CN110982226B - Structured high-elasticity buffer composite resin material and preparation method thereof - Google Patents
Structured high-elasticity buffer composite resin material and preparation method thereof Download PDFInfo
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- CN110982226B CN110982226B CN201911279707.XA CN201911279707A CN110982226B CN 110982226 B CN110982226 B CN 110982226B CN 201911279707 A CN201911279707 A CN 201911279707A CN 110982226 B CN110982226 B CN 110982226B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/24—Homopolymers or copolymers of amides or imides
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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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
Abstract
The invention relates to a structured high-elasticity buffer composite resin material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) preparing a PDMA hydrogel reinforcement material; (2) cutting and structural design of the hydrogel material; (3) modifying the epoxy resin material; (4) and (3) carrying out composite treatment on the hydrogel shearing structure and the epoxy resin system. The hydrogel material is compounded with the modified epoxy resin by virtue of high elasticity of the hydrogel material and structural cutting design, and the prepared modified epoxy resin-based composite material combines the advantages of the hydrogel and the epoxy resin material, and has high elasticity, self-repairing performance, high strength and related mechanical properties. The invention can be realized in the field with great demand on elastic performance, such as automobile bumpers and the like.
Description
Technical Field
The invention relates to the field of preparation of high polymer materials, in particular to a structured high-elasticity buffer composite resin material and a preparation method thereof.
Background
The elastic buffer material is one of indispensable materials in aerospace, automobile industry, electronic industry and instruments and meters. The requirement of the shock absorption and buffering function of the bumper in the automobile industry is particularly important. The existing automobile bumper has a certain buffering effect when an automobile collides, but the protection force for passengers in the automobile at high speed is still insufficient, more than 90% of the materials of the automobile bumper in China are PP plastics, and the automobile bumper has a certain protection effect when bearing impact. The existing bumper can play a role in buffering protection, but the buffer effect is limited, the expected target cannot be achieved, the protection effect is poor for the collision with large force, the bumper is easy to damage after the collision, and the self-repairing and self-healing capability is not available. Few structural modifications of the cushioning material region in combination with other high elastomers have been made to achieve a highly resilient cushioning composite system. The invention utilizes the high elasticity behavior of the hydrogel, and realizes the characteristics of high elasticity, high strength and automatic recovery after being pressed after being compounded with resin by carrying out structural design on the hydrogel, so as to meet the application of shock absorption and impact resistance occasions in the fields of automobile industry, instruments, aviation and the like.
Disclosure of Invention
The invention aims to compound the hydrogel material with modified epoxy resin by virtue of high elasticity of the hydrogel material through structural cutting design, and the prepared modified epoxy resin-based composite material combines the advantages of the hydrogel and the epoxy resin material, and not only has high elasticity and self-repairing performance, but also has high strength and related mechanical properties. The invention can be realized in the field with great demand on elastic performance, such as automobile bumpers and the like.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of the structured high-elasticity buffer composite resin material comprises the following steps:
(1) preparing a PDMA hydrogel reinforcement material;
(2) cutting and structural design of the hydrogel material;
(3) modifying the epoxy resin material;
(4) carrying out composite treatment on the hydrogel shearing structure and the epoxy resin system;
the epoxy resin material is modified by adopting the following raw materials in percentage by weight: epoxy resin E5130.32-38.60%, polyamide resin HB-12524.46-30.87%, n-butanol 7.65-9.71%, xylene 20.94-28.13%, 50 mesh crystalline flake graphite powder 1.74-13.76%, tributyl phosphate 0.275-0.35%, and other auxiliary agents 0.275-0.35%.
In the step (1), firstly, 2.0-2.2 parts by mass of ammonium dodecyl sulfate and 0.86-0.88 part by mass of NaCl are weighed and dissolved in a proper amount of H at normal temperature2Adding 0.28-0.32 parts by mass of octadecyl methacrylate into O, and magnetically stirring in a 35 ℃ water bath for 3-4 hours; adding N, N-dimethylacrylamide, stirring and reacting for 1-2 h; then adding 0.22-0.24 parts by mass of an initiator KPS and an accelerant TEMED, stirring uniformly, transferring the solution obtained by the reaction into a glass test tube, carrying out thermal initiation at 50 ℃, and carrying out polymerization reaction for 12-13h to obtain the PDMA hydrogel reinforcement material.
In step (1), the mass/volume ratio of ammonium lauryl sulfate to N, N-dimethylacrylamide is 0.43-0.53 (g/mL).
In the step (2), the prepared PDMA hydrogel reinforcement material is taken out and cut into a plurality of equal-height small cylindrical columns with the length of 1.1-1.3 cm; or cutting into strips 8.3-8.5cm long and 0.7-0.8cm wide and rectangular sheets 2.5-2.6cm long and 0.7-0.8cm wide, and arranging the strips and rectangular sheets at the spacing layer.
