CN102585531A - Lignin-epoxy resin composite material and preparation method thereof - Google Patents
Lignin-epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN102585531A CN102585531A CN2011104174282A CN201110417428A CN102585531A CN 102585531 A CN102585531 A CN 102585531A CN 2011104174282 A CN2011104174282 A CN 2011104174282A CN 201110417428 A CN201110417428 A CN 201110417428A CN 102585531 A CN102585531 A CN 102585531A
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Abstract
The invention discloses a lignin-epoxy resin composite material and a preparation method thereof, relates to a lignin-polymer composite material and a preparation method thereof, and aims to solve the conventional problem of low effective utilization rate of lignin. The lignin-epoxy resin composite material uses the lignin as a substrate; epoxy resin, a curing agent, a toughening agent, and the like are evenly blended with the lignin; and through the processes of pre-pressing, hot-pressing and curing molding, the lignin-based composite material is obtained. The lignin-epoxy resin composite material disclosed by the invention has the advantages of little water absorption, good mechanical performance, degradability, and the like, is suitable for manufacturing floor boards, wall protection boards, construction formworks, door-window profiles, fences, guardrails, louvers, roof boards, and the like in the construction industry, can be used for manufacturing inner decorative boards of automobile doors, seat backing boards, automobile roof lining, and the like in the automobile industry, and can also be used in the fields of the packaging and transportation industry, the furniture industry, office articles, sports facilities, and the like.
Description
Technical field
The present invention relates to xylogen-polymer composites and preparation method thereof.
Background technology
Xylogen is that occurring in nature content is only second to cellulosic second largest renewable resources, and is annual with 5 * 10
10The speed regeneration of t is a kind of organic raw material that is rich in commercial value.In Mierocrystalline cellulose related industries (like plant hydrolyzed and pulp and paper industry); Xylogen is usually with a large amount of outputs of the form of by product; But up to the present; The recovery of the separating lignin above 95% is burnt after concentrating, and causes the significant wastage of resource on the one hand, and the discharging that contains the xylogen trade effluent on the other hand also can cause serious detrimentally affect to environment.Xylogen is effectively utilized, environment protection and Economic development are all had positive meaning.
It is one of effective ways that xylogen is made full use of that xylogen and polymer blending are prepared advanced composite material; But the blending amount of xylogen is less in the prepared composite material at present, generally is lower than 50%, in addition; Mostly the polymkeric substance that is adopted is the high molecule plastic of low-pole; And xylogen polarity is strong, and has stronger intramolecularly and intermolecular ydrogen bonding, and the polymer property of itself and low-pole differs greatly; Thereby this matrix material exists interface bonded defective, thereby influences its use properties.
Summary of the invention
The present invention will solve the existing low problem of xylogen effective rate of utilization.
A kind of xylogen-epoxy resin composite material of the present invention is to be processed by 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies.
Wherein, described xylogen is industrial lignin, high purity xylogen, alkali lignin or high-boiling alcohol lignin; Described epoxy resin is bisphenol A type epoxy resin, brominated bisphenol a type epoxy resin, amino four glycidyl epoxy resins, PARA AMINOPHENOL three-glycidyl epoxy resin or phenol aldehyde type epoxy resin; Described solidifying agent is polymeric amide 200#, polymeric amide 400#, polyamide 6 51#, polymeric amide 203#, kymene 00# or polyamide 6 00#; Described toughner is thiorubber, paracril, copolymer nylon, polyvinyl acetal, urethane, low molecular polyamides, epoxidized SBS or epoxidation pyridyl SBS; Described toughener is silica powder, mica powder, talcum powder, lime carbonate, permanent white, WHITE CARBON BLACK, nano silicon, nano titanium oxide, nano zine oxide, nano zircite, nano-sized iron oxide, Nano titanate, nano-carbide, nano nitride, nano aluminium oxide, thomel, xylon, hemp fibre, bamboo fibers, spun glass, tossa, flax fiber, sisal fibers or monkey grass.
