Manufacturing device of modified petroleum resin

Through the synergistic effect of twin-screw extrusion and electron beam irradiation technology, safety hazards and high energy consumption problems in the synthesis of modified interpentadiene resins are solved, efficient, green and economical continuous production is achieved, and product quality is improved.

CN223233787UActive Publication Date: 2025-08-19BEIJING WANBANGDA ENVIRONMENTAL PROTECTION TECH +1
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Patent Information

Application Number
CN202422280856.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-09-18
Publication Date
2025-08-19
Estimated Expiration
2034-09-18

AI Technical Summary

Technical Problem

In the synthesis process of modified mPentadene resin, the quality reduction and safety hazards caused by incomplete use of initiators or catalysts, and the reaction is difficult to control, and there are problems such as high energy consumption and "three wastes".

Method used

The twin-screw extrusion technology and electron beam irradiation technology are used to synergize free radicals by using the strong shear force and high-energy electron beam of the twin-screw to achieve the grafting reaction between petroleum resin and polarized monomer, avoid the use of initiators, and set up a polar monomer recovery tank for recycling.

Benefits of technology

Continuous production in an oxygen-free environment has been achieved, by-product generation and energy consumption have been reduced, costs have been reduced, product quality has been improved, and green production has been achieved.

✦ Generated by Eureka AI based on patent content.

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Abstract

Some embodiments of the present application provide an apparatus for manufacturing a modified petroleum resin, the apparatus comprising: a mixer; the double-screw extruder is communicated with the mixing machine, and an outlet of the mixing machine is connected to an inlet of the double-screw extruder; the devolatilization kettle is communicated with the double-screw extruder, and an outlet of the double-screw extruder is connected to an inlet of the devolatilization kettle; the recovery tank is communicated with the devolatilization kettle, and a first outlet of the devolatilization kettle is connected to an inlet of the recovery tank; the condenser is communicated with the recovery tank, a first outlet of the recovery tank is communicated with an inlet of the condenser in a two-way mode, and an electron beam irradiation device is arranged at the position of the double-screw extruder. The polar monomer is grafted by adopting the synergistic effect of a twin-screw extrusion technology and an electron beam irradiation technology, and the petroleum resin and the polar grafted monomer are fully mixed by utilizing the strong shearing force of twin screws.
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Description

Technical Field

[0001] The embodiments of the present application relate to a device for producing modified petroleum resin. Background Art

[0002] Petroleum resins, such as piperylene, are important chemical raw materials. Their polymers, piperylene resins, exhibit excellent heat resistance, weatherability, and electrical insulation properties, making them widely used in electronics, electrical equipment, aerospace, and other fields. However, because piperylene petroleum resins are non-polar hydrocarbon oligomers, they exhibit weak composite properties with polar materials, limiting their applications and the performance of their composites. Therefore, improving their properties through modification techniques is a current research hotspot. Introducing polar groups into the molecular chain can increase their adhesiveness and adhesion, raise their softening temperature, and improve their compatibility with polar resins, broadening their application range. Furthermore, the addition of antioxidants can further enhance the resin's stability and extend its service life.

[0003] Patent application CN104341555A discloses a method for synthesizing a modified piperylene resin. This method utilizes piperylene, a C5 monoolefin, and a terpene as copolymerization raw materials to produce a petroleum resin with a low molecular weight, a high softening point, and a low bromine value. The modified piperylene resin synthesis method comprises: adding piperylene, a C5 monoolefin, and a terpene in a weight ratio of 1:0.1-0.7:0.4-1.4 to form a copolymerization raw material; and conducting a cationic polymerization reaction in the presence of a catalyst and an inert aliphatic hydrocarbon as a solvent at a temperature of 30-70°C in an oxygen-free environment to synthesize the resin.

[0004] Patent application number CN115572353A discloses a modified petroleum resin, its preparation method, and application. The preparation method comprises the following steps: (1) mixing an initiator with heat-insulated isoprene to carry out a polymerization reaction to obtain a petroleum resin solution; and (2) mixing the petroleum resin solution after the polymerization reaction in step (1) with an initiator and a polar grafting monomer to carry out a grafting reaction to obtain a modified petroleum resin. The method described in this utility model is continuous and online from synthesis to modification, without any intermediate steps (as in the traditional method of first producing the petroleum resin, pelletizing and packaging, and then heating and melting for grafting). The method has low energy consumption, energy conservation, low cost, adjustable grafting rate, and high purity of the modified petroleum resin.

