CN108440941A - A kind of preparation method of graphene modified resin base ballistic composite - Google Patents
A kind of preparation method of graphene modified resin base ballistic composite Download PDFInfo
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- CN108440941A CN108440941A CN201810174732.0A CN201810174732A CN108440941A CN 108440941 A CN108440941 A CN 108440941A CN 201810174732 A CN201810174732 A CN 201810174732A CN 108440941 A CN108440941 A CN 108440941A
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- graphene
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- modified resin
- graphene modified
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The present invention relates to bullet resistant material preparing technical field, especially a kind of preparation method of graphene modified resin base ballistic composite includes the following steps：S1, graphene is pre-processed, makes the active functional group in its surface；S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin adhesive；S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers (UHMWPE) in uniformly being sprawled in continuous lines, 1 3m/min of hauling speed is set, impregnated by resin under conditions of stringent control；S4, it dries at 55 70 DEG C later, dry 8 10min, you can be made.The present invention adds graphene in matrix adhesive, to substantially improve the ballistic performance of composite material entirety.
Description
Technical field
The present invention relates to bullet resistant material preparing technical field more particularly to a kind of shellproof composite woods of graphene modified resin base
The preparation method of material.
Background technology
Superhigh molecular weight polyethylene fibers (UHMWPE) ballistic composite is by UHMWPE fiber impregnated resins, stringent
It is obtained after dry by uniform, parallel, straight and upright arrangement under conditions of control glue content.Wherein resin matrix generally comprises poly-
Ethylene, polypropylene, ethylenic copolymer, propylene copolymer, epoxy resin, phenolic resin, polyurethane, unsaturated polyester (UP) etc..
The elastomer of these low modulus is coated on each fiber, in addition to that can also improve the anti-of composite material other than anchoring fiber
Bullet, shock resistance.
However this compound laminated cloth, the shortcomings that due to matrix resin adhesive itself so that composite material it is comprehensive
It can be affected, be embodied in poor heat resistance, comprehensive mechanical intensity is not high, and creep-resistant property is small, the UHMWPE fibers being made from it
Composite material cannot effectively resist the impact force of bullet, can only reach protection effect, quality by increasing the number of plies or weight
Partially hard, comfort level is poor, reduces practicability.Therefore, the heat resistance for how changing UHMWPE ballistic composites, makes it same
Etc. there is under the premise of the numbers of plies higher anti-bullet impact performance, so that it is constantly had become bullet resistant material to lightweight development and grind
The inexorable trend studied carefully.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of graphene modified resin proposed
The preparation method of base ballistic composite.
To achieve the goals above, present invention employs following technical solutions：
A kind of preparation method of graphene modified resin base ballistic composite is designed, is included the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin glue
Glutinous agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers
(UHMWPE) in uniformly being sprawled in continuous lines, hauling speed 1-3m/min is set, is soaked by resin under conditions of stringent control
Stain；
S4, it dries at 55-70 DEG C later, dry 8-10min, you can be made.
Preferably, pretreatment includes in S1：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene
Powder:Ethyl alcohol=1:5, coupling agent is the proportional arrangement coupling agent solution of 1g-10g/100ml according to mass concentration in a solvent,
Then by a diameter of 0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing,
Heating reflux reaction under stiring, the graphene after being coupled.
Preferably, select organochromium complexes, alkanes, titante coupling agent as coupling agent.
Preferably, it is as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=
1-10:The weight ratio of 100-90 mixes dispersant and resin under the conditions of high-speed stirred, at room temperature, rotating speed 3000-
4000r/min connects circulating condensing water, and dispersant resin is made after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, is stirred at 70-90 DEG C
Graphene modified resin adhesive is made in 1-2h after mixing.
Preferably, the dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin,
Phenolic resin, polyacrylate or polymethacrylates.
Preferably, resin is Aqueous Polyurethane Adhesives in S2.
