Preparation method of C9 thermal polymerization petroleum resin

Abstract

The invention discloses a preparation method of C9 thermal polymerization petroleum resin, relates to the technical field of thermal polymerization petroleum resin preparation, and aims to solve the problems of low production efficiency, high energy consumption, unstable product quality and difficulty in considering the production requirements of light-color and dark-color products in the traditional preparation method in the prior art. Comprising the following steps: 1, raw material preparation: feeding a cracked C9 raw material into a rectifying tower for cutting; 2, continuous polymerization reaction: respectively feeding the pretreated bicyclic enrichment liquid and heavy C9 into respective corresponding continuous tandem reaction kettle systems, and generating corresponding light-color and dark-color thermal polymerization petroleum resin precursors through thermal initiation polymerization reaction; step 3, secondary flash evaporation solvent removal: feeding the resin precursor subjected to the polymerization reaction into a secondary flash evaporation solvent removal system to obtain light-color and dark-color thermal polymerization petroleum resin with low solvent residue; and 4, product collection and post-treatment.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of thermally polymerized petroleum resins, in particular to a preparation method of C9 thermally polymerized petroleum resins. Background Art

[0002] Industrial cracking C9 is a by-product of naphtha steam cracking ethylene production unit. Its yield varies with the different steam cracking raw material components, generally about 10%-15%. The industrial cracking C9 components are extremely complex and very dispersed, rich in more than 200 components such as dicyclopentadiene and indene. It is mainly used to produce two-stage hydrogenation C9 components, C9 thermal polymerization petroleum resin, dicyclopentadiene (high purity grade), etc. Among them, the two-stage hydrogenation C9 components can be used as gasoline raw materials, the by-product tower bottoms can produce diesel and 180# fuel oil, C9 thermal polymerization petroleum resin is used to produce paints, low-end hot melt adhesives and rubber adhesives, etc., the by-product tower bottoms can produce 180# fuel oil and coumarone resin, and dicyclopentadiene (high purity grade) is used to produce pesticides, pharmaceutical intermediates and ENB, etc.

[0003] Thermal polymer resin is made by thermal polymerization with the byproduct of ethylene plant as raw material. The product appearance is milky white to yellow flake or granular solid, transparent and shiny, with good solubility, mutual solubility, water resistance, insulation, chemical stability to acid and alkali, good bonding performance, low thermal conductivity, etc. Thermal polymer resin and natural rubber particles have good mutual solubility and have no great influence on the rubber vulcanization process. Adding petroleum resin to rubber can play the role of viscosity increase, reinforcement and softening. It is suitable for high-demand rubber products such as radial tires. Thermal polymer resin can replace rosin, synthesize hot melt adhesives, and is very suitable for other modified resins;

[0004] At present, there are some problems in the preparation process of C9 thermal polymerization petroleum resin, such as unstable product quality, high production energy consumption, and large amount of three wastes discharged. Traditional preparation methods often have problems such as low production efficiency, high energy consumption, and unstable product quality, and it is difficult to take into account the production needs of light-colored and dark-colored products. Therefore, the market urgently needs to develop a preparation method for C9 thermal polymerization petroleum resin to help people solve existing problems. Summary of the invention

[0005] The purpose of the present invention is to provide a method for preparing C9 thermally polymerized petroleum resin to solve the problems of low production efficiency, high energy consumption, unstable product quality, and difficulty in taking into account the production needs of light-colored and dark-colored products in the traditional preparation method proposed in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a method for preparing C9 thermally polymerized petroleum resin, comprising the following steps:

[0007] Step 1: Raw material preparation, sending the cracked carbon nine raw material into a distillation tower for cutting to obtain light carbon nine, dicyclopentadiene-rich dicyclopentadiene-rich liquid and heavy carbon nine;