In the step (3), firstly, mixing n-butanol and xylene to prepare a mixed solvent, then weighing an additive, namely crystalline flake graphite, adding the additive into the mixed solvent, and treating the solution added with the crystalline flake graphite for 1 hour by using a homogenizer to obtain a mixed homogenate; and then weighing the epoxy resin E51, the defoaming agent tributyl phosphate and the silane coupling agent, adding the epoxy resin E51, the defoaming agent tributyl phosphate and the silane coupling agent into the mixed homogenate, uniformly stirring, then adding the curing agent polyamide resin HB-125, uniformly mixing and stirring, standing and curing for 30min to obtain the graphite flake modified epoxy resin-based material.
In the step (4), firstly, uniformly pouring the epoxy resin material matrix emulsion on the bottom layer of the mould, and heating at 90 ℃ for slight curing for 15-20 min; then respectively arranging the cut hydrogel on the slightly cured emulsion layer, uniformly covering the hydrogel matrix with the epoxy resin material matrix emulsion, and heating at 90 ℃ for 5-10 min; covering the rest epoxy resin material matrix emulsion on the outermost layer, heating at 90 ℃ for 2-3h, and finally placing in an oven for drying.
Compared with the prior art, the invention has the beneficial effects that:
the internal structure of the structured high-elasticity buffer composite resin material prepared by the invention adopts a hydrogel system, so that the total mass of the system is reduced, the weight of a vehicle body can be directly reduced, and the oil consumption is reduced.
Secondly, the structural high-elasticity buffer composite resin material prepared by the invention has higher rigidity, adopts resin curing materials, can ensure no deformation under small impact, and can keep certain mechanical properties in large impact.
The structured high-elasticity buffer composite resin material prepared by the invention has certain toughness, the matrix deforms when the material bears impact, and the hydrogel has high elasticity and self-repairing function, so that the maintenance cost is reduced.
The resin and hydrogel layer of the cured structured high-elasticity buffer composite resin material prepared by the invention is softer, and the high elasticity of the hydrogel plays an obvious buffer role when the material collides with pedestrians, so that the injury to the pedestrians is reduced.
Drawings
FIG. 1 shows a columnar hydrogel arranged in an epoxy material.
FIG. 2 shows the rectangular strips of hydrogel interleaved in the epoxy material.
FIG. 3 shows the structural arrangement of different hydrogels.
Detailed Description
The present invention will be further described with reference to the following specific examples.
(1) And (3) preparing an elastic hydrogel material. The preparation process of reinforced PDMA hydrogel material includes weighing Ammonium Dodecyl Sulfate (ADS) in 2.1g and NaCl in 0.878g dissolved in 25mLH at normal temperature2O, 0.30g of Stearyl Methacrylate (SMA) is added, and the mixture is placed in a 35 ℃ water bath and stirred magnetically for 3 hours. 4.4mL of N, N-dimethylacrylamide (DMAAm) was added, and the reaction was stirred for 1 to 2 hours. Then, 0.23g of the initiator KPS and 120. mu.L of the accelerant TEMED were added and stirred uniformly. Transferring the solution obtained by the reaction into a glass test tube with the diameter of 13mm, thermally initiating at 50 ℃, and carrying out polymerization reaction for 12h to prepare the PDMA hydrogel reinforcement material.
(2) Cutting and structural design of the hydrogel. This aspect allows for shearing and alignment of the hydrogel structure in the manner of the alignment of figure 3. The prepared PDMA hydrogel was taken out of the test tube, cut into a strip-shaped sheet having a length of 8.4cm and a width of 0.7cm, and arranged.
(3) And (5) modifying the epoxy resin material. The preparation method relates to the preparation of a diluent and the preparation of an epoxy resin matrix, and comprises the following specific operations:
firstly, mixing n-butanol (8.00%) and xylene (25.33%) to prepare a mixed solvent of 10 g; and preparing mixed homogenate of the graphite flake, weighing 50 meshes of the graphite flake according to 25% of the mass fraction of the mixed solvent, and treating the mixed solvent added with the graphite flake for 1h by using a refiner to obtain the mixed homogenate.
Secondly, weighing epoxy resin E5113.36g, a plurality of antifoaming agents tributyl phosphate and silane coupling agents according to the prepared mixed homogenate and epoxy resin ratio of 1:1, adding the weighed epoxy resin E5113.36g, the antifoaming agents tributyl phosphate and the silane coupling agents into the mixed homogenate, uniformly stirring, then adding 10.048g of curing agents (polyamide resin HB-125) with the mass fraction of 80% of the total mass of the epoxy resin, uniformly mixing and stirring, standing and curing for 30min, and preparing the graphite flake modified epoxy resin base material.
