CN111574858A - Method for removing organic matters in carbon black by-product in preparation of acetylene by partial oxidation of natural gas - Google Patents
Method for removing organic matters in carbon black by-product in preparation of acetylene by partial oxidation of natural gas Download PDFInfo
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- CN111574858A CN111574858A CN201910117196.5A CN201910117196A CN111574858A CN 111574858 A CN111574858 A CN 111574858A CN 201910117196 A CN201910117196 A CN 201910117196A CN 111574858 A CN111574858 A CN 111574858A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
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Abstract
The invention belongs to the technical field of separation of gas or steam by injecting a reactant, and particularly relates to a method for removing organic matters in a byproduct carbon black generated in preparation of acetylene by partial oxidation of natural gas, which comprises the following steps: A. and (3) drying: reducing the water content in the carbon black to be less than or equal to 30 percent; B. removing: placing the carbon black with the water content of less than or equal to 30% in an activation furnace, adding inert gas for reaction, and adding a weak oxidant into the activation furnace for oxidation reaction after the reaction is finished. The method well modifies the structure of the carbon black, can effectively remove organic matters in the carbon black, and improves the quality of the carbon black; reduces the environmental pollution, recycles the carbon black and improves the resource utilization rate.
Description
Technical Field
The invention belongs to the technical field of separation of gas or steam by injecting a reactant, and particularly relates to a method for removing organic matters in a byproduct carbon black in preparation of acetylene by partial oxidation of natural gas.
Background
Acetylene is a very important organic chemical raw material, and is widely used in the fields of metal processing, welding, cutting and the like, and the preparation of chemical products such as ethylene, vinyl chloride, trichloroethylene, vinyl acetate, acrylonitrile, polyacrylonitrile, 1, 4-butanediol and the like ("the acetylene is newly developed in organic synthetic chemistry", step winning, China chemical trade, No. 7, No. 22, No. 103, published Japanese 2015, 12 and 31 days; "research progress of acetylene preparation by low-carbon alkane pyrolysis by thermal plasma", Subaogen and the like, chemical reaction engineering and processes, No. 29, No. 3, No. 230, 236 pages, and published Japanese 2013, 06 and 30 months). The preparation method of acetylene mainly comprises a non-catalytic partial oxidation method, an electric arc method, a plasma method and the like, wherein the electric arc method is eliminated due to high energy consumption, the plasma method is still in a test stage (the current state of research of natural gas acetylene, thinking, angry, vinylon communication, No. 33, No. 2, No. 15-20, No. 2013, No. 12, No. 31 in 2013), the power consumption is high, the requirements on equipment are harsh, the method is difficult to popularize and apply so far, and the non-catalytic partial oxidation method is a main method for producing acetylene.
The process for preparing acetylene by partial oxidation of natural gas mainly comprises a desulfurization device process, an oxygen preparation device process, a cracking section process and a concentration section process. Wherein, the natural gas in the cracking process passes through an acetylene furnace to generate cracked gas through partial oxidation reaction, and the generated byproduct carbon black passes through carbon black water formed by spray water in an electric filter and a cooling tower. The carbon black water enters the degassing tank through the carbon black water main pipe and then enters the carbon black separation tank, and the carbon black water is subjected to treatment by the method of separation, sedimentation, concentration and the like of the device to remove carbon black in the carbon black water, so that the carbon black water is recycled. The carbon black as a byproduct has high water content, contains more organic matters and other impurities (collectively referred to as impurities), and the organic matters mainly comprise polycyclic aromatic hydrocarbons.
At present, the by-product carbon black produced by acetylene preparation from natural gas is treated as solid waste in China by adopting methods of landfill and boiler incineration, so that the environment is polluted and carbon black resources are wasted. And the carbon black is directly dried and removed, so that the application effect of the obtained byproduct carbon black product is not ideal, and the organic matter contained in the carbon black can cause poor quality of the carbon black, block the gaps of the carbon black and influence the service performance, so that the acetylene byproduct carbon black cannot be directly used after being dried and dehydrated.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for removing organic matters from carbon black, which is a byproduct of acetylene production by partial oxidation of natural gas, and the method can effectively remove organic matters from carbon black, improve the quality of carbon black, reduce environmental pollution, recover carbon black, and improve the resource utilization rate.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method for removing organic matters in the carbon black byproduct in the preparation of acetylene by partial oxidation of natural gas comprises the following steps:
A. and (3) drying: reducing the water content in the carbon black to be less than or equal to 30 percent;
B. removing: placing the carbon black with the water content of less than or equal to 30% in an activation furnace, adding inert gas for reaction, and adding a weak oxidant into the activation furnace for oxidation reaction after the reaction is finished.
The water content is a mass content.
