Single-component biomass resin synthesis process

Abstract

The present invention relates to the technical field of composite materials, and discloses a single-component biomass resin synthesis process, comprising the following steps, in an inert gas (such as nitrogen N2 or argon Ar) protective environment, hydroxyl-containing polyols and polyisocyanates are mixed in a certain proportion, and polymerization reaction is carried out at a suitable temperature (usually not more than 80°C) to synthesize a prepolymer, and the synthesized prepolymer is mixed with a capping agent (such as cardanol and butanone oxime), and end-capping treatment is carried out to close the polyisocyanate groups in the prepolymer. The single-component biomass resin synthesis process uses biomass raw materials, reduces the impact on the environment, has a wide range of raw material sources, is simple in synthesis process, has mild conditions, and is low in cost. By optimizing the formula and preparation process, the resin has good mechanical strength and toughness, and by optimizing the formula and preparation process, the resin has good mechanical strength and toughness, and the single-component system does not need to be mixed on site, simplifies the operation steps, and improves production efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of composite materials, in particular to a single-component biomass resin synthesis process. Background Art

[0002] In the field of composite materials, conductive resins are more widely used. By compounding conductive resins with other materials (such as carbon fiber, glass fiber, etc.), composite materials with excellent conductive properties and mechanical properties can be prepared. These composite materials are not only light in weight and high in strength, but also have good conductivity and corrosion resistance, and are suitable for aerospace, automobiles, electronics and electrical appliances and other fields.

[0003] With the rapid development of science and technology and the increasing demand for high-performance materials, the application prospects of conductive resins in electronic equipment, coatings, composite materials and other fields will be broader. Traditional conductive resins mainly achieve conductive properties by adding conductive fillers (such as carbon black, metal powder, etc.), but these traditional resins have many problems, including high cost, environmental unfriendliness, poor mechanical properties, etc. Therefore, there is an urgent need for a single-component biomass resin with a simple preparation process, environmental protection and excellent mechanical properties. Summary of the invention

[0004] The purpose of the present invention is to provide a single-component biomass resin synthesis process to solve the problems of high cost, unfriendly environment and poor mechanical properties mentioned in the above background technology.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a single-component biomass resin synthesis process, comprising the following steps:

[0006] S1: In an inert gas (such as nitrogen N 2 In an atmosphere of argon (Ar) protection, hydroxyl-containing polyol and polyisocyanate are mixed in a certain proportion, and polymerization reaction is carried out at a suitable temperature (usually not exceeding 80°C) to synthesize prepolymer. During the reaction, parameters such as temperature, pressure, stirring speed, etc. need to be controlled to ensure reaction efficiency and product quality;

[0007] S2: The synthesized prepolymer is mixed with a capping agent (such as cardanol and butanone oxime) and capped to block the polyisocyanate groups in the prepolymer. The capping rate is 100% to improve the stability and storage of the resin. The capping reaction needs to be carried out at a suitable temperature and the reaction time is controlled to ensure complete capping.

[0008] S3: adding a conductive functional body, including conductive graphene, carbon nanotubes and nano-metal particles, to the biomass polyurethane prepolymer in a ratio of 1% to 5% by weight of the resin matrix, and uniformly dispersing the conductive functional body in the resin matrix by physical or chemical means (such as ultrasonic dispersion, high-speed stirring, etc.);

[0009] S4: adding small molecule polyol and diamine to the obtained mixture to adjust the crosslinking density and flexibility of the resin, and controlling the reaction time to ensure the stability of the resin performance, and adjusting the R value (isocyanate index) to between 1.05 and 1.1 to obtain a single-component biomass conductive resin;

[0010] S5: Unsealing at high temperature and allowing the resin to react rapidly with a small molecule curing agent to cure into a shape.

[0011] Preferably, the hydroxyl-containing polyol is selected from one or more of polyethylene glycol, polypropylene glycol, and polytetrahydrofuran diol, preferably polyethylene glycol.

[0012] Preferably, the polyisocyanate is selected from one or more of toluene diisocyanate (TDI) and diphenylmethane diisocyanate (MDI), preferably toluene diisocyanate (TDI).