The preparation method of xylogen-epoxy resin composite material of the present invention carries out according to the following steps: one, take by weighing 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies; Two, the xylogen that step 1 is taken by weighing carries out drying treatment 3～12h under 90 ℃～120 ℃ temperature; Three, dried xylogen mixes 30min～60min in the epoxy resin that step 1 is taken by weighing, solidifying agent, toughner, toughener and the step 2, promptly gets mixture; Four, the mixture that step 3 is obtained is put into thermocompressor, and hot-pressing processing is carried out in first precompressed then, promptly gets matrix material; Five, the matrix material that makes in the step 4 is carried out after fixing 1～2h, promptly get xylogen-epoxy resin composite material; Wherein, step 3 is described to mix, and mixing velocity is 20～40rpm, and mixing temperature is 20 ℃～30 ℃; The described precompressed of step 4 is handled, and pressure is 2～6MPa, and squeeze time is 10～20min, and the precompressed temperature is 40 ℃～50 ℃; The described hot-pressing processing of step 4, pressure are 6～20MPa, and hot pressing temperature is 50 ℃～60 ℃, and hot pressing time is the THICKNESS CALCULATION of the matrix material of four gained set by step, and every millimeter keeps 3～5min; The described after fixing temperature of step 5 is 70 ℃～100 ℃.
The present invention utilizes xylogen to do main body material (content surpasses 50%), through compound with strong polar thermosetting epoxy resin, and preparation xylogen-epoxy resin composite material, thus realize that xylogen efficiently utilizes.
The present invention is base material with the xylogen, and through forming matrix material with blend such as epoxy resin, this matrix material not only has the mechanical property that satisfies general operational requirement, can process different shape easily through hot pressing again simultaneously, processes easy.Have complementary advantages through composite modified making between the differing materials; And obtain the different performance of matrix material through the content of regulating each composition; Make it have good heat-resisting, anti-uv-ray; HS, high rigidity and degradable performance etc. can be widely used in the every field of daily life.
Specific embodiments
Specify the present invention below in conjunction with specific examples.Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of xylogen-epoxy resin composite material of this embodiment is to be processed by 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies.
This embodiment is base material with the xylogen, and through forming matrix material with blend such as epoxy resin, this matrix material not only has the mechanical property that satisfies general operational requirement, can process different shape easily through hot pressing again simultaneously, processes easy.Have complementary advantages through composite modified making between the differing materials; And obtain the different performance of matrix material through the content of regulating each composition; Make it have good heat-resisting, anti-uv-ray; HS, high rigidity and degradable performance etc. can be widely used in the every field of daily life.
Embodiment two: what this embodiment and embodiment one were different is: described xylogen is industrial lignin, high purity xylogen, alkali lignin or high-boiling alcohol lignin.Other is identical with embodiment one.
The industrial lignin of this embodiment, alkali lignin, high purity xylogen and high-boiling alcohol lignin are the commercially available prod.
Embodiment three: what this embodiment and embodiment one to two were different is: described epoxy resin is bisphenol A type epoxy resin, brominated bisphenol a type epoxy resin, amino four glycidyl epoxy resins, PARA AMINOPHENOL three-glycidyl epoxy resin or phenol aldehyde type epoxy resin.Other is identical with embodiment one to two.
Embodiment four: what this embodiment was different with one of embodiment one to three is: described solidifying agent is polymeric amide 200#, polymeric amide 400#, polyamide 6 51#, polymeric amide 203#, kymene 00# or polyamide 6 00#.Other is identical with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is: described toughner is thiorubber, paracril, copolymer nylon, polyvinyl acetal, urethane, low molecular polyamides, epoxidized SBS or epoxidation pyridyl SBS.Other is identical with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is: described toughener is a silica powder; Mica powder; Talcum powder; Lime carbonate; Permanent white; WHITE CARBON BLACK; Nano silicon; Nano titanium oxide; Nano zine oxide; Nano zircite; Nano-sized iron oxide; Nano titanate; Nano-carbide; Nano nitride; Nano aluminium oxide; Thomel; Xylon; Hemp fibre; Bamboo fibers; Spun glass; Tossa; Flax fiber; Sisal fibers or monkey grass.Other is identical with one of embodiment one to five.
