A production method for improving the content of anthracene and carboline in crude anthracene product by using crystal nucleus seed

Abstract

This invention belongs to the technical field of anthracene oil processing and production, and discloses a production method for increasing the anthracene and carbide content in crude anthracene products using crystal nucleus seeds. The method mainly involves cooling the heated raw anthracene oil to 75°C, then adding high-quality crystal nucleus seeds (70% anthracene content, 17% carbide content, and ≤1% mechanical impurities) to a crystallization tank at a mass ratio of 1:75. At this point, the high-quality crystal nucleus seeds promote the formation of new crystal nuclei in the anthracene oil liquid. As the temperature decreases, the newly formed crystal nuclei gradually grow. Simultaneously, the temperature is naturally lowered to below 65°C through stirring, and the cooling system in the crystallization tank is activated to further cool the temperature to 35-40°C. The mixture is then repeatedly fed and dried in a centrifuge to produce high-quality crude anthracene. This invention utilizes unique high-quality crystal nucleus seeds to achieve an anthracene content of over 40% and a carbide content of over 14% in crude anthracene even when the anthracene and carbide content in the raw anthracene oil is low or unstable, resulting in a superior-grade crude anthracene product.

Description

Technical Field

[0001] This invention belongs to the technical field of anthracene oil processing and production, specifically relating to a production method that utilizes crystal seed nuclei to increase the anthracene and carbide content in crude anthracene products. Background Technology

[0002] Currently, the quality of anthracene oil produced by domestic and international coal tar processing enterprises is unstable due to the influence of coal tar quality and processing technology, which significantly impacts the production of crude anthracene by downstream anthracene oil processing enterprises. For example, our company uses the traditional physical crystallization method for producing crude anthracene. This involves first heating the raw anthracene oil to 90°C in a heating tank, then injecting it into an anthracene oil crystallization tank (15m³), stirring, and cooling it to approximately 40°C for about 16 hours. The raw anthracene oil in the crystallization tank is then centrifuged in batches for drying and packaging, producing crude anthracene and anthracene oil emulsion.

[0003] However, the quality of crude anthracene produced by the traditional physical crystallization method depends entirely on factors such as the anthracene content, carbide content, and oil content of the raw material anthracene oil. Therefore, it cannot consistently produce high-quality crude anthracene, which seriously affects the sales of crude anthracene products and restricts the normal and continuous production of downstream crude anthracene processing enterprises.

[0004] In conclusion, effectively increasing the anthracene and carbide content of crude anthracene when the anthracene and carbide content of raw anthracene oil is low or unstable is of great significance for practical production. Simultaneously, achieving an anthracene content of over 40% and a carbide content of over 14% in crude anthracene, thus ensuring the product quality reaches superior grade, has become one of our company's key research topics for improving the anthracene and carbide content in crude anthracene products. This is also crucial for ensuring stable product quality and meeting the market demands of downstream anthracene oil processing enterprises. Summary of the Invention

[0005] In response to the problem of unstable anthracene oil quality caused by the traditional physical crystallization method for producing crude anthracene in the background technology when the anthracene oil has low or unstable anthracene and carbide content in the raw material anthracene oil, which in turn affects the production of downstream anthracene oil processing enterprises and the quality of subsequent products, and in order to effectively solve the impact of the unstable quality of raw material anthracene oil on our company, our company's technical center professionals have independently developed a crystal nucleus seed method to improve product quality.

[0006] Based on this, the present invention provides a production method for increasing the anthracene and carbide content in crude anthracene products by using crystal seed nuclei.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: a production method for increasing the anthracene and carbide content in crude anthracene products using crystal seeding, comprising the following steps:

[0008] Step 1: Heat the raw anthracene oil in the heating tank to 93-95℃;

[0009] Step 2: Inject the heated anthracene oil from Step 1 into a crystallization tank and stir at a rate of 16 r / min for 4 hours to reduce the temperature of the anthracene oil to 75°C.