[0005] Because piperyl resin contains a large number of unsaturated double bonds, it facilitates the introduction of polar groups. Current technologies primarily rely on free radical polymerization or cationic polymerization. By adding initiators or catalysts, polar monomers react with piperyl resin or piperyl monomers to polymerize. This requires additional initiator or catalyst removal, and incomplete removal can also reduce the quality of the modified resin. Free radical polymerization also presents safety risks due to its violent and uncontrollable nature. Utility Model Content

[0006] This application utilizes twin-screw extrusion technology and electron beam irradiation technology to synergistically graft polar monomers. The strong shear force of the twin screws is used to thoroughly mix the resin and the polarized grafting monomer. The high-energy electron beam is then used to excite the resin to produce free radicals, thereby initiating the grafting reaction. Specifically, this application utilizes the strong shear force of the twin screws to thoroughly mix the petroleum resin and the polarized monomer. The high-energy electron beam is then used to graft the petroleum resin and the polarized monomer. The reaction conditions are mild, eliminating safety risks. The process is simple, resulting in high yield and high-quality products.

[0007] Specifically, some embodiments of the present application provide a manufacturing device for modified petroleum resin, comprising: a mixer; a twin-screw extruder, connected to the mixer, wherein the outlet of the mixer is connected to the inlet of the twin-screw extruder; a devolatilizer, connected to the twin-screw extruder, wherein the outlet of the twin-screw extruder is connected to the inlet of the devolatilizer; a recovery tank, connected to the devolatilizer, wherein the first outlet of the devolatilizer is connected to the inlet of the recovery tank; and a condenser, connected to the recovery tank, wherein the first outlet of the recovery tank is bidirectionally connected to the inlet of the condenser, wherein an electron beam irradiation device is provided at the twin-screw extruder.

[0008] In some embodiments, the electron beam irradiation device is disposed at the tail end of the twin-screw extruder close to the devolatilizer.

[0009] In some embodiments, the outlet of the twin-screw extruder is connected to the devolatilizer through a pipeline, wherein the material in the twin-screw extruder enters the devolatilizer through the pipeline after being irradiated by the electron beam of the electron beam irradiation device.

[0010] In some embodiments, the manufacturing device further includes: a finished product tank connected to the devolatilizer, wherein the second outlet of the devolatilizer is connected to the inlet of the finished product tank, wherein the second outlet of the devolatilizer is different from the first outlet of the devolatilizer; and a tail gas absorption tank connected to the recovery tank, wherein the second outlet of the recovery tank is connected to the inlet of the tail gas absorption tank, and the third outlet of the recovery tank is connected to the inlet of the mixer, wherein the first outlet, second outlet and third outlet of the recovery tank are all different.

[0011] In some embodiments, the electron beam irradiation device is disposed above the twin-screw extruder.

[0012] In some embodiments, the finished product tank is further connected to the granulation device, wherein the outlet of the finished product tank is connected to the inlet of the granulation device.

[0013] In some embodiments, the first outlet and the second outlet of the devolatilizer are connected to the inlet of the recovery tank and the inlet of the finished product tank respectively through different pipelines.

[0014] In some embodiments, the second outlet and the third outlet of the recovery tank are connected to the inlet of the tail gas absorption tank and the inlet of the mixer through different pipelines. In some embodiments, the recovery tank is an unreacted polarized grafted monomer recovery tank, specifically, a maleic anhydride (MA) recovery tank.

[0015] Compared with the existing technology, the beneficial effects of this technical solution are as follows:

[0016] 1) The modified petroleum resin manufacturing device provided in this application combines a twin-screw extruder and an electron beam irradiation device. Utilizing a synergistic processing technology of twin-screw extrusion and electron beam irradiation, it eliminates the use of initiators, reduces the generation of by-products, and eliminates the need for additional heating, thus reducing energy consumption. Furthermore, a polar monomer recovery tank is provided to collect the devolatilized components for subsequent recycling. Compared to existing technologies, this device can save approximately 40% of costs.

