An impregnating pitch and a method for producing an impregnating pitch using ethylene tar

Abstract

The application provides an impregnant pitch and a method for producing the impregnant pitch by using ethylene tar, and the method is as follows: 1. The ethylene tar is subjected to rectification, light components B1 with a distillation range of less than 180-210 DEG C are separated out, and heavy components A1 of the tar are collected; 2. The heavy components A1 of the tar obtained in step 1 are subjected to rectification again, light components B2 with a distillation range of 210-360 DEG C and heavy components A2 are separated out; 3. The light components B2 obtained in step 2 are subjected to catalytic polymerization and then subjected to negative pressure separation, the light components B3 obtained by the negative pressure separation are extracted, and heavy components A3 are collected; 4. The heavy components A3 obtained in step 3 are subjected to centrifugation, and the upper components C in the first 50% are collected according to the mass fraction; and 5. The upper components C obtained in step 4 and the heavy components A2 are subjected to condensation reaction to obtain the impregnant pitch. The impregnant pitch provided by the application simultaneously satisfies quinoline insoluble QI < 0.3%, and beta resin > 15%.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of petroleum chemical industry, in particular to a kind of impregnant pitch and the method for producing impregnant pitch using ethylene tar. BACKGROUND

[0002] Impregnant pitch requires quinoline insoluble QI <0.3%, beta resin >15%. Currently, coal tar is generally selected for producing impregnant pitch, because coal tar contains a large amount of condensed polycyclic aromatic hydrocarbons, and the beta resin content of the impregnant pitch made from coal tar is high. However, the original QI in coal pitch is relatively high, generally 3-5%. The original QI content in ethylene tar is low, almost none, but the beta resin content of the pitch produced by simply following the method of producing impregnant pitch from coal tar is low, which cannot meet the requirements of customers. Therefore, the prior art needs to be further developed. SUMMARY

[0003] The present application aims to overcome the above technical deficiencies, and provide a kind of impregnant pitch and the method for producing impregnant pitch using ethylene tar, to solve the technical problem that the impregnant pitch in the related art cannot simultaneously satisfy quinoline insoluble QI <0.3%, beta resin >15%.

[0004] To achieve the above technical purpose, the present application adopts the following technical scheme: a method for producing impregnant pitch using ethylene tar is provided, and the steps are as follows: (1) distill the ethylene tar to separate out light component B1 with a distillation range of less than 180-210℃, and collect heavy component A1 of the tar; (2) distill the heavy component A1 of the tar obtained in step (1) again to separate out light component B2 with a distillation range of 210-360℃ and heavy component A2; (3) catalytically polymerize the light component B2 obtained in step (2) and then perform negative pressure separation, extract the light component B3 obtained by negative pressure separation, and collect heavy component A3; (4) centrifuge the heavy component A3 obtained in step (3), and collect the upper component C with a mass fraction of the first 50%; and (5) perform condensation reaction on the upper component C obtained in step (4) and the heavy component A2 to obtain impregnant pitch.

[0005] Further, the temperature for catalytic polymerization in step (3) is 130-200℃, and the time for catalytic polymerization is 3-8 hours.

[0006] Further, the temperature for negative pressure separation in step (3) is 200-240℃, and the pressure for negative pressure separation is -100 to -90 kpa.

[0007] Further, the catalyst for catalytic polymerization in step (3) is Lewis acid.

[0008] Further, the Lewis acid can be boron trifluoride, aluminum trichloride or ferrous chloride.

[0009] Further, the rotation speed of centrifugation in step (4) is 1000-5000 rpm, and the centrifugation time is 5-10 min.

[0010] Further, the mass ratio of the recombined component A2 and the upper component C in step (5) is 1:1 to 5:1.

[0011] Further, the temperature of the condensation reaction in step (5) is 340-380℃, and the reaction time of the condensation reaction is 3-5 hours.

[0012] Further, the pressure of the condensation reaction in step (5) is -10 kPa to 10 kPa.

[0013] Further, high-temperature filtration is performed after the condensation reaction in step (5), and the temperature is 320℃ to 350℃.

[0014] In addition, the application also provides a dipping agent pitch prepared by the above method.

[0015] Beneficial effects:

[0016] 1. The dipping agent pitch produced by ethylene tar in the application is obtained by component subdivision and multi-step polymerization, which meets the requirements of quinoline insoluble QI <0.3% and beta resin >15%.

