A production method of high aromatic hydrocarbon environment-friendly rubber plasticizer and lubricating oil base oil

By using a continuous production method with two extraction towers connected in series, and utilizing specific feed ratios and temperature gradients for dual-solvent and single-solvent extraction, the problem of low CA value in existing rubber plasticizers has been solved, enabling the production of high-aromatic environmentally friendly rubber plasticizers and improving the aromatic carbon content and compatibility of the products.

CN118085918BActive Publication Date: 2025-12-05CHINA UNIV OF PETROLEUM (EAST CHINA)
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Patent Information

Application Number
CN202410077075.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-19
Publication Date
2025-12-05
Estimated Expiration
2044-01-19

AI Technical Summary

Technical Problem

Existing technologies cannot improve the aromatic carbon content (CA value) of rubber plasticizers while meeting environmental protection requirements, resulting in low product compatibility with rubber and failing to meet the demand for environmentally friendly rubber plasticizers with high aromatic content.

Method used

A continuous production method using two extraction towers connected in series is employed. Using lubricating oil solvent-refined extract as raw material, dual-solvent and single-solvent extractions are carried out through specific feed ratios and temperature gradients. Extraction is carried out in the first and second extraction towers respectively to obtain high-aromatic environmentally friendly rubber plasticizers and lubricating oil base oils.

Benefits of technology

While meeting environmental protection standards, it significantly improved the CA value of environmentally friendly rubber plasticizers, while also increasing the yield and quality of lubricating oil base oils, thus meeting the demand for environmentally friendly rubber plasticizers with higher aromatic content.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to a production method of high aromatic hydrocarbon environment-friendly rubber plasticizer and lubricating oil base oil. Its characteristics are that two extraction towers are combined in series to form a continuous high aromatic hydrocarbon environment-friendly rubber plasticizer extraction production process, lubricating oil solvent refined extracted oil is used as raw material, two extraction towers respectively carry out double-solvent extraction process and single-solvent extraction process, the lubricating oil base oil obtained by single-solvent extraction process is blended with raw oil, then double-solvent extraction is carried out, the refined oil obtained by double-solvent extraction is subjected to single-solvent extraction to separate out lubricating oil base oil, and high aromatic hydrocarbon environment-friendly rubber plasticizer product is obtained at the same time. The process can improve the C A value of the product under the premise of meeting the requirements of other properties of the product.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of petroleum chemical industry, more particularly to a production method of high aromatic environmental rubber plasticizer and lubricating oil base oil, and belongs to the international patent classification C10G. BACKGROUND

[0002] The rubber plasticizer is a kind of additive used in the rubber processing process, and the addition of the rubber plasticizer can well reduce the interaction between the rubber molecular chains, increase the plasticity of the rubber compound, thereby improving the mechanical properties of the rubber, and the addition of the rubber plasticizer can effectively reduce the cost of the rubber processing process.

[0003] The rapid development of the tire industry promotes the development of the rubber industry, thereby further promoting the development of the rubber plasticizer, but with the increasingly prominent global environmental problems, the rubber plasticizer faces new requirements of environmental protection. Various kinds of environmental protection regulations related thereto are successively issued, the 2005 / 69 / EC directive is issued in 2005, the REACH regulation is issued by the European Union in 2010, the content of the specific eight polycyclic aromatic hydrocarbons in the product is required to be less than 10 mg / kg, and the content of benzene[a]pyrene (BaP) is required to be less than 1 mg / kg, and the GB T33322-2016 rubber plasticizer aromatic mineral oil standard is also formulated in China, in addition to the above restrictions, it is also stipulated that the polycyclic aromatic hydrocarbon content (PCA) is less than or equal to 3%. In order to meet these environmental protection requirements, various production processes sacrifice the C A value of the product, and at the same time, it also causes the problems of low compatibility of the product with rubber.