[0017] 2) The manufacturing device of the modified petroleum resin provided in this application can realize continuous production from feeding to discharging, and no "three wastes" are generated in the production process, truly achieving green, economical and efficient production. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Various aspects of the present invention are best understood from the following detailed description when read with the accompanying figures.

[0019] Figure 1 Shown is a production apparatus for modified petroleum resin. DETAILED DESCRIPTION

[0020] The following disclosure provides many different embodiments or examples for implementing the different features of the present invention. Specific examples of components and arrangements are described below to simplify the present invention. Of course, these are merely examples and are not intended to limit the present invention. For example, in the following description, forming a first component above or on a second component may include an embodiment in which the first component and the second component are directly in contact with each other, and may also include an embodiment in which an additional component may be formed between the first component and the second component so that the first component and the second component may not be in direct contact. In addition, the present invention may repeat reference numerals and / or characters in various embodiments. This repetition is for the purpose of simplicity and clarity and does not itself indicate the relationship between the various embodiments and / or configurations discussed.

[0021] Furthermore, for ease of description, spatially relative terms such as "below," "beneath," "lower," "above," and "upper" may be used herein to describe the relationship of one element or component to another (or additional) elements or components as illustrated in the figures. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. The device may be otherwise oriented (rotated 90 degrees or at other orientations), and the spatially relative descriptors used herein should be interpreted accordingly.

[0022] The modified petroleum resin manufacturing apparatus provided herein combines a twin-screw extruder with an electron beam irradiation device. This technology utilizes the synergistic effects of twin-screw extrusion and electron beam irradiation to graft polar monomers. The strong shear force of the twin screws thoroughly mixes the resin and polarized grafting monomer. The high-energy electron beam then excites the resin to generate free radicals, initiating the grafting reaction. Furthermore, compared to existing technologies, the manufacturing process provided by this modified petroleum resin manufacturing apparatus requires no additional initiator or catalyst, eliminating the need for initiator or catalyst removal and avoiding the potential generation of byproducts from initiator-induced free radical reactions. The technical solution provided herein eliminates the need for organic solvents to dissolve the resin or polarized monomer, eliminating the need for solvent removal. Furthermore, the reaction process does not consume additional energy and is equipped with a polar grafting monomer recovery tank, enabling the recycling of unreacted monomer, thus reducing costs. Furthermore, the modified petroleum resin manufacturing apparatus provided herein enables continuous production, increasing productivity. This technology eliminates the generation of "three wastes" during the reaction, making it a green, economical, and efficient production process.

[0023] Some embodiments of the present application provide a manufacturing device for a modified petroleum resin, which includes: a mixer; a twin-screw extruder connected to the mixer, wherein the outlet of the mixer is connected to the inlet of the twin-screw extruder; a devolatilizer connected to the twin-screw extruder, wherein the outlet of the twin-screw extruder is connected to the inlet of the devolatilizer; a recovery tank connected to the devolatilizer, wherein the first outlet of the devolatilizer is connected to the inlet of the recovery tank; and a condenser connected to the recovery tank, wherein the first outlet of the recovery tank is bidirectionally connected to the inlet of the condenser, wherein an electron beam irradiation device is provided at the twin-screw extruder. Specifically, the electron beam irradiation device is provided at the tail end of the twin-screw extruder near the devolatilizer, and further, the electron beam irradiation device is provided above the tail end of the twin-screw extruder. In some embodiments, the outlet of the twin-screw extruder is connected to the devolatilizer through a pipeline, wherein the material in the twin-screw extruder enters the devolatilizer through the pipeline after being irradiated with the electron beam of the electron beam irradiation device. In some embodiments, the manufacturing device further includes: a finished product tank, connected to the devolatilizer, wherein the second outlet of the devolatilizer is connected to the inlet of the finished product tank, wherein the second outlet of the devolatilizer is different from the first outlet of the devolatilizer, and the first outlet and the second outlet of the devolatilizer are respectively connected to the inlet of the recovery tank and the inlet of the finished product tank through different pipelines; and a tail gas absorption tank, connected to the recovery tank, wherein the second outlet of the recovery tank is connected to the inlet of the tail gas absorption tank, and the third outlet of the recovery tank is connected to the inlet of the mixer, wherein the first outlet, the second outlet and the third outlet of the recovery tank are different, and the second outlet and the third outlet of the recovery tank are connected to the inlet of the tail gas absorption tank and the inlet of the mixer through different pipelines.