The method can effectively remove organic matters in the carbon black and improve the quality of the carbon black.
The method reduces environmental pollution, recovers carbon black, and improves resource utilization rate.
Further, the temperature of the carbon black in the drying process is 100-125 ℃.
Further, the drying is realized by electric heating, steam heating or high-temperature flue gas heating.
Further, the drying is drying in a high-temperature flue gas heating mode.
Further, the inert gas refers to nitrogen, helium, neon, argon, krypton, xenon or radon.
Further, the reaction temperature of the carbon black and the inert gas is 150-800 ℃, and the time is 10-150 min.
Further, the amount of the inert gas is 1.1-5% of the mass of the carbon black.
Further, the weak oxidant refers to water vapor, carbon dioxide, hydrogen peroxide or calcium carbonate.
The hydrogen peroxide is of any concentration.
Further, the reaction temperature of the carbon black and the weak oxidant is 500-1000 ℃, and the reaction time is 30-180 min.
Further, the dosage of the weak oxidant is 2.3-7.9% of the mass of the carbon black.
Furthermore, the relative pressure of the activation furnace is less than 0.04 MPa.
Further, the relative pressure of the activation furnace is 0-0.04 MPa.
Further, in the removing process, the gas is isolated from the strong oxidant.
Further, the gas strong oxidant refers to oxygen, air or ozone.
The invention has the beneficial effects that:
the method of the invention well modifies the structure of the carbon black.
The method can effectively remove organic matters in the carbon black and improve the quality of the carbon black. The iodine absorption value and the oil absorption value of the carbon black treated by the method are obviously improved; the heating decrement is greatly reduced, and the toluene light transmittance is obviously improved.
The method of the invention reduces the environmental pollution, recycles the carbon black and improves the resource utilization rate.
The invention provides a feasible method for the treatment of the byproduct carbon black in the preparation of acetylene from natural gas at present, effectively protects the environment, changes waste into valuable, and has certain environmental protection benefit and economic benefit.
Drawings
Fig. 1 is a flow chart of the process for removing organic matters from the carbon black by-product of acetylene preparation by partial oxidation of natural gas, wherein 1 is a dryer, 2 is an activation furnace, 1 is an inert gas, and 2 is a weak oxidant.
Detailed Description
The examples are provided for better illustration of the present invention, but the present invention is not limited to the examples. Therefore, those skilled in the art should make insubstantial modifications and adaptations to the embodiments of the present invention in light of the above teachings and remain within the scope of the invention.
The following water contents were measured in accordance with GB/T3780.8-2008 determination of heating loss of carbon black part 8;
the iodine uptake value was measured according to GB/T3780.1-2015 carbon black part 1 iodine uptake value test method;
the following oil absorption values are detected according to GB/T3780.2-2017 determination of oil absorption value of part 2 of carbon black;
the toluene light transmittance is detected according to GB/T3780.15-2016 determination of 15 th part toluene extract light transmittance of carbon black;
the heating weight loss was measured in accordance with GB/T3780.8-2008 about measurement of heating weight loss of carbon black part 8;
specific surface area measurement according to the nitrogen adsorption method for measuring the total surface area and the external surface area of GBT/10722-2014 carbon black, and then according to the formula
Calculating the specific surface area;
the 45 μm sieve residue was measured according to GB/T3780.21-2016 method for measuring Water flushing of part 21 carbon black sieve residue, and the mesh size was 45 μm.
Example 1
Organic matters in the acetylene byproduct carbon black are removed according to the flow shown in figure 1, and the specific process flow is as follows:
A. and (3) drying: putting carbon black (a by-product from partial oxidation of natural gas to acetylene) with water content of 50% into an electric heating drying device at 100 ℃ to reduce the water content of the carbon black to 30%;
B. removing: controlling the relative pressure of the activation furnace to be 0.4MPa, isolating oxygen, air and ozone, filling carbon black with the water content of 30% into the activation furnace, adding nitrogen with the mass of 1.12% of that of the carbon black, heating the activation furnace to 500 ℃, and reacting for 90min at the temperature of 500 ℃; after the reaction is finished, adding water vapor with the mass of 2.37 percent of that of the carbon black into the activation furnace, heating the activation furnace to 900 ℃, and reacting for 150min at the temperature of 900 ℃.