[0004] For some extract oils with large viscosity, low aromatic content, high alkane and cycloalkane content, the traditional extraction process can be used to produce the environmental rubber plasticizer product meeting the requirements, but the aromatic carbon rate (C A ) is low, and the C A value of the product cannot be further improved, thereby the demand for environmental rubber plasticizer with higher aromatic content cannot be met. SUMMARY

[0005] The present application provides a production method of high aromatic environmental rubber plasticizer and lubricating oil base oil, as follows:

[0006] 1. A production method of high aromatic hydrocarbon environment-friendly rubber plasticizer and lubricating oil base oil, characterized in that two extraction towers are used, a specific continuous production method is formed by using two towers in series, lubricating oil solvent refined extracted oil is used as raw material oil, the lubricating oil base oil obtained from the second extraction tower (2) is mixed with the raw material oil in a suitable ratio and then enters the middle part of the first extraction tower (1), the main solvent enters the upper part of the first extraction tower (1), the auxiliary solvent enters the lower part of the tower, the material at the top of the tower is recovered to obtain the first refined oil, and the material at the bottom of the tower is recovered to obtain the second extracted oil; the first refined oil from the first extraction tower (1) enters the lower part of the second extraction tower (2), the main solvent enters the upper part of the second extraction tower (2), the material at the top of the tower is recovered to obtain the second refined oil, part of the second refined oil is extracted as the lubricating oil base oil, and the other part is mixed with the raw material oil and then enters the first extraction tower (1), and the material at the bottom of the second extraction tower (2) is recovered to obtain the high aromatic hydrocarbon environment-friendly rubber plasticizer product.

[0007] 2. The production method of the high aromatic hydrocarbon environment-friendly rubber plasticizer according to 1, characterized in that the mass ratio of the solvent to the oil in the first extraction tower (1) is: main solvent: raw material oil: auxiliary solvent = 1.5-3: 1: 0.3-1.0; and the mass ratio of the solvent to the oil in the second extraction tower (2) is: main solvent: first refined oil = 1.5-4: 1.

[0008] 3. The production method of the high aromatic hydrocarbon environment-friendly rubber plasticizer according to 1, characterized in that the mixing mass ratio of the lubricating oil base oil obtained from the second extraction tower (2) to the raw material oil is between 0.5 and 1.

[0009] 4. The production method of the high aromatic hydrocarbon environment-friendly rubber plasticizer according to 1, characterized in that the extraction temperature at the bottom of the first extraction tower (1) is 40-75℃, the temperature at the top of the tower is 60-100℃, the temperature at the top of the tower is high, the temperature at the bottom of the tower is low, and the temperature gradually decreases from the top of the tower to the bottom of the tower.

[0010] 5. The production method of the high aromatic hydrocarbon environment-friendly rubber plasticizer according to 1, characterized in that the extraction temperature at the bottom of the second extraction tower (2) is 60-100℃, the temperature at the top of the tower is 80-120℃, the temperature at the top of the tower is high, the temperature at the bottom of the tower is low, and the temperature gradually decreases from the top of the tower to the bottom of the tower.

[0011] 6. The production method of the high aromatic hydrocarbon environment-friendly rubber plasticizer according to 1, characterized in that the main solvent is furfural or N-methyl pyrrolidone (NMP), and the auxiliary solvent (solvent D) is an alkane with a carbon number of 6-14.

[0012] Advantages of the invention

[0013] The production process provided by the present application can further improve the C A value of the environment-friendly rubber plasticizer product under the condition of meeting the environmental protection and other property indexes compared with other extraction processes. Attached Figure Description

[0014] Appendix Figure 1 This is a schematic diagram of the production process of this invention patent, wherein: 1. First extraction tower; 2. Second extraction tower; 3, 4, and 5 are storage tanks for co-solvent, raw material oil, and main solvent, respectively; 6, 7, and 8 are pumps; 9. Lubricating oil base oil; 10. Environmentally friendly rubber plasticizer; 11. Secondary extracted oil. Detailed Implementation

[0015] The following detailed description is provided in conjunction with the accompanying drawings and embodiments: This embodiment is implemented based on the process flow scheme of the present invention, and provides detailed implementation methods and processes. However, the scope of protection of the present invention is not limited to the following embodiments. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions.