[0024] The manufacturing process of the modified petroleum resin manufacturing device provided by the present application mainly adopts the following steps: using inert gas to replace the gas in the twin-screw extruder, the devolatilization kettle, the product tank and the connected pipelines to ensure that the entire production environment is an oxygen-free environment; adding petroleum resin such as isoprene resin and a polarized grafting monomer and an antioxidant in a specific ratio into a high-speed mixer (the mixer used in the present application is a high-speed mixer with a rotation speed of more than 1500rpm / min), stirring at a rotation speed of 1500-3500rpm / min for 3-5 minutes to obtain a mixed material; while the high-speed mixer is running, stirring for 3-5 minutes to obtain a mixed material. During the mixing process, the high-speed mixer is cooled with cooling water to keep the material temperature at room temperature (between 22°C and 25°C) to prevent the grafted polar monomer from volatilizing and the resin from softening due to excessive temperature during the mixing process; the obtained mixed material is added to the feeding port of the twin-screw extruder through a material lifting belt, the speed of the twin-screw is set to 170-300rpm / min, and the module temperature is set to 190-210°C; an electron beam irradiation device is provided at the tail end of the twin-screw extruder, and the discharge port of the twin-screw extruder is connected to the devolatilization reactor through a pipeline, and the material is advanced to the electron beam irradiation area through the twin screws, and after the electron beam irradiation, the material is passed through the electron beam irradiation device. The resin enters the devolatilizer at the rear end through a pipeline, wherein the polarized grafting monomer includes one or more unsaturated olefin functionalized monomers such as maleic anhydride and itaconic anhydride; the antioxidant includes one of 2,6-di-tert-butyl-4-methylphenol (antioxidant 264) or 3,5-di-tert-butylphenyl-4-hydroxyphenylpropionic acid isooctyl ester (antioxidant 1135); the mass of the polarized grafting monomer is 1%-10% of the mass of the isoprene resin, and the mass of the antioxidant is 0.1%-1% of the mass of the isoprene resin; the electron beam irradiation dose is 100-1000 kGy, and the electron energy of the electron beam irradiation is 0.6-1 MeV; the devolatilizer has The process is equipped with a stirring device and a heat preservation device. After the material enters the devolatilization reactor, the stirring device is turned on at a speed of 70-90 rpm / min. Unreacted polarized grafted monomers and oligomers are condensed in a condenser and recovered in a recovery tank through vacuum distillation. The pressure is (-0.07)-(-0.09) MPa, the devolatilization temperature (vacuum distillation temperature) is the temperature of the material (this temperature refers to the temperature of the material extruded from the twin-screw extruder), and the vacuum distillation time is 30-60 minutes. The recovered polarized grafted monomer is reused in the reaction, and the inert gas or nitrogen in the devolatilization reactor is adsorbed in an exhaust gas adsorption tank. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product. This simple and efficient process enables continuous resin production, adjustable acid value of the modified resin, recyclable polarized grafted monomer, and eliminates the generation of "three wastes", truly achieving green and economical production.

[0025] To more clearly illustrate the modified petroleum resin produced by the modified petroleum resin production apparatus provided by the present invention, the following examples provide detailed descriptions and measurements. The modified petroleum resins produced in these examples were tested using the following methods: softening point: Ring and Ball method (GB / T4507); color: GB / T22295 (Gardner color); acid value: GB / T2895; melt viscosity: GB / T24148.4. These test methods are commonly used in the art.

[0026] Example 1

[0027] The gas in the twin-screw extruder, the devolatilization reactor, the product tank and the connected pipeline is replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 1 kg of maleic anhydride and 0.1 kg of antioxidant 264 are added to a high-speed mixer at a rotation speed of 1500 rpm and a stirring time of 3 minutes to fully mix them to obtain a mixture; the mixture enters the feeding port of the twin-screw extruder through a material lifting belt, and the twin-screw extruder is started with a rotation speed set to 170 rpm / min and a module temperature of 190° C. The electron beam irradiation device is 0.6 MeV and the electron beam irradiation dose is set to 100 KGy; the grafted resin enters the rear-end devolatilization reactor, and unreacted polarized grafted monomers and oligomers are vacuum distilled to a recovery tank under the conditions of a pressure of -0.07 MPa and a rotation speed of 90 rpm / min by vacuum distillation for 30 minutes; after the vacuum distillation is completed, the modified resin is granulated to obtain a modified resin product.