[0017] 2. The softening point of the dipping agent pitch produced by ethylene tar in the application is 80℃ to 100℃.

[0018] 3. The method for producing the dipping agent pitch by ethylene tar in the application is simple and easy to operate, and greatly improves the comprehensive utilization rate of the dipping agent pitch. DETAILED DESCRIPTION

[0019] Figure 1 is a process flow chart of the dipping agent pitch produced by ethylene tar in the application. DETAILED DESCRIPTION

[0020] In order to enable the personnel in the art to better understand the present application, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by the person skilled in the art without creative labor should be within the scope of protection of the present application.

[0021] According to the embodiments of the present application, a dipping agent pitch produced by ethylene tar is provided, please refer to Figure 1A method for producing impregnating bitumen using ethylene tar, comprising the following steps: (1) distilling ethylene tar to separate light component B1 with a distillation range of less than 180-210℃ and collecting heavy component A1; (2) distilling the heavy component A1 obtained in step (1) again to separate light component B2 with a distillation range of 210-360℃ and heavy component A2; (3) catalytically polymerizing the light component B2 obtained in step (2) and then separating it under negative pressure, extracting the light component B3 obtained under negative pressure and collecting heavy component A3; (4) centrifuging the heavy component A3 obtained in step (3) and collecting the first 50% of the upper layer component C by mass fraction; (5) condensing the upper layer component C obtained in step (4) and the heavy component A2 to obtain impregnating bitumen. Impregnating agent pitch is obtained through component subdivision and multi-step polymerization. The impregnating agent pitch simultaneously satisfies the requirements of quinoline insoluble matter QI < 0.3% and β resin > 15%, solving the technical problem in related technologies where impregnating agent pitch cannot simultaneously satisfy quinoline insoluble matter QI < 0.3% and β resin > 15%, thus limiting the comprehensive utilization of impregnating agent pitch. Specifically, in step (1), after the ethylene tar is distilled and separated, the main components of the separated heavy tar component A1 are polycyclic aromatic hydrocarbons and polymers, and the separated light tar components include indene, methyl indene, and trimethylbenzene. In step (2), the heavy component A2 includes polymers and the light component B2 includes polycyclic aromatic hydrocarbons such as naphthalene, anthracene, pyrene, and tetramethylbenzene. In step (3), the light component B3 includes unreacted components such as tetramethylbenzene and catalyst. In step (4), the first 50% of the upper component C is collected because some large molecular insoluble substances, such as quinoline insoluble matter QI, must be removed after centrifugation.

[0022] The following will illustrate this with specific examples.

[0023] Example 1

[0024] A method for producing impregnating bitumen using ethylene tar, comprising the following steps:

[0025] 1. Ethylene tar is separated by distillation to separate the light component B1 with a distillation range of up to 210°C, which is used as a raw material for the production of other resins, while the heavy component A1 of the tar is collected.

[0026] 2. The heavy tar component A1 from step 1 is further distilled and separated to obtain the light component B2 with a distillation range of 210-360℃, which is used as the raw material for the next step. The heavy component A2 is used to make the impregnating agent pitch.

[0027] 3. The light component B2 in step 2 is subjected to catalytic polymerization at 180°C using boron trifluoride as catalyst for 5 hours. After 5 hours of reaction, the temperature is heated to 220°C and negative pressure is extracted. The pressure of the negative pressure separation is -100 kPa. The boron trifluoride and the light component B3 are extracted. When there is no longer any light component B3 distilled, the remaining component, the heavy component A3, is centrifuged. The centrifugal speed is 3000 revolutions per minute and the centrifugal time is 8 minutes. The upper layer component C is taken from the upper 50% by mass for standby;

[0028] 4. The heavy component A2 in step 2 and the upper layer component C prepared in step 3 are subjected to dry distillation at 360°C and a pressure of -10 kPa for 3 hours. The components inside are subjected to thermal cracking and thermal condensation reaction during the dry distillation. Finally, the impregnating pitch is obtained by filtration at 330°C. The quinoline insoluble QI content of the impregnating pitch is 0.26%, the β resin content is 18%, and the softening point is 91°C.

