CN112359605B - Unsaturated carbon fiber sizing agent and preparation method thereof - Google Patents
Unsaturated carbon fiber sizing agent and preparation method thereof Download PDFInfo
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/693—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural or synthetic rubber, or derivatives thereof
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention provides an unsaturated carbon fiber sizing agent and a preparation method thereof, wherein main sizing agent, diluent, emulsifier and penetrant are uniformly mixed at 40-60 ℃, then ionized water is dropwise added at the rotating speed of 8000-12000 r/min, and stirring is continued for 30-60 min after water is added, so as to obtain the unsaturated carbon fiber sizing agent; wherein the mass of the emulsifier is 5-15% of the mass of the main slurry, the mass of the penetrating agent is 2-5% of the mass of the main slurry, and the mass ratio of the diluent to the main slurry is (10-50): (50-90), wherein the mass ratio of the deionized water to the main slurry is (80-90): (10-20); the main slurry is prepared from a compound A and a compound B, wherein the compound A is any one of 4,4' -diaminodiphenylmethane, 4,4' -diaminodiphenyl ether, 4,4' -diaminodiphenyl sulfone and m-phenylenediamine, and the compound B is any one of glycidyl methacrylate and epoxy-terminated reactive liquid nitrile rubber. The invention can improve the interface performance of the carbon fiber reinforced vinyl ester resin composite material.
Description
Technical Field
The invention relates to an unsaturated sizing agent.
Background
The sizing is a necessary procedure in the preparation process of the carbon fiber, and aims to introduce a polymer transition layer between the carbon fiber and matrix resin, and has the main functions of: (1) protecting the carbon fibers; (2) improving the wettability of the carbon fiber and the resin; (3) Chemical bonds are formed between the carbon fibers and the resin, so that the interface bonding strength is improved. At present, most sizing agents on the surface of carbon fibers are epoxy sizing agents, and the vinyl ester resin sizing agents are rarely researched. The university of Jinan has conducted a systematic study on this, and has applied for two inventions: (1) An emulsion type carbon fiber sizing agent with an authorization notice number of CN101858037B and a preparation method and application thereof; (2) A carbon fiber emulsion sizing agent with the publication number of CN101858038B and a preparation method and application thereof.
In both patents, the main sizing agent is a mixture of two resin molecules, wherein the former is a mixture of a vinyl ester resin and a modified epoxy resin (epoxidized polybutadiene), and the latter is a mixture of an epoxy resin and an epoxy aliphatic polyolefin (epoxidized polybutadiene). The compatibility of the two main sizing agents and the compatibility of the sizing agent and the resin matrix are important factors for determining the performance of the sizing agent, but according to the similar compatibility principle, the compatibility of the epoxidized polybutadiene with the epoxy resin and the vinyl ester resin is poor, so that the effect of the sizing agent on improving the interfacial performance of the carbon fiber reinforced vinyl ester resin composite material is limited, and the interfacial bonding strength caused by the lack of chemical bond connection between the carbon fiber and the vinyl ester resin is low.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an unsaturated carbon fiber sizing agent which can form stronger connection strength with fibers and a resin matrix, has limited solubility in liquid resin, and forms an interface with stronger toughness.
The technical scheme adopted by the invention for solving the technical problem is as follows: an unsaturated carbon fiber sizing agent comprises main sizing agent, emulsifier, penetrant, diluent and deionized water, wherein the mass of the emulsifier is 5-15% of the mass of the main sizing agent, the mass of the penetrant is 2-5% of the mass of the main sizing agent, and the mass ratio of the diluent to the main sizing agent is (10-50): (50-90), wherein the mass ratio of the deionized water to the main slurry is (80-90): (10-20); the main slurry is prepared by reacting A and B compounds, wherein the compound A is any one of 4,4' -diaminodiphenylmethane, 4,4' -diaminodiphenyl ether, 4,4' -diaminodiphenyl sulfone and m-phenylenediamine, and the compound B is any one of glycidyl methacrylate and epoxy-terminated reaction type liquid nitrile rubber.