[0028] Example 2

[0029] The gas in the twin-screw extruder, the devolatilizer, the product tank and the connected pipeline is replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 1 kg of maleic anhydride and 0.1 kg of antioxidant 264 are added to a high-speed mixer at a speed of 3000 rpm / min and a stirring time of 5 minutes to fully mix them to obtain a mixture; the mixture enters the feeding port of the twin-screw extruder through a material lifting belt, and the twin-screw extruder is started with a speed set to 300 rpm / min and a module temperature of 210°C; the electron beam irradiation device is 1 MeV and the electron beam irradiation dose is set to 1000 KGy; the grafted resin enters the rear-end devolatilizer, and unreacted polarized grafted monomers and oligomers are vacuum distilled to a recovery tank under the conditions of a pressure of -0.09 MPa and a speed of 90 rpm / min by vacuum distillation for 40 minutes; after the vacuum distillation is completed, the modified resin is sent to a granulation workshop for granulation to obtain a modified resin product.

[0030] Example 3

[0031] The gas in the twin-screw extruder, the devolatilization kettle, the product tank and the connected pipeline is replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 5 kg of maleic anhydride and 0.5 kg of antioxidant 264 are added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample; the mixture enters the feeding port of the twin-screw extruder through a material lifting belt, the twin-screw extruder is turned on, the speed is set to 170 rpm / min, and the module temperature is 190°C; the electron beam irradiation device is 0.6 MeV, and the electron beam irradiation dose is set to 100 KGy; the grafted resin enters the rear-end devolatilization kettle, and under the conditions of a pressure of -0.07 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomers and oligomers are vacuum distilled to a recovery tank by vacuum distillation for 30 minutes; after the vacuum distillation work is completed, the modified resin is sent to a granulation workshop for granulation to obtain a modified resin product.

[0032] Example 4

[0033] The gases in the twin-screw extruder, the devolatilization reactor, the product tank and the connected pipelines were replaced with nitrogen. After the replacement, 100 kg of isopentadiene resin, 5 kg of maleic anhydride and 0.5 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample. The mixture entered the feeding port of the twin-screw extruder through a material lifting belt. The twin-screw extruder was started, the speed was set to 300 rpm / min, and the module temperature was 190°C. The electron beam irradiation device was 0.6 MeV, and the electron beam irradiation dose was set to 100 KGy. The grafted resin entered the rear-end devolatilization reactor, and under the conditions of a pressure of -0.07 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 30 minutes. The recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0034] Example 5

[0035] The gases in the twin-screw extruder, the devolatilizer, the product tank and the connected pipelines were replaced with nitrogen. After replacement, 100 kg of isopentylene resin, 5 kg of maleic anhydride and 0.5 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample. The mixture entered the feeding port of the twin-screw extruder through a material lifting belt. The twin-screw extruder was started, the speed was set to 300 rpm / min, and the module temperature was 210°C. The electron beam irradiation device was 0.6 MeV, and the electron beam irradiation dose was set to 100 KGy. The grafted resin entered the rear-end devolatilizer, and under the conditions of a pressure of -0.07 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 30 minutes. The recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0036] Example 6

[0037] The gases in the twin-screw extruder, the devolatilization reactor, the product tank and the connected pipelines were replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 5 kg of maleic anhydride and 0.5 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample; the mixture entered the feeding port of the twin-screw extruder through a material lifting belt, the twin-screw extruder was turned on, the speed was set to 300 rpm / min, and the module temperature was 210°C; the electron beam irradiation device was 0.8 MeV, and the electron beam irradiation dose was set to 500 KGy; the grafted resin entered the rear-end devolatilization reactor, and under the conditions of a pressure of -0.07 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 30 minutes; the recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0038] Example 7

