on the pipeline communicated with the feed inlet of the low-temperature tubular reactor (16) along the flow direction of sulfuric acid on the pipeline; the outside of the low-temperature tubular reactor (16) is wrapped with a temperature control jacket (23), and two ends of the temperature control jacket (23) are respectively provided with a low-temperature circulating liquid interface (A1, A2);
a discharge hole is formed in the upper end of the medium-temperature reactor (17), a feed hole is formed in the lower end of the medium-temperature reactor (17), the discharge hole of the low-temperature tubular reactor (16) is communicated with the feed hole of the medium-temperature reactor (17) through a pipeline, a temperature control jacket (24) is wrapped outside the medium-temperature reactor (17), and medium-temperature circulating liquid interfaces (B1 and B2) are respectively arranged on the upper portion and the lower portion of the temperature control jacket (24);
a discharge hole is formed in the upper end of the solvent mixer (18), a feed hole is formed in the lower end of the solvent mixer (18), the discharge hole of the medium-temperature reactor (17) is communicated with the feed hole of the solvent mixer (18) through a pipeline (29), the solvent storage tank (4) is communicated with the feed hole of the solvent mixer (18) through a pipeline (30), and a conveying pump (14), an adjusting valve (7) and a flow meter (11) are sequentially arranged on the pipeline (30) along the flowing direction of the solvent; the solvent mixer (18) is externally wrapped with a temperature control jacket (25), and the upper part and the lower part of the temperature control jacket (25) are respectively provided with medium-temperature circulating liquid interfaces (B3 and B4);
a discharge hole is formed in the upper end of the high-temperature reactor (19), a feed hole is formed in the lower end of the high-temperature reactor (19), the discharge hole of the solvent mixer (18) is communicated with the feed hole of the high-temperature reactor (19) through a pipeline (31), a temperature control jacket (26) is wrapped outside the high-temperature reactor (19), and high-temperature circulating liquid interfaces (C1 and C2) are respectively arranged on the upper portion and the lower portion of the temperature control jacket (26);
a discharge hole is formed in the upper end of the cooling reactor (20), a feed hole is formed in the lower end of the cooling reactor (20), the discharge hole of the high-temperature reactor (19) is communicated with the feed hole of the cooling reactor (20) through a pipeline (32), a temperature control jacket (27) is wrapped outside the cooling reactor (20), and medium-temperature circulating liquid interfaces (B5 and B6) are respectively arranged on the upper portion and the lower portion of the temperature control jacket (27);
a discharge hole is formed in the upper end of the reducing agent mixer (21), a feed hole is formed in the lower end of the reducing agent mixer (21), the discharge hole of the cooling reactor (20) is communicated with the feed hole of the reducing agent mixer (21) through a pipeline (33), the reducing agent storage tank (5) is communicated with the feed hole of the reducing agent mixer (21) through a pipeline (34), and a conveying pump (15), an adjusting valve (8) and a flowmeter (12) are sequentially arranged on the pipeline (34) along the flow direction of the reducing agent;
the upper end of buffer tank (22) is provided with the feed inlet, and the lower extreme of buffer tank (22) is provided with the discharge gate, and discharge gate department is provided with baiting valve (9), the discharge gate of reductant blender (21) passes through the feed inlet intercommunication of pipeline (35) and buffer tank (22), and the discharge gate of buffer tank (22) passes through the feed inlet intercommunication of pipeline (36) and aftertreatment system (37).
2. The apparatus for continuously preparing graphite oxide according to claim 1, wherein: the low-temperature reactor comprises at least two low-temperature kettle type reactors connected in parallel, and each low-temperature kettle type reactor is alternately communicated with the medium-temperature reactor (17).