When the main slurry is prepared, firstly, dissolving a compound A in absolute ethyl alcohol to prepare a solution, wherein the mass of the absolute ethyl alcohol in the solution is 10-20 times of that of the compound A; heating the solution to 60-90 ℃, and then dropwise adding a compound B, wherein the molar ratio of the compound A to the compound B is (1.0-1.2): 1.0; after the dripping is finished, continuously stirring for 20-40 minutes and then cooling to room temperature; finally, the ethanol solvent in the product was removed by evaporation.
The dropping speed of the compound B is 0.1-0.4 ml/min.
The emulsifier adopts a compound emulsifier, the compound emulsifier is any two of octyl phenol polyoxyethylene ether, nonyl phenol polyoxyethylene ether, castor oil polyoxyethylene ether and polyoxyethylene sorbitan monolaurate, and the weight ratio of the compound emulsifier is (50-80): (20 to 50) in terms of mass ratio.
The penetrating agent is sec-octyl alcohol polyoxyethylene ether.
The diluent is hydroxypropyl methacrylate.
The solid content of the unsaturated carbon fiber sizing agent is 10-35 wt%.
The invention also provides a preparation method of the unsaturated carbon fiber sizing agent, which comprises the following steps: uniformly mixing the main slurry with a diluent, an emulsifier and a penetrant at 40-60 ℃, then dropwise adding ionized water at the rotating speed of 8000-12000 r/min, and continuously stirring for 30-60 min after water is added to obtain the unsaturated carbon fiber sizing agent.
The invention has the beneficial effects that: the main sizing agent contains a polar functional group which can form a chemical bond or a hydrogen bond with the surface of the carbon fiber and a vinyl functional group which can chemically react with the vinyl ester resin in the molecular structure, and can form strong connection with the carbon fiber and a resin matrix; the molecular structure is similar to that of vinyl ester resin, so that better compatibility is ensured; the main sizing agent contains flexible chain segments in the molecular chain, so that the sizing agent has certain toughness. The carbon fiber sized by the sizing agent has good bundling property, moderate stiffness and better wear resistance. The interface strength and the interface toughness of the carbon fiber and the vinyl ester resin after sizing treatment are improved simultaneously, and the improvement effect of the interface performance is more obvious.
Drawings
FIG. 1 is a schematic view of a main slurry reactor of the present invention.
Detailed Description
The present invention will be further described with reference to the following drawings and examples, which include, but are not limited to, the following examples.
(1) An unsaturated carbon fiber sizing agent is characterized in that the sizing agent comprises the following components: the slurry comprises main slurry, an emulsifier, a penetrant, a diluent and deionized water, wherein the mass of the emulsifier is 5-15% of that of the main slurry, the mass of the penetrant is 2-5% of that of the main slurry, and the mass ratio of the diluent to the main slurry is 10-50: 50-90, wherein the mass ratio of the deionized water to the main slurry is 80-90: 10 to 20.
(2) The unsaturated carbon fiber sizing agent according to claim 1, characterized in that the main sizing agent is prepared from two compounds of a and B by chemical reaction;
the compound A is any one of 4,4' -diaminodiphenylmethane, 4,4' -diaminodiphenyl ether, 4,4' -diaminodiphenyl sulfone and m-phenylenediamine;
the compound B is any one of glycidyl methacrylate and epoxy-terminated reactive liquid nitrile rubber.
The schematic diagram of the reaction device is shown in figure 1, and the reaction steps are as follows: firstly, dissolving a compound A in absolute ethyl alcohol to prepare a solution, starting a stirrer and cooling water, heating the ethanol solution of the compound A to 60-90 ℃, and then dropwise adding a compound B at the dropping speed of 0.1-0.4 ml/min. After the dripping is finished, stirring is continued for 20-40 minutes and then cooling is carried out to the room temperature. And finally, removing the ethanol solvent in the product through a rotary evaporator to obtain unsaturated sizing agent main slurry.
The mass of the absolute ethyl alcohol is 10 to 20 times of that of the compound A.
The molar ratio of the compound A to the compound B is 1.0-1.2: 1.0.