[0029] Example 2

[0030] A method for producing impregnating pitch using ethylene tar is provided. The steps are as follows:

[0031] 1. The ethylene tar is separated by rectification to separate the light component B1 with a distillation range of 200°C or less, which is used as raw material for producing other resins, and the heavy component A1 is collected.

[0032] 2. The heavy component A1 in step 1 is separated by rectification again to separate the light component B2 with a distillation range of 210-360°C, which is used as raw material for the next step, and the heavy component A2 is used to produce impregnating pitch.

[0033] 3. The light component B2 in step 2 is subjected to catalytic polymerization at 200°C using boron trifluoride as catalyst for 3 hours. After 3 hours of reaction, the temperature is heated to 240°C and negative pressure is extracted. The pressure of the negative pressure separation is -90 kPa. The boron trifluoride and the light component B3 are extracted. When there is no longer any light component B3 distilled, the remaining component, the heavy component A3, is centrifuged. The centrifugal speed is 1000 revolutions per minute and the centrifugal time is 10 minutes. The upper layer component C is taken from the upper 50% by mass for standby.

[0034] 4. The heavy component A2 in step 2 and the upper layer component C prepared in step 3 are subjected to dry distillation at 380°C and a pressure of 10 kPa for 4 hours. The components inside are subjected to thermal cracking and thermal condensation reaction during the dry distillation. Finally, the impregnating pitch is obtained by filtration at 320°C. The quinoline insoluble QI content of the impregnating pitch is 0.29%, the β resin content is 22%, and the softening point is 101°C.

[0035] Example 3

[0036] A method for producing impregnating pitch from ethylene tar, comprising the following steps:

[0037] 1. The ethylene tar is separated by rectification to obtain a light component B1 with a distillation range of below 180°C, which is used as raw material for producing other resins, and a heavy component A1 which is collected;

[0038] 2. The heavy component A1 from step 1 is separated by rectification again to obtain a light component B2 with a distillation range of 210-360°C, which is used as raw material for the next step, and a heavy component A2 which is used for producing impregnating pitch;

[0039] 3. The light component B2 from step 2 is subjected to catalytic polymerization at 130°C using aluminum chloride as catalyst for 8 hours, after which the temperature is raised to 200°C and maintained while negative pressure is applied, the pressure for the separation by negative pressure being -95 kPa, the aluminum chloride and the light component B3 being removed, and when no light component B3 is distilled, the remaining component, the heavy component A3, is centrifuged at a speed of 5000 rpm for 5 minutes, and 50% of the upper component C is taken as standby;

[0040] 4. The heavy component A2 from step 2 and the upper component C from step 3 are dry-distilled at 340°C and a pressure of -1 kPa for 5 hours, during which the components inside are subjected to thermal cracking and thermal condensation, and finally, impregnating pitch is obtained by filtration at 350°C, the quinoline insoluble QI content of the impregnating pitch being 0.16%, the β resin content being 16%, and the softening point being 89°C.

[0041] Example 4

[0042] A method for producing impregnating pitch from ethylene tar, comprising the following steps:

[0043] 1. The ethylene tar is separated by rectification to obtain a light component B1 with a distillation range of below 210°C, which is used as raw material for producing other resins, and a heavy component A1 which is collected;

[0044] 2. The heavy component A1 from step 1 is separated by rectification again to obtain a light component B2 with a distillation range of 210-360°C, which is used as raw material for the next step, and a heavy component A2 which is used for producing impregnating pitch;

[0045] 3. The light component B2 from step 2 is subjected to catalytic polymerization at 150°C using ferrous chloride as catalyst for 6 hours, after which the temperature is raised to 210°C and maintained while negative pressure is applied, the pressure for the separation by negative pressure being -98 kPa, the ferrous chloride and the light component B3 being removed, and when no light component B3 is distilled, the remaining component, the heavy component A3, is centrifuged at a speed of 2000 rpm for 7 minutes, and 50% of the upper component C is taken as standby;

[0046] 4. The recombined component A2 in step 2 and the prepared upper component C in step 3 are mass ratio 2:1 dry distillation at 360℃, pressure -10kPa for 4 hours, during which the components inside undergo thermal cracking, thermal condensation reaction, and finally filtered at 320℃ to obtain impregnant pitch. The quinoline insoluble QI content of the impregnant pitch is 0.25%, the β resin content is 19%, and the softening point is 94℃.