Embodiment seven: the preparation method of the xylogen-epoxy resin composite material of this embodiment carries out according to the following steps: one, take by weighing 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies; Two, the xylogen that step 1 is taken by weighing carries out drying treatment 3～12h under 90 ℃～120 ℃ temperature; Three, dried xylogen mixes 30min～60min in the epoxy resin that step 1 is taken by weighing, solidifying agent, toughner, toughener and the step 2, promptly gets mixture; Four, the mixture that step 3 is obtained is put into thermocompressor, and hot-pressing processing is carried out in first precompressed then, promptly gets matrix material; Five, the matrix material that makes in the step 4 is carried out after fixing 1～2h, promptly get xylogen-epoxy resin composite material; Wherein, step 3 is described to mix, and mixing velocity is 20～40rpm, and mixing temperature is 20 ℃～30 ℃; The described precompressed of step 4 is handled, and pressure is 2～6MPa, and squeeze time is 10～20min, and the precompressed temperature is 40 ℃～50 ℃; The described hot-pressing processing of step 4, pressure are 6～20MPa, and hot pressing temperature is 50 ℃～60 ℃, and hot pressing time is the THICKNESS CALCULATION of the matrix material of four gained set by step, and every millimeter keeps 3～5min; The described after fixing temperature of step 5 is 70 ℃～100 ℃.
This embodiment utilizes xylogen to do main body material (content surpasses 50%), through compound with strong polar thermosetting epoxy resin, and preparation xylogen-epoxy resin composite material, thus realize that xylogen efficiently utilizes.
This embodiment is base material with the xylogen, and through forming matrix material with blend such as epoxy resin, this matrix material not only has the mechanical property that satisfies general operational requirement, can process different shape easily through hot pressing again simultaneously, processes easy.Have complementary advantages through composite modified making between the differing materials; And obtain the different performance of matrix material through the content of regulating each composition; Make it have good heat-resisting, anti-uv-ray; HS, high rigidity and degradable performance etc. can be widely used in the every field of daily life.
Embodiment eight: this embodiment and embodiment seven are different: described the mixing of step 3 is in kneader or mill, to carry out.Other is identical with embodiment seven.
Through following verification experimental verification effect of the present invention:
Test 1:
Prepare xylogen-epoxy resin composite material through following steps: one, take by weighing the high Vinsol of 60g, the bisphenol A type epoxy resin of 60g and the polymeric amide 200# of 48g; Two, the high Vinsol that step 1 is taken by weighing carries out drying treatment 3h under 120 ℃ of temperature; Three, the dried high Vinsol of the bisphenol A type epoxy resin that step 1 is taken by weighing, polymeric amide 200# and step 2 puts into kneader, with the rotating speed of 20rpm, under 30 ℃ of temperature, mixes 40min, promptly gets material; Four, the material that step 3 is obtained is put into thermocompressor, is 2MPa at pressure, and temperature is under 50 ℃ the condition, and 10min is handled in precompressed; After precompressed is handled, be 8MPa at pressure, temperature is under 60 ℃ the condition, to carry out hot-pressing processing 20min, promptly gets matrix material, and the thickness of matrix material is 4.8mm; Five, matrix material that step 4 is hot-forming carries out after fixing 1h under 85 ℃ of temperature, promptly get xylogen-epoxy resin composite material.
The high Vinsol of this test buys from Songyuan Laihe Chemicals Co., Ltd..
Wherein epoxy resin adopts bisphenol A type epoxy resin, and oxirane value is 0.51.
Xylogen-epoxy resin composite material that this test is obtained carries out the sample Mechanics Performance Testing: flexural strength on CMT6104 microcomputer control electronics universal testing machine according to the GB/T9341-2000 standard testing; According to the GB/T1043-93 standard testing, density is according to the GB/T17657-1999 standard test on XJJ-50 charpy impact test machine for shock strength; The result sees table 1.