[0016] The lubricating oil base oil obtained from the second extraction tower (2) is blended with the feed oil at a specific mass ratio and then enters the first extraction tower (1). The main solvent, blended feed oil, and co-solvent are fed into the upper, middle, and lower parts of the first extraction tower (1) respectively. Under a specific feed ratio and a suitable temperature gradient, a dual solvent extraction process is carried out. The raffinate oil is obtained at the top of the first extraction tower (1), and the secondary extracted oil is obtained at the bottom of the tower.

[0017] The second extraction tower (2) is a single-solvent extraction process where the main solvent and the residue oil obtained from the first extraction tower (1) are extracted under specific temperature gradients and feed ratios. The lower part of the second extraction tower (2) is the feed location for the residue oil obtained from the first extraction tower (1), and the upper part is the feed location for the main solvent. The residue oil obtained at the top of the tower is the lubricating oil base oil; part of it is collected, and part is used to blend the raw material oil for continuous dual-solvent extraction. The bottom of the tower yields a high-aromatic environmentally friendly rubber plasticizer product. Using this process, a portion of C... A Components with low C values ​​are extracted from the top of the second extraction column (2), which increases the C value of the rubber plasticizer at the bottom of the column. A Value, while obtaining low C A Value of lubricating oil base oil.

[0018] To further illustrate the present invention, a detailed description is provided below with reference to specific embodiments:

[0019] Example 1

[0020] The process is carried out in a continuous process, and the same reduced four-line extracted oil as in Comparative Example 1 is used as the raw material, and furfural and solvent D are used as the main solvent and the cosolvent, respectively, and the cosolvent is an alkane with a carbon number of 6-8. The first extraction tower (1) is composed of 5 temperature control sections from top to bottom, and the temperature gradient is 40-60°C, and the main process is a double-solvent extraction process. The lubricating oil base oil prepared in the second extraction tower (2) is blended with the raw oil in a mass ratio of 1:2, and then used as the raw oil of the extraction tower 1. The blended oil, furfural and cosolvent are fed in a mass ratio of 1:1.5:0.3. The raffinate oil at the top of the first extraction tower (1) is recovered by evaporation to obtain the solvent, and then the raffinate oil enters the extraction tower 2 for a single-solvent extraction process. The main solvent furfural is fed into the upper part of the second extraction tower (2), and the extracted oil obtained at the top and bottom of the tower is collected.

[0021] The temperature gradient of the second extraction tower (2) is 60-100°C from bottom to top, and the raffinate oil obtained from the first extraction tower (1) is the feed of the second extraction tower (2), and the mass ratio of the raffinate oil to furfural is 1:1.5. The single-solvent extraction process is carried out under the experimental conditions. The raffinate oil obtained at the top is the lubricating oil base oil, part of which is blended with the raw oil and then continues to be extracted, and the product of high aromatic rubber plasticizer is obtained at the bottom. The yield of the obtained high aromatic rubber plasticizer product is 50.5%, the PCA value is 2.98%, the C A value is 24%, and the content of eight polycyclic aromatic hydrocarbons is 2.3 mg / kg, which meets the European Union and national standards. The yield of the lubricating oil base oil is 29.7%, the acid value of the lubricating oil base oil is 0.05 mgKOH / g, the viscosity index is 95, and the viscosity (100°C) is 8.9 mm 2 / s, which meets the standard of lubricating oil base oil.

[0022] Comparative Example 1

[0023] The same equipment and raw oil, main solvent and cosolvent D as in Example 1 are used, and the temperature gradient of the first extraction tower (1) is also the same, which is 40-60°C, and a double-solvent extraction process is carried out, and the second extraction tower (2) is not working. The first extraction tower (1) is not used for base oil, only reduced four-line extracted oil, and the raw oil, furfural and cosolvent are fed in the same mass ratio as in Example 1, which is 1:1.5:0.3. The raffinate oil at the top of the first extraction tower (1) is recovered by evaporation to obtain the solvent, and the yield of the raffinate oil is 81.0%, the PCA value is 2.87%, and the C A value is 21%.

[0024] It is shown that the C A value can be increased from 21% to 24% by the double-tower extraction of the present patent.