[0013] Preferably, the conductive functional body comprises conductive graphene, carbon nanotubes and nano-metal particles, wherein the content of conductive graphene is 0.5% to 2%, the content of carbon nanotubes is 0.5% to 2%, and the content of nano-metal particles is 1% to 3%.

[0014] Preferably, the small molecule polyol is selected from one or more of ethylene glycol, propylene glycol, and butylene glycol, preferably ethylene glycol.

[0015] Preferably, the diamine is selected from one or more of ethylenediamine, hexamethylenediamine, and diethylenetriamine, preferably ethylenediamine.

[0016] Preferably, the temperature range of the high temperature desealing is 120-150°C, preferably 130-140°C.

[0017] Preferably, the curing time is 1-3 hours, preferably 1.5-2.5 hours.

[0018] Preferably, the addition amount, form (such as powder, solution, dispersion) and surface treatment method of the conductive functional body can be adjusted according to specific needs to achieve optimal conductive performance and dispersion uniformity.

[0019] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0020] First, the present invention uses biomass raw materials, which reduces the impact on the environment. The raw materials are widely available, the synthesis process is simple, the conditions are mild, and the cost is low. By optimizing the formula and preparation process, the resin has good mechanical strength and toughness. By optimizing the formula and preparation process, the resin has good mechanical strength and toughness. The single-component system does not require on-site mixing, simplifies the operation steps, and improves production efficiency.

[0021] Second, the present invention, the single-component resin replaces the existing two-component polyurethane resin, can be used for pultrusion molding of profiles with complex cross-sections, and pultrusion molding of profiles with small-sized cross-sections, such as composite material door and window profiles replacing aluminum alloy, photovoltaic frame profiles, vegetable greenhouse poles, prefabricated building profiles, energy fields, greatly improving the yield and production efficiency, overcoming the two-component resin must use a glue injection machine, proprietary molds, and reduce production equipment investment.

[0022] Second, the present invention introduces conductive graphene, carbon nanotubes and nano-metal particles to make the prepared resin have excellent conductive function, overcoming the insulation characteristics of conventional composite materials, the surface treatment can only be done by grinding, plasma burning and then water-based paint coating, which brings high cost shortcomings. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is the overall flow chart of the present invention. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] The present invention provides the following technical solutions:

[0026] Embodiment 1

[0027] The single-component biomass resin synthesis process comprises the following materials in parts by weight:

[0028] Polyol: polyethylene glycol;

[0029] Polyisocyanate: toluene diisocyanate (TDI);

[0030] Conductive functional body: conductive graphene 1%, carbon nanotubes 1%, nano metal particles 3%;

[0031] Small molecule polyols: ethylene glycol;

[0032] Diamine: ethylenediamine;

[0033] R value: 1.05;

[0034] High temperature unsealing temperature: 120℃;

[0035] Curing time: 1 hour.

[0036] Preparation process of single-component biomass resin:

[0037] S1: Under nitrogen protection, polyethylene glycol and toluene diisocyanate are reacted at 70°C for 2 hours to form a prepolymer;

[0038] S2: Cardanol and butanone oxime were used to terminate the polyisocyanate groups in the prepolymer, with a termination rate of 100%;

[0039] S3: adding conductive graphene, carbon nanotubes and nano-metal particles into the prepolymer in proportion and stirring evenly;

[0040] S4: mixing ethylene glycol and ethylenediamine, controlling the R value to 1.05, and preparing a single-component biomass conductive resin;

[0041] S5: Unblocking at 120°C and allowing the resin to react rapidly with the small molecule curing agent, with a curing time of 1 hour.

[0042] Embodiment 2

[0043] The single-component biomass resin synthesis process comprises the following materials in parts by weight:

[0044] Polyol: polypropylene glycol;

[0045] Polyisocyanate: diphenylmethane diisocyanate (MDI);

[0046] Conductive functional body: conductive graphene 2%, carbon nanotubes 2%, nano metal particles 1%;

[0047] Small molecule polyols: propylene glycol;

[0048] Diamine: hexamethylenediamine;

[0049] R value: 1.1;

[0050] High temperature unsealing temperature: 150℃;

[0051] Curing time: 3 hours.