(3) The unsaturated carbon fiber sizing agent according to claim 1, characterized in that the emulsifier is a compound emulsifier, the compound emulsifier is any two of octyl phenol polyoxyethylene ether (OP-10), nonyl phenol polyoxyethylene ether (NP-10), castor oil polyoxyethylene ether (EL-40), polyoxyethylene sorbitan monolaurate (Tween-20), and the mass ratio of the two emulsifiers is 50-80: 20 to 50.
(4) The unsaturated carbon fiber sizing agent according to claim 1, characterized in that the penetrant is a sec-octanol polyoxyethylene ether.
(5) The unsaturated carbon fiber sizing agent according to claim 1, characterized in that the diluent is hydroxypropyl methacrylate.
(6) The unsaturated carbon fiber sizing agent according to claims 1 to 5, characterized by being prepared by a phase inversion emulsification method, comprising the steps of: uniformly mixing the main slurry with a diluent, an emulsifier and a penetrant at 40-60 ℃, then dropwise adding ionized water at the rotating speed of 8000-12000 r/min, and continuously stirring for 30-60 min after water is added to obtain the unsaturated carbon fiber sizing agent.
(7) The unsaturated carbon fiber sizing agent and the preparation method thereof according to claim 6, characterized in that the solid content of the unsaturated carbon fiber sizing agent is 10-35 wt%.
The first embodiment is as follows:
the embodiment is an unsaturated carbon fiber sizing agent and a preparation method thereof, wherein the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenylmethane and glycidyl methacrylate through chemical reaction. The synthesis steps are as follows: firstly, mixing 4,4' -diaminodiphenylmethane and absolute ethyl alcohol uniformly in a three-neck flask; then starting cooling water of an electric stirrer and a condenser pipe, heating the three-mouth bottle to 60-90 ℃ by a water bath method, and dripping glycidyl methacrylate into the three-mouth bottle at the speed of 0.1-0.4 ml/min; and after the dropwise addition is finished, continuously stirring for 20-40 minutes, cooling to room temperature, and removing the ethanol solvent in the product through a rotary evaporator to obtain the unsaturated sizing agent main slurry. 5363 and 4,4' -diaminodiphenylmethane and glycidyl methacrylate in a molar ratio of 1.0 to 1.2.
The preparation steps of the sizing agent emulsion are as follows: uniformly mixing the prepared sizing agent main slurry with a diluent, an emulsifier and a penetrating agent at 40-60 ℃, then dropwise adding ionized water at the rotating speed of 8000-12000 r/min, and continuously stirring for 30-60 min after water is added to obtain the unsaturated carbon fiber sizing agent. Wherein the mass ratio of the diluent hydroxypropyl methacrylate to the main slurry is 10-50: 50 to 90 percent; the emulsifier is a compound of OP-10 and Tween-20, the total mass of the emulsifier is 5-15% of the mass of the main slurry, and the mass ratio of the OP-10 to the Tween-20 is 50-80; the mass of the penetrating agent, namely the polyoxyethylene ether of the secondary octanol, is 2 to 5 percent of the mass of the main slurry; the mass ratio of the deionized water to the main slurry is 80-90.
The second embodiment is as follows:
the difference between the present embodiment and the first embodiment is: the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenyl ether and glycidyl methacrylate through chemical reaction. The rest is the same as the first embodiment.
The third concrete implementation mode:
the present embodiment differs from the first embodiment in that: the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenyl sulfone and glycidyl methacrylate through chemical reaction. The rest is the same as the first embodiment.
The fourth concrete implementation mode is as follows:
the present embodiment differs from the first embodiment in that: the sizing agent main sizing agent is synthesized by m-phenylenediamine and glycidyl methacrylate through chemical reaction. The rest is the same as the first embodiment.
The fifth concrete implementation mode:
the present embodiment differs from the first embodiment in that: the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenylmethane and epoxy-terminated reactive liquid nitrile rubber through chemical reaction. The rest is the same as the first embodiment.
The sixth specific implementation mode:
the present embodiment is different from the fifth embodiment in that: the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenyl ether and epoxy-terminated reactive liquid nitrile rubber through chemical reaction. The rest is the same as the fifth embodiment.
The seventh concrete implementation mode:
the present embodiment is different from the fifth embodiment in that: the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenyl sulfone and epoxy-terminated reactive liquid nitrile rubber through chemical reaction. The rest is the same as the fifth embodiment.