[0025] Example 2

[0026] The process is carried out in a continuous process, using the reduced four-line extracted oil of Example 1 as raw material, using furfural and solvent D as the main solvent and the cosolvent, respectively, and the cosolvent being an alkane with a carbon number of 8-10. The first extraction column (1) is composed of 5 temperature control sections from top to bottom, with a temperature gradient of 55-75°C, and mainly carries out a double-solvent extraction process. The lubricating oil base oil obtained from the second extraction column (2) is blended with the raw material oil in a mass ratio of 1:2, and the blended oil, furfural and cosolvent are fed in a mass ratio of 1:2:0.6. After the double-solvent extraction process in the first extraction column (1), raffinate oil is obtained at the top of the column, which is then fed into the second extraction column (2) for a single-solvent extraction process, and the extracted oil obtained at the bottom of the column is collected.

[0027] The second extraction column (2) is also composed of 5 temperature control sections from bottom to top, with a temperature gradient of 75-95°C, and the raffinate oil obtained from the first extraction column (1) is fed into the column in a mass ratio of 1:2.5 with furfural, and a single-solvent extraction process is carried out under the experimental conditions. The raffinate oil obtained at the top of the column is lubricating oil base oil, part of which is collected and blended with the raw material oil for further extraction, and the product of high aromatic rubber plasticizer is obtained at the bottom of the column. The yield of the product is 51.3%, the PCA value is 2.93%, the C A value is 23%, and the yield of the lubricating oil base oil is 29.1%. The lubricating oil base oil has an acid value of 0.05 mgKOH / g, a viscosity index of 95, and a viscosity (100°C) of 8.6 mm 2 / s, which meets the standard of lubricating oil base oil.

[0028] Comparative Example 2

[0029] The same equipment and raw material oil, main solvent and cosolvent D are used as in Example 2, and the temperature gradient of the first extraction column (1) is also the same, i.e. 55-75°C, for a double-solvent extraction process, and the second extraction column (2) is not used. The first extraction column (1) is fed only with the reduced four-line extracted oil, and the raw material oil, furfural and cosolvent are fed in the same mass ratio as in Example 2, i.e. 1:2:0.6. The raffinate oil obtained by evaporating the solvent from the raffinate liquid at the top of the first extraction column (1) has a yield of 80.5%, a PCA value of 2.89% and a C A value of 20.5%.

[0030] It is shown that the C A value can be increased from 20.5% to 23% by the double-column extraction of the present application.

[0031] Example 3

[0032] The process is carried out in a continuous process, using the reduced four-line extracted oil of Example 1 as raw material, using furfural and solvent D as the main solvent and the cosolvent, respectively, and the cosolvent being an alkane with a carbon number of 10-12. The first extraction column (1) is composed of 5 temperature control sections from top to bottom, with a temperature gradient of 70-100°C, and mainly carries out a double-solvent extraction process. The lubricating oil base oil obtained from the second extraction column (2) is blended with the raw material oil in a mass ratio of 1:2, and the blended oil, furfural and cosolvent are fed in a mass ratio of 1:3:1.

[0033] The second extraction column (2) is also composed of 5 temperature control sections from bottom to top, with a temperature gradient of 90-120°C, and the raffinate oil obtained from the first extraction column (1) and furfural are fed in a mass ratio of 1:3.5, and a single-solvent extraction process is carried out under the experimental conditions. The raffinate oil obtained at the top is the lubricating oil base oil, part of which is blended with the raw material oil and then subjected to extraction, and the product of high aromatic rubber plasticizer is obtained at the bottom. The yield of the product is 50.1%, the PCA value is 2.81%, the C A value is 22%, and the yield of the lubricating oil base oil is 26.0%. The lubricating oil base oil has an acid value of 0.05 mgKOH / g, a viscosity index of 95, and a viscosity (100°C) of 8.5 mm 2 / s, which meets the standard of lubricating oil base oil.

[0034] Comparative Example 3

[0035] The same equipment and raw material oil, main solvent and cosolvent D as in Example 3 are used, and the temperature gradient of the first extraction column (1) is also the same, i.e. 70-100°C, to carry out a double-solvent extraction process, and the second extraction column (2) is not used. The first extraction column (1) is fed only with the reduced four-line extracted oil, and the raw material oil, furfural and cosolvent are fed in the same mass ratio as in Example 3, i.e. 1:3:1. The raffinate oil obtained at the top of the first extraction column (1) is recovered by evaporation of the solvent, and the yield of the raffinate oil is 75.5%, the PCA value is 2.5%, and the C A value is 18.5%.

