A method for preparing a petroleum resin
Patent Information
- Application Number
- CN202310908419.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-24
- Publication Date
- 2026-10-23
- Estimated Expiration
- 2043-07-24
AI Technical Summary
但其产生的副产物及对环境的影响并未考虑
[0026]1、本发明一种石油树脂制备方法通过优化催化剂的成分、结构和表面性质,实现了石油树脂制备反应的高效催化,传统的石油树脂制备常采用酸性或碱性催化剂,但这些催化剂通常具有使用寿命短、废弃物产生多、反应选择性差等问题,本发明中的新型催化剂具有良好的催化活性、高选择性和长使用寿命,能够在相对温和的反应条件下实现高效的石油树脂制备。
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Abstract
Description
Technical Field
[0001] This invention relates to methods for preparing petroleum resins, particularly green and environmentally friendly methods, and belongs to the field of petrochemicals. Background Technology
[0002] Petroleum resins are an important class of chemical raw materials, widely used in various industrial fields such as coatings, adhesives, plastics, inks, and binders. They play a crucial role in industrial production, endowing products with specific properties and functions.
[0003] There are various methods for preparing petroleum resins, including thermal polymerization, catalytic polymerization, and oxidative polymerization. Traditional petroleum resin preparation often uses petroleum derivatives as raw materials, such as cracked oil, dewaxed oil, and aromatics. However, traditional preparation methods present several environmental and sustainability challenges, such as environmental impact, resource consumption, and byproduct generation.
[0004] Chinese invention patent CN105585666B discloses a "method for preparing dicyclopentadiene hydrogenated petroleum resin," which improves product yield and ensures that the resin prepared by this method is free of impurities such as gel and sulfur. It can be directly used for hydrogenation reactions without further treatment, and yields hydrogenated petroleum resin products with excellent performance and stable quality while ensuring catalyst lifespan. However, the byproducts and environmental impact are not considered.
[0005] Therefore, in recent years, green and environmentally friendly methods for preparing petroleum resins have attracted much attention. These methods aim to reduce environmental impact, decrease reliance on non-renewable resources, and improve the sustainability and eco-friendliness of petroleum resins. Summary of the Invention
[0006] The technical problem to be solved by the present invention is to provide a method for preparing petroleum resin, which achieves an efficient, environmentally friendly and sustainable petroleum resin preparation process by optimizing reaction conditions, improving catalyst design and applying green solvents.
[0007] This invention is achieved through the following scheme: a method for preparing petroleum resin, comprising the following steps:
[0008] s1. Prepare petroleum raw materials, including naphtha as a raw material for petroleum resin. The naphtha components include: 60%-70% alkanes, 20%-30% aromatics, 4%-5% alkenes, 1%-5% alicyclic hydrocarbons, and 1% heterocyclic compounds.
[0009] s2. Decolorize and deodorize the naphtha;
[0010] s3. Select a catalyst;
[0011] s4. Adjust the reaction conditions, adjust the reaction temperature of the reactor to 160-180℃ and stabilize the temperature through the temperature control device, the pressure to 8-10MPa, and the stirring speed to 300-500rpm;
[0012] s5. Add a green solvent to improve the selectivity and efficiency of the reaction;
[0013] s6. Microwave-assisted preparation: A microwave heating system is used to place the reaction system in a microwave field for heating. The reaction rate and product quality are controlled by adjusting the microwave power and radiation time.
[0014] s7. Separate and purify the reaction mixture to obtain the target petroleum resin product;
[0015] s8. Recycling and utilizing waste and by-products;
[0016] s9. Testing and evaluation: Testing and evaluation of the final petroleum resin product, including the determination of performance indicators such as density, viscosity, softening point, tensile strength, and abrasion resistance.
[0017] The decolorization treatment in step s2 is performed by activated carbon adsorption, and the deodorization treatment is performed by vacuum distillation.
[0018] The catalyst in step s3 is a platinum / iron oxide composite catalyst, and its preparation steps are as follows:
[0019] s31. Preparation of catalyst precursors;
[0020] s32, Preparation of catalyst composites;
[0021] s33, precipitation treatment and catalyst formation;
[0022] Activation of S34 catalyst.
[0023] The green solvent in step s5 is one of ethanol, dimethyl sulfoxide, and N-methylpyrrolidone.
[0024] The separation in step s7 is one of extraction or distillation, and the purification is a membrane separation process.