A kind of preparation method of graphene modified resin base ballistic composite proposed by the present invention, advantageous effect are：
The present invention adds graphene in matrix adhesive, to substantially improve the ballistic performance of composite material entirety.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1
A kind of preparation method of graphene modified resin base ballistic composite, includes the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin glue
Glutinous agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers
(UHMWPE) in uniformly being sprawled in continuous lines, hauling speed 1m/min is set, is impregnated by resin under conditions of stringent control；
S4, it dries at 55 DEG C later, dry 8min, you can be made.The composite material of above-mentioned gained is pressed into (0/90 °) two
Layer staggeredly overlaps.By 50 layers, 40cm*40cm, the UD composite materials superposition that surface density is 110g/m2 is placed in the target that backing is clay
On frame, by GA141-2010 testing standards, using 54 formula 7.62mm pistols, the test of 51 formula pistol lead for retractable pencil bullets, back lining materials recess
As a result depth ＜ 25mm meet the standard requirement of GA141-2010.About reduce 10% compared to weight before.Thus it proves,
The UHMWPE ballistic composites of the present invention can largely reduce overall weight, improve the mechanicalness of resin matrix
Can, obtain bulletproof effect preferably ballistic composite.After measured, 100% stretching strength is up to 25Mpa for the modified resin of gained
Left and right.This method principle is reliable, and preparation process is simple, and cost is relatively low, and controllability is strong, is suitble to large-scale production.
It is pre-processed in S1 and includes：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene powder:Second
Alcohol=1:5, coupling agent, then will be a diameter of according to the proportional arrangement coupling agent solution that mass concentration in a solvent is 1g/100ml
0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing, heats under stiring
Back flow reaction, the graphene after being coupled.
Select organochromium complexes, alkanes, titante coupling agent as coupling agent.
It is as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=
1:100 weight ratio mixes dispersant and resin under the conditions of high-speed stirred, and at room temperature, rotating speed 3000r/min connects cycle
Dispersant resin is made in condensed water after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, and 1h is stirred at 70 DEG C,
Graphene modified resin adhesive is made after mixing.
Dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin, phenolic aldehyde tree
Fat, polyacrylate or polymethacrylates.
Resin is Aqueous Polyurethane Adhesives in S2.
Embodiment 2
A kind of preparation method of graphene modified resin base ballistic composite, includes the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin glue
Glutinous agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers
(UHMWPE) in uniformly being sprawled in continuous lines, hauling speed 2m/min is set, is impregnated by resin under conditions of stringent control；
S4, it dries at 58 DEG C later, dry 9min, you can be made.The composite material of above-mentioned gained is pressed into (0/90 °) two
Layer staggeredly overlaps.By 50 layers, 40cm*40cm, the UD composite materials superposition that surface density is 110g/m2 is placed in the target that backing is clay
On frame, by GA141-2010 testing standards, using 54 formula 7.62mm pistols, the test of 51 formula pistol lead for retractable pencil bullets, back lining materials recess
As a result depth ＜ 25mm meet the standard requirement of GA141-2010.About reduce 10% compared to weight before.Thus it proves,
The UHMWPE ballistic composites of the present invention can largely reduce overall weight, improve the mechanicalness of resin matrix
Can, obtain bulletproof effect preferably ballistic composite.After measured, 100% stretching strength is up to 25Mpa for the modified resin of gained
Left and right.This method principle is reliable, and preparation process is simple, and cost is relatively low, and controllability is strong, is suitble to large-scale production.
It is pre-processed in S1 and includes：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene powder:Second
Alcohol=1:5, coupling agent, then will be a diameter of according to the proportional arrangement coupling agent solution that mass concentration in a solvent is 2g/100ml
0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing, heats under stiring
Back flow reaction, the graphene after being coupled.
Select organochromium complexes, alkanes, titante coupling agent as coupling agent.
It is as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=
2:100 weight ratio mixes dispersant and resin under the conditions of high-speed stirred, and at room temperature, rotating speed 3200r/min connects cycle
Dispersant resin is made in condensed water after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, and 1h is stirred at 75 DEG C,
Graphene modified resin adhesive is made after mixing.
Dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin, phenolic aldehyde tree
Fat, polyacrylate or polymethacrylates.
Resin is Aqueous Polyurethane Adhesives in S2.