[0036] It is shown that the double-column extraction according to the present application can increase the C A value from 18.5% to 22%.

[0037] Example 4

[0038] The process is carried out in a continuous process, using the reduced four-line extracted oil of Example 1 as raw material, using furfural and solvent D as the main solvent and the cosolvent, respectively, and the cosolvent being an alkane with a carbon number of 12-14. The first extraction column (1) is composed of five temperature control sections from top to bottom, with a temperature gradient of 60-80°C, and mainly carries out a double-solvent extraction process. The lubricating oil base oil obtained from the second extraction column (2) is blended with the raw material oil in a mass ratio of 1:2, and the blended oil, furfural and cosolvent are fed in a mass ratio of 1:3:0.3. After the double-solvent extraction process in the first extraction column (1), raffinate oil is obtained at the top, which is then fed into the second extraction column (2) for a single-solvent extraction process, and the extracted oil obtained at the bottom is collected.

[0039] The second extraction column (2) is also composed of five temperature control sections from bottom to top, with a temperature gradient of 100-120°C, and the raffinate oil obtained from the first extraction column (1) is fed in a mass ratio of 1:4 with furfural, and a single-solvent extraction process is carried out under the experimental conditions. The raffinate oil obtained at the top is lubricating oil base oil, part of which is collected and blended with the raw material oil for further extraction, and the product of high aromatic rubber plasticizer is obtained at the bottom. The yield of the product is 47.3%, the PCA value is 2.72%, the C A value is 22%, and the yield of the lubricating oil base oil is 25.1%. The acid value of the lubricating oil base oil is 0.05 mgKOH / g, the viscosity index is 95, and the viscosity (100°C) is 8.8 mm 2 / s, which meets the standard of lubricating oil base oil.

[0040] Comparative Example 4

[0041] The same equipment and raw material oil, main solvent and cosolvent D as in Example 4 are used, and the temperature gradient of the first extraction column (1) is also the same, i.e. 60-80°C, for a double-solvent extraction process, and the second extraction column (2) is not used. The first extraction column (1) is fed only with the reduced four-line extracted oil, and the raw material oil, furfural and cosolvent are fed in the same mass ratio as in Example 4, i.e. 1:3:0.3. The raffinate oil obtained at the top of the first extraction column (1) is recovered by evaporation of the solvent, and the yield of the raffinate oil is 72.0%, the PCA value is 2.7%, and the C A value is 18.5%.

[0042] It is shown that the C A value can be increased from 18.5% to 22% by the double-column extraction of the present application.

[0043] Example 5

[0044] The process is carried out in a continuous process, and the reduced four-line extracted oil in Example 1 is used as the raw material, and the solvents NMP and D are used as the main solvent and the cosolvent, respectively, and the cosolvent is an alkane with a carbon number of 6-8. The first extraction tower (1) is composed of 5 temperature control sections from top to bottom, and the temperature gradient is 40-60°C, and the main process is a double-solvent extraction process. The lubricating oil base oil prepared in the second extraction tower (2) is blended with the raw oil in a mass ratio of 1:1, and then used as the raw oil of the extraction tower 1. The blended oil, the solvent NMP and the cosolvent are fed in a mass ratio of 1:1.5:0.3. After the double-solvent extraction process in the first extraction tower (1) is completed, the raffinate oil is obtained at the top of the tower, and then enters the second extraction tower (2) for a single-solvent extraction process. The extracted oil obtained at the bottom of the tower is collected.

[0045] The second extraction tower (2) is also composed of 5 temperature control sections from bottom to top, and the temperature gradient is 60-80°C. The raffinate oil obtained from the first extraction tower (1) is fed with the solvent NMP in a mass ratio of 1:1.5, and a single-solvent extraction process is carried out under the experimental conditions. The raffinate oil obtained at the top of the tower is lubricating oil base oil, part of which is collected and blended with the raw oil for further extraction, and the product of high aromatic rubber plasticizer is obtained at the bottom of the tower. The yield of the product is 50.4%, the PCA value is 2.93%, the C A value is 24%, and the yield of the lubricating oil base oil is 25.0%.

