A method for preparing a carbon five petroleum resin

Abstract

The application belongs to the technical field of petroleum resin, and provides a preparation method of C5 petroleum resin, which comprises the following steps: S1, 3.2-3.5 g of a catalyst and 160-175 g of a functional reagent are added into a reactor and heated in a 50 DEG C water bath; when the temperature reaches 45 DEG C, a mixed solution is added dropwise into the reactor, and constant temperature is maintained to obtain a base resin solution; the mass of the catalyst is 1.2-1.5% of the mass of the mixed solution; the mixed solution is composed of piperylene and alpha-methylstyrene, and the mass of the alpha-methylstyrene is 10.7-11.2% of the mass of the mixed solution; the functional reagent is prepared by dissolving hydrogenated rosin glyceride in a solvent; S2, after the base resin is sequentially subjected to alkali washing and water washing, an antioxidant is added to obtain an intermediate resin solution; and S3, the intermediate resin solution is subjected to distillation, and the C5 petroleum resin is obtained.

Description

Technical Field

[0001] This invention belongs to the field of petroleum resin technology, and in particular relates to a method for preparing C5 petroleum resin. Background Technology

[0002] C5 petroleum resin has an aliphatic structure as its main chain segment. It has the characteristics of low acid value, good miscibility, water resistance, ethanol resistance and chemical corrosion resistance. It also has the characteristics of good viscosity adjustment and thermal stability. It is widely used in rubber, coatings, traffic paint, ink, papermaking and other industries.

[0003] In the prior art, in order to expand the application fields of C5 petroleum resin, such as its better application in the adhesive industry, it is required that its softening point be in a lower range and that it have a lower melting temperature. This helps to improve the initial tack and processing performance of adhesives, and is especially suitable for applications requiring high flexibility. In the process of preparing C5 petroleum resin, an aromatic monoolefin (α-methylstyrene) is added. As the amount of α-methylstyrene added increases, the content of diene in the component decreases, the ratio of diene and monoolefin decreases, the active component of the system decreases, the reaction is relatively slow, and the softening point decreases accordingly.

[0004] However, aromatic monoolefins (α-methylstyrene) themselves contain benzene rings (and also alkenyl side chains that are more easily oxidized than benzene rings), which will cause the degree of unsaturation in the structure to deepen and affect the color of the product; as the amount added increases, the color of the resin deteriorates, affecting the aesthetics of the adhesive when it is used. Summary of the Invention

[0005] To address the aforementioned problems, this invention proposes a method for preparing C5 petroleum resin. By increasing the amount of aromatic monoolefin (α-methylstyrene) added, the softening point of the prepared C5 petroleum resin is lowered, while its appearance color (color number) is reduced to improve its aesthetics in actual use.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.2-3.5g of catalyst and 160-175g of functional reagent to the reactor and heat in a 50℃ water bath; when the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30-35 minutes to obtain the basic resin solution. The mass of the catalyst is 1.2-1.5% of the mass of the mixture. The mixture is composed of isoprene and α-methylstyrene, wherein the mass of α-methylstyrene is 10.7-11.2% of the mass of the mixture. The functional reagent is prepared by dissolving hydrogenated rosin glycerol ester in a solvent; S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. An antioxidant is added to the organic layer to obtain the intermediate resin solution. S3. The intermediate resin solution obtained in S2 is distilled to obtain the C5 petroleum resin.

[0007] Furthermore, the preparation method of the functional reagent is as follows: after pulverizing hydrogenated rosin glycerol ester to a particle size ≥80 mesh, the specific surface area can be increased, the dissolution rate in the solvent can be accelerated, and uniform mixing can be ensured; add it to the solvent, the mass of hydrogenated rosin glycerol ester is 4.5-5.5% of the solvent mass, stir to dissolve, and the reagent is obtained.

[0008] This avoids the problem of uneven dispersion caused by direct solid-state addition, while preventing the initial violent reaction from affecting the overall polymerization equilibrium.

[0009] Furthermore, the solvent includes toluene and / or xylene.