[0008] Step 2: Continuous polymerization reaction, the pre-treated bicyclic enriched liquid and heavy carbon nine are respectively sent into their corresponding continuous series reactor systems, and through thermal initiation polymerization reaction, under certain temperature, pressure and catalyst conditions, a stable and continuous polymerization process is achieved to generate corresponding light-colored and dark-colored thermally polymerized petroleum resin precursors;

[0009] Step 3: Secondary flash desolventization, the resin precursor after the polymerization reaction is sent to the secondary flash desolventization system, and the solvent is quickly evaporated by rapid pressure reduction and heating to achieve efficient desolventization, and obtain light-colored and dark-colored thermally polymerized petroleum resins with low solvent residue;

[0010] Step 4: Product collection and post-processing: the resin product after desolventization is processed to obtain light-colored and dark-colored C9 thermally polymerized petroleum resin products that meet quality standards.

[0011] Preferably, in the raw material preparation step, the operating conditions of the distillation tower include temperature gradient setting, pressure control and reflux ratio adjustment to ensure effective separation and purification of the raw materials.

[0012] Preferably, in the continuous polymerization reaction step, the number of continuous series reactor systems is at least two, and the temperature and pressure in each reactor can be independently regulated to achieve more precise reaction control and product performance optimization.

[0013] Preferably, the catalyst for the thermally initiated polymerization reaction is a free radical initiator, and the type and amount of the catalyst are precisely adjusted according to the characteristics of the raw materials and the performance of the target product.

[0014] Preferably, in the secondary flash desolventizing step, the temperature and pressure conditions of the primary flash chamber and the secondary flash chamber are optimized to ensure rapid evaporation of the solvent and low solvent residue in the resin product.

[0015] Preferably, the product collection and post-processing steps also include steps of quality testing and performance evaluation of the products to ensure that the product quality meets preset standards.

[0016] Preferably, in the product collection and post-processing steps, the processing of the resin product includes cooling, filtering and drying steps to remove impurities and improve product quality.

[0017] Preferably, the cracked carbon nine raw material is a cracked carbon nine fraction with a high concentration of dicyclopentadiene.

[0018] Preferably, in the continuous polymerization reaction step, the pretreatment of the bicyclic enriched liquid and the heavy carbon nine is a ratio adjustment, and the ratio of the bicyclic enriched liquid and the heavy carbon nine is adjusted by adjusting the ratio of the bicyclic enriched liquid and the heavy carbon nine and adding an appropriate amount of molecular weight regulating component.

[0019] Preferably, the molecular weight regulating component includes a chain transfer agent and a cross-linking agent, and the molecular weight distribution and performance of the resin product can be regulated by controlling the addition amount of the molecular weight regulating component.

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

[0021] 1. The invention realizes effective separation of raw materials through distillation cutting, ensures the purity and stability of raw materials, and lays a solid foundation for subsequent reactions. At the same time, the application of continuous polymerization reaction improves production efficiency and operational flexibility, reduces energy consumption, simplifies the process flow, and reduces the discharge of three wastes. In addition, the efficient desolventizing capacity of the secondary flash desolventizing system not only improves product quality, but also reduces solvent residue, meets environmental protection requirements, and can take into account the production needs of light-colored and dark-colored products, solving the problems of low production efficiency, high energy consumption, unstable product quality and difficulty in meeting diversified product needs in traditional preparation methods.

[0022] 2. The invention processes the resin product in the product collection and post-processing steps, including cooling, filtering, and drying steps. The filtering operation uses equipment such as a filter press or a vacuum filter to remove solid impurities in the resin product. The drying operation can use methods such as hot air drying or vacuum drying to evaporate the moisture in the resin product. Through these post-processing steps, the purity and stability of the product can be further improved, providing strong guarantees for the subsequent application of the product and improving product quality. At the same time, by removing impurities and moisture, the processing performance and weather resistance of the product can also be improved, thereby extending the service life of the product.