[0046] Comparative Example 5

[0047] The same equipment, raw oil, main solvent and cosolvent D as in Example 5 are used, and the temperature gradient of the first extraction tower (1) is also the same, i.e. 40-60°C, for a double-solvent extraction process, and the second extraction tower (2) is not used. The first extraction tower (1) is fed with only the reduced four-line extracted oil, and the raw oil, NMP and cosolvent are fed in the same mass ratio as in Example 5, i.e. 1:1.5:0.3. The raffinate oil is obtained by evaporating and recovering the solvent from the raffinate liquid at the top of the first extraction tower (1), and the yield of the raffinate oil is 72.0%, the PCA value is 2.8%, and the C A value is 18.0%.

[0048] It is shown that the double-tower extraction according to the present application can increase the C A value from 18.0% to 24%.

[0049] Example 6

[0050] The process is carried out in a continuous process, using the reduced four-line extracted oil of Example 1 as the raw material, using solvent NMP and solvent D as the main solvent and the cosolvent, respectively, and the cosolvent being an alkane with a carbon number of 8-10. The first extraction tower (1) is composed of five temperature control sections from top to bottom, with a temperature gradient of 55-75°C, and mainly carries out a double-solvent extraction process. The lubricating oil base oil obtained from the second extraction tower (2) is blended with the raw material oil in a mass ratio of 1:1, and then used as the raw material oil of the first extraction tower (1). The blended oil, solvent NMP (containing 8% water), and cosolvent are fed in a mass ratio of 1:2:0.6. After the double-solvent extraction process is completed in the first extraction tower (1), raffinate oil is obtained at the top of the tower, which is then fed into the second extraction tower (2) to carry out a single-solvent extraction process, and the extracted oil obtained at the bottom of the tower is collected.

[0051] The second extraction tower (2) is also composed of five temperature control sections from bottom to top, with a temperature gradient of 75-95°C. The raffinate oil obtained from the first extraction tower (1) is fed into the second extraction tower (2) in a mass ratio of 1:2.5 with solvent NMP, and a single-solvent extraction process is carried out under the experimental conditions. Raffinate oil, i.e., lubricating oil base oil, is obtained at the top of the tower, part of which is blended with the raw material oil and then subjected to extraction, and the high-aromatic rubber plasticizer product is obtained at the bottom of the tower. The yield of the product is 60.0%, the PCA value is 2.82%, the C A value is 23%, and the yield of the lubricating oil base oil is 20.3%.

[0052] Comparative Example 6

[0053] Using the same equipment and raw material oil, main solvent, and cosolvent D as in Example 6, and the temperature gradient of the first extraction tower (1) being the same as in Example 6, i.e., 55-75°C, a double-solvent extraction process is carried out, and the second extraction tower (2) is not used. The first extraction tower (1) is fed only with the reduced four-line extracted oil, and the raw material oil, NMP, and cosolvent are fed in the same mass ratio as in Example 6, i.e., 1:2:0.6. The raffinate oil obtained at the top of the first extraction tower (1) is evaporated to recover the solvent, and the yield of the raffinate oil is 80.0%, the PCA value is 2.84%, and the C A value is 20.0%.

[0054] It can be seen that, by using the double-tower extraction of the present application, the C A value can be increased from 20.0% to 23%.

[0055] Example 7

[0056] The process is carried out in a continuous process, using the reduced four-line extracted oil of Example 1 as the raw material, using solvent NMP (water content 8%) as the main solvent and solvent D as the cosolvent, the cosolvent being an alkane with carbon number 10-12. The first extraction tower (1) is composed of 5 temperature control sections from top to bottom, with a temperature gradient of 70-100°C, and mainly carries out a double-solvent extraction process. The lubricating oil base oil obtained from the second extraction tower (2) is blended with the raw material oil according to a mass ratio of 1:2, and then used as the raw material oil of the first extraction tower (1). The blended oil, solvent NMP (water content 8%) and cosolvent are fed according to a mass ratio of 1:3:1. After the double-solvent extraction process is completed in the first extraction tower (1), raffinate oil is obtained at the top of the tower, which is then fed into the second extraction tower (2) to carry out a single-solvent extraction process, and the extracted oil obtained at the bottom of the tower is collected.