[0010] Further, in S2, the specific operation of the alkaline washing treatment is as follows: the base resin solution is transferred into the washing tank, heated in a water bath until there is reflux, 480-510g of 50℃ 10wt% NaOH aqueous solution and 3.7-4.2mL of 1wt% demulsifier aqueous solution are added to the washing tank, stirred for 5min and then stopped, and sedimentation begins. After sedimentation for 5-15min according to the stratification effect, the alkaline water layer is separated, and the organic layer is left in the tank.

[0011] Furthermore, in S2, the specific operation of the water washing treatment is as follows: the organic layer is washed with water in the same way (with demulsifier added), and then the water washing is repeated without demulsifier until sedimentation, and the pH value of the water layer is measured to be 7-8 using test paper.

[0012] Furthermore, the demulsifier is PFA8311.

[0013] Further, in S3, the specific operation of the distillation process is as follows: the intermediate resin liquid is distilled under normal pressure. When the bottom temperature reaches 200°C, water vapor is introduced and the vacuum pump is turned on for reduced pressure distillation. When the temperature rises to 220°C, the heating power is turned off and the heating jacket is removed. When the temperature drops to 200°C, the venting valve is opened to release the air and the vacuum pump is turned off. After weighing, the liquid is poured out and cooled to room temperature.

[0014] Furthermore, the catalyst is AlCl3 solid powder.

[0015] Furthermore, the antioxidant is antioxidant 1010.

[0016] Compared with the prior art, the present invention has the following beneficial effects: In the preparation of the C5 petroleum resin of the present invention, the softening point of the obtained C5 petroleum resin is reduced by increasing the amount of α-methylstyrene added, while hydrogenated rosin glycerol ester is introduced by pre-dissolving.

[0017] On the one hand, hydrogenated rosin glycerol contains multiple long-chain aliphatic structures with significant steric hindrance. During cationic polymerization, it can act as a mild chain transfer agent or end-capping agent, limiting excessive growth and cross-linking of the polymer backbone, thereby effectively controlling the molecular weight distribution and slightly reducing the average molecular weight. Simultaneously, its polar ester groups may slightly interfere with the coordination environment of the catalyst (AlCl3) active center, making the reaction more stable and reducing the risk of explosive polymerization. Furthermore, α-methylstyrene itself has high steric hindrance due to methyl substitution, tending to form short-branched structures. When coexisting with hydrogenated rosin glycerol, the combined effect further weakens the cross-linking tendency between dienes (isopentadiene), resulting in higher linearity of the final product, macroscopically manifested as a decrease in the softening point. In other words, through steric hindrance and chain transfer, it inhibits high cross-linking, regulates molecular weight distribution, weakens diene activity, promotes α-methylstyrene insertion, forms flexible segments, and thus synergistically lowers the softening point.

[0018] On the other hand, the benzene ring in α-methylstyrene undergoes oxidation under high-temperature (aerobic) conditions (it also contains alkenyl side chains, which are more easily oxidized than the benzene ring), generating chromophores. Hydrogenated rosin glycerol esters, due to their highly saturated polycyclic structure and residual trace amounts of phenolic substances, possess a certain free radical scavenging ability, which can inhibit thermo-oxidative degradation in the later stages of polymerization and during vacuum distillation, thus mitigating discoloration caused by thermo-oxidative aging. Furthermore, residual AlCl3 catalyst is one of the important factors leading to later yellowing (Fe...). 3+ / Cu 2+ (Impurities can catalyze oxidation). The carboxylic acid ester groups in hydrogenated rosin glycerol ester can chelate with metal ions, reducing their catalytic activity and thus lowering the risk of color deepening. Hydrogenated rosin glycerol ester itself also helps to improve the thermal stability of the resin liquid, reducing local charring during distillation and indirectly improving transparency and brightness. That is, by scavenging free radicals, chelating metal ions, and improving thermal stability, it inhibits oxidation side reactions, prevents high-temperature carbonization, and thus synergistically reduces the appearance color (Gardner color). Attached Figure Description

[0019] Figure 1 This is a comparative trend chart of the softening point (°C) data of the C5 petroleum resins prepared in Examples 1-3 and Comparative Examples 1-5 of the present invention. Figure 2 This is a comparative trend chart showing the appearance and color (color number) data of the C5 petroleum resins prepared in Examples 1-3 and Comparative Examples 1-5 of the present invention. Detailed Implementation

[0020] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] Unless otherwise specified, the raw materials used in the embodiments and comparative examples of this application are all commercially available.