Test 2:
Prepare xylogen-epoxy resin composite material through following steps: one, take by weighing the high Vinsol of 90g, the bisphenol A type epoxy resin of 60g and the polymeric amide 200# of 48g; Two, the high Vinsol that step 1 is taken by weighing carries out drying treatment 3h under 120 ℃ of temperature; Three, the dried high Vinsol of the bisphenol A type epoxy resin that step 1 is taken by weighing, polymeric amide 200# and step 2 puts into kneader, with the rotating speed of 20rpm, under 30 ℃ of temperature, mixes 40min, promptly gets material; Four, the material that step 3 is obtained is put into thermocompressor, is 2MPa at pressure, and temperature is under 50 ℃ the condition, and 10min is handled in precompressed; After precompressed is handled, be 8MPa at pressure, temperature is under 60 ℃ the condition, to carry out hot-pressing processing 20min, promptly gets matrix material, and the thickness of matrix material is 5.4mm; Five, matrix material that step 4 is hot-forming carries out after fixing 1h under 85 ℃ of temperature, promptly get xylogen-epoxy resin composite material.
The high Vinsol of this test buys from Songyuan Laihe Chemicals Co., Ltd..
Wherein epoxy resin adopts bisphenol A type epoxy resin, and oxirane value is 0.51.
Xylogen-epoxy resin composite material that this test is obtained carries out the sample Mechanics Performance Testing: flexural strength on CMT6104 microcomputer control electronics universal testing machine according to the GB/T9341-2000 standard testing; According to the GB/T1043-93 standard testing, density is according to the GB/T17657-1999 standard test on XJJ-50 charpy impact test machine for shock strength.The result sees table 1.
Test 3:
Prepare xylogen-epoxy resin composite material through following steps: one, take by weighing the high Vinsol of 90g, the bisphenol A type epoxy resin of 60g and the polymeric amide 200# of 48g; Two, the high Vinsol that step 1 is taken by weighing carries out drying treatment 3h under 120 ℃ of temperature; Three, the dried high Vinsol of the bisphenol A type epoxy resin that step 1 is taken by weighing, polymeric amide 200# and step 2 puts into kneader, with the rotating speed of 20rpm, under 30 ℃ of temperature, mixes 40min, promptly gets material; Four, the material that step 3 is obtained is put into thermocompressor, is 2MPa at pressure, and temperature is under 50 ℃ the condition, and 10min is handled in precompressed; After precompressed is handled, be 6MPa at pressure, temperature is under 60 ℃ the condition, to carry out hot-pressing processing 20min, promptly gets matrix material, and the thickness of matrix material is 5.3mm; Five, matrix material that step 4 is hot-forming carries out after fixing 1h under 85 ℃ of temperature, promptly get xylogen-epoxy resin composite material.
The high Vinsol of this test buys from Songyuan Laihe Chemicals Co., Ltd..
Wherein epoxy resin adopts bisphenol A type epoxy resin, and oxirane value is 0.51.
Xylogen-epoxy resin composite material that this test is obtained carries out the sample Mechanics Performance Testing: flexural strength on CMT6104 microcomputer control electronics universal testing machine according to the GB/T9341-2000 standard testing; According to the GB/T1043-93 standard testing, density is according to the GB/T17657-1999 standard test on XJJ-50 charpy impact test machine for shock strength.The result sees table 1.