(4) And (3) carrying out composite treatment on the hydrogel shearing structure and the epoxy resin system. Firstly, uniformly pouring an epoxy resin material matrix emulsion on a bottom layer of a mould, and slightly curing for 15min by heating at 90 ℃; then respectively arranging the cut hydrogel on the slightly cured emulsion layer, as shown in figure 3, uniformly covering the hydrogel matrix with the epoxy resin material matrix emulsion, and heating at 90 ℃ for 5-10 min; covering the rest epoxy resin material matrix emulsion on the outermost layer, heating at 90 ℃ for 2h, and finally placing in an oven for drying.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (2)
1. A structured high-elasticity buffer composite resin material is characterized in that: the preparation method comprises the following steps:
(1) preparing a PDMA hydrogel reinforcement material;
(2) cutting and structural design of the hydrogel material;
(3) modifying the epoxy resin material;
(4) carrying out composite treatment on the hydrogel shearing structure and the epoxy resin system;
the epoxy resin material is modified by adopting the following raw materials in percentage by weight: epoxy resin E5130.32-38.60%, polyamide resin HB-12524.46-30.87%, n-butanol 7.65-9.71%, xylene 20.94-28.13%, 50 mesh crystalline flake graphite powder 1.74-13.76%, tributyl phosphate 0.275-0.35%, and other auxiliary agents 0.275-0.35%;
in the step (1), firstly, 2.0-2.2 parts by mass of ammonium dodecyl sulfate and 0.86-0.88 part by mass of NaCl are weighed and dissolved in a proper amount of H at normal temperature2Adding 0.28-0.32 parts by mass of octadecyl methacrylate into O, and magnetically stirring in a 35 ℃ water bath for 3-4 hours; adding N, N-dimethylacrylamide, and stirring to react for 1-2 h; then adding 0.22-0.24 parts by mass of an initiator KPS and an accelerant TEMED, uniformly stirring, transferring the solution obtained by reaction into a glass test tube, carrying out thermal initiation at 50 ℃, and carrying out polymerization reaction for 12-13h to obtain the PDMA hydrogel reinforcement material;
in the step (2), the prepared PDMA hydrogel reinforcement material is taken out and cut into a plurality of equal-height small cylindrical columns with the length of 1.1-1.3 cm; or cutting into strips 8.3-8.5cm long and 0.7-0.8cm wide and rectangular sheets 2.5-2.6cm long and 0.7-0.8cm wide, and arranging the strips and rectangular sheets according to the spacing layer;
in the step (3), firstly, mixing n-butanol and xylene to prepare a mixed solvent, then weighing additive flake graphite powder, adding the additive flake graphite powder into the mixed solvent, and treating the solution added with the flake graphite powder for 1h by using a homogenizer to obtain a mixed homogenate; then weighing epoxy resin E51, a defoaming agent tributyl phosphate and a silane coupling agent, adding the epoxy resin E51, the defoaming agent tributyl phosphate and the silane coupling agent into the mixed homogenate, uniformly stirring, then adding curing agent polyamide resin HB-125, uniformly mixing and stirring, standing and curing for 30min to obtain epoxy resin material matrix emulsion;
in the step (4), firstly, uniformly pouring the epoxy resin material matrix emulsion on the bottom layer of the mould, and heating at 90 ℃ for slight curing for 15-20 min; then respectively arranging the cut hydrogel on the slightly cured emulsion layer, uniformly covering the hydrogel matrix with the epoxy resin material matrix emulsion, and heating at 90 ℃ for 5-10 min; covering the rest epoxy resin material matrix emulsion on the outermost layer, heating at 90 ℃ for 2-3h, and finally placing in an oven for drying.
2. The structured high elastic cushioning composite resin material of claim 1, wherein: in the step (1), the mass/volume ratio of the ammonium dodecyl sulfate to the N, N-dimethylacrylamide is 0.43-0.53 g/mL.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104861755A (en) * | 2015-05-11 | 2015-08-26 | 哈尔滨工程大学 | Novel hydrogel anti-fouling coating preparation method |
| WO2017116598A1 (en) * | 2015-12-30 | 2017-07-06 | The Regents Of The University Of Michigan | Gels and nanocomposites containing aramid nanofibers |
| CN110358004A (en) * | 2019-07-08 | 2019-10-22 | 南京信息工程大学 | A kind of Intelligent Composite hydrogel of doped graphene and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104861755A (en) * | 2015-05-11 | 2015-08-26 | 哈尔滨工程大学 | Novel hydrogel anti-fouling coating preparation method |
| WO2017116598A1 (en) * | 2015-12-30 | 2017-07-06 | The Regents Of The University Of Michigan | Gels and nanocomposites containing aramid nanofibers |
| CN110358004A (en) * | 2019-07-08 | 2019-10-22 | 南京信息工程大学 | A kind of Intelligent Composite hydrogel of doped graphene and preparation method thereof |
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