Functional resin capable of being polymerized and produced at normal temperature and preparation method of functional resin

Abstract

The invention belongs to the technical field of functional resin, and discloses functional resin capable of being polymerized and produced at normal temperature and a preparation method thereof, and the preparation method comprises the following steps: step 1, preparing and mixing raw materials; 2, adding a catalyst; step 3, starting a reaction; step 4, reaction monitoring: analyzing the composition and property of a reaction system by sampling every 1 hour so as to judge the reaction process and the resin quality; step five, treatment and product preparation: when the reaction reaches a preset degree, adding a terminating agent to terminate the polymerization reaction, and controlling the stirring speed to be 200-300 revolutions per minute and the stirring time to be 10-15 minutes; step 6, product separation: filtering and washing the reaction liquid to remove impurities such as unreacted raw materials, the catalyst and the solvent; the invention not only solves the technical problem of normal temperature polymerization production of functional resin, but also provides a new thought and technical path for realizing green, efficient and sustainable development of resin materials.

Description

Technical Field

[0001] The invention belongs to the technical field of functional resins, and specifically relates to a functional resin that can be polymerized and produced at room temperature and a preparation method thereof. Background Art

[0002] In the field of materials science, functional resins have always been a hot topic of research and development due to their unique physical and chemical properties and broad application prospects. Functional resins not only play an important role in traditional industries such as coatings, adhesives, and plastic processing, but also show great potential in emerging fields such as electronic information, new energy, and biomedicine. However, the production process of traditional functional resins often relies on high-temperature polymerization conditions, which not only consumes a lot of energy, but may also cause environmental pollution and safety hazards. In addition, high-temperature polymerization may also lead to excessive cross-linking of resin molecular chains, affecting the adjustability of its performance. Therefore, developing a method for preparing functional resins that can be polymerized at room temperature is of great significance for energy conservation and emission reduction, improving production efficiency, and expanding the application fields of resins.

[0003] Traditional room temperature polymerization methods are often limited by the narrow selection range of raw materials, low polymerization efficiency, unstable product performance and other problems. In particular, for resin precursors with complex structures, such as bicyclic compounds, their polymerization activity at room temperature is low, and it is difficult to achieve efficient polymerization directly through simple methods. Therefore, raw material selection and ratio: how to screen out a system suitable for room temperature polymerization from a large number of raw materials and determine the optimal ratio to improve polymerization efficiency and product performance. Summary of the invention

[0004] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides a functional resin that can be produced by polymerization at room temperature and a preparation method thereof, which effectively solves the problems raised by the background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing a functional resin that can be polymerized at room temperature, comprising the following steps:

[0006] Step 1: Raw material preparation and mixing:

[0007] 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system;

[0008] 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed;

[0009] Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction;

[0010] Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 200-300 rpm, and the stirring time is 3-5 hours;

[0011] Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality;

[0012] Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 200-300 rpm, and the stirring time is 10-15 minutes;

[0013] Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

[0014] Preferably, in the step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 1-3:3-6:5-20:5-15.

[0015] Preferably, the stirring speed in step 1 is controlled at 200-300 rpm, and the stirring time is 30-50 minutes.

[0016] Preferably, the catalyst in step 2 is triethylamine, and the amount used is 1-3% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 200-300 rpm, and the stirring time is 10-15 minutes.

[0017] Preferably, the initiator in step three is benzoyl peroxide, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

[0018] Preferably, the terminator in step five is thiol, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

[0019] A functional resin that can be produced by polymerization at room temperature is prepared by a method for preparing a functional resin that can be produced by polymerization at room temperature.

