CN112959790A - Preparation method of high-performance plate cocoon composite material - Google Patents
Preparation method of high-performance plate cocoon composite material Download PDFInfo
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- CN112959790A CN112959790A CN202110228075.5A CN202110228075A CN112959790A CN 112959790 A CN112959790 A CN 112959790A CN 202110228075 A CN202110228075 A CN 202110228075A CN 112959790 A CN112959790 A CN 112959790A
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- cocoon
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- epoxy resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1207—Heat-activated adhesive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0012—Mechanical treatment, e.g. roughening, deforming, stretching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0036—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/0076—Curing, vulcanising, cross-linking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/08—Animal fibres, e.g. hair, wool, silk
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Fluid Mechanics (AREA)
- Thermal Sciences (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a preparation method of a high-performance plate cocoon composite material, which comprises the following steps: the method comprises the following steps: the silkworms spin in a two-dimensional plane by adjusting the silkworm cocooning environment; step two: plate cocoons with different areas, sizes and thicknesses are prepared by changing the number of the mature silkworms and the spinning time; step three: optimizing the cocoon shell structure by a hot pressing method; step four: and alternately laying the hot-pressed flat cocoon shells and the resin films and preparing the high-performance flat cocoon composite material by a hot pressing process. The invention utilizes the instinct of silkworm spinning to prepare the flat cocoon layer, adopts the flat cocoon layer with a natural cocoon layer structure as the reinforcement of the composite material, and can obtain the composite material with excellent mechanical property. The size and thickness of the plate cocoon can be adjusted by changing the number of the cooked silkworms and the spinning time, and the plate cocoon has compact structure after hot pressing, can be cut at will, is convenient to manufacture, and fully overcomes the defects of small volume, irregular shape and the like of the common silkworm cocoon.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of a high-performance plate cocoon composite material.
Background
Silkworm enters and develops special ability for spinning and cocooning to protect silkworm pupa through long-term natural selection process, so that the silkworm pupa is prevented from being invaded by predators, irradiation, moisture, germs and the like. The silkworm cocoon as an important protection device is a natural multi-layer structure composite material (the main components of the composite material are fibroin and sericin) with a porous microscopic structure, and the composite material has the advantages of being porous, comfortable, breathable, tough, environment-friendly, reproducible and excellent in impact resistance. However, the defects of small volume, irregular shape, uneven quality, irregular cocoon layer and the like of the silkworm cocoons seriously limit the deep research and development and large-scale application of the silkworm cocoons as protective structure materials.
The existing large amount of research is to prepare the toughened impact-resistant composite material by adopting the idea of compounding the silk obtained by the silk reeling process and the resin matrix, and a series of achievements with great effect are obtained. In the publication "Integrating the tussah silk and carbon fiber mixed as tough phase" disclosed in article No. 3786 of No. 10 of Nature communications journal in 2019, tussah silk and carbon fiber are used as tough phase to construct a series of high-strength and high-modulus epoxy resin-based composite materials, which are expected to be used as structural materials with high buffering and energy absorption requirements, such as military helmets. Ude in the publication "An experimental initiation on the response of the same in the atmospheric natural fiber/epoxy composite panel under low-level vacuum impact effect" of Ude et al, published in 2013, 127-132 of the journal of Fibers and Polymers, systematically studied the low-speed impact properties and failure mechanisms of a silk/epoxy resin laminate using An instrumented drop hammer test, which showed that the impact failure modes mainly included inter-layer matrix cracking, inter-layer debonding, delamination and fiber breakage. A study by Shah et al in the publication "Can side book an effective recovery of fiber A properties Composites with a flax and glass recovered Composites" published in 2014, the Composites Science & Technology journal, No. 101, page 173-183, shows that silk reinforced epoxy resin based Composites having a non-woven or plain weave structure possess superior impact resistance properties to flax reinforced epoxy resin based Composites.