[0057] The second extraction tower (2) is also composed of 5 temperature control sections from bottom to top, with a temperature gradient of 90-120°C. The raffinate oil obtained from the first extraction tower (1) and solvent NMP (without water) are fed according to a mass ratio of 1:3.5, and a single-solvent extraction process is carried out under the experimental conditions. Raffinate oil, i.e. lubricating oil base oil, is obtained at the top of the tower, part of which is blended with the raw material oil and then used for extraction, and the high-aromatic rubber plasticizer product is obtained at the bottom of the tower. The yield of the product is 52.4%, the PCA value is 2.70%, the C A value is 22%, and the yield of the lubricating oil base oil is 10.1%.

[0058] Comparative Example 7

[0059] Using the same equipment and raw material oil, main solvent and cosolvent D as in Example 7, and the temperature gradient of the first extraction tower (1) being the same as in Example 7, i.e. 55-75°C, a double-solvent extraction process is carried out, and the second extraction tower (2) is not used. The feed of the first extraction tower (1) does not contain base oil, but only reduced four-line extracted oil. The raw material oil, NMP (water content 8%) and cosolvent are fed according to the same mass ratio as in Example 7, i.e. 1:2:0.6. The raffinate obtained at the top of the first extraction tower (1) is evaporated to recover the solvent, and the yield of the raffinate oil is 71.0%, the PCA value is 2.88%, and the C A value is 20.0%.

[0060] It can be seen that, by using the double-tower extraction of the present application, the C A value can be increased from 20.0% to 22%.

[0061] Example 8

[0062] The process is carried out in a continuous process, and the feedstock is the reduced four-line extracted oil in Example 1, the solvent NMP (containing 8% water) is the main solvent, the solvent D is the cosolvent, and the cosolvent is an alkane with carbon number of 12-14. The first extraction tower (1) is composed of 5 temperature control sections from top to bottom, and the temperature gradient is 75-95°C, and the main process is the double-solvent extraction process. The lubricating oil base oil obtained from the second extraction tower (2) is blended with the feedstock oil according to the mass ratio of 1:1, and then the blended oil, the solvent NMP (containing 8% water) and the cosolvent are fed according to the mass ratio of 1:3:0.3. After the double-solvent extraction process in the first extraction tower (1) is completed, the raffinate oil is obtained at the top of the tower, and then the raffinate oil enters the second extraction tower (2) to perform the single-solvent extraction process, and the extracted oil obtained at the bottom of the tower is collected.

[0063] The second extraction tower (2) is also composed of 5 temperature control sections from bottom to top, and the temperature gradient is 75-95°C. The raffinate oil obtained from the first extraction tower (1) and the solvent NMP (without water) are fed according to the mass ratio of 1:3, and the single-solvent extraction process is performed under the experimental conditions. The raffinate oil obtained at the top of the tower is the lubricating oil base oil, part of which is blended with the feedstock oil to continue the extraction, and the high-aromatic rubber plasticizer product is obtained at the bottom of the tower. The yield of the product is 50.6%, the PCA value is 2.67%, the C A value is 23%, and the yield of the lubricating oil base oil is 17.7%.

[0064] Comparative Example 8

[0065] The same equipment, feedstock oil, main solvent and cosolvent D as in Example 8 are used, and a two-step extraction process is adopted. The temperature gradient of the first extraction tower (1) is also the same, which is 55-75°C, and the double-solvent extraction process is performed. The feedstock of the second extraction tower (2) is the reduced four-line extracted oil, and the second extraction tower (2) is also composed of 5 temperature control sections from bottom to top, and the temperature gradient is 80-110°C. The feedstock oil and the solvent NMP (without water) are fed according to the mass ratio of 1:2, and the single-solvent extraction process is performed under the experimental conditions. The material at the bottom of the second extraction tower (2) is the feedstock of the first extraction tower (1), and the three materials at the bottom of the tower, i.e. the oil, the NMP and the cosolvent, are fed according to the same mass ratio as in Example 8, which is 1:3:0.3. The raffinate oil is obtained by evaporating and recovering the solvent from the raffinate liquid at the top of the first extraction tower (1), and the yield of the raffinate oil is 50.0%, the PCA value is 2.84%, and the C A value is 21.0%.