[0010] Step 3: When the temperature of the anthracene oil in the crystallization tank cools to 75°C, high-quality crystal nuclei with an anthracene content of 70%, a carbide content of 17%, and mechanical impurities of ≤1% are added to the crystallization tank at a mass ratio of 1:75. At this time, the high-quality crystal nuclei can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases.

[0011] Step 4: When the raw material anthracene oil in the crystallization tank cools down to 65°C naturally through stirring, turn on the cooling system in the crystallization tank to continue cooling down to 35-40°C.

[0012] Step 5: After the anthracene oil with added crystal seeds is cooled, it is put into a centrifuge for drying. The process of feeding, drying and packaging is repeated to produce high-quality crude anthracene.

[0013] As a further supplement to the above technical solution, in step 3 of the above technical solution, the raw material crystal seed with an anthracene content of 34.7% and a carb content of 11.6% is used to produce high-quality crystal seed with an anthracene content of 70%, a carb content of 17%, and mechanical impurities of ≤1% by solvent method.

[0014] As a further supplement to the above technical solution, the method for producing high-quality crystal nuclei seeds in the above technical solution includes the following steps:

[0015] Step 2.1: Add the organic solvent and the crystal seed raw material to the reaction vessel at a mass ratio of 1:1 and heat and stir. At this time, the material is a solid-liquid mixture.

[0016] Step 2.2: Heat the mixture in the reactor for 4 hours using heat transfer oil until the temperature reaches 120°C. At this point, the material in the reactor changes from a solid-liquid state to a liquid solution with good fluidity.

[0017] Step 2.3: Stop heating the reactor and turn on the cooling system to cool it for 6 hours until the temperature of the mixed solution in the reactor drops to 50°C. At this time, the material in the reactor consists of both solution and crystals.

[0018] Step 2.4: The cooled mixed solution is injected into a centrifuge in batches for solid-liquid separation. The solid crystalline material is weighed by a scale and packaged by a packaging machine to produce high-quality crystal seeds with an anthracene content of 70%, a carbide content of 17%, and mechanical impurities of ≤1%.

[0019] As a further explanation and limitation of the above technical solution, in step 2.1, the organic solvent is any one or a combination of two of the phenolic oil solvent and DMF solvent.

[0020] Compared with the prior art, the present invention has the following advantages:

[0021] 1. This invention utilizes our company's proprietary high-quality crystal nucleus seeds to effectively increase the anthracene and carbide content of crude anthracene when the anthracene oil and carbide content of the raw materials are low or unstable. This results in an anthracene content of over 40% and a carbide content of over 14% in the crude anthracene, thus achieving a superior grade of crude anthracene product.

[0022] 2. The crude anthracene production method provided by this invention is easy to operate, produces stable product quality, and is beneficial to downstream customers in producing subsequent products. Therefore, this method for improving the quality of crude anthracene products has significant implications for practical production. Attached Figure Description

[0023] Figure 1 This is a process flow diagram of producing high-quality anthracene oil products using crystal nucleus seeds in this invention;

[0024] Figure 2 This is a process flow diagram of producing high-quality crystal nuclei seeds using the solvent method in this invention;

[0025] Figure 3 This is a quality inspection report for the crude anthracene product produced using the optimal embodiment of the present invention.

[0026] Figure 4 The chromatogram of the anthracene oil sample used in this invention is obtained by area normalization method.

[0027] Figure 5 The chromatogram of the crude anthracene product used in this invention is obtained using the area normalization method. Detailed Implementation

[0028] To further illustrate the technical solution of the present invention, the following is in conjunction with the appendix. Figures 1 to 5 Our company's technical center personnel further illustrate the present invention by selecting multiple sets of embodiments.

[0029] First, we used raw material crystal seeds with an anthracene content of 34.7% and a carb content of 11.6% to produce high-quality crystal seeds with an anthracene content of 70%, a carb content of 17%, and mechanical impurities of ≤1% using a solvent method.

[0030] As attached Figure 2 As shown, in this embodiment, the method for producing high-quality crystal nuclei using a solvent method includes the following steps:

[0031] The first step involves adding phenolic oil solvent and the crystal nucleus seed raw material with the above quality requirements into a reaction vessel at a mass ratio of 1:1 and heating and stirring. At this time, the material is a solid-liquid mixture.