[0052] Preparation process of single-component biomass resin:

[0053] S1: Under nitrogen protection, polypropylene glycol and diphenylmethane diisocyanate are reacted at 75°C for 2.5 hours to form a prepolymer;

[0054] S2: Cardanol and butanone oxime were used to terminate the polyisocyanate groups in the prepolymer, with a termination rate of 100%;

[0055] S3: adding conductive graphene, carbon nanotubes and nano-metal particles into the prepolymer in proportion and stirring evenly;

[0056] S4: mixing propylene glycol and hexamethylenediamine, controlling the R value to 1.1, and preparing a single-component biomass conductive resin;

[0057] S5: Unblocking at 150°C and allowing the resin to react rapidly with the small molecule curing agent, with a curing time of 3 hours.

[0058] Embodiment 3

[0059] The single-component biomass resin synthesis process comprises the following materials in parts by weight:

[0060] Polyol: polytetramethylene glycol;

[0061] Polyisocyanate: toluene diisocyanate (TDI);

[0062] Conductive functional body: conductive graphene 1.5%, carbon nanotubes 1.5%, nano metal particles 2%;

[0063] Small molecule polyols: butanediol;

[0064] Diamine: diethylenetriamine;

[0065] R value: 1.08;

[0066] High temperature unsealing temperature: 130℃;

[0067] Curing time: 2 hours.

[0068] Preparation process of single-component biomass resin:

[0069] S1: Under nitrogen protection, polytetrahydrofuran diol and toluene diisocyanate are reacted at 70° C. for 2 hours to form a prepolymer;

[0070] S2: Cardanol and butanone oxime were used to terminate the polyisocyanate groups in the prepolymer, with a termination rate of 100%;

[0071] S3: adding conductive graphene, carbon nanotubes and nano-metal particles into the prepolymer in proportion and stirring evenly;

[0072] S4: mixing butanediol and diethylenetriamine, controlling the R value to 1.08, to prepare a single-component biomass conductive resin;

[0073] S5: Unblocking at 130°C and allowing the resin to react rapidly with the small molecule curing agent, with a curing time of 2 hours.

[0074] Embodiment 4

[0075] The single-component biomass resin synthesis process comprises the following materials in parts by weight:

[0076] Polyol: polyethylene glycol;

[0077] Polyisocyanate: diphenylmethane diisocyanate (MDI);

[0078] Conductive functional body: conductive graphene 1.2%, carbon nanotubes 1.2%, nano metal particles 2.6%;

[0079] Small molecule polyols: ethylene glycol;

[0080] Diamine: ethylenediamine;

[0081] R value: 1.06;

[0082] High temperature unsealing temperature: 135℃;

[0083] Curing time: 2 hours;

[0084] Preparation process of single-component biomass resin:

[0085] S1: Under nitrogen protection, polyethylene glycol and diphenylmethane diisocyanate are reacted at 75°C for 2 hours to form a prepolymer;

[0086] S2: Cardanol and butanone oxime were used to terminate the polyisocyanate groups in the prepolymer, with a termination rate of 100%;

[0087] S3: adding conductive graphene, carbon nanotubes and nano-metal particles into the prepolymer in proportion and stirring evenly;

[0088] S4: mixing ethylene glycol and ethylenediamine, controlling the R value to 1.06, and preparing a single-component biomass conductive resin;

[0089] S5: Unblocking at 135°C and allowing the resin to react rapidly with the small molecule curing agent, with a curing time of 2 hours.

[0090] Embodiment 5

[0091] The single-component biomass resin synthesis process comprises the following materials in parts by weight:

[0092] Polyol: polypropylene glycol;

[0093] Polyisocyanate: toluene diisocyanate (TDI);

[0094] Conductive functional body: conductive graphene 1.8%, carbon nanotubes 1.8%, nano metal particles 1.4%;

[0095] Small molecule polyols: propylene glycol;

[0096] Diamine: hexamethylenediamine;

[0097] R value: 1.07;

[0098] High temperature unsealing temperature: 140℃;

[0099] Curing time: 2.5 hours.