[0047] Comparative Example 1

[0048] Impregnant pitch is prepared according to the method of producing impregnant pitch from coal tar in the prior art, using ethylene tar as raw material.

[0049] The method for preparing needle coke raw material pitch from coal tar by one-step solvent method includes the following steps:

[0050] 1) After desalination and dehydration, the coal tar is subjected to vacuum distillation to remove light oil before 230℃, and heavy oil is obtained;

[0051] 2) The heavy oil is mixed with aromatic hydrocarbon extractant, and then extracted and separated to obtain a soluble phase;

[0052] 3) The soluble phase is subjected to vacuum distillation to recover the aromatic hydrocarbon extractant, and then the fraction before 330℃ is removed, and a polycyclic aromatic hydrocarbon oil is obtained;

[0053] 4) The polycyclic aromatic hydrocarbon oil is subjected to inert gas stripping to obtain needle coke raw material pitch.

[0054] The softening point of the needle coke raw material pitch is 15-40℃, the toluene insoluble (β resin) component content is 0.1wt%-1wt%, and the quinoline insoluble component content is 0-0.1wt%.

[0055] As can be seen from Comparative Example 1, it is difficult for impregnant pitch to simultaneously meet the requirements of quinoline insoluble QI <0.3%, and β resin >15%. The present application obtains impregnant pitch that simultaneously meets the requirements of quinoline insoluble QI <0.3%, and β resin >15% through component subdivision and multi-step polymerization, and the method is simple and easy to operate, and greatly improves the comprehensive utilization rate of impregnant pitch.

[0056] In addition, it should be understood that although the present specification is described in terms of embodiments, not every embodiment contains only one independent technical solution, and the specification is described in this way only for the sake of clarity, and 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 those skilled in the art can understand.

Claims

1. A process for producing impregnant pitch from ethylene tar, characterized by, The steps are as follows: (1) subjecting the ethylene tar to rectification to separate out light component B1 with a distillation range of less than 210℃, and collect heavy component A1 of the tar; (2) subjecting the heavy component A1 of the tar obtained in step (1) to rectification again to separate out light component B2 with a distillation range of 210-360℃ and heavy component A2; (3) subjecting the light component B2 obtained in step (2) to catalytic polymerization, and then to negative pressure separation, and collecting light component B3 obtained by the negative pressure separation, and collecting heavy component A3; (4) subjecting the heavy component A3 obtained in step (3) to centrifugation, and collecting the upper component C in the first 50% by mass; (5) subjecting the upper component C obtained in step (4) and the heavy component A2 to condensation reaction to obtain impregnant pitch.

2. The method for producing impregnating pitch from ethylene tar according to claim 1, characterized by, The temperature for the catalytic polymerization in step (3) is 130-200℃, and the time for the catalytic polymerization is 3-8 hours.

3. The method for producing impregnating pitch from ethylene tar according to claim 1, characterized by, The temperature for the negative pressure separation in step (3) is 200-240℃, and the pressure for the negative pressure separation is -100 to -90 kPa.

4. The method for producing impregnating pitch from ethylene tar according to claim 1, characterized by, The catalyst for the catalytic polymerization in step (3) is Lewis acid.

5. The method for producing impregnating pitch from ethylene tar according to claim 4, characterized by, The Lewis acid is boron trifluoride, aluminum trichloride or ferrous chloride.

6. The method of producing impregnating pitch from ethylene tar according to claim 1, characterized in that, The rotation speed for the centrifugation in step (4) is 1000-5000 rpm, and the time for the centrifugation is 5-10 min.

7. The method of producing impregnating pitch from ethylene tar according to claim 1, characterized in that, The mass ratio of the heavy component A2 to the upper component C in step (5) is 1:1 to 5:

1.

8. The method of producing impregnating pitch from ethylene tar according to claim 1, characterized in that, The temperature for the condensation reaction in step (5) is 340-380℃, and the reaction time for the condensation reaction is 3-5 hours.

9. The method of producing impregnating pitch from ethylene tar according to claim 1, characterized in that, The pressure for the condensation reaction in step (5) is -10 kPa to 10 kPa.

10. Impregnant pitch produced by the method of any one of claims 1-9 using ethylene tar.

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