CN116215044A - Basalt fabric polybutylene succinate composite board and preparation method thereof - Google Patents

Basalt fabric polybutylene succinate composite board and preparation method thereof Download PDF

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Publication number
CN116215044A
CN116215044A CN202310384079.1A CN202310384079A CN116215044A CN 116215044 A CN116215044 A CN 116215044A CN 202310384079 A CN202310384079 A CN 202310384079A CN 116215044 A CN116215044 A CN 116215044A
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basalt
polybutylene succinate
fabric
composite board
fiber
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李莺
孙世元
张志娟
詹建朝
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Jiaxing University
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Jiaxing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/36Layered products comprising a layer of synthetic resin comprising polyesters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/12Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/08Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the cooling method
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10Methods 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered 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
    • B32B5/02Layered 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10Inorganic fibres
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

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  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention provides a basalt fabric polybutylene succinate composite board and a preparation method thereof, and belongs to the technical field of composite material preparation. The invention ultrasonically cleans basalt fiber with acetone solution, then cleans and dries with deionized water, separates into single fiber, then carries out plasma treatment to obtain modified basalt fabric, then lays the modified basalt fabric in a hot-pressing mould in a warp-weft crossing mode, lays 8 layers, lays a layer of polybutylene succinate film between every two layers, preheats and presses for 1 minute at 118 ℃ and 2.5MPa, and then adjusts the temperature to 120 ℃ and hot presses for 10 minutes to prepare the composite board. The basalt fabric polybutylene succinate composite board prepared by the method is formed at one time, does not need to be compounded layer by layer, can be completely degraded, has no harm to the environment, and has the strength as high as 235.5MPa.