3. The apparatus for continuously preparing graphite oxide according to claim 2, wherein: the low-temperature kettle type reactor comprises a first low-temperature kettle type reactor (16A) and a second low-temperature kettle type reactor (16B) which are connected in parallel, the upper end of the first low-temperature kettle type reactor (16A) and the upper end of the second low-temperature kettle type reactor (16B) are arranged as feed inlets, the lower end of the first low-temperature kettle type reactor (16A) and the lower end of the second low-temperature kettle type reactor (16B) are arranged as discharge outlets, the discharge outlets are communicated with a conveying pump (38) through a pipeline (28), and discharge valves (41 and 42) are arranged at the discharge outlets; the first feeding machines (2A, 2B) and the second feeding machines (3A, 3B) are respectively communicated with the feeding holes of the first low-temperature kettle type reactor (16A) and the second low-temperature kettle type reactor (16B) through pipelines, the sulfuric acid storage tank (1) is respectively communicated with the feeding holes of the first low-temperature kettle type reactor (16A) and the second low-temperature kettle type reactor (16B) through pipelines, and a conveying pump (13), a regulating valve (6) and a flow meter (10) are sequentially arranged on a main pipeline of the sulfuric acid storage tank (1) communicated with the first low-temperature kettle type reactor (16A) and the second low-temperature kettle type reactor (16B); the first low-temperature kettle type reactor (16A) and the second low-temperature kettle type reactor (16B) are respectively wrapped with temperature control jackets (23A, 23B), and the upper part and the lower part of each temperature control jacket (23A, 23B) are respectively provided with a low-temperature circulating liquid interface (A1, A2, A3, A4); the conveying pump (38) is communicated with a feed inlet of the medium-temperature reactor (17) through a pipeline, and a flow meter (39) and an adjusting valve (40) are sequentially arranged on the pipeline through which the conveying pump (38) is communicated with the feed inlet of the medium-temperature reactor (17).
4. The apparatus for continuously preparing graphite oxide according to claim 1, wherein: the medium-temperature reactor (17), the solvent mixer (18), the high-temperature reactor (19), the cooling reactor (20) and the reducing agent mixer (21) are all tubular reactors.
5. The apparatus for continuously preparing graphite oxide according to claim 1, wherein: the first feeders (2A, 2B) are graphite powder and sodium nitrate mixture feeders, and the second feeders (3A, 3B) are potassium permanganate feeders.
6. The apparatus for continuously preparing graphite oxide according to claim 1, wherein: the low-temperature circulating liquid interfaces (A1, A2, A3 and A4) are communicated with the low-temperature tank through pipelines to form a low-temperature circulating liquid loop, the medium-temperature circulating liquid interfaces (B5 and B6) are communicated with the medium-temperature tank through pipelines to form a medium-temperature circulating liquid loop, and the high-temperature circulating liquid interfaces (C1 and C2) are communicated with the high-temperature tank through pipelines to form a high-temperature circulating loop.
7. A method for continuously preparing graphite oxide using the apparatus for continuously preparing graphite oxide according to claim 1, comprising the steps of:
s1, weighing raw materials including graphite powder, sodium nitrate, sulfuric acid and potassium permanganate, wherein the mass ratio of the graphite powder to the sodium nitrate to the sulfuric acid to the potassium permanganate is 1 (0.1-1) to 30-80 (1-5), adding the raw materials into a low-temperature reactor, and mixing at the temperature of-5 ℃ for 1-2 hours to prepare a first mixture;
s2, conveying the first mixture prepared in the step S1 to a medium-temperature reactor (17), and reacting at the temperature of 30-45 ℃ for 1-5 hours to prepare a second mixture;
s3, conveying the second mixture prepared in the step S2 to a solvent mixer (18), and diluting the second mixture by using a solvent to prepare a third mixture; the solvent is deionized water, and the mass ratio of the solvent to the graphite powder is 40-100: 1;
s4, conveying the third mixture prepared in the step S3 to a high-temperature reactor (19), and reacting at the temperature of 90-110 ℃ for 1-5 hours to prepare a fourth mixture;
s5, conveying the fourth mixture prepared in the step S4 to a cooling reactor (20), and cooling to 30-45 ℃ to prepare a fifth mixture;
s6, conveying the fifth mixture prepared in the step S5 to a reducing agent mixer (21), and reducing the fifth mixture by using a reducing agent to prepare a sixth mixture;
and S7, carrying out post-treatment on the sixth mixture prepared in the step S6 by a post-treatment system (37) to prepare a graphite oxide solution, and drying the graphite oxide solution to prepare graphite oxide powder.
8. The method for continuously preparing graphite oxide according to claim 7, wherein: in the step S2, the flow rate of the first mixture in the medium temperature reactor is 0.7-3.5 m/min.
9. The method for continuously preparing graphite oxide according to claim 7, wherein: in the step S6, the reducing agent is hydrogen peroxide, and the mass ratio of the reducing agent to the graphite powder is 1-20: 1.
10. The method for continuously preparing graphite oxide according to claim 7, wherein: in step S7, the post-treatment includes one or more of sedimentation, centrifugation, and filtration.