[0022] Example 1: (a) The functional reagent was prepared by dissolving hydrogenated rosin glycerol ester in a solvent; The specific preparation method is as follows: After pulverizing hydrogenated rosin glycerol ester to a particle size of 80 mesh, add it to the solvent toluene, where the mass of hydrogenated rosin glycerol ester is 5.0% of the mass of solvent toluene, stir to dissolve, and the product is obtained.

[0023] (II) A method for preparing a C5 petroleum resin, comprising the following steps: S1. Add 3.5g of catalyst and 170g of functional reagent to the reactor and heat in a 50℃ water bath. When the reactor temperature reaches 45℃, start adding the mixture dropwise to the reactor. After the addition is complete, continue to keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0024] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture; that is, the mass of the mixture added is 250g.

[0025] The mixture is composed of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 11% of the mass of the mixture; that is, in 250g of the mixture, α-methylstyrene is 27.5g and isoprene is 222.5g.

[0026] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0027] The specific operation of the alkaline washing treatment is as follows: the base resin solution is transferred into the washing tank and heated in a water bath until there is reflux. Then, 500g of 10wt% NaOH aqueous solution at 50℃ and 4.0mL of 1wt% demulsifier aqueous solution (PFA8311) are added to the washing tank. After stirring for 5 minutes, the stirring is stopped and sedimentation begins. After sedimentation for 12 minutes, the alkaline water layer is separated, and the organic layer remains in the tank.

[0028] The specific operation of the water washing treatment is as follows: wash the organic layer with water in the same way (with demulsifier added), and then repeat the water washing without demulsifier until sedimentation. Then use test paper to measure the pH value of the water layer to be 7-8.

[0029] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0030] The specific operation of the distillation process is as follows: the intermediate resin liquid is distilled under normal pressure. When the bottom temperature reaches 200°C, water vapor is introduced and the vacuum pump is turned on for reduced pressure distillation. When the temperature rises to 220°C, the heating power is turned off and the heating jacket is removed. When the temperature drops to 200°C, the venting valve is opened to release the air and the vacuum pump is turned off. After weighing, the liquid is poured out and cooled to room temperature.

[0031] Example 2: The difference between this example and Example 1 is that: (i) the functional reagent is prepared by dissolving hydrogenated rosin glycerol ester in a solvent; The specific preparation method is as follows: After pulverizing hydrogenated rosin glycerol ester to a particle size of 80 mesh, add it to the solvent toluene. The mass of hydrogenated rosin glycerol ester is 4.5% of the mass of the solvent toluene. Stir to dissolve, and the product is obtained.

[0032] (II) A method for preparing a C5 petroleum resin, comprising the following steps: S1. Add 3.2g of catalyst and 175g of functional reagent to the reactor and heat in a 50℃ water bath. When the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0033] The mass of the catalyst is 1.2% of the mass of the mixture.

[0034] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 10.7% of the mass of the mixture.

[0035] S2. Transfer the base resin solution obtained in S1 into a washing tank, and perform alkali washing and water washing treatment in sequence. Then, add 1.25g of antioxidant 1010 to the organic layer to obtain the intermediate resin solution.

[0036] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0037] Example 3: The difference between this example and Example 1 is that: (i) the functional reagent is prepared by dissolving hydrogenated rosin glycerol ester in a solvent; The specific preparation method is as follows: After pulverizing hydrogenated rosin glycerol ester to a particle size of 80 mesh, add it to the solvent toluene, where the mass of hydrogenated rosin glycerol ester is 5.5% of the mass of solvent toluene, stir to dissolve, and the product is obtained.