[0025] The beneficial effects of this invention are as follows:
[0026] 1. The present invention provides a method for preparing petroleum resin, which achieves highly efficient catalysis of the petroleum resin preparation reaction by optimizing the composition, structure and surface properties of the catalyst. Traditional petroleum resin preparation often uses acidic or basic catalysts, but these catalysts usually have problems such as short service life, high waste generation and poor reaction selectivity. The novel catalyst in the present invention has good catalytic activity, high selectivity and long service life, and can achieve efficient petroleum resin preparation under relatively mild reaction conditions.
[0027] 2. The present invention introduces a green solvent to replace the traditional organic solvent in a method for preparing petroleum resin. This not only helps to reduce the emission of volatile organic compounds, but also improves the safety and sustainability of the reaction system. The green solvent has good solubility and reactivity in the petroleum resin preparation process, which can effectively promote the reaction and improve the quality and purity of the product.
[0028] 3. This invention introduces microwave radiation as an energy source into a method for preparing petroleum resin, accelerating the petroleum resin preparation reaction. Microwave-assisted preparation has the advantages of rapid heating and accelerated reaction, which can greatly shorten the reaction time and improve the quality of the product. At the same time, due to the efficient utilization of microwave radiation energy, energy consumption is also significantly reduced. In this invention, through the rational design of the reaction system and the control of microwave power, efficient heating and control of the petroleum resin preparation reaction are achieved.
[0029] 4. This invention's method for preparing petroleum resin fully considers the principles of a circular economy, achieving the recycling of waste and by-products during the petroleum resin preparation process. By optimizing the reaction system and separation process, waste is transformed into valuable by-products, which are then recycled in other processes or products, reducing resource waste and environmental burden. The waste and by-products in this invention, after appropriate treatment and purification, can be used as raw materials or additives in other chemical production processes, maximizing resource utilization. Detailed Implementation
[0030] The present invention will be further described below, but the scope of protection of the present invention is not limited to the content described.
[0031] For clarity, not all features of the actual embodiments will be described. In the following description, well-known functions and structures will not be described in detail, as they would confuse the invention with unnecessary details. It should be understood that in the development of any actual embodiment, a great deal of implementation detail must be made to achieve the developer’s specific goals, such as changing one embodiment to another according to the limitations of the system or business. In addition, it should be understood that such development work may be complex and time-consuming, but is merely routine work for those skilled in the art.
[0032] The preparation method of petroleum resin is as follows:
[0033] Step 1: Prepare petroleum raw materials
[0034] Prepare naphtha as a raw material for petroleum resins. Ensure the naphtha meets quality standards and is free of impurities and contaminants. Table 1 shows the percentage of naphtha raw material components (by mass) in each example.
[0035] Step 2: Petroleum feedstock pretreatment
[0036] Naphtha undergoes decolorization and deodorization treatment to remove impurities and odors. Decolorization can be achieved using activated carbon adsorbents; the naphtha is contacted with activated carbon and stirred, then the activated carbon and adsorbed impurities are removed by filtration or centrifugation. Deodorization can be carried out by methods such as distillation or vacuum distillation.
[0037] Step 3: Selecting a catalyst
[0038] The catalyst used is a platinum / iron oxide composite catalyst.
[0039] Step 4: Adjusting reaction conditions
[0040] Temperature: Based on the characteristics of the selected catalyst and reaction system, an appropriate reaction temperature is determined and controlled within the range of 60-180℃. The reaction system can be heated using equipment such as heaters or reaction vessels, and the temperature can be stabilized using a temperature control device.
[0041] Pressure: The reaction is carried out at 8-10 MPa atmospheric pressure, but it can be adjusted within a certain range depending on the catalyst and the needs of the reaction system. The reaction pressure can be controlled using a pressure regulator.
[0042] Stirring speed: 300-500 rpm.
[0043] Step 5: Introduce green solvent
[0044] Introducing green solvents to replace traditional organic solvents. Adding an appropriate amount of green solvent to the reaction system can improve the selectivity and efficiency of the reaction. The selection of green solvents should consider their impact on catalyst activity and the stability of the reaction system.
[0045] Step 6: Microwave-assisted preparation
[0046] Microwave radiation equipment provides energy to accelerate the reaction process. A microwave reactor or microwave heating system can be used to place the reaction system in a microwave field for heating. The reaction rate and product quality can be controlled by adjusting the microwave power and radiation time.
[0047] Step 7: Separation and purification
[0048] The reaction mixture is separated and purified to obtain the target petroleum resin product. Common separation methods include distillation and extraction. Distillation is a commonly used method, separating different components at different boiling points by controlling temperature and pressure. Extraction utilizes solvents to selectively extract the target components, followed by distillation or removal of the extractant to obtain pure petroleum resin. After product separation, further purification may be required to obtain a high-purity product; membrane separation processes are often used for purification.
