CN105646945A - Method for preparing nanometer silicon dioxide grafted carbon fiber reinforcements by aid of mercapto-alkene click reaction - Google Patents
Method for preparing nanometer silicon dioxide grafted carbon fiber reinforcements by aid of mercapto-alkene click reaction Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to a method for preparing nanometer silicon dioxide grafted carbon fiber reinforcements by the aid of mercapto-alkene click reaction. The method includes particular steps of 1), carrying out sulfhydrylation treatment on nanometer silicon dioxide; 2), carrying out acidification treatment on carbon fibers; 3), carrying out amination treatment on the surfaces of the carbon fibers; 4), preparing allyl glycidyl ether grafted carbon fibers; 5), preparing the nanometer silicon dioxide grafted carbon fiber reinforcements by the aid of the mercapto-alkene click reaction. The method has the advantages that the surface roughness can be improved after the nanometer silicon dioxide is grafted on the surfaces of the carbon fibers, the carbon fiber and resin wettability can be obviously improved, the method is favorable for increasing interface binding force between the carbon fibers and resin matrixes, and mechanical properties of carbon fiber reinforcement composite materials can be improved; the heat stability of the carbon fibers can be obviously improved after the nanometer silicon dioxide is grafted on the surfaces of the carbon fibers; the method is short in reaction period, high in yield and favorable for large-scale production, and byproducts are harmless.
Description
Technical field
The present invention relates to a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement.
Background technology
Carbon fiber is a kind of new material with advantages such as low-density, high specific strength, high ratio modulus, endurance, heat conduction, conductions, has been widely used for the fields such as Aeronautics and Astronautics, stationery sports goods and textile machine. But due to carbon fiber own structural characteristics so that it is poor with the caking property of resin matrix, firm not with resin matrix compound tense interface, a lot of excellent properties of composite can not be brought into play well. Therefore, the key issue that to be carbon fiber to carbon fiber surface modification encountered in polymer matrix composite is applied.
Traditional surface treatment of carbon fibers technology is higher to the requirement of equipment and technique, and treatment effect is not good. Utilizing sulfydryl-alkene click-reaction that inorganic material surface is modified is work as the method for modifying that former is new, and the method has the advantages such as applied range, productivity is high, by-product is harmless, the response time is short. The method avoids the tradition method of modifying process time long, process is toxic, it is difficult to the problems such as industrialized mass production. After nano silicon being grafted to carbon fiber surface by sulfydryl-alkene click-reaction, the interface binding power between carbon fiber and resin matrix can be significantly improved, improve the thermal stability of carbon fiber simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of method simply, quickly preparing nano silicon grafting carbon fiber reinforcement, the party's ratio juris is mainly based upon sulfydryl-alkene click-reaction, this reaction time is short, productivity is high, and prepared nano silicon grafting carbon fiber reinforcement has the advantages such as surface roughness is big and resin wellability is good, thermal stability is good.
The present invention is achieved like this, the preparation method of nano silicon grafting carbon fiber reinforcement, it is characterized in that method step is:
The first step: 1g nano silicon and 0.4g deionized water are joined in 30 ~ 60mL ethanol, ultrasonic Treatment adds 2 ~ 4g containing mercaptosilane coupling agents after 60 ~ 120 minutes, put in oil bath pan 60��75 DEG C of back flow reaction 4 ~ 6 hours, reaction terminate after with ethanol purge 4 times remove non-grafted on containing mercaptosilane coupling agents, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing mercaptosilane coupling agents engrafted nanometer silicon dioxide;
Second step: 5g carbon fiber is immersed in 100 ~ 160mL nitration mixture, ultrasonic Treatment 60 ~ 120 minutes, then move in oil bath pan 80 ~ 100 DEG C to react 2 ~ 4 hours, it is washed till neutrality after completion of the reaction with deionized water, it is subsequently placed in 100 DEG C of vacuum drying ovens dry 24 hours, namely obtains acid treatment carbon fiber;
3rd step: 5g acid treatment carbon fiber is dispersed in 150 ~ 200mL mixed solvent, with second acid for adjusting pH value to 4 ~ 5, ultrasonic Treatment adds 10 ~ 30g containing amino silicane coupling agent after 30 ~ 60 minutes, 60 DEG C are reacted 2 ~ 4 hours, reaction clean 4 times with the mixed solution of ethanol, acetone and deionized water after terminating remove non-grafted on containing amino silicane coupling agent, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing amino silicane coupling agent grafting carbon fiber;
4th step: 2g grafting carbon fiber containing amino silicane coupling agent is dispersed in 30��60mL ethanol, it is subsequently adding 4 ~ 8g allyl glycidyl ether, room temperature magnetic agitation 48 ~ 72 hours, with ethanol purge 4 times, then dry 24 hours in 40 DEG C of vacuum drying ovens, allyl glycidyl ether grafting carbon fiber can be obtained;
5th step: 0.4g is dispersed in the dimethylformamide of 30 ~ 60mL containing mercaptosilane coupling agents engrafted nanometer silicon dioxide and 1g allyl glycidyl ether grafting carbon fiber, ultrasonic Treatment 60 ~ 120 minutes, it is subsequently adding the light trigger of 0.1g, the irradiation under ultraviolet ray adopting wavelength to be 365nm 1 ~ 2 hour, then ethanol purge is used 4 times, 80 DEG C of vacuum drying ovens dry 24 hours, nano silicon grafting carbon fiber reinforcement can be obtained.