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

[0021] By selecting the ring-free carbon nine fraction with a high content of dicyclic components as the main raw material, and combining it with indene resin oil and methyl indene resin oil as auxiliary raw materials, it not only broadens the source of raw materials, but also reduces the production cost and improves the polymerization efficiency;

[0022] High-efficiency catalysis and initiation system: triethylamine is used as a catalyst and benzoyl peroxide as an initiator, which effectively promotes the polymerization reaction at room temperature, shortens the reaction time, improves the polymerization efficiency, and the product has a uniform molecular weight distribution and stable performance;

[0023] Fine process control: By precisely controlling parameters such as stirring speed and reaction time, the polymerization process can be finely regulated to ensure the stability and consistency of product quality;

[0024] Environmental protection and energy saving: The polymerization reaction carried out at room temperature not only reduces energy consumption, but also reduces the risk of environmental pollution, which is in line with the development trend of green chemistry;

[0025] Product purification technology: through filtering, washing and drying, impurities are effectively removed, the purity and performance of the product are improved, and reliable guarantee is provided for the wide application of functional resins;

[0026] In summary, the preparation method of the present invention not only solves the technical difficulties in producing functional resins by room temperature polymerization, but also provides a new idea and technical path for achieving green, efficient and sustainable development of resin materials. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0028] The present invention relates to a method for preparing a functional resin that can be polymerized at room temperature, comprising the following steps:

[0029] Step 1: Raw material preparation and mixing:

[0030] 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system;

[0031] 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed;

[0032] Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction;

[0033] Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 200-300 rpm, and the stirring time is 3-5 hours;

[0034] Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality;

[0035] Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 200-300 rpm, and the stirring time is 10-15 minutes;

[0036] Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

[0037] In step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 1-3:3-6:5-20:5-15.

[0038] The stirring speed in step 1 is controlled at 200-300 rpm, and the stirring time is 30-50 minutes.

[0039] The catalyst in step 2 is triethylamine, and the amount used is 1-3% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 200-300 rpm, and the stirring time is 10-15 minutes.

[0040] The initiator in step three is benzoyl peroxide, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

[0041] The terminator in step five is thiol, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

[0042] A functional resin that can be produced by polymerization at room temperature is prepared by a method for preparing a functional resin that can be produced by polymerization at room temperature.

[0043] Embodiment 1:

[0044] This embodiment relates to a method for preparing a functional resin that can be polymerized at room temperature, comprising the following steps:

[0045] Step 1: Raw material preparation and mixing:

[0046] 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system;

[0047] 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed;

[0048] Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction;

[0049] Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 200 rpm, and the stirring time is 5 hours;

[0050] Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality;

[0051] Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 200 rpm, and the stirring time is 15 minutes;

[0052] Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

[0053] In step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 1:3:5:5.

[0054] The stirring speed in step 1 was controlled at 200 rpm and the stirring time was 50 minutes.

[0055] The catalyst in step 2 is triethylamine, and the amount used is 1% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 200 rpm, and the stirring time is 15 minutes.

[0056] The initiator in step 3 is benzoyl peroxide, and the amount used is 0.1% of the total mass of the reaction system.

[0057] The terminator in step 5 is thiol, and the amount used is 0.1% of the total mass of the reaction system.

[0058] The final resin product is quality tested to ensure it meets customer requirements.

[0059] Embodiment 2:

[0060] This embodiment relates to a method for preparing a functional resin that can be polymerized at room temperature, comprising the following steps:

[0061] Step 1: Raw material preparation and mixing:

[0062] 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system;

[0063] 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed;

[0064] Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction;

[0065] Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 300 rpm, and the stirring time is 3 hours;

[0066] Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality;

[0067] Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 300 rpm, and the stirring time is 10 minutes;

[0068] Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

[0069] In step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 3:6:20:15.

[0070] The stirring speed in step 1 is controlled at 300 rpm and the stirring time is 30 minutes.

[0071] The catalyst in step 2 is triethylamine, and the amount used is 1-3% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 300 rpm, and the stirring time is 10 minutes.

[0072] The initiator in step 3 is benzoyl peroxide, and the amount used is 0.5% of the total mass of the reaction system.

[0073] The terminator in step 5 is thiol, and the amount used is 0.5% of the total mass of the reaction system.

[0074] The final resin product is quality tested to ensure it meets customer requirements.