Description

Basalt fabric polybutylene succinate composite board and preparation method thereof
The application is a divisional application of a patent application named basalt fabric reinforced polybutylene succinate composite material plate preparation method, and the application date of the original application is 2021, 03 and 06, and the application number is 202110247800.3.
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a basalt fabric polybutylene succinate composite board and a preparation method thereof.
Background
The polybutylene succinate is obtained by condensation polymerization of succinic acid and butanediol, is easy to be decomposed and metabolized by enzymes in animals and plants or microorganisms in nature, has excellent biodegradability and good processability, has tensile strength between polyethylene and polypropylene and rigidity between low-density polyethylene and high-density polyethylene, and is a very promising biodegradable high polymer material. However, since the polybutylene succinate has low strength, the application range is greatly limited, and therefore, the polybutylene succinate must be modified.
The basalt fiber is a high-performance fiber, has strength higher than that of the E glass fiber and slightly lower than that of the S glass fiber, has excellent high temperature resistance, good electrical insulation and good sound insulation, is an environment-friendly material, and can be directly degraded in soil, so that the basalt fiber is widely applied to the fields of water body treatment, heat insulation and temperature resistance, aerospace, transportation, petrochemical industry, automobiles, ships and the like. But basalt fiber is inorganic mineral fiber, has very smooth surface, is chemically inert, lacks active oxygen-containing groups, has poor surface hydrophilicity, and limits the application field.
At present, basalt fibers and polybutylene succinate are compounded into fully-degradable plates with very good performances in all aspects.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the basalt fabric polybutylene succinate composite board and the preparation method thereof, and the composite board prepared by the method is formed at one time, does not need to be composited layer by layer, can be completely degraded, has no harm to the environment, and has the strength as high as 235.5MPa.
The aim of the invention is achieved by the following technical scheme:
the invention provides a preparation method of a basalt fabric polybutylene succinate composite board, which comprises the following steps:
(1) Film formation of polybutylene succinate
(2) Modification
Firstly, ultrasonically cleaning basalt fibers by using an acetone solution, then cleaning and drying by using deionized water, and then separating into single fibers; then carrying out plasma treatment on the basalt single fiber for 60s with the power of 200-300W, and obtaining modified basalt fabric after the treatment;
(3) Laying down
Laying the modified basalt fabric in a hot-pressing die in a warp-weft crossing mode, laying 8 layers, laying a layer of polybutylene succinate film between every two layers, wherein the volume content of the modified basalt fiber is 30-35%;
(4) Hot pressing
Firstly, the temperature is increased to 118 ℃, the pressure is set to 2.5MPa, the resin is preheated after 1 minute of heat preservation, then the temperature is increased to 120 ℃, and the heat preservation is carried out for 10 minutes;
(5) Cooling and demoulding
The basalt fabric polybutylene succinate composite board is formed at one time, does not need to be compounded layer by layer, can be completely degraded, has no harm to the environment, and has the strength as high as 235.5MPa.
Preferably, the basalt fiber in the step (2) is a desized basalt fiber.
The acetone in the step (2) may be other organic solvents or a mixed solvent of several organic solvents. The drying adopts equipment such as a baking oven and the like.
Preferably, the plasma treatment in the step (2) is performed by using a radio frequency plasma generator.
Preferably, the plasma treatment in the step (2) adopts the following method: fixing the basalt single fiber on a paper frame, placing the paper frame in a plasma processing chamber, and turning on a radio frequency power supply and an automatic radio frequency matcher to perform plasma processing.
Preferably, in the step (4), a stainless steel spacer plate with a certain thickness is placed between two pressing plates of a hot pressing mold to ensure that a composite material plate with a consistent thickness is obtained, and polyimide is used as release paper. The stainless steel can also be replaced by other hard materials; the polyimide can also be replaced by release paper made of other materials.
The invention also provides the basalt fabric polybutylene succinate composite board manufactured by the method.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method provided by the invention can be used for manufacturing the basalt reinforced polybutylene succinate composite material with the strength of up to 235.5MPa, and the obtained reinforced composite material plate has the advantage of high strength of the basalt reinforced composite material, can be recycled, and belongs to an environment-friendly material.
2. The invention adopts hot press molding, and has the advantages of short molding time, simple molding process and manufacturing process. The process parameters can be accurately controlled and adjusted at any time. Furthermore, the hot pressing process of the invention comprises a preheating process and a forming process, so that the product quality can be further improved.
3. The invention adopts the woven fabric as the reinforcing material, and the strength is obviously improved, especially in the direction of warp and weft yarns. In addition, the direction of the fabric can be adjusted according to the requirements, so that the plate has the characteristic of anisotropic strength, and the designability of the composite material is improved.
4. The basalt fabric is woven by adopting basalt fibers modified by hydrophilic plasmas. Through a simpler reaction system, the surface of basalt fiber is modified by utilizing radio frequency plasma, and the hydrophilicity of the basalt fiber is increased through the effects of etching the surface of the basalt fiber, introducing active oxygen-containing groups and the like.
5. Compared with other basalt fiber modification methods, the modification method adopted by the invention has the following advantages: (1) the modification method only modifies the surface of the fiber, and has no damage to the strength of the fiber; (2) the modification time is relatively short, and the operation is simple and convenient; (3) the oxygen element with extremely high proportion is introduced in the plasma modification process, so that the hydrophilicity of the fiber is obviously improved.
6. According to the invention, the modified basalt fabric is laid in the hot-pressing die according to the one-time layer by layer with the polybutylene succinate film, so that layer-by-layer compounding and one-time molding are not needed, and the time, labor, energy and other costs are greatly saved.
Drawings
FIG. 1 is a surface topography of a first embodiment of the present invention;
FIG. 2 is a surface topography of a second embodiment of the present invention;
FIG. 3 is a surface topography of a third embodiment of the present invention;
FIG. 4 is a surface topography of a fourth embodiment of the present invention;
FIG. 5 is a surface topography of a comparative example of the present invention;
FIG. 6 is a graph of filament strength statistics for a first embodiment of the present invention;
FIG. 7 is a statistical plot of the strength of single fibers of embodiment two of the present invention;
FIG. 8 is a statistical plot of the strength of single fibers of embodiment three of the present invention;
FIG. 9 is a statistical plot of the strength of single fibers of example four of the present invention;
FIG. 10 is a statistical plot of the strength of the filaments of the comparative example of the present invention;
FIG. 11 is a statistical plot of the water droplet absorption time of the present invention;
FIG. 12 is a diagram of chemical element composition of basalt fiber according to an embodiment of the present invention;