Described is the one in ��-mercaptopropyl trimethoxysilane, ��-mercapto hydroxypropyl methyl dimethoxysilane or gamma-mercaptopropyltriethoxysilane containing mercaptosilane coupling agents.
Described nitration mixture is that ratio for 3:1 mixes by volume by the concentrated nitric acid that mass percent concentration is 65% and concentrated sulphuric acid that mass percent concentration is 96%.
Described mixed solvent is to be mixed by the ratio that dehydrated alcohol and deionized water are 4:1 by volume.
Described is the one in gamma-aminopropyl-triethoxy-silane, ��-aminopropyltriethoxy diethoxy silane or ��-aminopropyltrimethoxysilane containing amino silicane coupling agent.
Described light trigger is the one in benzoin dimethylether or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
The solution have the advantages that: it is big that nano silicon grafting carbon fiber reinforcement provided by the invention has surface roughness, nano silicon percent grafting is high, good with resin matrix caking property, the advantages such as thermal stability is good.
Detailed description of the invention
Embodiment 1:
This example demonstrates that a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement provided by the invention.
The first step: 1g nano silicon and 0.4g deionized water are joined in 30mL ethanol, ultrasonic Treatment adds 2g containing mercaptosilane coupling agents (��-mercapto hydroxypropyl methyl dimethoxysilane) after 120 minutes, put in oil bath pan 70 DEG C of back flow reaction 5 hours, reaction terminate after with ethanol purge 4 times remove non-grafted on containing mercaptosilane coupling agents, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing mercaptosilane coupling agents engrafted nanometer silicon dioxide;
Second step: 5g carbon fiber is immersed in 160mL nitration mixture, ultrasonic Treatment 60 minutes, then moves in oil bath pan 80 DEG C and reacts 4 hours, be washed till neutrality with deionized water after completion of the reaction, it is subsequently placed in 100 DEG C of vacuum drying ovens dry 24 hours, namely obtains acid treatment carbon fiber;
3rd step: 5g acid treatment carbon fiber is dispersed in 180mL mixed solvent, with second acid for adjusting pH value to 4, ultrasonic Treatment adds 10g containing amino silicane coupling agent (gamma-aminopropyl-triethoxy-silane) after 45 minutes, 60 DEG C are reacted 3 hours, reaction clean 4 times with the mixed solution of ethanol, acetone and deionized water after terminating remove non-grafted on containing amino silicane coupling agent, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing amino silicane coupling agent grafting carbon fiber;
4th step: 2g grafting carbon fiber containing amino silicane coupling agent is dispersed in 45mL ethanol, it is subsequently adding 4g allyl glycidyl ether, room temperature magnetic agitation 48 hours, with ethanol purge 4 times, then dry 24 hours in 40 DEG C of vacuum drying ovens, allyl glycidyl ether grafting carbon fiber can be obtained;
5th step: 0.4g is dispersed in the dimethylformamide of 30mL containing mercaptosilane coupling agents engrafted nanometer silicon dioxide and 1g allyl glycidyl ether grafting carbon fiber, ultrasonic Treatment 120 minutes, it is subsequently adding the benzoin dimethylether of 0.1g, the irradiation under ultraviolet ray adopting wavelength to be 365nm 1 hour, then ethanol purge is used 4 times, 80 DEG C of vacuum drying ovens dry 24 hours, nano silicon grafting carbon fiber reinforcement can be obtained.