[0039] The gases in the twin-screw extruder, the devolatilizer, the product tank and the connected pipelines were replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 5 kg of maleic anhydride and 0.5 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample. The mixture entered the feeding port of the twin-screw extruder through a material lifting belt. The twin-screw extruder was started, the speed was set to 300 rpm / min, and the module temperature was 210°C. The electron beam irradiation device was 0.8 MeV, and the electron beam irradiation dose was set to 500 KGy. The grafted resin entered the rear-end devolatilizer, and under the conditions of a pressure of -0.09 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 40 minutes. The recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0040] Example 8

[0041] The gases in the twin-screw extruder, the devolatilizer, the product tank and the connected pipelines were replaced with nitrogen. After the replacement, 100 kg of isopentylene resin, 10 kg of maleic anhydride and 1 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample. The mixture entered the feeding port of the twin-screw extruder through a material lifting belt. The twin-screw extruder was started, the speed was set to 300 rpm / min, and the module temperature was 210°C. The electron beam irradiation device was 1 MeV, and the electron beam irradiation dose was set to 1000 KGy. The grafted resin entered the rear-end devolatilizer, and under the conditions of a pressure of -0.09 MPa and a speed of 80 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 60 minutes. The recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0042] Example 9

[0043] The gases in the twin-screw extruder, the devolatilization reactor, the product tank and the connected pipelines were replaced with nitrogen. After the replacement, 100 kg of isopentadiene resin, 5 kg of itaconic anhydride and 0.5 kg of antioxidant 1135 were added to a high-speed mixer at a speed of 3000 rpm / min for 5 minutes to fully mix them to obtain a mixed sample. The mixture entered the feeding port of the twin-screw extruder through a material lifting belt. The twin-screw extruder was started, the speed was set to 300 rpm / min, and the module temperature was 210°C. The electron beam irradiation device was 0.8 MeV, and the electron beam irradiation dose was set to 500 KGy. The grafted resin entered the rear-end devolatilization reactor, and under the conditions of a pressure of -0.09 MPa and a speed of 90 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank by vacuum distillation for 40 minutes. The recovered polarized grafted monomer was continuously reused in the reaction. After the vacuum distillation is completed, the modified resin is sent to the granulation workshop for granulation to obtain the modified resin product.

[0044] Example 10

[0045] The gas in the twin-screw extruder, devolatilization reactor, product tank and connected pipeline was replaced with nitrogen. After replacement, 100 kg of isoprene resin, 5 kg of itaconic anhydride and 5 kg of maleic anhydride, as well as 0.5 kg of antioxidant 1135 and 0.5 kg of antioxidant 264 were added to the high-speed mixer at a speed of 3500 rpm / min for 40 minutes to fully mix and obtain a mixed sample. The mixed material entered the feeding port of the twin-screw extruder through the material lifting belt, and the twin-screw extruder was started. The speed was set to 200 rpm / min, and the module temperature was 200°C. The electron beam irradiation device was 0.8 MeV, and the electron beam irradiation dose was set to 500 kGy. The grafted resin entered the back-end devolatilization reactor. Under the conditions of -0.08 MPa pressure and 70 rpm / min, the unreacted polarized grafted monomer and oligomer were vacuum distilled to a recovery tank for 40 minutes. The recovered polarized grafted monomer was reused in the reaction. After the vacuum distillation, the modified resin was sent to the granulation workshop for granulation to obtain the modified resin product.

[0046] The test results of the modified piperylene resins in Examples 1 to 10 are shown in Table 1 below.

[0047] Table 1 Test results of modified piperylene resins of Examples 1 to 10

[0048]

[0049]

[0050] As can be seen from the above table, the present application can effectively improve the reaction efficiency and product quality by precisely controlling the ratio of the polarized grafting monomer and the antioxidant, the rotation speed of the twin-screw extruder and the dose of electron beam irradiation, the reaction time, and the temperature and time of the reduced pressure distillation. Specifically, the chromaticity of the modified isoprene resin manufactured by the manufacturing device of the present application can be improved to 3 to 7, the acid value can be improved to 1.2 to 29.31 mg KOHg, the softening point can be between 100 and 110°C, and the melt viscosity can be between 145.5 and 239.5 mPa·s.