11. The method for continuously preparing graphite oxide according to claim 7, wherein: in the step S7, the oxygen content of the prepared graphite oxide powder is 25 to 48 wt%.
Technical Field
The invention belongs to the technical field of graphite oxide preparation, and particularly relates to a device and a method for continuously preparing graphite oxide.
Background
Graphene is a novel carbon material with a two-dimensional honeycomb lattice structure composed of a single layer of carbon atoms. Due to the unique structure and excellent performance, the composite material has wide application in the fields of composite materials, energy storage, corrosion prevention, electromagnetic shielding and the like. The redox method is a mainstream method for preparing graphene powder on a large scale at present, and has the advantages of low cost and high stripping degree. The graphite oxide is an important intermediate for preparing graphene by a redox method, and the performance of the graphite oxide directly determines the quality of the prepared graphene material. In addition, the special properties of the polymer also enable the polymer to be widely applied to biomedicine, modified polymer materials and the like.
The first synthesis of graphite oxide dates back to the Brodie method in 1898, after which Staudenmaier and Hummers methods, etc. appeared. In all three oxidation methods, graphite is treated with a strong protonic acid to form a graphite intercalation compound, and then a strong oxidant is added to oxidize the graphite intercalation compound. Wherein the Brodie method adopts fuming HNO3And KClO3As oxidizing agent, the Staudemaier process uses concentrated H2SO4And fuming HNO3The mixed acid of (2) is used for treating graphite, and KClO is also adopted3As an oxidizing agent. Both the Staudenmeier and Brodie processes produce toxic ClO2Gas, both reactions should be carried out in a fume hood. Hummers' law uses concentrated H2SO4、NaNO3And KMnO4As an oxidizing agent, the method is superior to other two methodsThe method is safer, the excessive high manganese acid radical ions used in the method can cause pollution, and H is required to be used2O2The treatment was carried out and then the separation was carried out thoroughly by washing with water. The preparation process of Hummers method is deeply studied by Friedel and the like, and is divided into three stages of low-temperature, medium-temperature and high-temperature reaction, and graphite and KMnO are pointed out4Dosage, concentration H2SO4The volume, the reaction time at low temperature, the water addition method in the reaction at high temperature are the main factors affecting the structure and performance of the final product, and the reaction starts from the edge of graphite and is oxidized at KMnO4Driven to form H2SO4-a graphite intercalation compound. In the Hummers method, concentrated sulfuric acid and potassium permanganate are mixed to generate high-activity manganese dioxide, and when a traditional kettle-type reactor is adopted, the reaction temperature needs to be strictly controlled, otherwise, safety accidents are easily caused. In addition, the graphite oxide prepared by the kettle type reactor has the defects of uneven material mixing and the like.
CN106882803B discloses a method and an apparatus for preparing graphene oxide, but the method only uses a mixing kettle for mixing graphite, acid and oxidant, and when continuous feeding and discharging, the materials enter the subsequent pipeline reactor without being mixed uniformly, which affects the consistency of the product; after the reaction of the first pipeline reactor is finished, the temperature of the materials is 20-150 ℃, the concentrated acid can be diluted after the solvent is added into the mixer, so that a large amount of dilution heat is generated, and the temperature of the reaction liquid in the mixer is further increased to be far higher than the decomposition temperature (55 ℃) of manganese sesquioxide due to the fact that the mixer is not externally connected with a cooler, so that explosion can be caused. In addition, in the patent, a reducing agent (hydrogen peroxide) and a solvent are added into a mixer at the same time, the hydrogen peroxide is decomposed violently at an excessively high temperature, potassium permanganate and manganese dioxide cannot be reduced into soluble divalent manganese ions, and a large amount of manganese impurities still exist in the obtained graphene oxide after subsequent purification treatment.
Disclosure of Invention
In order to overcome the defects of the technical problems, the invention provides a device and a method for continuously preparing graphite oxide.
The invention is realized by the following technical scheme.