[0038] (II) A method for preparing a C5 petroleum resin, comprising the following steps: S1. Add 3.3g of catalyst and 160g of functional reagent to the reactor and heat in a 50℃ water bath. When the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 35 minutes to obtain the basic resin solution.

[0039] The mass of the catalyst is 1.5% of the mass of the mixture.

[0040] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 11.2% of the mass of the mixture.

[0041] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.4g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0042] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0043] Comparative Example 1: The difference between this comparative example and Example 1 is that the functional reagent is replaced with the solvent toluene, that is, hydrogenated rosin glycerol ester is not added; and the mass of α-methylstyrene is 10% of the mass of the mixture.

[0044] Specifically, a method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.5g of catalyst and 162g of solvent toluene to the reactor and heat in a 50°C water bath. When the reactor temperature reaches 45°C, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0045] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture.

[0046] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 10% of the mass of the mixture.

[0047] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0048] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0049] Comparative Example 2: The difference between this comparative example and Example 1 is that the functional reagent is replaced with the solvent toluene, that is, hydrogenated rosin glycerol ester is not added.

[0050] Specifically, a method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.5g of catalyst and 162g of solvent toluene to the reactor and heat in a 50°C water bath. When the reactor temperature reaches 45°C, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0051] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture.

[0052] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 11% of the mass of the mixture.

[0053] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0054] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0055] Comparative Example 3: The difference between this comparative example and Example 1 is that the mass of α-methylstyrene is 10% of the mass of the mixture.

[0056] Specifically, a method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.5g of catalyst and 170g of functional reagent to the reactor and heat in a 50℃ water bath. When the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0057] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture.

[0058] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 10% of the mass of the mixture.

[0059] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0060] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0061] Comparative Example 4: The difference between this comparative example and Example 1 is that the mass of α-methylstyrene is 12% of the mass of the mixture.

[0062] Specifically, a method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.5g of catalyst and 170g of functional reagent to the reactor and heat in a 50℃ water bath. When the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0063] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture.

[0064] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 12% of the mass of the mixture.

[0065] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0066] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0067] Comparative Example 5: The difference between this comparative example and Example 1 is that hydrogenated rosin glycerol ester was added in solid form.

[0068] Specifically, a method for preparing a C5 petroleum resin includes the following steps: S1. Add 3.5g of catalyst, 8g of hydrogenated rosin glycerol ester and 162g of solvent toluene to the reactor and heat in a 50°C water bath. When the reactor temperature reaches 45°C, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30 minutes to obtain the basic resin solution.

[0069] The catalyst is AlCl3 solid powder; the mass of the catalyst is 1.4% of the mass of the mixture.

[0070] The mixture consists of isoprene and α-methylstyrene, with the mass of α-methylstyrene being 11% of the mass of the mixture.

[0071] S2. The base resin solution obtained in S1 is transferred into a washing tank and subjected to alkali washing and water washing in sequence. Then, 1.3g of antioxidant 1010 is added to the organic layer to obtain the intermediate resin solution.

[0072] S3. The intermediate resin solution obtained in S2 is distilled to obtain C5 petroleum resin.

[0073] Test Example: Test Subjects: C5 petroleum resin samples prepared in Examples 1-3 and Comparative Examples 1-5. Test Items and Methods: ① Softening Point - determined according to GB / T 4507-2014. ② Appearance and Color - determined according to GB / T22295-2008; the resin sample was dissolved in toluene to prepare a homogeneous solution, with a mass ratio of resin sample to toluene of 1:1. Test Results: See Table 1.

[0074] Table 1. Test Data for Experimental Examples Softening point (°C) Appearance and color (color code) Example 1 87.8 4 Example 2 88.0 4 Example 3 87.7 4 Comparative Example 1 91.1 4 Comparative Example 2 89.2 5 Comparative Example 3 90.7 4 Comparative Example 4 87.5 5 Comparative Example 5 88.5 5 Results Analysis: Combining the data in Table 1 and... Figures 1-2 Analysis of Examples 1-3 shows that the softening point of the C5 petroleum resin prepared by the present invention (Examples 1-3) is as low as 87.7-88.0℃, and the appearance color (Gardner color) is as low as No. 4.

