CN113912997A - Modified corn straw fiber reinforced PBS (Poly Butylene succinate) composite material and preparation method thereof - Google Patents
Modified corn straw fiber reinforced PBS (Poly Butylene succinate) composite material and preparation method thereof Download PDFInfo
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- CN113912997A CN113912997A CN202111325354.XA CN202111325354A CN113912997A CN 113912997 A CN113912997 A CN 113912997A CN 202111325354 A CN202111325354 A CN 202111325354A CN 113912997 A CN113912997 A CN 113912997A
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- 240000008042 Zea mays Species 0.000 title claims abstract description 264
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 264
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 264
- 235000005822 corn Nutrition 0.000 title claims abstract description 264
- 239000010902 straw Substances 0.000 title claims abstract description 180
- 239000000835 fiber Substances 0.000 title claims abstract description 141
- 229920002961 polybutylene succinate Polymers 0.000 title claims abstract description 94
- 239000004631 polybutylene succinate Substances 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- -1 Poly Butylene succinate Polymers 0.000 title claims abstract description 10
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 32
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 32
- 239000000314 lubricant Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims description 69
- 238000001035 drying Methods 0.000 claims description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- 238000002791 soaking Methods 0.000 claims description 36
- 238000009210 therapy by ultrasound Methods 0.000 claims description 33
- 238000005406 washing Methods 0.000 claims description 31
- 239000003513 alkali Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 230000008878 coupling Effects 0.000 claims description 7
- 238000010168 coupling process Methods 0.000 claims description 7
- 238000005859 coupling reaction Methods 0.000 claims description 7
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 239000002023 wood Substances 0.000 abstract description 4
- 229920001587 Wood-plastic composite Polymers 0.000 abstract description 2
- 239000004566 building material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000011155 wood-plastic composite Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract 1
- 229920003023 plastic Polymers 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 36
- 230000000704 physical effect Effects 0.000 description 22
- 239000011347 resin Substances 0.000 description 22
- 229920005989 resin Polymers 0.000 description 22
- 239000011159 matrix material Substances 0.000 description 21
- 238000005303 weighing Methods 0.000 description 20
- 238000004140 cleaning Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 18
- 229910021641 deionized water Inorganic materials 0.000 description 18
- 238000012986 modification Methods 0.000 description 11
- 230000004048 modification Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000002028 Biomass Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
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- 239000002154 agricultural waste Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZMKVBUOZONDYBW-UHFFFAOYSA-N 1,6-dioxecane-2,5-dione Chemical compound O=C1CCC(=O)OCCCCO1 ZMKVBUOZONDYBW-UHFFFAOYSA-N 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a corn straw fiber reinforced PBS straw-plastic composite material and a preparation method thereof, belonging to the technical field of biodegradable composite materials. Solves the environmental problems caused by wood shortage and straw burning of the existing wood-plastic composite material. The composite material comprises the following components in percentage by weight: 60-95% of Poly Butylene Succinate (PBS), 40-5% of Modified Corn Straw Fiber (MCSF), 0-1% of lubricant and 0-1% of antioxidant. The corn stalk fiber reinforced PBS composite material is safe, nontoxic, biodegradable and excellent in mechanical property, can be applied to the fields of packaging, furniture, aerospace, various plates, automotive interiors, building materials and the like, and has a good market prospect.
Description
Technical Field
The invention belongs to the technical field of biodegradable composite materials, and particularly relates to a biodegradable modified corn straw fiber reinforced PBS composite material and a preparation method thereof.