An apparatus for continuously preparing graphite oxide, wherein: the system comprises a low-temperature reactor, a medium-temperature reactor, a solvent mixer, a high-temperature reactor, a cooling reactor, a reducing agent mixer, a buffer tank and an aftertreatment system which are connected in sequence;
the low-temperature reactor is a low-temperature tubular reactor, one end of the low-temperature tubular reactor is provided with a feed inlet, the other end of the low-temperature tubular reactor is provided with a discharge outlet, the first feeder 2 and the second feeder 3 are communicated with the feed inlet of the low-temperature tubular reactor through pipelines, the sulfuric acid storage tank is communicated with the feed inlet of the low-temperature tubular reactor through a pipeline, and a
the upper end of the medium-temperature reactor is provided with a discharge hole, the lower end of the medium-temperature reactor is provided with a feed hole, the discharge hole of the low-temperature tubular reactor is communicated with the feed hole of the medium-temperature reactor through a pipeline, the outside of the medium-temperature reactor is wrapped by a
the upper end of the solvent mixer is provided with a discharge hole, the lower end of the solvent mixer is provided with a feed hole, the discharge hole of the medium temperature reactor is communicated with the feed hole of the solvent mixer through a pipeline, the solvent storage tank is communicated with the feed hole of the solvent mixer through a
the upper end of the high-temperature reactor is provided with a discharge hole, the lower end of the high-temperature reactor is provided with a feed hole, the discharge hole of the solvent mixer is communicated with the feed hole of the high-temperature reactor through a
the upper end of the cooling reactor is provided with a discharge hole, the lower end of the cooling reactor is provided with a feed hole, the discharge hole of the high-temperature reactor is communicated with the feed hole of the cooling reactor through a
the upper end of the reducing agent mixer is provided with a discharge hole, the lower end of the reducing agent mixer is provided with a feed hole, the discharge hole of the cooling reactor is communicated with the feed hole of the reducing agent mixer through a
the upper end of buffer tank is provided with the feed inlet, and the lower extreme of buffer tank is provided with the discharge gate, and discharge gate department is provided with
Further, the low-temperature reactor comprises at least two low-temperature kettle type reactors connected in parallel, and each low-temperature kettle type reactor is alternately communicated with the medium-temperature reactor.
Further, the low-temperature kettle type reactor comprises a first low-temperature kettle type reactor and a second low-temperature kettle type reactor which are connected in parallel, the upper end of the first low-temperature kettle type reactor and the upper end of the second low-temperature kettle type reactor are set as feed inlets, the lower end of the first low-temperature kettle type reactor and the lower end of the second low-temperature kettle type reactor are set as discharge outlets, the discharge outlets are communicated with the
Further, the medium temperature reactor, the solvent mixer, the high temperature reactor, the cooling reactor and the reducing agent mixer are all tubular reactors.
Further, the
Furthermore, low-temperature circulating liquid ports A1, A2, A3 and A4 are communicated with the low-temperature tank through pipelines to form a low-temperature circulating liquid loop, medium-temperature circulating liquid ports B5 and B6 are communicated with the medium-temperature tank through pipelines to form a medium-temperature circulating liquid loop, and high-temperature circulating liquid ports C1 and C2 are communicated with the high-temperature tank through pipelines to form a high-temperature circulating loop.
A method for continuously preparing graphite oxide using an apparatus for continuously preparing graphite oxide, comprising the steps of:
s1, weighing raw materials including graphite powder, sodium nitrate, sulfuric acid and potassium permanganate, wherein the mass ratio of the graphite powder to the sodium nitrate to the sulfuric acid to the potassium permanganate is 1 (0.1-1) to 30-80 (1-5), adding the raw materials into a low-temperature reactor, and mixing at the temperature of-5 ℃ for 1-2 hours to prepare a first mixture;
s2, conveying the first mixture prepared in the step S1 to a medium-temperature reactor, and reacting at the temperature of 30-45 ℃ for 1-5 hours to prepare a second mixture;
s3, conveying the second mixture obtained in the step S2 to a solvent mixer, and diluting the second mixture by using a solvent to obtain a third mixture; the solvent is deionized water, and the mass ratio of the solvent to the graphite powder is 40-100: 1;
s4, conveying the third mixture prepared in the step S3 to a high-temperature reactor, and reacting at the temperature of 90-110 ℃ for 1-5 hours to prepare a fourth mixture;
s5, conveying the fourth mixture prepared in the step S4 to a cooling reactor, and cooling to 30-45 ℃ to prepare a fifth mixture;
s6, conveying the fifth mixture prepared in the step S5 to a reducing agent mixer, and reducing the fifth mixture by using a reducing agent to prepare a sixth mixture;
and S7, carrying out post-treatment on the sixth mixture prepared in the step S6 by a post-treatment system to prepare a graphite oxide solution, and drying the graphite oxide solution to prepare graphite oxide powder.
Further, in the step S2, the flow rate of the first mixture in the medium temperature reactor is 0.7-3.5 m/min.