FIG. 13 is a diagram of the chemical element composition of basalt fiber according to the second embodiment of the present invention;
FIG. 14 is a chemical element composition diagram of basalt fiber of example three of the present invention;
FIG. 15 is a chemical element composition diagram of basalt fiber of example four of the present invention;
FIG. 16 is a chemical element composition diagram of basalt fiber of comparative example of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples, which, however, do not limit the scope of the invention. Further, any modification of the present invention by those skilled in the relevant art will be equivalent to those falling within the scope of the present invention as defined in the appended claims, without departing from the spirit of the present invention.
Basalt fibers used in the embodiments of the present invention were purchased from Zhejiang gold basalt fiber limited.
The plasma equipment used in the invention is a radio frequency plasma generator manufactured by Chinese sciences and having the model number of RFG-1000.
The matcher used in the invention is an automatic radio frequency matcher manufactured by Chinese sciences and having the model number of RFM-1000.
The tensile strength of the invention was tested using a universal tester, test standard reference GB/T1447-2005.
Preparation of modified basalt fiber
Example 1
Fixing basalt fibers on a paper frame, placing the paper frame in a plasma processing chamber, turning on a radio frequency power supply and an automatic radio frequency matcher, setting the processing power of plasma to be 50W, setting the processing time to be 60S, automatically stopping a plasma device after processing, taking out the paper frame, and putting the paper frame into a clean sample bag to complete the processing. The basalt fiber with very smooth surface morphology, single fiber strength statistics value of 4397Mpa, surface oxygen element content of 41.59%, water drop absorption time of 29.3S and hydrophilicity enhancement is obtained.
Example two
Fixing basalt fibers on a paper frame, placing the paper frame in a plasma processing chamber, turning on a radio frequency power supply and an automatic radio frequency matcher, setting the processing power of plasma to be 100W, setting the processing time to be 60s, automatically stopping a plasma device after the processing is finished, taking out the paper frame, and putting the paper frame into a clean sample bag to finish the processing. The basalt fiber with the surface Xu Cucao, the single fiber strength statistical value of 4716MPa, the surface oxygen element content of 44.31 percent, the water drop absorption time of 17.3S and the hydrophilicity enhanced is obtained.
Example III
Fixing basalt fibers on a paper frame, placing the paper frame in a plasma processing chamber, turning on a radio frequency power supply and an automatic radio frequency matcher, setting the processing power of plasma to be 200W, setting the processing time to be 60s, automatically stopping a plasma device after the processing is finished, taking out the paper frame, and putting the paper frame into a clean sample bag to finish the processing. The basalt fiber with increased surface particles, single fiber strength statistics of 4322MP, surface oxygen element content of 53.53%, water drop absorption time of 4.6S and hydrophilicity is obtained.
Example IV
Fixing basalt fibers on a paper frame, placing the paper frame in a plasma processing chamber, turning on a radio frequency power supply and an automatic radio frequency matcher, setting the processing power of plasma to 300W, processing time to 60s, automatically stopping a plasma device after processing is completed, taking out the paper frame, and placing the paper frame into a clean sample bag to complete the processing. The basalt fiber with increased surface particles, single fiber strength statistics of 4421MPa, surface oxygen element content of 53.14%, water drop absorption time of 3.2S and hydrophilicity is obtained.
Comparative examples
The basalt fiber is measured to have very smooth surface morphology, surface oxygen element content of 33.74%, water drop absorption time of 60.4S and single fiber strength statistic value of 4415MPa without plasma treatment.
The chemical element composition table of basalt fiber implemented above is shown in the following table
Figure BDA0004173246810000051
1-16, compared with the comparative examples, the surface roughness of the basalt fiber after treatment is obviously increased, the statistical value of the single fiber strength is not obviously different, the oxygen element content is obviously increased, the water drop absorption time is obviously reduced, and the hydrophilicity is obviously increased.
Preparation of basalt fabric reinforced polybutylene succinate composite material plate
Example five
The basalt woven fabric is respectively paved in a hot-pressing die according to the set paving angles and the layer number, 8 layers are paved in the embodiment, and the warp-weft crossed paving is adopted. The volume content of basalt fiber is 31%. And paving a polybutylene succinate film between adjacent layers of fabrics. During hot pressing, the temperature is firstly increased to 118 ℃, the pressure is 2.5MPa, the resin is preheated after 1 minute of heat preservation, and then the temperature is increased to 120 ℃ and the heat preservation is carried out for 10 minutes. And finally, cooling the pressed composite material plate to room temperature and demolding to obtain the basalt fabric polybutylene succinate composite plate. Through detection, the strength of the basalt fabric reinforced polybutylene succinate composite board is 223.7MPa.
Example six
The basalt woven fabric is respectively paved in a hot-pressing die according to the set paving angles and the layer number, 8 layers are paved in the embodiment, and the warp-weft crossed paving is adopted. The volume content of basalt fiber is 35%. And paving a polybutylene succinate film between every two layers of fabrics. During hot pressing, the temperature is firstly increased to 118 ℃, the pressure is 2.5MPa, the resin is preheated after 1 minute of heat preservation, and then the temperature is increased to 120 ℃ and the heat preservation is carried out for 10 minutes. And finally, cooling the pressed composite material plate to room temperature and demolding to obtain the basalt fabric polybutylene succinate composite plate. Through detection, the strength of the basalt fabric reinforced polybutylene succinate composite board is 235.5MPa.
Example seven
The basalt woven fabric is respectively paved in a hot-pressing die according to the set paving angles and the layer number, 8 layers are paved in the embodiment, and the warp-weft crossed paving is adopted. The volume content of basalt fiber is 38%. And paving a polybutylene succinate film between every two layers of fabrics. During hot pressing, the temperature is firstly increased to 118 ℃, the pressure is 2.5MPa, the resin is preheated after 1 minute of heat preservation, and then the temperature is increased to 120 ℃ and the heat preservation is carried out for 10 minutes. And finally, cooling the pressed composite material plate to room temperature and demolding to obtain the basalt fabric polybutylene succinate composite plate. Through detection, the strength of the basalt fabric reinforced polybutylene succinate composite board is 221.7MPa.
Example eight
The basalt woven fabric is respectively paved in a hot-pressing die according to the set paving angles and the layer number, 8 layers are paved in the embodiment, and the warp-weft crossed paving is adopted. The volume content of basalt fiber was 41%. And paving a polybutylene succinate film between every two layers of fabrics. During hot pressing, the temperature is firstly increased to 118 ℃, the pressure is 2.5MPa, the resin is preheated after 1 minute of heat preservation, and then the temperature is increased to 120 ℃ and the heat preservation is carried out for 10 minutes. And finally, cooling the pressed composite material plate to room temperature and demolding to obtain the basalt fabric polybutylene succinate composite plate. Through detection, the strength of the basalt fabric reinforced polybutylene succinate composite board is 216.8MPa.
Therefore, the strength of the basalt fabric polybutylene succinate composite board manufactured by the method is at least more than 200MPa and is up to 235.5MPa.