Embodiment 3
A kind of preparation method of graphene modified resin base ballistic composite, includes the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin glue
Glutinous agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers
(UHMWPE) in uniformly being sprawled in continuous lines, hauling speed 3m/min is set, is impregnated by resin under conditions of stringent control；
S4, it dries at 60 DEG C later, dry 9min, you can be made.The composite material of above-mentioned gained is pressed into (0/90 °) two
Layer staggeredly overlaps.By 50 layers, 40cm*40cm, the UD composite materials superposition that surface density is 110g/m2 is placed in the target that backing is clay
On frame, by GA141-2010 testing standards, using 54 formula 7.62mm pistols, the test of 51 formula pistol lead for retractable pencil bullets, back lining materials recess
As a result depth ＜ 25mm meet the standard requirement of GA141-2010.About reduce 10% compared to weight before.Thus it proves,
The UHMWPE ballistic composites of the present invention can largely reduce overall weight, improve the mechanicalness of resin matrix
Can, obtain bulletproof effect preferably ballistic composite.After measured, 100% stretching strength is up to 25Mpa for the modified resin of gained
Left and right.This method principle is reliable, and preparation process is simple, and cost is relatively low, and controllability is strong, is suitble to large-scale production.
It is pre-processed in S1 and includes：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene powder:Second
Alcohol=1:5, coupling agent, then will be a diameter of according to the proportional arrangement coupling agent solution that mass concentration in a solvent is 8g/100ml
0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing, heats under stiring
Back flow reaction, the graphene after being coupled.
Select organochromium complexes, alkanes, titante coupling agent as coupling agent.
It is as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=
8:100 weight ratio mixes dispersant and resin under the conditions of high-speed stirred, and at room temperature, rotating speed 3500r/min connects cycle
Dispersant resin is made in condensed water after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, and 2h is stirred at 80 DEG C,
Graphene modified resin adhesive is made after mixing.
Dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin, phenolic aldehyde tree
Fat, polyacrylate or polymethacrylates.
Resin is Aqueous Polyurethane Adhesives in S2.
Embodiment 4
A kind of preparation method of graphene modified resin base ballistic composite, includes the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin glue
Glutinous agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers
(UHMWPE) in uniformly being sprawled in continuous lines, hauling speed 3m/min is set, is impregnated by resin under conditions of stringent control；
S4, it dries at 70 DEG C later, dry 10min, you can be made.The composite material of above-mentioned gained is pressed into (0/90 °)
Two layers staggeredly overlap.By 50 layers, 40cm*40cm, it is clay that the superposition of UD composite materials that surface density is 110g/m2, which is placed in backing,
On target holder, by GA141-2010 testing standards, using 54 formula 7.62mm pistols, the test of 51 formula pistol lead for retractable pencil bullets, back lining materials are recessed
Depth ＜ 25mm are fallen into, the standard requirement of GA141-2010 is as a result met.About reduce 10% compared to weight before.Thus it demonstrate,proves
Bright, UHMWPE ballistic composites of the invention can largely reduce overall weight, improve the machinery of resin matrix
Performance obtains bulletproof effect preferably ballistic composite.After measured, 100% stretching strength is reachable for the modified resin of gained
25Mpa or so.This method principle is reliable, and preparation process is simple, and cost is relatively low, and controllability is strong, is suitble to large-scale production.
It is pre-processed in S1 and includes：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene powder:Second
Alcohol=1:5, coupling agent is according to the proportional arrangement coupling agent solution that mass concentration in a solvent is 10g/100ml, then by diameter
It it is 0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing, adds under stiring
Hot back flow reaction, the graphene after being coupled.
Select organochromium complexes, alkanes, titante coupling agent as coupling agent.
It is as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=
10:90 weight ratio mixes dispersant and resin under the conditions of high-speed stirred, and at room temperature, rotating speed 4000r/min connects cycle
Dispersant resin is made in condensed water after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, and 2h is stirred at 90 DEG C,
Graphene modified resin adhesive is made after mixing.
Dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin, phenolic aldehyde tree
Fat, polyacrylate or polymethacrylates.