[0051] Compared with the existing technology, the beneficial effects of this technical solution are as follows:

[0052] 1) The modified petroleum resin manufacturing device provided in this application combines a twin-screw extruder and an electron beam irradiation device. Utilizing a synergistic processing technology of twin-screw extrusion and electron beam irradiation, it eliminates the use of initiators, reduces the generation of by-products, and eliminates the need for additional heating, thus reducing energy consumption. Furthermore, a polar monomer recovery tank is provided to collect the devolatilized components for subsequent recycling. Compared to existing technologies, this device can save approximately 40% of costs.

[0053] 2) The manufacturing device of the modified petroleum resin provided in this application has a simple process flow, a short reaction time, and can also realize continuous production from feeding to discharging. In addition, no "three wastes" are generated in the production process, truly achieving green, economical and efficient production.

[0054] 3) The process flow provided by the manufacturing device of the present application can effectively improve the reaction efficiency and product quality by precisely controlling the ratio of the polarized grafting monomer and the antioxidant, the speed and time of the high-speed mixer, the speed of the twin-screw extruder, the dose of electron beam irradiation, and the temperature and time of the vacuum distillation. The grafting rate of maleic anhydride in the isobutylene-modified resin produced by this patent can reach 0.2-5%.

[0055] The features of several embodiments are summarized above so that those skilled in the art can better understand aspects of the present invention. Those skilled in the art will appreciate that they can easily use the present invention as a basis to design or modify other processes and structures for implementing the same purposes and / or achieving the same advantages as the embodiments described herein. Those skilled in the art will also appreciate that such equivalent constructions do not depart from the spirit and scope of the present invention, and that various variations, substitutions, and changes may be made herein without departing from the spirit and scope of the present invention.

Claims

1. A device for producing modified petroleum resin, characterized in that: include: Mixer; a twin-screw extruder, connected to the mixer, wherein the outlet of the mixer is connected to the inlet of the twin-screw extruder; a devolatilizer, connected to the twin-screw extruder, wherein the outlet of the twin-screw extruder is connected to the inlet of the devolatilizer; a recovery tank, connected to the devolatilizer, wherein a first outlet of the devolatilizer is connected to an inlet of the recovery tank; and A condenser is connected to the recovery tank, wherein the first outlet of the recovery tank is connected to the inlet of the condenser in a two-way manner. Wherein, an electron beam irradiation device is provided at the twin-screw extruder.

2. The manufacturing device according to claim 1, wherein The electron beam irradiation device is arranged at the tail end of the twin-screw extruder close to the devolatilizer.

3. The manufacturing device according to claim 2, characterized in that The outlet of the twin-screw extruder is connected to the devolatilizer through a pipeline. The material in the twin-screw extruder is irradiated by the electron beam of the electron beam irradiation device and then enters the devolatilization reactor through the pipeline.

4. The manufacturing device according to claim 1, wherein Also includes: A finished product tank is connected to the devolatilizer, wherein a second outlet of the devolatilizer is connected to an inlet of the finished product tank, and wherein the second outlet of the devolatilizer is different from the first outlet of the devolatilizer.

5. The manufacturing device according to claim 1, wherein Also includes: A tail gas absorption tank is connected to the recovery tank, wherein the second outlet of the recovery tank is connected to the inlet of the tail gas absorption tank, wherein the first outlet of the recovery tank is different from the second outlet of the recovery tank.

6. The manufacturing device according to claim 5, characterized in that The third outlet of the recovery tank is connected to the inlet of the mixer, wherein the first outlet of the recovery tank, the second outlet of the recovery tank and the third outlet of the recovery tank are all different.

7. The manufacturing device according to claim 2, characterized in that The electron beam irradiation device is arranged above the tail end of the twin-screw extruder.

8. The manufacturing device according to claim 4, characterized in that The finished product tank is further connected to a granulation device, wherein the outlet of the finished product tank is connected to the inlet of the granulation device.

9. The manufacturing device according to claim 4, characterized in that The first outlet and the second outlet of the devolatilizer are connected to the inlet of the recovery tank and the inlet of the finished product tank respectively through different pipelines.

10. The manufacturing device according to claim 6, characterized in that The second outlet and the third outlet of the recovery tank are connected to the inlet of the tail gas absorption tank and the inlet of the mixer through different pipelines.

Citation Information

Patent Citations

  • Synthesis method for modified m-pentadiene resin

    CN104341555A

  • Modified petroleum resin as well as preparation method and application thereof

    CN115572353A