[0032] The second step is to use heat transfer oil to heat the mixture in the reactor for 4 hours, so that the temperature of the mixture in the reactor reaches 120°C. At this time, the material in the reactor changes from a solid-liquid state to a liquid solution with good fluidity.

[0033] The third step is to stop heating the reactor and turn on the cooling system to cool it for 6 hours to reduce the temperature of the mixed solution in the reactor to 50°C. At this time, the material in the reactor consists of both solution and crystals.

[0034] The fourth step involves injecting the cooled mixed solution into a centrifuge in batches for solid-liquid separation. The solid crystalline material is weighed by a scale and then packaged by a packaging machine to produce high-quality crystal seeds with an anthracene content of 70%, a carbide content of 17%, and mechanical impurities of ≤1%.

[0035] In the above specific embodiments, the phenolic oil solvent can be replaced with DMF solvent, or a mixture of both can be used. It should be noted that the method or even the type of organic solvent used has no impact on the quality of the finished seeds. Therefore, those skilled in the art who refer to the above production method and change the method and type of organic solvent used without departing from the spirit or basic characteristics of the present invention should be considered to fall within the scope of protection disclosed in the technical solution of the present invention.

[0036] Secondly, based on the above embodiments, high-quality crystal nuclei are produced with an anthracene content of 70%, a carbide content of 17%, and mechanical impurities ≤1%. Since the anthracene oil with added crystal nuclei is easily dried by centrifugation at 35-40°C, we list four embodiments to further illustrate the key technical points of this invention by examining the effects of temperature control when adding high-quality crystal nuclei and the cooling method of the crystallizer on the anthracene and carbide content in the crude anthracene product. This aims to enable those skilled in the art to implement and select the optimal embodiment for production. Example 1

[0037] As attached Figure 1 As shown, a production method for increasing the anthracene and carbide content in crude anthracene products using crystal seeding includes the following steps:

[0038] Step 1: Heat the raw anthracene oil in the heating tank to 90-95℃;

[0039] Step 2: Inject the heated anthracene oil from Step 1 into the crystallization tank and stir at a rate of 16 r / min for 4 hours to lower the temperature of the anthracene oil to below 70°C. Then, turn on the cooling system inside the crystallization tank to cool the anthracene oil.

[0040] Step 3: When the temperature of the anthracene oil in the crystallization tank is cooled to 73°C, the high-quality crystal nuclei produced above are added into the crystallization tank at a mass ratio of 1:75. At this time, the high-quality crystal nuclei can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases.

[0041] Step 4: When the raw material anthracene oil in the crystallization tank cools down naturally to below 70°C through stirring, turn on the cooling system in the crystallization tank to continue cooling down to 35-40°C;

[0042] Step 5: After the anthracene oil with added crystal seeds is cooled, it is put into a centrifuge for drying. The process of feeding, drying and packaging is repeated to produce high-quality crude anthracene.

[0043] In this embodiment, the crude anthracene product produced passed our company's quality inspection, with an anthracene content of approximately 37% and a carboxylic acid content of approximately 8.5%. Example 2

[0044] As attached Figure 1 As shown, a production method for increasing the anthracene and carbide content in crude anthracene products using crystal seeding includes the following steps:

[0045] Step 1: Heat the raw anthracene oil in the heating tank to 90-95℃;

[0046] Step 2: Inject the heated anthracene oil from Step 1 into the crystallization tank and stir at a rate of 16 r / min for 4 hours to lower the temperature of the anthracene oil to below 70°C. Then, turn on the cooling system inside the crystallization tank to cool the anthracene oil.

[0047] Step 3: When the temperature of the anthracene oil in the crystallization tank cools to 75°C, the high-quality crystal nuclei produced above are added into the crystallization tank at a mass ratio of 1:75. At this time, the high-quality crystal nuclei can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases.