Background
Nowadays, in order to improve environmental pollution and get rid of dependence on petroleum resources, the development of biodegradable polymer materials is a research hotspot of numerous researchers. Among them, wood-plastic composite materials have attracted much attention, and such materials are widely used in the fields of packaging, furniture, various boards, automotive interiors, building materials, and the like because of having the advantages of low cost, no abrasion, biodegradability, renewability, good mechanical properties, and the like. However, along with the gradual shortage of forest resources and the environmental problems caused by excessive chopping and cutting, the replacement of wood by straw becomes a new development trend. In the field of traditional natural fiber reinforced polymers, the selection of biomass feedstocks has gradually shifted from wood resources to agricultural wastes (including rice hulls, corn stover, peanut hulls, wheat straw, and other wastes). The agricultural residues are large in quantity, short in growth period, wide in distribution and easy to process, and the biomass is an excellent biomass resource for replacing wood. China is a traditional agricultural big country, and the annual output of various crop straws reaches about 9 hundred million tons according to estimation, the annual output of Corn Straws (CSF) also reaches 2.4 hundred million tons, but the utilization rate is less than 30 percent. A large amount of corn straws are not reasonably and effectively applied for a long time, most of the corn straws are treated in a local burying or burning mode, and only a small amount of corn straws are used for producing feed. This not only causes waste of a large amount of biomass resources, but also causes a serious problem of air pollution, and does not meet the requirements of sustainable development. The corn stalk fiber is selected as the reinforcing material, so that the material is convenient to obtain, the source is wide, and the price is low. Polybutylene succinate (PBS) is an aliphatic polyester with great development potential, has the advantages of complete biodegradability, no toxicity, no harm, good comprehensive performance and the like, but has the defects of high cost, low melt strength, low crystallization rate, poor toughness and the like of the PBS, so that the further application of the PBS is limited. Therefore, the PBS/corn straw fiber composite material with excellent performance is prepared, and has certain economic benefit for effectively utilizing corn straws while expanding the application field of PBS.
Disclosure of Invention
The invention aims to provide a modified corn straw fiber reinforced PBS composite material and a preparation method thereof. In order to achieve the above purpose, the invention provides the following technical scheme:
the invention firstly provides a modified corn straw fiber reinforced PBS composite material, which comprises the following components in percentage by weight: 60-95% polybutylene succinate; 40-5% of modified corn straw fiber; 0-1% of a lubricant; 0-1% of antioxidant.
Wherein the modified corn stalk fiber comprises the following components in percentage by weight: 95-99% of corn straw fiber and 5-1% of silane coupling agent;
preferably, the preparation method of the modified corn stalk fiber comprises the following steps:
(1) crushing corn straws into 100 meshes, adding the crushed corn straws into alkali liquor for soaking treatment, performing ultrasonic treatment (ultrasonic treatment is performed for 50min at the temperature of 60 ℃), then washing to be neutral, and drying for 12 hours at the temperature of 80 ℃ to obtain pretreated corn straws;
(2) preparing a silane coupling agent hydrolysis solution in advance, adding the pretreated corn straw into the silane coupling agent hydrolysis solution, carrying out magnetic stirring treatment, and drying to obtain the modified corn straw fiber. The drying was carried out at 80 ℃ for 12 hours.
Preferably, the silane coupling agent is selected from one or more of KH550, KH560, KH570, KH580, VTES, VTS and the like;
preferably, the concentration of the self-made alkali liquor is 3-7%, and the proportion of the corn straws to the alkali liquor is 1: (4-12), and the soaking time is 2-7 hours.
Preferably, the concentration of the silane coupling agent-ethanol aqueous solution is 1-5%; the proportion of the corn straw to the silane coupling agent-ethanol aqueous solution is 1: (4-12), soaking in the silane coupling agent-ethanol aqueous solution for 2-7 hours.
Preferably, the lubricant is selected from one or more of sodium stearate, zinc stearate and calcium stearate.
Preferably, the antioxidant is selected from one or more of antioxidant 2112, antioxidant 1076 and antioxidant 1010.
The invention also provides a preparation method of the modified corn straw fiber reinforced PBS composite material, which comprises the following steps: and (3) carrying out melt blending on the polybutylene succinate, the modified corn straw fiber, the lubricant and the antioxidant to obtain the PBS/corn straw composite material.
Preferably, the melt blending temperature is 150 ℃, and the melt blending time is 5-12 min.