However, the traditional silk reeling process thoroughly destroys the biological structure of the silkworm cocoons, and in the aspect of directly utilizing the silkworm cocoons to prepare the composite material product with special protective performance: in a preparation method of a high-strength silkworm cocoon structure composite material disclosed in 2017, the patent CN201710243121.2 of the Chinese invention discloses that Wang et al cut silkworm cocoons into square blocks, then splice the square blocks into complete large-area silkworm cocoon sheets, then lay the silkworm cocoon sheets in odd layers, finally apply an adhesive to the laminated material, and prepare the silkworm cocoon structure composite material with excellent mechanical properties by hot press molding; in a academic thesis published in 2015, "design and characterization of high-performance fiber/natural non-woven material composite product" Zhongxianxiang cuts natural tussah cocoons into strips, and then combines the strips with aramid fibers through a special "two-system warp" weaving means, so that the prepared cocoon/aramid composite product has good low-speed impact resistance, but has limited high-speed ballistic impact resistance. Because the traditional silkworm cocoons are limited in size, in the existing research of directly utilizing the silkworm cocoons to prepare the composite material, the silkworm cocoons have to be cut into strip-shaped, sheet-shaped or granular cocoon sheets, the methods cannot fully utilize the porous continuous biological structure and the excellent impact resistance characteristic of the natural silkworm cocoons, and the existing technology is to cut the natural silkworm cocoons and then splice the natural silkworm cocoons into plane cocoons, so that the operation is complex, the production efficiency is low, and the splicing of the plane cocoons is more due to the fact that the single silkworm cocoon is too small, and the performance of the joint is seriously influenced.
Disclosure of Invention
In order to overcome the problems, the invention provides a preparation method of a high-performance plate cocoon composite material.
The technical scheme adopted by the invention is as follows:
the preparation method of the high-performance plate cocoon composite material comprises the following steps:
the method comprises the following steps: after defecation, placing the mature five-instar silkworms on a two-dimensional silking flat plate for silking, and preparing flat plate cocoon sheets with different areas and thicknesses by changing the number of the mature silkworms and the silking time;
step two: carrying out hot-pressing treatment on the flat cocoon sheets to optimize the structure of the flat cocoon sheets;
step three: and (3) alternately laying the hot-pressed flat cocoon sheets and the resin films, and preparing the resin/flat cocoon composite material by a hot pressing process.
As one of the embodiments: the method specifically comprises the following steps:
the method comprises the following steps: cutting the obtained fluffy plate cocoons to the size of a hot-pressing die for hot pressing, wherein the hot-pressing environmental parameters are as follows: preheating for 30s at 80-130 deg.C under 4-12 MPa for 4-7 min;
step two: selecting epoxy resin and a curing agent thereof as matrix materials, and mixing the epoxy resin and the curing agent according to the ratio of 5: 1, uniformly mixing the components in a mass ratio, coating the mixture on the surface of a smooth polytetrafluoroethylene plate, putting the polytetrafluoroethylene plate into a vacuum machine for vacuumizing, taking out the polytetrafluoroethylene plate after vacuumizing until bubbles completely disappear, floating grooves caused by the air-exhausted bubbles, standing for 15-24 h, taking down a semi-cured epoxy resin thin layer, and cutting the semi-cured epoxy resin thin layer to the size of a hot-pressing mold for later use;
step three: sequentially and alternately putting the semi-cured epoxy resin thin layer and the hot-pressed flat cocoon layer into a hot-pressing die, putting into a vacuum hot-pressing machine, and performing hot-pressing environmental parameter: preheating for 30s at 100-150 deg.C under 10-15 MPa for 15-75 min, and hot-press molding;
step four: and (4) after the epoxy resin is fully cured by hot pressing, stopping heating the vacuum hot press, cooling, demoulding and taking out the test piece to obtain the high-performance plate cocoon composite material.