The specific implementation mode is eight:
the present embodiment is different from the fifth embodiment in that: the sizing agent main sizing agent is synthesized by m-phenylenediamine and epoxy-terminated reactive liquid nitrile rubber through chemical reaction. The rest is the same as the fifth embodiment.
The specific implementation method nine:
the difference between the present embodiment and the first embodiment is: the emulsifier used for preparing the sizing agent emulsion is the compound of OP-10 and EL-40. The rest is the same as the first embodiment.
The detailed implementation mode is ten:
the present embodiment differs from the first embodiment in that: the emulsifier used for preparing the sizing agent emulsion is the compound of OP-10 and NP-10. The rest is the same as the first embodiment.
The effect of the invention is demonstrated by the following examples:
in the embodiment, the sizing agent main sizing agent is synthesized by 4,4' -diaminodiphenylmethane and glycidyl methacrylate through chemical reaction. The synthesis steps are as follows: firstly, 4.356g of 4,4' -diaminodiphenylmethane and 100ml of ethanol are uniformly mixed in a 250ml three-neck flask; then starting cooling water of an electric stirrer and a condenser pipe, heating the three-mouth bottle to 80 ℃ by a water bath method, and dropwise adding 2.840g glycidyl methacrylate into the three-mouth bottle at the speed of 0.3 ml/min; after the dropwise addition, stirring is continued for 20 minutes, cooling is carried out to room temperature, and then the ethanol solvent in the product is removed through a rotary evaporator, so as to obtain the unsaturated sizing agent main slurry.
The preparation steps of the sizing agent emulsion are as follows: uniformly mixing the prepared sizing agent main slurry with hydroxypropyl methacrylate, polyoxyethylene octylphenol ether, tween-20 and polyoxyethylene secondary octanol at 50 ℃, dropwise adding ionized water at the rotating speed of 10000r/min, and continuously stirring for 30min after the water is added to obtain the unsaturated carbon fiber sizing agent. The mass of the diluent is 50% of the mass of the main slurry; the mass of the emulsifier is 10 percent of that of the main slurry, wherein the mass ratio of the polyoxyethylene octylphenol ether to the Tween-20 is 7:3; the mass of the penetrating agent is 2% of that of the main slurry, and the mass ratio of the deionized water to the main slurry is 80.
The carbon fiber sizing treatment steps are as follows: diluting the unsaturated sizing agent to the solid content of 0.5%, sizing the carbon fiber for 30s, drying in a furnace at 100 ℃ for 10 minutes, and rolling to obtain the sized carbon fiber.
And weighing the mass of the carbon fiber before and after sizing, and calculating to obtain the mass fraction of the sizing agent on the surface of the carbon fiber to be 1.02%. The carbon fiber after sizing treatment has good bundling property, the stiffness is 66mm, the abrasion resistance times are 1334 times, and the wool amount is 0.16mg/m. The surface roughness of the carbon fiber after sizing treatment was slightly improved by atomic force microscopy. The surface energy of the carbon fiber is measured and calculated by adopting an OWKR theoretical model, and the result shows that the surface energy of the carbon fiber treated by the sizing agent is obviously increased. The interfacial shear strength of the carbon fiber/vinyl ester resin composite material is measured by a micro-debonding method, and the result shows that the interfacial shear strength of the composite material prepared by the carbon fiber treated by the sizing agent reaches 62MPa, while the interfacial shear strength of the composite material prepared by the untreated carbon fiber is 32MPa, which is improved by 96.9%.
Claims (8)
1. An unsaturated carbon fiber sizing agent comprises main sizing agent, an emulsifier, a penetrant, a diluent and deionized water, and is characterized in that the mass of the emulsifier is 5-15% of that of the main sizing agent, the mass of the penetrant is 2-5% of that of the main sizing agent, and the mass ratio of the diluent to the main sizing agent is (10-50): (50-90), wherein the mass ratio of the deionized water to the main slurry is (80-90): (10-20); the main slurry is prepared by reacting A and B compounds, wherein the compound A is any one of 4,4' -diaminodiphenylmethane, 4,4' -diaminodiphenyl ether, 4,4' -diaminodiphenyl sulfone and m-phenylenediamine, and the compound B is any one of glycidyl methacrylate and epoxy-terminated reaction type liquid nitrile rubber.