The invention has the advantages of
The invention firstly provides a modified corn straw fiber reinforced PBS composite material, which comprises the following components in percentage by weight: 60-95% polybutylene succinate; 40-5% of modified corn straw fiber; 0-1% of a lubricant; 0-1% of antioxidant. Wherein the modified corn stalk fiber comprises the following components in percentage by weight: 95-99% of corn straw fiber and 5-1% of silane coupling agent; compared with the prior art, the modified corn straw fiber is modified by the alkali liquor and the silane coupling agent together, so that the modified corn straw fiber can be uniformly dispersed in the PBS matrix resin, the interfacial tension is reduced, the compatibility of two phases is improved, the interfacial binding force is improved, and the processing is convenient. Therefore, the composite material has good toughness and rigidity, and the experimental result shows that: the impact strength of the composite material can reach 60J/m, the tensile strength can reach 45MPa, and the modulus can reach 1422 MPa.
The invention also provides a preparation method of the modified corn straw fiber reinforced PBS composite material, the preparation method has simple process and easily obtained raw materials, and the prepared composite material is safe, non-toxic, biodegradable and excellent in mechanical property.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The invention firstly provides a modified corn straw fiber reinforced PBS composite material, which comprises the following components in percentage by weight: 60-95% of poly (butylene succinate), preferably 70-92%, more preferably 80-90%; 40-5% of modified corn straw fiber, preferably 30-8%, more preferably 20-10%; 0-1% lubricant, preferably 0.3-0.7%, more preferably 0.5%; 0-1% of antioxidant, preferably 0.3-0.7%, more preferably 0.5%.
Wherein the modified corn stalk fiber comprises the following components in percentage by weight: 95-99% of corn stalk fiber, preferably 96-98%, more preferably 97%; 5-1% of a silane coupling agent, preferably 4-2%, more preferably 3%.
The PBS resin according to the present invention is a commercial product commonly used by those skilled in the art, and the corn stalks are agricultural wastes.
The preparation method of the modified corn stalk fiber according to the invention preferably comprises the following steps:
(1) crushing corn straws into 100 meshes, adding the crushed corn straws into alkali liquor for soaking treatment, performing ultrasonic treatment (ultrasonic treatment is performed for 50min at the temperature of 60 ℃), then washing to be neutral, and drying for 12 hours at the temperature of 80 ℃ to obtain pretreated corn straws;
(2) preparing a silane coupling agent hydrolysis solution in advance, adding the pretreated corn straw into the silane coupling agent hydrolysis solution, carrying out magnetic stirring treatment, and drying to obtain the modified corn straw fiber. The drying was carried out at 80 ℃ for 12 hours.
According to the invention, the silane coupling agent is preferably one or more of gamma-aminopropyltriethoxysilane (KH 550), gamma-glycidoxypropyltrimethoxysilane (KH 560), gamma-methacryloxypropylsilane (KH 570), gamma-mercaptopropyltriethoxysilane (KH 580), Vinyltriethoxysilane (VTES), Vinyltrimethoxysilane (VTS) and the like;
according to the invention, the concentration of the self-made alkali liquor is preferably 3-7%, more preferably 4-6%, and more preferably 5%; the preferable proportion of the corn straws to the alkali liquor is 1: (4-12), more preferably 1: (6-10), more preferably 1: 8; the soaking time in the alkali liquor is 2-7h, more preferably 3-6h, and more preferably 4 h.
According to the present invention, the concentration of the silane coupling agent-ethanol aqueous solution is preferably 1 to 5%, more preferably 2 to 4%, and still more preferably 3%; the proportion of the corn straw to the silane coupling agent-ethanol aqueous solution is preferably 1: (4-12), more preferably 1: (6-10), more preferably 1: 8; the soaking time in the silane coupling agent-ethanol aqueous solution is 2-7h, more preferably 3-6h, and even more preferably 4 h.
According to the invention, the lubricant is preferably one or more of sodium stearate, zinc stearate and calcium stearate.
According to the invention, the antioxidant is preferably one or more of antioxidant 2112, antioxidant 1076 and antioxidant 1010.