Embodiment 2:
This example demonstrates that a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement provided by the invention.
The first step: 1g nano silicon and 0.4g deionized water are joined in 60mL ethanol, ultrasonic Treatment adds 3g containing mercaptosilane coupling agents (gamma-mercaptopropyltriethoxysilane) after 60 minutes, put in oil bath pan 75 DEG C of back flow reaction 6 hours, reaction terminate after with ethanol purge 4 times remove non-grafted on containing mercaptosilane coupling agents, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing mercaptosilane coupling agents engrafted nanometer silicon dioxide;
Second step: 5g carbon fiber is immersed in 120mL nitration mixture, ultrasonic Treatment 90 minutes, then moves in oil bath pan 100 DEG C and reacts 2 hours, be washed till neutrality with deionized water after completion of the reaction, it is subsequently placed in 100 DEG C of vacuum drying ovens dry 24 hours, namely obtains acid treatment carbon fiber;
3rd step: 5g acid treatment carbon fiber is dispersed in 150mL mixed solvent, with second acid for adjusting pH value to 5, ultrasonic Treatment adds 20g containing amino silicane coupling agent (��-aminopropyltrimethoxysilane) after 60 minutes, 60 DEG C are reacted 4 hours, reaction clean 4 times with the mixed solution of ethanol, acetone and deionized water after terminating remove non-grafted on containing amino silicane coupling agent, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing amino silicane coupling agent grafting carbon fiber;
4th step: 2g grafting carbon fiber containing amino silicane coupling agent is dispersed in 30mL ethanol, it is subsequently adding 6g allyl glycidyl ether, room temperature magnetic agitation 72 hours, with ethanol purge 4 times, then dry 24 hours in 40 DEG C of vacuum drying ovens, allyl glycidyl ether grafting carbon fiber can be obtained;
5th step: 0.4g is dispersed in the dimethylformamide of 60mL containing mercaptosilane coupling agents engrafted nanometer silicon dioxide and 1g allyl glycidyl ether grafting carbon fiber, ultrasonic Treatment 60 minutes, it is subsequently adding the 2-hydroxy-2-methyl-1-phenyl-1-acetone of 0.1g, the irradiation under ultraviolet ray adopting wavelength to be 365nm 2 hours, then ethanol purge is used 4 times, 80 DEG C of vacuum drying ovens dry 24 hours, nano silicon grafting carbon fiber reinforcement can be obtained.
Embodiment 3:
This example demonstrates that a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement provided by the invention.
The first step: 1g nano silicon and 0.4g deionized water are joined in 45mL ethanol, ultrasonic Treatment adds 4g containing mercaptosilane coupling agents (��-mercaptopropyl trimethoxysilane) after 90 minutes, put in oil bath pan 60 DEG C of back flow reaction 4 hours, reaction terminate after with ethanol purge 4 times remove non-grafted on containing mercaptosilane coupling agents, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing mercaptosilane coupling agents engrafted nanometer silicon dioxide;
Second step: 5g carbon fiber is immersed in 100mL nitration mixture, ultrasonic Treatment 120 minutes, then moves in oil bath pan 90 DEG C and reacts 3 hours, be washed till neutrality with deionized water after completion of the reaction, it is subsequently placed in 100 DEG C of vacuum drying ovens dry 24 hours, namely obtains acid treatment carbon fiber;
3rd step: 5g acid treatment carbon fiber is dispersed in 200mL mixed solvent, with second acid for adjusting pH value to 4, ultrasonic Treatment adds 30g containing amino silicane coupling agent (��-aminopropyltriethoxy diethoxy silane) after 30 minutes, 60 DEG C are reacted 2 hours, reaction clean 4 times with the mixed solution of ethanol, acetone and deionized water after terminating remove non-grafted on containing amino silicane coupling agent, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing amino silicane coupling agent grafting carbon fiber;
4th step: 2g grafting carbon fiber containing amino silicane coupling agent is dispersed in 60mL ethanol, it is subsequently adding 8g allyl glycidyl ether, room temperature magnetic agitation 60 hours, with ethanol purge 4 times, then dry 24 hours in 40 DEG C of vacuum drying ovens, allyl glycidyl ether grafting carbon fiber can be obtained;
5th step: 0.4g is dispersed in the dimethylformamide of 45mL containing mercaptosilane coupling agents engrafted nanometer silicon dioxide and 1g allyl glycidyl ether grafting carbon fiber, ultrasonic Treatment 90 minutes, it is subsequently adding the benzoin dimethylether of 0.1g, the irradiation under ultraviolet ray adopting wavelength to be 365nm 1 hour, then ethanol purge is used 4 times, 80 DEG C of vacuum drying ovens dry 24 hours, nano silicon grafting carbon fiber reinforcement can be obtained.