[0048] Step 4: When the raw material anthracene oil in the crystallization tank cools down naturally to below 70°C through stirring, turn on the cooling system in the crystallization tank to continue cooling down to 35-40°C;

[0049] Step 5: After the anthracene oil with added crystal seeds is cooled, it is put into a centrifuge for drying. The process of feeding, drying and packaging is repeated to produce high-quality crude anthracene.

[0050] In this embodiment, the crude anthracene product produced passed our company's quality inspection, with an anthracene content of approximately 35.5% and a carbide content of approximately 7%. Example 3

[0051] As attached Figure 1As shown, a production method for increasing the anthracene and carbide content in crude anthracene products using crystal seeding includes the following steps:

[0052] Step 1: Heat the raw anthracene oil in the heating tank to 93-95℃;

[0053] Step 2: Inject the heated anthracene oil from Step 1 into a crystallization tank and stir at a rate of 16 r / min for 4 hours to reduce the temperature of the anthracene oil to 75°C.

[0054] Step 3: When the temperature of the anthracene oil in the crystallization tank cools to 75°C, the high-quality crystal nuclei produced above are added into the crystallization tank at a mass ratio of 1:75. At this time, the high-quality crystal nuclei can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases.

[0055] Step 4: When the raw material anthracene oil in the crystallization tank cools down to 65°C naturally through stirring, turn on the cooling system in the crystallization tank to continue cooling down to 35-40°C.

[0056] Step 5: After the anthracene oil with added crystal seeds is cooled, it is put into a centrifuge for drying. The process of feeding, drying and packaging is repeated to produce high-quality crude anthracene.

[0057] As attached Figures 3 to 5 As shown in this embodiment, the crude anthracene product produced has passed our company's quality inspection, with anthracene content of over 40% and carbide content of over 14%, and its quality has reached the superior grade. Example 4

[0058] As attached Figure 1 As shown, a production method for increasing the anthracene and carbide content in crude anthracene products using crystal seeding includes the following steps:

[0059] Step 1: Heat the raw anthracene oil in the heating tank to 90-95℃;

[0060] Step 2: Inject the heated anthracene oil from Step 1 into the crystallization tank and stir at a rate of 16 r / min for 4 hours to lower the temperature of the anthracene oil to below 70°C. Then, turn on the cooling system inside the crystallization tank to cool the anthracene oil.

[0061] Step 3: When the temperature of the anthracene oil in the crystallization tank cools to 75°C, the high-quality crystal nuclei produced above are added into the crystallization tank at a mass ratio of 1:75. At this time, the high-quality crystal nuclei can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases.

[0062] Step 4: When the raw material anthracene oil in the crystallization tank is cooled down to below 65°C by stirring, we use natural cooling instead of the cooling system to continue cooling down to 35-40°C.

[0063] Step 5: After the anthracene oil with added crystal seeds is cooled, it is put into a centrifuge for drying. The process of feeding, drying and packaging is repeated to produce high-quality crude anthracene.

[0064] However, in this embodiment, the crude anthracene product produced passed our company's quality inspection, with an anthracene content of about 29% and a carbide content of about 5.5%.

[0065] Compared to the traditional physical crystallization method for producing crude anthracene, which involves heating the raw anthracene oil to 90°C in a heating tank, then pouring it into a 15m³ anthracene oil crystallization tank, stirring and cooling it to approximately 40°C for about 16 hours, and then centrifuging and packaging the raw anthracene oil in batches to produce crude anthracene and anthracene oil emulsions, the crude anthracene product has an anthracene content of only 22.8% and a carboxylic acid content of 6.55%. However, after comparing the above examples, we found that the crude anthracene product produced in Example 3 has an anthracene content of over 40% and a carboxylic acid content of over 14%, making it the optimal example for this production method. Furthermore, through experiments in Examples 3 and 4, we concluded that different cooling methods in the crystallization tank significantly affect the anthracene and carboxylic acid content in the crude anthracene product. Specifically, the high-quality anthracene oil product produced by naturally cooling the raw anthracene oil in the crystallization tank to below 70°C through stirring, followed by rapid cooling to 35-40°C using a cooling system, has a significantly higher anthracene and carboxylic acid content than the high-quality anthracene oil product produced by natural cooling.