Test 4:
Prepare xylogen-epoxy resin composite material through following steps: one, take by weighing the high Vinsol of 90g, the bisphenol A type epoxy resin of 60g, the polymeric amide 200# of 36g and the thiorubber of 1.8g; Two, the high Vinsol that step 1 is taken by weighing carries out drying treatment 3h under 120 ℃ of temperature; Three, the dried high Vinsol of the bisphenol A type epoxy resin that step 1 is taken by weighing, polymeric amide 200#, thiorubber and step 2 puts into kneader, with the rotating speed of 20rpm, under 30 ℃ of temperature, mixes 40min, promptly gets material; Four, the material that step 3 is obtained is put into thermocompressor, is 2MPa at pressure, and temperature is under 50 ℃ the condition, and 10min is handled in precompressed; After precompressed is handled, be 6MPa at pressure, temperature is under 60 ℃ the condition, to carry out hot-pressing processing 20min, promptly gets matrix material, and the thickness of matrix material is 5.3mm; Five, matrix material that step 4 is hot-forming carries out after fixing 1h under 85 ℃ of temperature, promptly get xylogen-epoxy resin composite material.
The high Vinsol of this test buys from Songyuan Laihe Chemicals Co., Ltd..
Wherein epoxy resin adopts bisphenol A type epoxy resin, and oxirane value is 0.51.
Xylogen-epoxy resin composite material that this test is obtained carries out the sample Mechanics Performance Testing: flexural strength on CMT6104 microcomputer control electronics universal testing machine according to the GB/T9341-2000 standard testing; According to the GB/T1043-93 standard testing, density is according to the GB/T17657-1999 standard test on XJJ-50 charpy impact test machine for shock strength.The result sees table 1.
Test 5:
Prepare xylogen-epoxy resin composite material through following steps: one, take by weighing the high Vinsol of 90g, the bisphenol A type epoxy resin of 60g, the polymeric amide 200# of 48g, the thiorubber of 1.8g and the 120 purpose xylons of 30g; Two, the high Vinsol and the 120 purpose xylons that step 1 are taken by weighing carry out drying treatment 3h under 120 ℃ of temperature, then dried xylogen and xylon are mixed, and get material just; Three, the dried material just of the bisphenol A type epoxy resin that step 1 is taken by weighing, polymeric amide 200#, thiorubber and step 2 is put into kneader, with the rotating speed of 20rpm, under 30 ℃ of temperature, mixes 40min, promptly gets material; Four, the material that step 3 is obtained is put into thermocompressor, is 2MPa at pressure, and temperature is under 50 ℃ the condition, and 10min is handled in precompressed; After precompressed is handled, be 6MPa at pressure, temperature is under 60 ℃ the condition, to carry out hot-pressing processing 20min, promptly gets matrix material, and the thickness of matrix material is 6.5mm; Five, matrix material that step 4 is hot-forming carries out after fixing 1h under 85 ℃ of temperature, promptly get xylogen-epoxy resin composite material.
The high Vinsol of this test buys from Songyuan Laihe Chemicals Co., Ltd..
Wherein epoxy resin adopts bisphenol A type epoxy resin, and oxirane value is 0.51.
Xylogen-epoxy resin composite material that this test is obtained carries out the sample Mechanics Performance Testing: flexural strength on CMT6104 microcomputer control electronics universal testing machine according to the GB/T9341-2000 standard testing, shock strength on XJJ-50 charpy impact test machine according to the GB/T1043-93 standard testing; Density is according to the GB/T17657-1999 standard test.The result sees table 1.
The performance of the prepared xylogen-epoxy resin composite material of table 1
| Test | Flexural strength/(MPa) | Shock strength/(KJ/m 2) | Density/(g/cm 3) |
| 1 | 35.39 | 2.80 | 1.09 |
| 2 | 34.22 | 3.22 | 1.13 |
| 3 | 33.59 | 1.94 | 1.09 |
| 4 | 27.23 | 5.83 | 1.01 |
| 5 | 41.27 | 3.05 | 1.12 |
Claims (8)
1. an xylogen-epoxy resin composite material is characterized in that described xylogen-epoxy resin composite material is to be processed by 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies.
2. xylogen-epoxy resin composite material according to claim 1 is characterized in that described xylogen is industrial lignin, high purity xylogen, alkali lignin or high-boiling alcohol lignin.