[0100] Preparation process of single-component biomass resin:

[0101] S1: Under nitrogen protection, polypropylene glycol and toluene diisocyanate are reacted at 70°C for 2.5 hours to form a prepolymer;

[0102] S2: Cardanol and butanone oxime were used to terminate the polyisocyanate groups in the prepolymer, with a termination rate of 100%;

[0103] S3: adding conductive graphene, carbon nanotubes and nano-metal particles into the prepolymer in proportion and stirring evenly;

[0104] S4: mixing propylene glycol and hexamethylenediamine, controlling the R value to 1.07, and preparing a single-component biomass conductive resin;

[0105] S5: Unblocking at 140°C and allowing the resin to react rapidly with the small molecule curing agent, with a curing time of 2.5 hours.

[0106] While 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 alterations may be made to the embodiments without departing from the principles and spirit thereof, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A single-component biomass resin synthesis process, characterized in that: The following steps are involved: S1: In an inert gas (such as nitrogen N2 or argon Ar) protective environment, hydroxyl-containing polyol and polyisocyanate are mixed in a certain proportion, and polymerization reaction is carried out at a suitable temperature (usually not exceeding 80°C) to synthesize prepolymer. During the reaction, parameters such as temperature, pressure, stirring speed, etc. need to be controlled to ensure reaction efficiency and product quality; S2: The synthesized prepolymer is mixed with a capping agent (such as cardanol and butanone oxime) and capped to block the polyisocyanate groups in the prepolymer. The capping rate is 100% to improve the stability and storage of the resin. The capping reaction needs to be carried out at a suitable temperature and the reaction time is controlled to ensure complete capping. S3: adding a conductive functional body, including conductive graphene, carbon nanotubes and nano-metal particles, to the biomass polyurethane prepolymer in a ratio of 1% to 5% by weight of the resin matrix, and uniformly dispersing the conductive functional body in the resin matrix by physical or chemical means (such as ultrasonic dispersion, high-speed stirring, etc.); S4: adding small molecule polyol and diamine to the obtained mixture to adjust the crosslinking density and flexibility of the resin, and controlling the reaction time to ensure the stability of the resin performance, and adjusting the R value (isocyanate index) to between 1.05 and 1.1 to obtain a single-component biomass conductive resin; S5: Unsealing at high temperature and allowing the resin to react rapidly with a small molecule curing agent to cure into a shape.

2. The single-component biomass resin synthesis process according to claim 1, characterized in that: The hydroxyl-containing polyol is selected from one or more of polyethylene glycol, polypropylene glycol, and polytetramethylene glycol, preferably polyethylene glycol.

3. The single-component biomass resin synthesis process according to claim 1, characterized in that: The polyisocyanate is selected from one or more of toluene diisocyanate (TDI) and diphenylmethane diisocyanate (MDI), preferably toluene diisocyanate (TDI).

4. The single-component biomass resin synthesis process according to claim 1, characterized in that: The conductive functional body comprises conductive graphene, carbon nanotubes and nano metal particles, wherein the content of the conductive graphene is 0.5% to 2%, the content of the carbon nanotubes is 0.5% to 2%, and the content of the nano metal particles is 1% to 3%.

5. The single-component biomass resin synthesis process according to claim 1, characterized in that: The small molecule polyol is selected from one or more of ethylene glycol, propylene glycol, and butylene glycol, preferably ethylene glycol.

6. The single-component biomass resin synthesis process according to claim 1, characterized in that: The diamine is selected from one or more of ethylenediamine, hexamethylenediamine, and diethylenetriamine, preferably ethylenediamine.

7. The single-component biomass resin synthesis process according to claim 1, characterized in that: The temperature range of the high temperature desealing is 120-150°C, preferably 130-140°C.

8. The single-component biomass resin synthesis process according to claim 1, characterized in that: The curing time is 1-3 hours, preferably 1.5-2.5 hours.

9. The single-component biomass resin synthesis process according to claim 1, characterized in that: The addition amount, form (such as powder, solution, dispersion) and surface treatment method of the conductive functional body can be adjusted according to specific needs to achieve optimal conductive performance and dispersion uniformity.

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