[0066] In summary, the crude anthracene product produced by this invention has significantly increased anthracene and carbide content. Furthermore, it is the first in the industry to utilize crystal seeding to increase the anthracene and carbide content in crude anthracene products, effectively solving the problem of unstable quality of raw anthracene oil in actual production.

[0067] The foregoing has shown and described the main features and advantages of the present invention. It will be apparent to those skilled in the art that the specific embodiments of the present invention are not limited to the details of the exemplary embodiments described above. Furthermore, without departing from the spirit or essential characteristics of the present invention, the inventive concept and design ideas of the present invention can be implemented in other specific forms, and these should be equivalently included within the protection scope disclosed in the technical solutions of the present invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects. The scope of the present invention is defined by the appended claims rather than the foregoing description, and thus all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included within the present invention.

[0068] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A production method for increasing the contents of anthracene and carbazole in crude anthracene products by using crystal nucleus seeds, characterized in that, It includes the following steps: Step 1: Heat the raw anthracene oil in the raw material anthracene oil heating tank to 93 - 95°C; Step 2: Inject the heated raw material anthracene oil in Step 1 into the crystallization tank for stirring. The stirring rate is 16 r / min, and the stirring time is 4 hours to make the temperature of the raw material anthracene oil drop to 75°C; Step 3: When the temperature of the anthracene oil in the crystallization tank cools to 75°C, put high-quality crystal nucleus seeds with a purity of 70% anthracene content, 17.3% carbazole content, and mechanical impurities ≤ 1% into the crystallization tank according to a mass ratio of 1:

75. At this time, the high-quality crystal nucleus seeds can promote the generation of new crystal nuclei in the anthracene oil liquid, and the newly generated crystal nuclei gradually grow as the temperature decreases; Step 4: When the raw material anthracene oil in the crystallization tank naturally cools to below 65°C through stirring, start the cooling system in the crystallization tank to continue cooling to 35 - 40°C; Step 5: After cooling the anthracene oil added with crystal nucleus seeds, put it into a centrifuge for centrifugal dehydration, and repeatedly feed and dehydrate and package to produce high-quality crude anthracene.

2. The production method for increasing the contents of anthracene and carbazole in crude anthracene products by using crystal nucleus seeds according to claim 1, wherein In Step 3, raw material crystal nucleus seeds with a purity of 34.7% anthracene content and 11.6% carbazole content are used to produce high-quality crystal nucleus seeds with a purity of 70% anthracene content, 17% carbazole content, and mechanical impurities ≤ 1% by the solvent method.

3. The production method for increasing the contents of anthracene and carbazole in crude anthracene products by using crystal nucleus seeds according to claim 2, wherein The production method of high-quality crystal nucleus seeds includes the following steps: Step 2.1: Inject the organic solvent and the crystal nucleus seed raw material into the reaction kettle for heating and stirring according to a mass ratio of 1:

1. At this time, the material is a solid-liquid mixture; Step 2.2: Use heat-conducting oil to heat up for 4 hours to make the temperature of the mixed solution in the reaction kettle reach 120°C. At this time, the material in the reaction kettle changes from a solid-liquid state to a liquid solution with good fluidity; Step 2.3: Stop heating the reaction kettle, and start the cooling system to cool for 6 hours to make the temperature of the mixed solution in the reaction kettle drop to 50°C. At this time, the material in the reaction kettle is a coexistence of solution and crystal; Step 2.4: Inject the cooled mixed solution into the centrifuge in batches for centrifugal dehydration for solid-liquid separation. The solid crystal material is weighed by a weighing scale and packaged by a packaging machine to produce high-quality crystal nucleus seeds with a purity of 70% anthracene content, 17% carbazole content, and mechanical impurities ≤ 1%.

4. A production method for increasing the contents of anthracene and carbazole in crude anthracene products by using crystal nucleus seeds according to claim 3, characterized in that: In Step 2.1, the organic solvent is any one or a combination of two of phenol oil solvent and DMF solvent.

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