Further, in the step S6, the reducing agent is hydrogen peroxide, and the mass ratio of the reducing agent to the graphite powder is 1-20: 1.
Further, in the step S7, the post-treatment includes one or a combination of sedimentation, centrifugation and filtration.
Further, in the step S7, the oxygen content of the prepared graphite oxide powder is 25 to 48 wt%.
According to the technical scheme, raw materials of graphite powder, sodium nitrate, sulfuric acid and potassium permanganate are added into a low-temperature reactor to perform low-temperature reaction, then the mixture is conveyed into a medium-temperature reactor to perform medium-temperature reaction, a second mixture of a product obtained through the medium-temperature reaction is conveyed into a solvent mixer to be diluted by a solvent, then the mixture is conveyed into the high-temperature reactor to perform high-temperature reaction, a fourth mixture of a product obtained after the high-temperature reaction is cooled in a cooling reactor, a fifth mixture obtained after the cooling is subjected to reduction reaction in a reducing agent mixer, and then the sixth mixture is subjected to post-treatment such as settling, centrifuging and filtering to obtain a graphite oxide solution. The raw materials are carried out under the coordination of the reaction conditions, the graphite oxide solution with stable product quality can be continuously prepared, the oxygen content of the graphite oxide powder obtained after drying can reach 25-48wt%, the purity is more than or equal to 99.9 wt%, the content of metal impurities is extremely low, and the manganese content is less than or equal to 50 ppm.
Meanwhile, the invention also provides a special device for realizing the preparation method, which comprises a low-temperature reactor, a medium-temperature tubular reactor, a solvent tubular mixer, a high-temperature tubular reactor, a cooling tubular reactor, a reducing agent tubular mixer, a buffer tank and a post-treatment system which are connected in sequence, wherein the low-temperature reactor is a low-temperature tubular reactor and/or a low-temperature kettle type reactor.
If the low-temperature reactors are low-temperature kettle type reactors, the number of the low-temperature kettle type reactors is at least two, the outlet ends of the two low-temperature kettle type reactors are connected with the inlet end of the medium-temperature tubular reactor, and the outlet ends of the two low-temperature kettle type reactors are provided with regulating valves so as to realize the alternate communication of the two low-temperature kettle type reactors and the medium-temperature tubular reactor and further realize the continuous production of the graphite oxide. If the low-temperature reactor is a low-temperature tubular reactor, the low-temperature tubular reactor is directly mixed with the medium-temperature tubular reactor, the raw materials are fully mixed by controlling the reaction of the raw materials in the low-temperature tubular reactor, and then the raw materials are continuously fed into the medium-temperature tubular reactor, so that the continuous production of the graphite oxide is realized.
Furthermore, the low-temperature reactor in the device provided by the invention is provided with a feed inlet, a feeder and a liquid conveyor are arranged at the feed inlet, and the liquid conveyor comprises a liquid storage tank, a conveying pump, a flowmeter and an adjusting valve which are communicated with the low-temperature reactor through a pipeline; wherein, the peripheries of the low-temperature reactor, the medium-temperature tubular reactor, the solvent tubular mixer and the high-temperature tubular reactor are all provided with constant-temperature jackets.
The constant-temperature jackets are arranged on the peripheries of the low-temperature reactor, the medium-temperature tubular reactor, the solvent tubular mixer and the high-temperature tubular reactor, and the temperature of the constant-temperature jackets on the periphery of the low-temperature reactor is kept between-5 ℃ and 5 ℃, so that reaction materials can be fully and uniformly mixed before the medium-temperature reaction starts.
If a low-temperature kettle type reactor is adopted, the feeder is positioned at the upper part of the feed inlet of the low-temperature reaction kettle and is connected with the feed inlet through a pipeline; if a low-temperature tubular mixer is adopted, the guide pipes connected with the low-temperature tubular mixer are respectively provided with a feeding machine; the liquid storage tank is a sulfuric acid storage tank, the input end of the low-temperature kettle type reactor (or the low-temperature tubular mixer) is connected with the sulfuric acid storage tank through a pipeline, and a sulfuric acid delivery pump, a flow meter and an adjusting valve are sequentially arranged on the pipeline connecting the sulfuric acid storage tank and the low-temperature kettle type reactor (or the low-temperature tubular mixer).