[0049] Step 8: Recycling and utilizing waste and by-products
[0050] The generated waste and byproducts are treated and utilized to achieve the application of a circular economy. Waste treatment can employ appropriate methods such as incineration, catalytic combustion, and catalytic cracking. Byproducts can be purified and processed for use in other chemical production processes or as an energy source.
[0051] Step 9: Testing and Evaluation
[0052] The final petroleum resin product is tested and evaluated, including the determination of performance indicators such as density, viscosity, softening point, tensile strength, and abrasion resistance. Standard testing methods or self-developed testing methods can be used for evaluation to ensure the product meets quality requirements. The performance indicators of the tested petroleum resin are shown in Table 3.
[0053] The preparation process of the platinum / iron oxide composite catalyst in step 3 is as follows:
[0054] 1. Preparation of catalyst precursor:
[0055] Preparation of platinum precursor: Dissolve 0.5g of chloroplatinic acid in 50mL of deionized water to obtain an aqueous solution of platinum.
[0056] Preparation of iron oxide precursor: Dissolve 0.5g of ferrous sulfate in 50mL of deionized water to obtain an aqueous solution of iron.
[0057] 2. Preparation of catalyst composites:
[0058] The platinum solution and the iron solution were mixed and stirred at 500 rpm at 60°C until homogeneous.
[0059] Reaction time: 2 hours.
[0060] 3. Precipitation treatment and catalyst formation:
[0061] The reaction mixture is separated by centrifugation or filtration to remove unreacted salts and solvents.
[0062] Wash the precipitate with deionized water to remove impurities.
[0063] Drying temperature: 80℃.
[0064] Drying time: 12 hours.
[0065] 4. Catalyst activation:
[0066] The prepared platinum / iron oxide composite catalyst was heated to 300°C under a nitrogen atmosphere and held at that temperature for 2 hours.
[0067] After cooling to room temperature, the catalyst was placed in a hydrogen atmosphere and reduced at 200°C for 4 hours.
[0068] Although the technical solutions of the present invention have been described and enumerated in detail, it should be understood that modifications to the above embodiments or the adoption of equivalent alternatives are obvious to those skilled in the art. Such modifications or improvements made without departing from the spirit of the present invention are all within the scope of protection claimed by the present invention.
[0069] Table 1: Percentage of Naphtha Raw Material Components in the Examples (by Mass)
[0070]
[0071]
[0072] Table 2: Green Solvents for Each Example
[0073] Example 1 ethanol Example 2 dimethyl sulfoxide Example 3 N-methylpyrrolidone
[0074] Table 3: Performance Indicators of Petroleum Resins
[0075]
Claims
1. A method for preparing petroleum resin, characterized in that, Includes the following steps: s1. Prepare petroleum raw materials, specifically naphtha as the raw material for petroleum resin. The naphtha composition includes: 60%-70% alkanes, 20%-30% aromatics, 4%-5% alkenes, 1%-5% alicyclic hydrocarbons, and 1% heterocyclic compounds. s2. Decolorize and deodorize the naphtha; s3. Catalysis is carried out using a platinum / iron oxide composite catalyst; s4. Adjust the reaction conditions: adjust the reaction temperature of the reactor to 160-180℃ and stabilize the temperature using a temperature control device; the pressure to 8-10MPa; and the stirring speed to 300-500 rpm. s5. Added solvent: selected from one or more of ethanol, dimethyl sulfoxide, and N-methylpyrrolidone; s6. Microwave-assisted preparation: A microwave heating system is used to place the reaction system in a microwave field for heating. The reaction rate and product quality are controlled by adjusting the microwave power and radiation time. s7. Separate and purify the reaction mixture to obtain the target petroleum resin product; s8. Recycling and utilizing waste and by-products; s9. Testing and evaluation: Testing and evaluation of the final petroleum resin product, including determination of density, viscosity, softening point, tensile strength, and abrasion resistance properties.
2. The method for preparing petroleum resin according to claim 1, characterized in that... The decolorization treatment in step s2 is performed by activated carbon adsorption, and the deodorization treatment is performed by vacuum distillation.
3. The method for preparing petroleum resin according to claim 1, characterized in that... The separation in step s7 is one of extraction or distillation, and the purification is a membrane separation process.
Citation Information
Patent Citations
A method for preparing dicyclopentadiene hydrogenated petroleum resin
CN105585666B
Naphtha raw material catalysis cracking method
CN105349173A
Preparation method of light-color modified petroleum resin with low softening point
CN108822257A