[0023] 3. The invention pre-treats the dicyclopentane enriched liquid and heavy carbon nine by adjusting the ratio in the continuous polymerization reaction step, adjusts the ratio of the dicyclopentane enriched liquid and heavy carbon nine, and adds an appropriate amount of molecular weight regulating components, and controls the amount of molecular weight regulating components added to regulate the molecular weight distribution and performance of the resin product. By adjusting the ratio, polymerization conditions and the amount of molecular weight regulating components added, light-colored and dark-colored thermal polymerization petroleum resin products with different softening points and melt viscosities can be flexibly produced to meet the diverse needs of the market. At the same time, by optimizing the ratio and polymerization conditions, the performance and quality of the product can be further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 The present invention is a flow chart of a method for preparing C9 thermally polymerized petroleum resin. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0026] See also Figure 1 The present invention provides an embodiment: a method for preparing a C9 thermally polymerized petroleum resin, comprising the following steps:

[0027] Step 1: Raw material preparation, sending the cracked carbon nine raw material into a distillation tower for cutting to obtain light carbon nine, dicyclopentadiene-rich bicyclic enriched liquid and heavy carbon nine, wherein the bicyclic enriched liquid and heavy carbon nine are used as the main raw materials for preparing light-colored and dark-colored thermally polymerized petroleum resins, respectively. By controlling the temperature and pressure conditions, the effective separation of the raw materials is achieved;

[0028] By sending the cracked C9 raw material into a distillation tower for cutting treatment, the complex cracked C9 components are separated according to their different boiling points, thereby obtaining three main components: light C9, dicyclopentadiene enriched liquid and heavy C9. Light C9 is mainly used in the production of other chemical products due to its lower boiling point, while dicyclopentadiene enriched liquid is rich in key ingredients such as dicyclopentadiene and is the main raw material for preparing C9 thermal polymerization petroleum resin. Heavy C9, due to its higher boiling point, contains more high molecular weight components and also plays an important role in the preparation of C9 thermal polymerization petroleum resin. Through precise cutting operations, the purity and stability of the raw materials can be ensured, laying a solid foundation for subsequent thermal polymerization reactions.

[0029] Step 2: Continuous polymerization reaction, the pre-treated bicyclic enriched liquid and heavy carbon nine are respectively sent into their corresponding continuous series reactor systems, and through thermal initiation polymerization reaction, under certain temperature, pressure and catalyst conditions, a stable and continuous polymerization process is achieved to generate corresponding light-colored and dark-colored thermally polymerized petroleum resin precursors;

[0030] Through the continuous production method, the production efficiency and operational flexibility are significantly improved, while the energy consumption is reduced, the process flow is simplified, and the discharge of three wastes is reduced;

[0031] Step 3: Secondary flash desolventization, the resin precursor after the polymerization reaction is sent to the secondary flash desolventization system, and the solvent is quickly evaporated by rapid pressure reduction and heating to achieve efficient desolventization, and obtain light-colored and dark-colored thermally polymerized petroleum resins with low solvent residue;

[0032] By sending the resin product into the flash tower, the solvent is evaporated quickly under high temperature and low pressure conditions, thereby achieving effective separation of the solvent and the resin. The setting of the flash tower should ensure that the material residence time is short to avoid over-reaction, thereby further improving the quality of the product. The setting of the two-stage flash evaporation not only improves the solvent removal efficiency, but also helps to reduce solvent residues, meeting environmental protection requirements;

[0033] Step 4: Product collection and post-processing: the resin product after desolventization is processed to obtain light-colored and dark-colored C9 thermally polymerized petroleum resin products that meet quality standards.

[0034] Furthermore, in the raw material preparation step, the operating conditions of the distillation tower include temperature gradient setting, pressure control and reflux ratio adjustment to ensure effective separation and purification of the raw materials. Precise operating conditions can minimize impurities in the raw materials, improve the purity and stability of the raw materials, and provide a high-quality raw material basis for subsequent thermal polymerization reactions, thereby ensuring the quality of the final product and improving the efficiency and reliability of the entire production process.