2. The unsaturated carbon fiber sizing agent according to claim 1, wherein the main sizing agent is prepared by first dissolving the compound A in absolute ethanol to prepare a solution, and the mass of the absolute ethanol in the solution is 10-20 times of that of the compound A; heating the solution to 60-90 ℃, and then dropwise adding a compound B, wherein the molar ratio of the compound A to the compound B is (1.0-1.2): 1.0; after the dripping is finished, continuously stirring for 20-40 minutes and then cooling to room temperature; finally, the ethanol solvent in the product was removed by evaporation.
3. The unsaturated carbon fiber sizing agent according to claim 2, wherein the dropping rate of the compound B is 0.1 to 0.4ml/min.
4. The unsaturated carbon fiber sizing agent according to claim 1, wherein the emulsifier is a compound emulsifier, and the compound emulsifier is any two of octylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether and polyoxyethylene sorbitan monolaurate according to the ratio of (50-80): (20 to 50) in terms of mass ratio.
5. The unsaturated carbon fiber sizing agent according to claim 1, wherein said penetrant is a para-octanol polyoxyethylene ether.
6. The unsaturated carbon fiber sizing agent according to claim 1, wherein the diluent is hydroxypropyl methacrylate.
7. The unsaturated carbon fiber sizing agent according to claim 1, wherein the solid content of the unsaturated carbon fiber sizing agent is 10 to 35wt%.
8. A method for preparing the unsaturated carbon fiber sizing agent according to claim 1, comprising the steps of: uniformly mixing the main slurry with a diluent, an emulsifier and a penetrant at 40-60 ℃, then dropwise adding ionized water at the rotating speed of 8000-12000 r/min, and continuously stirring for 30-60 min after water is added to obtain the unsaturated carbon fiber sizing agent.
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| JP2005146431A (en) * | 2003-11-11 | 2005-06-09 | Mitsubishi Rayon Co Ltd | Sizing agent for reinforcing fiber, carbon fiber bundle and method for producing the same, and thermoplastic resin composition and its molded article |
| CN101858037A (en) * | 2010-06-18 | 2010-10-13 | 济南大学 | A kind of emulsion type carbon fiber sizing agent and its preparation method and application |
| JP2015007300A (en) * | 2013-06-26 | 2015-01-15 | 東レ株式会社 | Sizing agent-coated carbon fibers, method for producing the same, and carbon fiber-reinforced composite material |
| CN105064030A (en) * | 2015-08-19 | 2015-11-18 | 国网智能电网研究院 | Carbon fiber sizing agent and preparation method thereof |
| JP2017155372A (en) * | 2016-03-03 | 2017-09-07 | 東レ株式会社 | Sizing agent applied carbon fiber, manufacturing method of sizing agent applied carbon fiber, prepreg and carbon fiber reinforced composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2583953A1 (en) * | 2011-10-20 | 2013-04-24 | 3B-Fibreglass SPRL | Sizing composition for glass fibres |
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| JP2005146431A (en) * | 2003-11-11 | 2005-06-09 | Mitsubishi Rayon Co Ltd | Sizing agent for reinforcing fiber, carbon fiber bundle and method for producing the same, and thermoplastic resin composition and its molded article |
| CN101858037A (en) * | 2010-06-18 | 2010-10-13 | 济南大学 | A kind of emulsion type carbon fiber sizing agent and its preparation method and application |
| JP2015007300A (en) * | 2013-06-26 | 2015-01-15 | 東レ株式会社 | Sizing agent-coated carbon fibers, method for producing the same, and carbon fiber-reinforced composite material |
| CN105064030A (en) * | 2015-08-19 | 2015-11-18 | 国网智能电网研究院 | Carbon fiber sizing agent and preparation method thereof |
| JP2017155372A (en) * | 2016-03-03 | 2017-09-07 | 東レ株式会社 | Sizing agent applied carbon fiber, manufacturing method of sizing agent applied carbon fiber, prepreg and carbon fiber reinforced composite material |
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