3. xylogen-epoxy resin composite material according to claim 1 is characterized in that described epoxy resin is bisphenol A type epoxy resin, brominated bisphenol a type epoxy resin, amino four glycidyl epoxy resins, PARA AMINOPHENOL three-glycidyl epoxy resin or phenol aldehyde type epoxy resin.
4. xylogen-epoxy resin composite material according to claim 1 is characterized in that described solidifying agent is polymeric amide 200#, polymeric amide 400#, polyamide 6 51#, polymeric amide 203#, kymene 00# or polyamide 6 00#.
5. xylogen-epoxy resin composite material according to claim 1 is characterized in that described toughner is thiorubber, paracril, copolymer nylon, polyvinyl acetal, urethane, low molecular polyamides, epoxidized SBS or epoxidation pyridyl SBS.
6. xylogen-epoxy resin composite material according to claim 1 is characterized in that described toughener is silica powder, mica powder, talcum powder, lime carbonate, permanent white, WHITE CARBON BLACK, nano silicon, nano titanium oxide, nano zine oxide, nano zircite, nano-sized iron oxide, Nano titanate, nano-carbide, nano nitride, nano aluminium oxide, thomel, xylon, hemp fibre, bamboo fibers, spun glass, tossa, flax fiber, sisal fibers or monkey grass.
7. the method for preparing a kind of xylogen-epoxy resin composite material as claimed in claim 1, the preparation method who it is characterized in that xylogen-epoxy resin composite material are to carry out according to the following steps: one, take by weighing 100 parts epoxy resin, 100～400 parts xylogen, 60～120 parts solidifying agent, 0～40 part toughener and 0～20 part toughner by ratio of quality and the number of copies; Two, the xylogen that step 1 is taken by weighing carries out drying treatment 3～12h under 90 ℃～120 ℃ temperature; Three, dried xylogen mixes 30min～60min in the epoxy resin that step 1 is taken by weighing, solidifying agent, toughner, toughener and the step 2, promptly gets mixture; Four, the mixture that step 3 is obtained is put into thermocompressor, and hot-pressing processing is carried out in first precompressed then, promptly gets matrix material; Five, the matrix material that makes in the step 4 is carried out after fixing 1～2h, promptly get xylogen-epoxy resin composite material; Wherein, step 3 is described to mix, and mixing velocity is 20～40rpm, and mixing temperature is 20 ℃～30 ℃; The described precompressed of step 4 is handled, and pressure is 2～6MPa, and squeeze time is 10～20min, and the precompressed temperature is 40 ℃～50 ℃; The described hot-pressing processing of step 4, pressure are 6～20MPa, and hot pressing temperature is 50 ℃～60 ℃, and hot pressing time is the THICKNESS CALCULATION of the matrix material of four gained set by step, and every millimeter keeps 3～5min; The described after fixing temperature of step 5 is 70 ℃～100 ℃.
8. the preparation method of a kind of xylogen-epoxy resin composite material according to claim 7 is characterized in that described the mixing in kneader or mill of step 3 carry out.
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| CN112408359A (en) * | 2020-11-18 | 2021-02-26 | 上海汉禾生物新材料科技有限公司 | Method for preparing battery negative electrode material by using enzymatic hydrolysis lignin-based epoxy resin |
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| CN113429862A (en) * | 2021-07-21 | 2021-09-24 | 安徽博纳新材料科技有限公司 | High-strength modified epoxy resin material and preparation method thereof |
| CN113429863A (en) * | 2021-04-10 | 2021-09-24 | 中海油常州涂料化工研究院有限公司 | Polyamide-amine type water-based lignin-based epoxy anticorrosive paint and preparation method thereof |
| CN113913081A (en) * | 2021-08-13 | 2022-01-11 | 深圳市深赛尔股份有限公司 | High-flexibility environment-friendly elastic resin coating and preparation method thereof |
| CN114085490A (en) * | 2021-09-02 | 2022-02-25 | 东北林业大学 | Reinforced compression-resistant anti-collision highway guardrail plate material |
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Application publication date: 20120718 |