The invention has the following advantages:
1. according to the invention, through adjusting the silkworm cocoon forming environment, silkworms spin in a two-dimensional plane to prepare flat cocoons with different areas, sizes and thicknesses, the sizes and the thicknesses of the flat cocoons can be adjusted by changing the number of the cooked silkworms and the spinning time, and the flat cocoons are fluffy and soft in structure, can be cut at will, are convenient to manufacture, fully overcome the defects of small volume, irregular shape, uneven cocoon layers and the like of the silkworm cocoons, simultaneously preserve the natural structure of the silkworm cocoons, are not required to be spliced after cutting because the silkworm directly spins the silk, have excellent mechanical properties and are uniformly distributed, and solve the problem that the performance of the silkworm cocoons is influenced by splicing in the prior art;
2. the hot-pressed flat cocoon shell and resin film are alternatively laid, and the hot-pressing method is used for preparing the high-performance flat cocoon composite material with a laminated structure.
Detailed Description
The present invention will be further described below, but the present invention is not limited to these.
Example 1
The preparation method of the high-performance plate cocoon composite material comprises the following steps:
the method comprises the following steps: cutting the obtained fluffy plate cocoons to the size of a hot-pressing die for hot-pressing for standby, wherein the hot-pressing environmental parameters are as follows: preheating for 30s at 80-130 deg.C under 4-12 MPa for 4-7 min;
step two: selecting epoxy resin E51 as a matrix material, and mixing the epoxy resin E51 and a curing agent T31 according to the weight ratio of 5: 1, uniformly mixing the components in a mass ratio, coating the mixture on the surface of a smooth polytetrafluoroethylene plate, putting the polytetrafluoroethylene plate into a vacuum machine for vacuumizing, taking out the polytetrafluoroethylene plate after vacuumizing until bubbles completely disappear, floating grooves caused by the air-exhausted bubbles, standing for 15-24 h, taking down a semi-cured epoxy resin thin layer, and cutting the semi-cured epoxy resin thin layer to the size of a hot-pressing mold for later use;
step three: alternately putting the epoxy resin thin layer and the hot-pressed flat cocoon layer into a hot-pressing mould in sequence, wherein the number of stacked layers is as follows: 3+2 or 9+8, placing the mixture into a vacuum-pumping hot-pressing forming machine, wherein the hot-pressing environmental parameters are as follows: preheating for 30s at 100-150 deg.C under 10-15 MPa for 15-75 min, and hot-press molding;
step four: and (4) after the epoxy resin is fully cured by hot pressing, stopping heating the vacuum hot press, cooling, demoulding and taking out the test piece to obtain the high-performance plate cocoon composite material.
The thickness of the composite material obtained in the embodiment is 2mm, the width is 20mm, the measured length is 80mm, the volume content of plate cocoons is about 20-25%, the average tensile strength is 40MPa, and the epoxy resin matrix with the same size is about 20 MPa.
The composite material obtained in this embodiment had a thickness of 10mm, a width of 4mm, a notch depth of 2mm, an average impact strength of 55J/m and an epoxy matrix of about 23J/m with the same dimensions.
It is noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (7)
1. The preparation method of the high-performance plate cocoon composite material is characterized by comprising the following steps of: the method comprises the following steps:
the method comprises the following steps: after defecation, placing the mature five-instar silkworms on a two-dimensional silking flat plate for silking, and preparing flat plate cocoon sheets with different areas and thicknesses by changing the number of the mature silkworms and the silking time;
step two: carrying out hot-pressing treatment on the flat cocoon sheets to optimize the structure of the flat cocoon sheets;
step three: and alternately laying the hot-pressed flat cocoon shells and the resin films, and preparing the resin/flat cocoon composite material by a hot pressing process.
2. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: the two-dimensional spinning flat plate is a flat plate cocoon sheet with a fluffy structure and a rough surface.
3. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: the hot-pressing conditions of the plate cocoons are that the temperature is 80-130 ℃, the pressure is 4-12 MPa, the time is 4-7 min, and the plate cocoons are preheated for 30 s.
4. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: the resin film is prepared by mixing epoxy resin and curing agent according to the ratio of 5: 1, coating the mixture on the surface of a smooth polytetrafluoroethylene plate after uniformly mixing, putting the polytetrafluoroethylene plate into a vacuum machine for vacuumizing, taking out the polytetrafluoroethylene plate after bubbles disappear completely, floating grooves caused by the air bubbles, standing the epoxy resin thin layer, taking the epoxy resin thin layer out, and cutting the epoxy resin thin layer to the size of a hot pressing mold for later use.
5. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: the epoxy resin film is semi-cured and molded under the condition of standing for 15-24 hours at the temperature of 25 ℃.
6. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: the stacking mode of the semi-cured epoxy resin thin layer and the hot-pressed flat cocoon layer is interactive stacking, wherein the epoxy resin film is arranged on the outer layer, and the number of layers of the interactive stacking of the epoxy resin and the flat cocoon layer comprises 3+2, 4+3, …, 15+14 and the like, and is changed according to the thickness of the required composite material.
7. The method for preparing a high-performance plate cocoon composite material according to claim 1, characterized in that: stacking the epoxy resin and the plate cocoons, and then putting the stacked epoxy resin and plate cocoons into a die for hot pressing, wherein the hot pressing process parameters are as follows: the temperature is 100-150 ℃, the pressure is 10-15 MPa, the time is 15-75 minutes, and the preheating is carried out for 30 s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110228075.5A CN112959790A (en) | 2021-03-02 | 2021-03-02 | Preparation method of high-performance plate cocoon composite material |
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| CN202110228075.5A CN112959790A (en) | 2021-03-02 | 2021-03-02 | Preparation method of high-performance plate cocoon composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234246A (en) * | 2021-07-01 | 2021-08-10 | 西南大学 | Preparation method of graphene/plate cocoon toughened carbon fiber composite material |
| CN114043754A (en) * | 2021-11-08 | 2022-02-15 | 盐城工业职业技术学院 | Processing method of planar cocoon high-pressure internal-permeation composite membrane material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103129042A (en) * | 2013-01-30 | 2013-06-05 | 广东生益科技股份有限公司 | Carbon fiber base fabric composite material and preparation method and application thereof |
| CN110818923A (en) * | 2019-11-15 | 2020-02-21 | 北京航空航天大学 | Preparation method of natural mulberry/tussah silk fabric reinforced epoxy resin composite material |
| CN111607196A (en) * | 2020-06-28 | 2020-09-01 | 浙江大学 | Method for enhancing anti-tearing performance of polymer membrane material by utilizing planar silkworm cocoon and composite membrane material thereof |
-
2021
- 2021-03-02 CN CN202110228075.5A patent/CN112959790A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103129042A (en) * | 2013-01-30 | 2013-06-05 | 广东生益科技股份有限公司 | Carbon fiber base fabric composite material and preparation method and application thereof |
| CN110818923A (en) * | 2019-11-15 | 2020-02-21 | 北京航空航天大学 | Preparation method of natural mulberry/tussah silk fabric reinforced epoxy resin composite material |
| CN111607196A (en) * | 2020-06-28 | 2020-09-01 | 浙江大学 | Method for enhancing anti-tearing performance of polymer membrane material by utilizing planar silkworm cocoon and composite membrane material thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234246A (en) * | 2021-07-01 | 2021-08-10 | 西南大学 | Preparation method of graphene/plate cocoon toughened carbon fiber composite material |
| CN114043754A (en) * | 2021-11-08 | 2022-02-15 | 盐城工业职业技术学院 | Processing method of planar cocoon high-pressure internal-permeation composite membrane material |
| CN114043754B (en) * | 2021-11-08 | 2024-05-21 | 盐城工业职业技术学院 | Processing method of plane cocoon high-pressure inner-permeation composite membrane material |
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Application publication date: 20210615 |