[0075] Combining the data in Table 1 and Figures 1-2 The analysis of Example 1 and Comparative Examples 1-5 was conducted, specifically comparing Comparative Examples 1 and 2. It was found that, compared to Comparative Example 1 where the mass of α-methylstyrene was 10% of the mass of the mixture, the mass of α-methylstyrene in Comparative Example 2 increased to 11% of the mass of the mixture. As a result, the softening point of the prepared C5 petroleum resin decreased from 91.1℃ (Comparative Example 1) to 89.2℃ (Comparative Example 2), but at the same time, the appearance color (Gardner color) increased from color No. 4 (Comparative Example 1) to color No. 5 (Comparative Example 2).

[0076] This is mainly because increasing the amount of α-methylstyrene reduces the content of dienes in the components, decreases the ratio of dienes and monoenes, reduces the active components in the system, makes the reaction relatively slow, and lowers the softening point. However, at the same time, α-methylstyrene itself contains benzene rings, which will cause the degree of unsaturation in the structure to deepen, affecting the color of the product. As its addition increases, the resin color deepens, and the color number tends to increase.

[0077] Specifically, by comparing Comparative Example 1 and Comparative Example 3, it can be seen that compared to Comparative Example 1 (the mass of α-methylstyrene is 10% of the mass of the mixture), Comparative Example 3 introduced hydrogenated rosin glycerol ester by pre-dissolving; as a result, the softening point of the prepared C5 petroleum resin decreased from 91.1℃ (Comparative Example 1) to 90.7℃ (Comparative Example 3), a decrease of 0.4℃; the appearance color (Gardner color) remained unchanged.

[0078] Comparing Comparative Example 2 and Example 1, it can be seen that, compared to Comparative Example 2 (where the mass of α-methylstyrene is 11% of the mass of the mixture), Example 1 also introduced hydrogenated rosin glycerol ester by pre-dissolving; as a result, the softening point of the prepared C5 petroleum resin decreased from 89.2℃ (Comparative Example 2) to 87.8℃ (Comparative Example 3), a decrease of 1.4℃; and the appearance color (Gardner color) decreased from color No. 5 (Comparative Example 2) to color No. 4 (Example 1).

[0079] This indicates that increasing the mass of α-methylstyrene to 11% of the mixture, compared to 10% of the mixture's mass, can synergistically reduce the softening point and appearance (Gardner color) of the resulting C5 petroleum resin, in conjunction with the pre-dissolved hydrogenated rosin glycerol ester. In other words, within a certain dosage range, more α-methylstyrene can better exert a synergistic effect with hydrogenated rosin glycerol ester, synergistically reducing the softening point of the resulting C5 petroleum resin.

[0080] By comparing with Comparative Example 5, it can be seen that when the mass of α-methylstyrene is 11% of the mass of the mixture, the method of introducing hydrogenated rosin glycerol ester is changed from pre-dissolving (Example 1) to solid addition (Comparative Example 5). As a result, the softening point of the C5 petroleum resin prepared in Comparative Example 5 is 88.5℃, which is between 89.2℃ of Comparative Example 2 and 87.8℃ of Example 1, and the appearance color (Gardner color) remains the same as color No. 5 of Comparative Example 2.

[0081] This indicates that, compared to solid addition, introducing hydrogenated rosin glycerol esters via pre-dissolution is more beneficial in reducing the softening point and appearance (Gardner color) of the prepared C5 petroleum resin.

[0082] This is mainly because pulverizing hydrogenated rosin glycerol ester to a particle size of 80 mesh can increase the specific surface area, accelerate its dissolution rate in the solvent, and ensure uniform mixing in the subsequent process. This can avoid the problem of uneven dispersion caused by direct solid addition, and at the same time prevent the initial violent reaction from affecting the overall polymerization balance, thereby better exerting its own role and synergistic effect.