Furthermore, the input end of the solvent tube mixer is connected with a solvent storage tank through a pipeline, and a solvent delivery pump, a flow meter and an adjusting valve are sequentially arranged on the pipeline connecting the solvent storage tank and the solvent tube mixer; the input end of the reducing agent tubular mixer is connected with a reducing agent storage tank through a pipeline, and a reducing agent delivery pump, a flowmeter and an adjusting valve are sequentially arranged on the pipeline connecting the reducing agent storage tank and the reducing agent tubular mixer.
In the invention, the output end of the low-temperature kettle type reactor (or the low-temperature tubular mixer) is connected with the input end of the medium-temperature tubular reactor through a connecting pipeline, a delivery pump, a flowmeter and a regulating valve are arranged on the connecting pipeline, the output end of the medium temperature tubular reactor is connected with the input end of the solvent tubular mixer through a connecting pipeline, the output end of the solvent tubular mixer is connected with the input end of the high-temperature tubular reactor through a connecting pipeline, the output end of the high-temperature tubular reactor is connected with the input end of the cooling tubular reactor through a connecting pipeline, the output end of the cooling tubular reactor is connected with the input end of the reducing agent tubular mixer through a connecting pipeline, the output end of the reducing agent tubular mixer is connected with the buffer tank through a connecting pipeline, and the input end of the post-treatment system is connected with a valve at the bottom of the buffer tank through a connecting pipeline.
According to the technical scheme of the invention, the inventor of the invention finds that the method for preparing the graphite oxide is matched with the device, so that the continuous preparation of the high-quality graphite oxide can be further effectively realized. The oxygen content of the graphite oxide powder obtained by drying the graphite oxide solution prepared by the method is 25-48wt%, the purity is more than or equal to 99.9 wt%, the content of metal impurities is extremely low, and the content of manganese is less than or equal to 50 ppm.
The invention has the beneficial effects that: the invention controls the mixing and reaction modes of materials through the pipeline and the pipeline mixer, overcomes the defects that the common kettle type reactor can not continuously produce and the material mixing of a simple pipeline reactor is not uniform, is carried out at the temperature of 30-45 ℃ in the stages of adding water and hydrogen peroxide, prevents the temperature of reaction liquid from being overhigh, ensures the safety and the high efficiency of the production process, has low manganese content of products, ensures the uniformity of material mixing in the reaction process, ensures the continuity and is beneficial to industrial production.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic view of the overall structure of a tubular reactor using a low temperature according to the present invention;
in the figure 1, 1 is a sulfuric acid storage tank, 2 is a graphite powder and sodium nitrate mixture feeder, 3 is a potassium permanganate feeder, 4 is a solvent storage tank, 5 is a reducing agent storage tank, 6-8 is a regulating valve, 9 is a discharge valve, 10-12 are flow meters, 13-15 are delivery pumps, 16 is a low-temperature tubular mixer, 17 is an intermediate-temperature tubular reactor, 18 is a solvent tubular mixer, 19 is a high-temperature tubular reactor, 20 is a cooling tubular reactor, 21 is a reducing agent tubular mixer, 22 is a buffer tank, 23-27 are temperature-control jackets, 28-36 are connecting pipes, 37 is a post-treatment system, A1 and A2 are low-temperature circulating liquid interfaces, B1, B2, B3, B4, B5 and B6 are intermediate-temperature circulating liquid interfaces, and C1 and C2 are high-temperature circulating liquid interfaces.
FIG. 2 is a schematic structural diagram of the present invention in which two low-temperature reaction vessels are alternately used;
in fig. 2, 1 is a sulfuric acid storage tank, 2A and 2B are graphite powder and sodium nitrate mixture feeders, 3A and 3B are potassium permanganate feeders, 4 is a solvent storage tank, 5 is a reducing agent storage tank, 9, 41 and 42 are discharge valves, 6 to 8 and 40 are regulating valves, 10 to 12 and 39 are flow meters, 13 to 15 and 38 are delivery pumps, 16A to 16B are low-temperature reaction kettles, 17 is a medium-temperature tubular reactor, 18 is a solvent tubular mixer, 19 is a high-temperature tubular reactor, 20 is a cooling tubular reactor, 21 is a reducing agent tubular mixer, 22 is a buffer tank, 23A and 23B, 24-27 are temperature control jackets, 28-36 are connecting pipes, 37 is a post-treatment system, A1, A2, A3 and A4 are low-temperature circulating liquid interfaces, B1, B2, B3, B4, B5 and B6 are medium-temperature circulating liquid interfaces, and C1 and C2 are high-temperature circulating liquid interfaces.
Detailed Description
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