Claims (6)

1. The preparation method of the basalt fabric polybutylene succinate composite board is characterized by comprising the following steps of:
(1) Film formation of polybutylene succinate
(2) Modification
Firstly, ultrasonically cleaning basalt fibers by using an acetone solution, then cleaning and drying by using deionized water, and then separating into single fibers; then carrying out plasma treatment on the basalt single fiber for 60s with the power of 200-300W, and obtaining modified basalt fabric after the treatment;
(3) Laying down
Laying the modified basalt fabric in a hot-pressing die in a warp-weft crossing mode, laying 8 layers, laying a layer of polybutylene succinate film between every two layers, wherein the volume content of the modified basalt fiber is 30-35%;
(4) Hot pressing
Firstly, the temperature is increased to 118 ℃, the pressure is set to 2.5MPa, the resin is preheated after 1 minute of heat preservation, then the temperature is increased to 120 ℃, and the heat preservation is carried out for 10 minutes;
(5) Cooling and demoulding
The basalt fabric polybutylene succinate composite board is formed at one time, does not need to be compounded layer by layer, can be completely degraded, has no harm to the environment, and has the strength as high as 235.5MPa.
2. The method of claim 1, wherein the basalt fibers of step (2) are desized basalt fibers.
3. The method of claim 2, wherein the plasma treatment in step (2) is performed using a radio frequency plasma generator.
4. A method according to claim 3, wherein the plasma treatment in step (2) is performed by: fixing the basalt single fiber on a paper frame, placing the paper frame in a plasma processing chamber, and turning on a radio frequency power supply and an automatic radio frequency matcher to perform plasma processing.
5. The method according to claim 4, wherein a stainless steel spacer plate having a certain thickness is placed between two pressing plates of a hot pressing mold at the time of hot pressing in the step (4) to ensure that a composite plate having a uniform thickness is obtained, and polyimide is used as a release paper.
6. A basalt fabric polybutylene succinate composite board prepared by the preparation method of any one of claims 1 to 5.
CN202310384079.1A 2021-03-06 2021-03-06 Basalt fabric polybutylene succinate composite board and preparation method thereof Withdrawn CN116215044A (en)

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