[0075] Embodiment 3:

[0076] This embodiment relates to a method for preparing a functional resin that can be polymerized at room temperature, comprising the following steps:

[0077] Step 1: Raw material preparation and mixing:

[0078] 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system;

[0079] 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed;

[0080] Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction;

[0081] Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 270 rpm, and the stirring time is 4 hours;

[0082] Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality;

[0083] Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 270 rpm, and the stirring time is 13 minutes;

[0084] Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

[0085] In step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 2:4:13:9.

[0086] The stirring speed in step 1 was controlled at 270 rpm and the stirring time was 40 minutes.

[0087] The catalyst in step 2 is triethylamine, and the amount used is 1-3% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 270 rpm, and the stirring time is 13 minutes.

[0088] The initiator in step 3 is benzoyl peroxide, and the amount used is 0.3% of the total mass of the reaction system.

[0089] The terminator in step 5 is thiol, and the amount used is 0.3% of the total mass of the reaction system.

[0090] The final resin product is quality tested to ensure it meets customer requirements.

[0091] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0092] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a functional resin that can be polymerized at room temperature, characterized in that: The following steps are involved: Step 1: Raw material preparation and mixing: 1) Raw material selection: select the carbon nine fraction with a high content of bicyclic components as the main raw material, prepare indene resin oil and methyl indene resin oil as auxiliary raw materials, and select a suitable solvent to adjust the viscosity of the reaction system; 2) Raw material mixing: Mix the carbon nine, indene resin oil, methyl indene resin oil and solvent in a certain proportion to form a premixed liquid; ensure that the raw materials are fully mixed; Step 2, adding catalyst: adding catalyst to the premixed liquid, stirring it thoroughly, and then placing the reaction system at room temperature for polymerization reaction; Step 3, reaction initiation: Initiate the polymerization reaction by using an initiator, adjust the stirring speed and reaction time to control the molecular weight and distribution of the resin, the stirring speed is controlled at 200-300 rpm, and the stirring time is 3-5 hours; Step 4, reaction monitoring: analyze the composition and properties of the reaction system by sampling every hour to determine the reaction progress and resin quality; Step 5, treatment and product preparation: when the reaction reaches a predetermined degree, the polymerization reaction is terminated by adding a terminator, the stirring speed is controlled at 200-300 rpm, and the stirring time is 10-15 minutes; Step six, product separation: filtering and washing the reaction solution to remove impurities such as unreacted raw materials, catalysts and solvents; drying the separated resin product to remove residual moisture and solvents.

2. The method for preparing a functional resin that can be polymerized at room temperature according to claim 1, characterized in that: In the step 1, the carbon nine, indene resin oil, methyl indene resin oil and solvent are trimethylbenzene, coumarone resin, methyl indene and toluene respectively; the mass ratio of trimethylbenzene, coumarone resin, methyl indene and toluene is 1-3:3-6:5-20:5-15.

3. The method for preparing a functional resin that can be polymerized at room temperature according to claim 1, characterized in that: The stirring speed in the step 1 is controlled at 200-300 rpm, and the stirring time is 30-50 minutes.

4. The method for preparing a functional resin that can be polymerized at room temperature according to claim 1, characterized in that: The catalyst in step 2 is triethylamine, and the amount used is 1-3% of the total mass of the reaction system. The stirring speed in step 2 is controlled at 200-300 rpm, and the stirring time is 10-15 minutes.

5. The method for preparing a functional resin that can be polymerized at room temperature according to claim 1, characterized in that: The initiator in step three is benzoyl peroxide, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

6. The method for preparing a functional resin that can be polymerized at room temperature according to claim 1, characterized in that: The terminator in step 5 is thiol, and the amount used is between 0.1-0.5% of the total mass of the reaction system.

7. A functional resin that can be polymerized at room temperature, characterized in that: The resin is prepared by the method for preparing a functional resin that can be polymerized at room temperature as described in any one of claims 1 to 6.