Claims (6)
1. one kind utilizes the method that sulfydryl-alkene click-reaction prepares nano silicon grafting carbon fiber reinforcement, it is characterised in that said method comprising the steps of:
The first step: 1g nano silicon and 0.4g deionized water are joined in 30 ~ 60mL ethanol, ultrasonic Treatment adds 2 ~ 4g containing mercaptosilane coupling agents after 60 ~ 120 minutes, put in oil bath pan 60��75 DEG C of back flow reaction 4 ~ 6 hours, reaction terminate after with ethanol purge 4 times remove non-grafted on containing mercaptosilane coupling agents, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing mercaptosilane coupling agents engrafted nanometer silicon dioxide;
Second step: 5g carbon fiber is immersed in 100 ~ 160mL nitration mixture, ultrasonic Treatment 60 ~ 120 minutes, then move in oil bath pan 80 ~ 100 DEG C to react 2 ~ 4 hours, it is washed till neutrality after completion of the reaction with deionized water, it is subsequently placed in 100 DEG C of vacuum drying ovens dry 24 hours, namely obtains acid treatment carbon fiber;
3rd step: 5g acid treatment carbon fiber is dispersed in 150 ~ 200mL mixed solvent, with second acid for adjusting pH value to 4 ~ 5, ultrasonic Treatment adds 10 ~ 30g containing amino silicane coupling agent after 30 ~ 60 minutes, 60 DEG C are reacted 2 ~ 4 hours, reaction clean 4 times with the mixed solution of ethanol, acetone and deionized water after terminating remove non-grafted on containing amino silicane coupling agent, it is placed in 100 DEG C of vacuum drying ovens dry 24 hours, can obtain containing amino silicane coupling agent grafting carbon fiber;
4th step: 2g grafting carbon fiber containing amino silicane coupling agent is dispersed in 30��60mL ethanol, it is subsequently adding 4 ~ 8g allyl glycidyl ether, room temperature magnetic agitation 48 ~ 72 hours, with ethanol purge 4 times, then dry 24 hours in 40 DEG C of vacuum drying ovens, allyl glycidyl ether grafting carbon fiber can be obtained;
5th step: 0.4g is dispersed in the dimethylformamide of 30 ~ 60mL containing mercaptosilane coupling agents engrafted nanometer silicon dioxide and 1g allyl glycidyl ether grafting carbon fiber, ultrasonic Treatment 60 ~ 120 minutes, it is subsequently adding the light trigger of 0.1g, the irradiation under ultraviolet ray adopting wavelength to be 365nm 1 ~ 2 hour, then ethanol purge is used 4 times, 80 DEG C of vacuum drying ovens dry 24 hours, nano silicon grafting carbon fiber reinforcement can be obtained.
2. a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement as claimed in claim 1, it is characterised in that described is the one in ��-mercaptopropyl trimethoxysilane, ��-mercapto hydroxypropyl methyl dimethoxysilane or gamma-mercaptopropyltriethoxysilane containing mercaptosilane coupling agents.
3. a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement as claimed in claim 1, it is characterised in that described nitration mixture is that ratio for 3:1 mixes by volume by the concentrated nitric acid that mass percent concentration is 65% and concentrated sulphuric acid that mass percent concentration is 96%.
4. a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement as claimed in claim 1, it is characterised in that described mixed solvent is that ratio for 4:1 mixes by volume by dehydrated alcohol and deionized water.
5. a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement as claimed in claim 1, it is characterised in that described is the one in gamma-aminopropyl-triethoxy-silane, ��-aminopropyltriethoxy diethoxy silane or ��-aminopropyltrimethoxysilane containing amino silicane coupling agent.
6. a kind of method utilizing sulfydryl-alkene click-reaction to prepare nano silicon grafting carbon fiber reinforcement as claimed in claim 1, it is characterised in that described light trigger is the one in benzoin dimethylether or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
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