The invention also provides a preparation method of the modified corn straw fiber reinforced PBS composite material, which comprises the following steps:
and (3) carrying out melt blending on the polybutylene succinate, the modified corn straw fiber, the lubricant and the antioxidant to obtain the PBS/corn straw composite material. The melt blending temperature is preferably 150 ℃, and the melt blending time is preferably 5-12 min.
The present invention will be further illustrated in detail by the following examples, but it should be noted that these examples should not be construed as limiting the scope of the present invention in any way.
Example 1
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 2
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
weighing 95 parts by weight of PBS matrix resin, 5 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 3
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
weighing 85 parts of PBS matrix resin, 15 parts of modified corn straw fiber and 0.5 part of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 4
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
weighing 80 parts by weight of PBS matrix resin, 20 parts by weight of modified corn straw fiber, and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 5
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of corn straw fibers to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning the corn stalk fiber, washing with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH570 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH570 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 6
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of corn straw fibers to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a VTES ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the VTES ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 7
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 6. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 8
Preparing modified corn stalk fiber:
firstly, crushing corn stalk fibers into 100-mesh particles, drying the crushed corn stalks, and then putting the dried crushed corn stalks into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of the corn stalks to the alkali liquor is 1: 10. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 9
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 2%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 10
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 7%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 3%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 11
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 1%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 12
Preparing modified corn stalk fiber:
firstly, crushing corn straws into 100-mesh particles, drying the crushed corn straws, and then putting the dried crushed corn straws into alkali liquor (with the concentration of 5%) for soaking ultrasonic treatment, wherein the weight ratio of the corn straws to the alkali liquor is 1: 8. performing ultrasonic treatment (ultrasonic treatment at 60 deg.C for 50min), soaking for 4 hr, cleaning corn stalk with clear water for 5-6 times to ensure clean surface of corn stalk, washing with deionized water, drying at 80 deg.C for 12 hr. And then putting the pretreated corn straws into a KH560 ethanol solution (with the concentration of 5%) for soaking modification treatment, wherein the weight ratio of the corn straws to the KH560 ethanol solution is 1: 8. and simultaneously stirring for 4 hours, then cleaning the modified corn straws, washing for 5-6 times by using clean water to ensure that the surfaces of the corn straws are clean, finally washing for one time by using deionized water, putting the cleaned corn straws into drying equipment, setting the drying temperature to be 80 ℃, and drying for 12 hours to obtain the modified corn straw fibers.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 13
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
weighing 75 parts by weight of PBS matrix resin, 25 parts by weight of modified corn straw fiber, and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 14
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
weighing 70 parts of PBS matrix resin, 30 parts of modified corn straw fiber and 0.5 part of antioxidant and lubricant by weight respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 15
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
and weighing 60 parts by weight of PBS matrix resin, 40 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 16
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 5min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 17
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 12min, thus obtaining the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 18
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin and 10 parts by weight of modified corn straw fiber, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
Example 19
Preparing modified corn stalk fiber:
same as in example 1.
Preparing a PBS/corn stalk fiber composite material:
and weighing 90 parts by weight of PBS matrix resin, 10 parts by weight of modified corn straw fiber and 0.5 part by weight of antioxidant and lubricant respectively, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS/corn straw fiber composite material. The physical properties of the composite material are shown in Table 1.
TABLE 1 physical Properties of composites made in examples 1-16
| Serial number | PBS/RH(wt/wt) | Impact Strength (J/m) | Tensile Strength (MPa) | Modulus (MPa) |
| Example 1 | 90/10 | 54 | 35 | 656 |
| Example 2 | 95/5 | 48 | 32 | 547 |
| Example 3 | 85/15 | 49 | 36 | 945 |
| Example 4 | 80/20 | 46 | 40 | 1057 |
| Example 5 | 90/10 | 44 | 30 | 624 |
| Example 6 | 90/10 | 43 | 29 | 637 |
| Example 7 | 90/10 | 52 | 30 | 633 |
| Example 8 | 90/10 | 51 | 29 | 610 |
| Example 9 | 90/10 | 45 | 28 | 587 |
| Example 10 | 90/10 | 52 | 32 | 591 |
| Example 11 | 90/10 | 46 | 27 | 574 |
| Example 12 | 90/10 | 48 | 30 | 630 |
| Example 13 | 75/25 | 43 | 43 | 1321 |
| Example 14 | 70/30 | 42 | 45 | 1244 |
| Example 15 | 60/40 | 40 | 46 | 1362 |
| Example 16 | 90/10 | 52 | 33 | 611 |
| Example 17 | 90/10 | 53 | 34 | 648 |
| Example 18 | 90/10 | 52 | 33 | 646 |
| Example 19 | 90/10 | 53 | 34 | 651 |
Comparative example 1
And weighing 100 parts by weight of PBS matrix resin, and carrying out melt blending, wherein the mixing temperature is fixed at 150 ℃, and the mixing time is 7min, so as to obtain the PBS material. The physical properties of the composite material are shown in Table 2.