Example 2
Organic matters in the acetylene byproduct carbon black are removed according to the flow shown in figure 1, and the specific process flow is as follows:
A. and (3) drying: putting the carbon black (a by-product from the partial oxidation of natural gas to acetylene) with the water content of 85 percent into steam heating drying equipment at 125 ℃ to reduce the water content of the carbon black to 25 percent;
B. removing: controlling the relative pressure of the activation furnace to be 0MPa, isolating oxygen, air and ozone, filling carbon black with the water content of 30% into the activation furnace, adding helium with the mass of 5% of the carbon black, heating the activation furnace to 800 ℃, and reacting for 60min at the temperature of 800 ℃; after the reaction is finished, adding carbon dioxide with the mass of 7.9% of that of the carbon black into the activation furnace, heating the activation furnace to 950 ℃, and reacting for 30min at the temperature of 950 ℃.
Example 3
Organic matters in the acetylene byproduct carbon black are removed according to the flow shown in figure 1, and the specific process flow is as follows:
A. and (3) drying: putting carbon black (a by-product from the partial oxidation of natural gas to acetylene) with the water content of 60% into steam heating drying equipment at the temperature of 110 ℃ to reduce the water content of the carbon black to 20%;
B. removing: controlling the relative pressure of the activation furnace to be 0.2MPa, isolating oxygen, air and ozone, filling carbon black with the water content of 20% into the activation furnace, adding radon gas with the mass of 3% of the carbon black, heating the activation furnace to 150 ℃, and reacting for 90min at the temperature of 150 ℃; after the reaction is finished, adding calcium carbonate accounting for 3% of the mass of the carbon black into the activation furnace, heating the activation furnace to 900 ℃, and reacting for 90min at the temperature of 900 ℃.
Example 4
Organic matters in the acetylene byproduct carbon black are removed according to the flow shown in figure 1, and the specific process flow is as follows:
A. and (3) drying: putting carbon black (a by-product from partial oxidation of natural gas to acetylene) with the water content of 70% into high-temperature flue gas heating and drying equipment at 115 ℃ to reduce the water content of the carbon black to 25%;
B. removing: controlling the relative pressure of the activation furnace to be 0.25MPa, isolating oxygen, air and ozone, filling carbon black with the water content of 25% into the activation furnace, adding neon with the mass of 1.5% of that of the carbon black, heating the activation furnace to 600 ℃, and reacting for 10min at the temperature of 600 ℃; after the reaction is finished, hydrogen peroxide with the mass fraction of 80 percent and the mass percent of 4 percent of carbon black is added into the activation furnace, the temperature of the activation furnace is raised to 600 ℃, and the reaction is carried out for 120min at the temperature of 600 ℃.
Example 5
Organic matters in the acetylene byproduct carbon black are removed according to the flow shown in figure 1, and the specific process flow is as follows:
A. and (3) drying: putting carbon black (a by-product from partial oxidation of natural gas to acetylene) with the water content of 65% into high-temperature flue gas heating and drying equipment at the temperature of 110 ℃ to reduce the water content of the carbon black to 20%;
B. removing: controlling the relative pressure of the activation furnace to be 0.2MPa, isolating oxygen, air and ozone, filling carbon black with the water content of 20% into the activation furnace, adding argon with the mass of 4.5% of that of the carbon black, heating the activation furnace to 400 ℃, and reacting at the temperature of 400 ℃ for 70 min; after the reaction is finished, hydrogen peroxide with the mass fraction of 10 percent and the mass fraction of 6.1 percent of the carbon black is added into the activation furnace, the temperature of the activation furnace is raised to 800 ℃, and the reaction is carried out for 80min at the temperature of 800 ℃.
Comparative example 1
Carbon black with a water content of 85% (by-product from the partial oxidation of natural gas to acetylene) without any treatment.
Performance testing
The carbon blacks obtained by the removing treatments of examples 1 to 5 and the carbon black of comparative example 1 were examined for iodine absorption value, oil absorption value, toluene light transmittance, heating loss, nitrogen adsorption specific surface area and 45 μm screen residue, and the results are shown in Table 1.
Table 1 results of performance testing
As can be seen from Table 1, the nitrogen adsorption specific surface area and 45 mesh screen residue of the carbon blacks treated in examples 1-5 were significantly improved. Thus, the method of the invention is proved to be good in modification of the structure of the carbon black.
As can be seen from Table 1, the iodine absorption and oil absorption values of the carbon blacks treated in examples 1-5 were significantly improved; the heating decrement is greatly reduced, and the toluene light transmittance is obviously improved. Thus, the method of the invention is proved to effectively remove organic matters in the carbon black.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (14)
1. The method for removing organic matters in the carbon black byproduct in the preparation of acetylene by partial oxidation of natural gas is characterized by comprising the following steps of: the method comprises the following steps:
A. and (3) drying: reducing the water content in the carbon black to be less than or equal to 30 percent;
B. removing: placing the carbon black with the water content of less than or equal to 30% in an activation furnace, adding inert gas for reaction, and adding a weak oxidant into the activation furnace for oxidation reaction after the reaction is finished.