[0066] It is shown that the C A value is increased from 21.0% to 23% through the double-tower extraction of the present application.

[0067] The environmental protection rubber plasticizer product prepared by the embodiment of the present application under the premise of using the reduced four-line extracted oil as the raw oil is compared with the key indicators of the best product of other processes:

[0068] One-step extraction process Two-step extraction process Process of the invention Product yield 83.8% 30.4% 10-53% Lubricating oil base oil yield 0% 25.0% 10-30% Product PCA value 2.82% 2.80% ≤3% Product C A values 18-21% 21% 22-24%

[0069] The product indicators of the one-step extraction process refer to the product indicators obtained by the one-step double-solvent extraction process of the raw oil directly using the main solvent and the auxiliary solvent under the best experimental condition. The two-step extraction process refers to that the raw oil is first extracted by the single solvent to obtain the extracted oil and the extracted oil, the extracted oil is desolventized to obtain the lubricating oil base oil, the extracted oil is desolventized and then double-solvent extracted to obtain the secondary extracted oil and the secondary extracted oil, the secondary extracted oil is desolventized to obtain the environmental protection rubber plasticizer product, and the product indicators in the table refer to the corresponding sample indicators obtained by the process under the best experimental condition.

[0070] Of course, the present application can have other various embodiments. The temperature gradient of each tower, the feeding ratio, the type of the filler, and the blending ratio of the refined oil of the extraction tower 2 and the raw oil can be adjusted according to the different raw oils. Those skilled in the art can make various corresponding changes and modifications according to the present application without departing from the spirit and essence of the present application, and these corresponding changes and modifications shall belong to the protection scope of the present application.

Claims

1. A method for producing a high aromatic environmentally friendly rubber plasticizer and a lubricating oil base oil, characterized by The two towers are combined in series to form a specific continuous production method. Lubricating oil solvent refined extracted oil is used as the raw oil. The lubricating oil base oil obtained from the second extraction tower (2) is mixed with the raw oil in a suitable ratio and then fed into the middle of the first extraction tower (1). The main solvent is fed into the upper part of the first extraction tower (1), and the auxiliary solvent is fed into the lower part of the tower. The material at the top of the tower is recovered to obtain the first refined oil, and the material at the bottom of the tower is recovered to obtain the second extracted oil. The first refined oil from the first extraction tower (1) is fed into the lower part of the second extraction tower (2), and the main solvent is fed into the upper part of the second extraction tower (2). The material at the top of the tower is recovered to obtain the second refined oil. Part of the second refined oil is extracted as lubricating oil base oil, and the other part is mixed with the raw oil and then fed into the first extraction tower (1). The material at the bottom of the second extraction tower (2) is recovered to obtain the high-aromatic rubber plasticizer product. The solvent / oil mass ratio of the first extraction tower (1) is: main solvent: raw oil: auxiliary solvent = 1.5-3: 1: 0.3-1.

0. The solvent / oil mass ratio of the second extraction tower (2) is: main solvent: first refined oil = 1.5-4:

1. The blending mass ratio of the lubricating oil base oil obtained from the second extraction tower (2) and the raw oil is between 0.5 and 1. The extraction temperature at the bottom of the first extraction tower (1) is 40-75℃, and the temperature at the top of the tower is 60-100℃. The temperature at the top of the tower is high, and the temperature at the bottom of the tower is low. The temperature gradually decreases from the top of the tower to the bottom of the tower. The extraction temperature at the bottom of the second extraction tower (2) is 60-100℃, and the temperature at the top of the tower is 80-120℃. The temperature at the top of the tower is high, and the temperature at the bottom of the tower is low. The temperature gradually decreases from the top of the tower to the bottom of the tower. The main solvent used is furfural or N-methyl pyrrolidone, and the auxiliary solvent is an alkane with a carbon number of 6-14.

Citation Information

Patent Citations

  • Production method of environment-friendly rubber oil

    CN109749772A