TABLE 2 physical Properties of PBS
| Serial number | PBS | Impact Strength (J/m) | Tensile Strength (MPa) | Modulus (MPa) |
| Comparative example 1 | 100 | 42 | 24 | 421 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and modifications and variations thereof within the spirit and scope of the invention will be apparent to those skilled in the art.
Claims (11)
1. The modified corn stalk fiber reinforced PBS composite material and the preparation method thereof are characterized by comprising the following components in percentage by weight:
60-95% polybutylene succinate;
40-5% of modified corn straw fiber;
0-1% of a lubricant;
0-1% of antioxidant;
the modified corn straw fiber comprises the following components in percentage by weight: 95-99% of corn straw fiber and 5-1% of silane coupling agent;
the preparation method of the modified corn stalk fiber comprises the following steps: (1) adding corn straws into alkali liquor, soaking, washing to be neutral after ultrasonic treatment, and drying to obtain pretreated corn straws; (2) preparing a silane coupling agent hydrolysis solution in advance, adding the pretreated corn straw into the silane coupling agent hydrolysis solution, performing magnetic stirring treatment, and drying to obtain modified corn straw fiber;
the preparation method of the modified corn stalk fiber reinforced PBS composite material comprises the following steps: and (3) melting and blending the polybutylene succinate, the modified corn straw fiber, the lubricant and the antioxidant to prepare the PBS/corn straw fiber composite material.
2. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the concentration of the homemade alkali solution is 3-7%, and the ratio of the corn stalk to the alkali solution is 1: (4-12), soaking for 2-7 hours, and performing ultrasonic treatment at 60 ℃ for 50 min.
3. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the drying temperature of the corn stalk treated by the alkali solution is 80 ℃ and the drying time is 12 hours.
4. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the ratio of the corn stalk to the silane coupling agent-ethanol aqueous solution is 1: (4-12), and the soaking time is 2-7 hours.
5. The method for preparing the modified corn stalk fiber reinforced PBS composite material according to claim 1, wherein the silane coupling agent is selected from one or more of gamma-aminopropyl triethoxysilane (KH 550), gamma-glycidoxypropyl trimethoxysilane (KH 560), gamma-methacryloxypropyl silane (KH 570), gamma-mercaptopropyl triethoxysilane (KH 580), Vinyltriethoxysilane (VTES), Vinyltrimethoxysilane (VTS), etc.
6. The method for preparing the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the size of the crushed corn stalk is 100 meshes.
7. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the lubricant is selected from one or more of sodium stearate, zinc stearate and calcium stearate.
8. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the antioxidant is selected from one or more of antioxidant 2112, antioxidant 1076 and antioxidant 1010.
9. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the drying temperature of the modified corn stalk fiber is 80 ℃ and the drying time is 12 hours.
10. The preparation method of the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the melt blending time is 5-12 min.
11. The method for preparing the modified corn stalk fiber reinforced PBS composite material as claimed in claim 1, wherein the melt blending temperature is 150 ℃.
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| CN103289334A (en) * | 2013-07-02 | 2013-09-11 | 河南省科学院同位素研究所有限责任公司 | Straw fiber/PBS (Poly Butylene Succinate) composite material based on radiation modification and preparation method thereof |
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