2. The method for removing organic matters from carbon black, which is a byproduct in the preparation of acetylene by partial oxidation of natural gas, according to claim 1, is characterized in that: the temperature of the carbon black in the drying process is 100-125 ℃.
3. The method for removing organic matters in carbon black as a by-product of acetylene preparation by partial oxidation of natural gas according to claim 1 or 2, wherein the drying is performed by electric heating, steam heating or high-temperature flue gas heating.
4. The method for removing organic matters in carbon black as a by-product of acetylene preparation by partial oxidation of natural gas according to claim 3, wherein the drying is drying by high-temperature flue gas heating.
5. The method for removing organic matters from carbon black, a by-product of acetylene production by partial oxidation of natural gas, according to claim 1, 2, 3 or 4, wherein the inert gas is nitrogen, helium, neon, argon, krypton, xenon or radon.
6. The method for removing organic matters in carbon black as a by-product of acetylene preparation by partial oxidation of natural gas according to claim 1, 2, 3, 4 or 5, wherein the reaction temperature of the carbon black and the inert gas is 150-800 ℃ and the reaction time is 10-150 min.
7. The method for removing organic matters from carbon black, a by-product of acetylene production by partial oxidation of natural gas, according to claim 1, 2, 3, 4, 5 or 6, characterized in that the amount of the inert gas is 1.1-5% by mass of the carbon black.
8. The method for removing organic matters in carbon black as a by-product of acetylene production by partial oxidation of natural gas according to claim 1, 2, 3, 4, 5, 6 or 7, wherein the weak oxidizing agent is steam, carbon dioxide, hydrogen peroxide or calcium carbonate.
9. The method for removing organic matters in carbon black as a by-product of producing acetylene by partial oxidation of natural gas according to claim 1, 2, 3, 4, 5, 6, 7 or 8, wherein the reaction temperature of carbon black and weak oxidant is 500-1000 ℃ and the reaction time is 30-180 min.
10. The method for removing organic matters from carbon black as a by-product of acetylene production by partial oxidation of natural gas according to claim 1, 2, 3, 4, 5, 6, 7, 8 or 9, wherein the amount of the weak oxidizing agent is 2.3 to 7.9% by mass of the carbon black.
11. The method for removing organic matters from carbon black as a by-product of acetylene production by partial oxidation of natural gas according to claim 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, wherein the relative pressure of the activation furnace is less than 0.04 MPa.
12. The method for removing organic matters from carbon black as a by-product of acetylene preparation by partial oxidation of natural gas according to claim 10, wherein the relative pressure of the activation furnace is 0 to 0.04 MPa.
13. The method for removing organic matters from carbon black as a by-product of acetylene production by partial oxidation of natural gas according to claim 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12, wherein the removing step is carried out while isolating the strong oxidizing agent from the gas.
14. The method for removing organic matters from carbon black, a by-product of acetylene production by partial oxidation of natural gas, according to claim 13, wherein the strong gas oxidizer is oxygen, air or ozone.
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Cited By (5)
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| CN113402905A (en) * | 2021-06-28 | 2021-09-17 | 青岛黑猫新材料研究院有限公司 | High-porosity carbon black, preparation method and preparation device thereof |
| CN114085555A (en) * | 2021-11-29 | 2022-02-25 | 苏州宝化炭黑有限公司 | High volume resistivity carbon black, process for its manufacture and its use |
| CN114426782A (en) * | 2020-10-14 | 2022-05-03 | 中国石油化工股份有限公司 | Activation method of byproduct carbon black for preparing acetylene by partial oxidation of natural gas |
| CN115537044A (en) * | 2022-09-19 | 2022-12-30 | 青岛黑猫新材料研究院有限公司 | Modified pyrolysis carbon black and preparation method and application thereof |
| CN116002946A (en) * | 2021-10-19 | 2023-04-25 | 中国石油化工股份有限公司 | Treatment device for carbon black-containing wastewater in process of preparing acetylene from natural gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114426782A (en) * | 2020-10-14 | 2022-05-03 | 中国石油化工股份有限公司 | Activation method of byproduct carbon black for preparing acetylene by partial oxidation of natural gas |
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| CN114085555A (en) * | 2021-11-29 | 2022-02-25 | 苏州宝化炭黑有限公司 | High volume resistivity carbon black, process for its manufacture and its use |
| CN114085555B (en) * | 2021-11-29 | 2023-03-14 | 苏州宝化炭黑有限公司 | High volume resistivity carbon black, process for its manufacture and its use |
| CN115537044A (en) * | 2022-09-19 | 2022-12-30 | 青岛黑猫新材料研究院有限公司 | Modified pyrolysis carbon black and preparation method and application thereof |
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Application publication date: 20200825 |