[0035] Furthermore, in the continuous polymerization reaction step, the number of continuous series reactor systems is at least two, and the temperature and pressure in each reactor can be independently regulated to achieve more precise reaction control and product performance optimization, which not only improves the flexibility and controllability of the production process, but also allows the reaction conditions to be more finely adjusted to optimize product performance. At the same time, the continuous production method significantly improves production efficiency, reduces energy consumption, and simplifies the process flow, bringing higher economic benefits to the enterprise.

[0036] Furthermore, the catalyst for the thermally initiated polymerization reaction is a free radical initiator, such as benzoyl peroxide, azobisisobutyronitrile, etc. The type and amount of the catalyst are precisely adjusted according to the characteristics of the raw materials and the performance of the target product. By precisely adjusting the type and amount of the catalyst, the efficient polymerization reaction can be ensured, while unnecessary side reactions can be reduced and the yield and purity of the product can be improved. In addition, according to the differences in raw materials and target products, flexible selection of catalysts can further optimize product performance and meet market demand.

[0037] Furthermore, in the secondary flash desolventizing step, the temperature and pressure conditions of the primary flash chamber and the secondary flash chamber are optimized to ensure rapid evaporation of the solvent and low solvent residue in the resin product. The optimization not only improves the solvent removal efficiency and reduces energy consumption, but also helps to reduce solvent residue and improve the environmental performance and safety of the product. At the same time, the product with low solvent residue has better processing performance and stability in subsequent applications.

[0038] Furthermore, the product collection and post-processing steps also include steps for quality inspection and performance evaluation of the products to ensure that the product quality meets the preset standards, ensuring that each batch of products meets the quality standards, improving the reliability and market competitiveness of the products. At the same time, through continuous quality inspection and performance evaluation, problems in the production process can be discovered and corrected in a timely manner, thereby continuously improving product quality and production efficiency.

[0039] Furthermore, in the product collection and post-processing steps, the processing of the resin product includes cooling, filtering, and drying steps to remove impurities. The filtering operation uses equipment such as a filter press or a vacuum filter to remove solid impurities in the resin product. The drying operation can use methods such as hot air drying or vacuum drying to evaporate the moisture in the resin product. Through these post-processing steps, the purity and stability of the product can be further improved, providing strong guarantees for the subsequent application of the product and improving product quality. At the same time, by removing impurities and moisture, the processing performance and weather resistance of the product can also be improved, thereby extending the service life of the product.

[0040] Furthermore, the cracked carbon nine raw material is a cracked carbon nine fraction with a high concentration of dicyclopentadiene. By selecting high-quality raw materials, it can be ensured that the product contains more key ingredients such as dicyclopentadiene, thereby improving the performance and quality of the product. At the same time, the high-concentration raw materials can also reduce energy consumption and costs in subsequent processing processes and improve production efficiency.

[0041] Furthermore, in the continuous polymerization reaction step, the pretreatment of the dicyclopentane enriched liquid and heavy carbon nine is a ratio adjustment, and the ratio of the dicyclopentane enriched liquid and heavy carbon nine is adjusted by adjusting the ratio of the dicyclopentane enriched liquid and heavy carbon nine and adding an appropriate amount of molecular weight regulating components, wherein the molecular weight regulating components include chain transfer agents and cross-linking agents, and the molecular weight distribution and performance of the resin product are regulated by controlling the addition amount of the molecular weight regulating components. By adjusting the ratio, polymerization conditions and the addition amount of the molecular weight regulating components, light-colored and dark-colored thermally polymerized petroleum resin products with different softening points and melt viscosities can be flexibly produced to meet the diverse needs of the market. At the same time, by optimizing the ratio and polymerization conditions, the performance and quality of the product can be further improved, which is conducive to enhancing market competitiveness.