[0083] In comparison with Comparative Example 4, it can be seen that by further increasing the mass of α-methylstyrene to 12% of the mass of the mixture, even with the introduction of hydrogenated rosin glycerol esters through pre-dissolution, the final C5 petroleum resin still achieves a color (Gardner chromaticity) of No. 5.

[0084] In summary, the present invention (Examples 1-3) reduces the softening point of the prepared C5 petroleum resin by increasing the mass of α-methylstyrene to 10.7-11.2% of the mass of the mixture, while simultaneously introducing hydrogenated rosin glycerol ester through pre-dissolution, thereby synergistically reducing the softening point and appearance (Gardner color) of the prepared C5 petroleum resin. The softening point of the prepared C5 petroleum resin is as low as 87.7-88.0℃, and the appearance (Gardner color) is as low as No. 4.

[0085] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing a C5 petroleum resin, characterized in that, Includes the following steps: S1. Add 3.2-3.5g of catalyst and 160-175g of functional reagent to the reactor and heat in a 50℃ water bath; when the reactor temperature reaches 45℃, add the mixture dropwise to the reactor. After the addition is complete, keep the temperature constant for 30-35 minutes to obtain the basic resin solution. The catalyst comprises 1.2-1.5% of the mass of the mixture; the mixture consists of isoprene and α-methylstyrene, with α-methylstyrene comprising 10.7-11.2% of the mass of the mixture; the functional reagent is prepared by dissolving hydrogenated rosin glycerol ester in a solvent. S2. Transfer the base resin solution obtained in S1 into a washing tank, and perform alkaline washing and water washing treatment in sequence. Then add an antioxidant to obtain a medium-grade resin solution. S3. The intermediate resin solution obtained in S2 is distilled to obtain the C5 petroleum resin.

2. The method for preparing C5 petroleum resin according to claim 1, characterized in that, The preparation method of the functional reagent is as follows: hydrogenated rosin glycerol ester is pulverized to a particle size ≥ 80 mesh, added to a solvent, the mass of hydrogenated rosin glycerol ester being 4.5-5.5% of the solvent mass, and stirred to dissolve, thereby obtaining the functional reagent.

3. The method for preparing C5 petroleum resin according to claim 1 or 2, characterized in that, The solvent includes toluene and / or xylene.

4. The method for preparing C5 petroleum resin according to claim 1, characterized in that, In S2, the specific operation of alkaline washing is as follows: the base resin solution is transferred into the washing tank, heated in a water bath until there is reflux, 480-510g of 10wt% NaOH aqueous solution and 3.7-4.2mL of 1wt% demulsifier aqueous solution are added to the washing tank, stirred, and after settling for 5-15min, the alkaline water layer is separated, and the organic layer is left in the tank.

5. The method for preparing C5 petroleum resin according to claim 4, characterized in that, In S2, the specific operation of the water washing treatment is as follows: the organic layer is washed with water once under the condition of adding a demulsifier, and then the water washing is repeated without adding a demulsifier until the pH value of the water layer after sedimentation is 7-8.

6. The method for preparing C5 petroleum resin according to claim 4, characterized in that, The demulsifier is PFA8311.

7. The method for preparing C5 petroleum resin according to claim 1, characterized in that, In S3, the specific operation of the distillation process is as follows: the intermediate resin liquid is distilled under normal pressure. When the bottom temperature reaches 200°C, water vapor is introduced and the vacuum pump is turned on for reduced pressure distillation. When the temperature rises to 220°C, the heating power is turned off and the heating jacket is removed. When the temperature drops to 200°C, the venting valve is opened to release the air and the vacuum pump is turned off. After weighing, the liquid is poured out and cooled to room temperature.

8. The method for preparing C5 petroleum resin according to claim 1, characterized in that, The catalyst is AlCl3 solid powder.

9. The method for preparing C5 petroleum resin according to claim 1, characterized in that, The antioxidant is antioxidant 1010.

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