Resin is Aqueous Polyurethane Adhesives in S2.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of graphene modified resin base ballistic composite, which is characterized in that include the following steps：
S1, graphene is pre-processed, makes the active functional group in its surface；
S2, graphene and adhesive are sufficiently mixed, it is made to be evenly distributed in resin, form graphene modified resin gluing
Agent；
S3, graphene modified resin adhesive is placed in glue groove, by reinforcement superhigh molecular weight polyethylene fibers in continuous lines
On uniformly sprawl, hauling speed 1-3m/min is set, is impregnated by resin under conditions of stringent control；
S4, it dries at 55-70 DEG C later, dry 8-10min, you can be made.
2. a kind of preparation method of graphene modified resin base ballistic composite according to claim 1, feature exist
In, in S1 pretreatment include：Graphene powder is dispersed under ultrasonication in alcohol solvent, graphene powder:Ethyl alcohol=
1:5, coupling agent, then will be a diameter of according to the proportional arrangement coupling agent solution that mass concentration in a solvent is 1g-10g/100ml
0.1 μm -300 μm, thickness is placed in coupling agent solution for the graphene of 0.5nm-5nm and carries out coupling processing, heats under stiring
Back flow reaction, the graphene after being coupled.
3. a kind of preparation method of graphene modified resin base ballistic composite according to claim 2, feature exist
In：Select organochromium complexes, alkanes, titante coupling agent as coupling agent.
4. a kind of preparation method of graphene modified resin base ballistic composite according to claim 1, feature exist
In being as follows in S2：
A1, dispersant resin is prepared：N-Methyl pyrrolidone (NMP) is selected to be used as dispersant, according to dispersant:Resin=1-
10:The weight ratio of 100-90 mixes dispersant and resin under the conditions of high-speed stirred, at room temperature, rotating speed 3000-4000r/
Min connects circulating condensing water, and dispersant resin is made after mixing；
A2, graphene modified resin is prepared：Graphene after coupling is mixed with dispersant resin, and 1-2h is stirred at 70-90 DEG C,
Graphene modified resin adhesive is made after mixing.
5. a kind of preparation method of graphene modified resin base ballistic composite according to claim 4, feature exist
In：Dispersant described in S2 is N-Methyl pyrrolidone (NMP), and resin is：Polyurethane, epoxy resin, phenolic resin, poly- third
Olefin(e) acid ester or polymethacrylates.
6. a kind of preparation method of graphene modified resin base ballistic composite according to claim 4, feature exist
In：Resin is Aqueous Polyurethane Adhesives in S2.
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| CN201810174732.0A CN108440941A (en) | 2018-03-02 | 2018-03-02 | A kind of preparation method of graphene modified resin base ballistic composite |
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| CN201810174732.0A CN108440941A (en) | 2018-03-02 | 2018-03-02 | A kind of preparation method of graphene modified resin base ballistic composite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220418A (en) * | 2019-06-21 | 2019-09-10 | 江西洪都航空工业集团有限责任公司 | A kind of composite material of microwell plate, microwell plate, light-duty bulletproof armour and preparation method thereof |
| CN110849215A (en) * | 2019-11-21 | 2020-02-28 | 北京航天雷特机电工程有限公司 | Graphene modified bulletproof composite non-woven fabric and preparation method thereof |
| WO2021092788A1 (en) * | 2019-11-13 | 2021-05-20 | 远景能源有限公司 | Method and apparatus for use in manufacturing graphene-modified fiber reinforced material |
-
2018
- 2018-03-02 CN CN201810174732.0A patent/CN108440941A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220418A (en) * | 2019-06-21 | 2019-09-10 | 江西洪都航空工业集团有限责任公司 | A kind of composite material of microwell plate, microwell plate, light-duty bulletproof armour and preparation method thereof |
| CN110220418B (en) * | 2019-06-21 | 2022-04-08 | 江西洪都航空工业集团有限责任公司 | Microporous plate composite material, microporous plate, light bulletproof armor and manufacturing method thereof |
| WO2021092788A1 (en) * | 2019-11-13 | 2021-05-20 | 远景能源有限公司 | Method and apparatus for use in manufacturing graphene-modified fiber reinforced material |
| CN110849215A (en) * | 2019-11-21 | 2020-02-28 | 北京航天雷特机电工程有限公司 | Graphene modified bulletproof composite non-woven fabric and preparation method thereof |
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Application publication date: 20180824 |