[0042] Working principle: When in use, the cracked carbon nine raw material is sent to the distillation tower, and the temperature gradient, pressure and reflux ratio are controlled to achieve effective separation and purification of the raw materials to obtain light carbon nine, dicyclopentadiene-rich dicyclopentadiene-rich dicyclopentadiene-enriched liquid and heavy carbon nine. Then, the pretreated dicyclopentadiene-enriched liquid and heavy carbon nine are respectively sent to the continuous series reactor system, and thermally initiated polymerization reactions are carried out under specific temperature, pressure and catalyst conditions to generate light and dark thermally polymerized petroleum resin precursors. Next, the resin precursor after the polymerization reaction is sent to the secondary flash desolventization system, and efficient desolventization is achieved through rapid pressure reduction and heating to obtain a resin product with low solvent residue. Finally, the product is subjected to post-processing steps such as cooling, filtering, and drying, and quality inspection and performance evaluation are carried out at the same time to ensure that the product meets quality standards, thereby obtaining high-performance, low-solvent-residue light and dark C9 thermally polymerized petroleum resin products to meet the diverse needs of the market.

[0043] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A method for preparing C9 thermally polymerized petroleum resin, It is characterized in that The following steps are involved: Step 1: Raw material preparation, sending the cracked carbon nine raw material into a distillation tower for cutting to obtain light carbon nine, dicyclopentadiene-rich bicyclic enriched liquid and heavy carbon nine; Step 2: Continuous polymerization reaction, the pre-treated bicyclic enriched liquid and heavy carbon nine are respectively sent into their corresponding continuous series reactor systems, and through thermal initiation polymerization reaction, under certain temperature, pressure and catalyst conditions, a stable and continuous polymerization process is achieved to generate corresponding light-colored and dark-colored thermally polymerized petroleum resin precursors; Step 3: Secondary flash desolventization, the resin precursor after the polymerization reaction is sent to the secondary flash desolventization system, and the solvent is quickly evaporated by rapid pressure reduction and heating to achieve efficient desolventization, and obtain light-colored and dark-colored thermally polymerized petroleum resins with low solvent residue; Step 4: Product collection and post-processing: the resin product after desolventization is processed to obtain light-colored and dark-colored C9 thermally polymerized petroleum resin products that meet quality standards.

2. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: In the raw material preparation step, the operating conditions of the distillation tower include temperature gradient setting, pressure control and reflux ratio adjustment to ensure effective separation and purification of the raw materials.

3. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: In the continuous polymerization reaction step, the number of continuous series reactor systems is at least two, and the temperature and pressure in each reactor can be independently regulated to achieve more precise reaction control and product performance optimization.

4. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: The catalyst for the thermally initiated polymerization reaction is a free radical initiator, and the type and amount of the catalyst are precisely adjusted according to the characteristics of the raw materials and the performance of the target product.

5. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: In the secondary flash desolventizing step, the temperature and pressure conditions of the primary flash chamber and the secondary flash chamber are optimized to ensure rapid evaporation of the solvent and low solvent residue of the resin product.

6. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: The product collection and post-processing steps also include steps of quality testing and performance evaluation of the products to ensure that the product quality meets the preset standards.

7. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: In the product collection and post-processing steps, the processing of the resin product includes cooling, filtering, and drying steps to remove impurities and improve product quality.

8. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: The cracked carbon nine raw material is a cracked carbon nine fraction with a high concentration of dicyclopentadiene.

9. A method for preparing a C9 thermally polymerized petroleum resin according to claim 1, Features: In the continuous polymerization reaction step, the pretreatment of the bicyclic enriched liquid and the heavy carbon nine is a ratio adjustment, and the ratio of the bicyclic enriched liquid and the heavy carbon nine is adjusted by adjusting the ratio of the bicyclic enriched liquid and the heavy carbon nine and adding an appropriate amount of molecular weight regulating components.

10. A method for preparing a C9 thermally polymerized petroleum resin according to claim 9, Features: The molecular weight regulating components include chain transfer agents and cross-linking agents. The molecular weight distribution and performance of the resin product can be regulated by controlling the addition amount of the molecular weight regulating components.

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