CN103554836A - Preparation method of SiO2 coated sisal cellulose crystallites and application thereof - Google Patents
Preparation method of SiO2 coated sisal cellulose crystallites and application thereof Download PDFInfo
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- CN103554836A CN103554836A CN201310510684.5A CN201310510684A CN103554836A CN 103554836 A CN103554836 A CN 103554836A CN 201310510684 A CN201310510684 A CN 201310510684A CN 103554836 A CN103554836 A CN 103554836A
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Abstract
The invention discloses a preparation method of SiO2 coated sisal cellulose crystallites and an application thereof. The preparation method comprises the following steps: by taking sisal as the raw material, preparing sisal cellulose crystallites by the methods of pretreatment, alkali treatment and acid treatment, and obtaining the SiO2 coated sisal cellulose crystallites by hydrolyzing SiO2 by a hydrothermal method and coating the surface of the sisal cellulose crystallites with the hydrolyzed SiO2; mixing an appropriate amount of SiO2 coated sisal cellulose crystallites with epoxy resin, and curing to obtain an epoxy resin hybrid material modified by the SiO2 coated sisal cellulose crystallites, wherein the epoxy resin hybrid material has excellent overall performance. The raw materials for the preparation method to prepare the sisal cellulose crystallites are wide in source, cheap and easy to get; the preparation method is easy to operate, and simple in process; the preparation of the SiO2 coated sisal cellulose crystallites is realized, so that the synergistic effect of the sisal cellulose crystallites and the SiO2 is achieved; the SiO2 coated sisal cellulose crystallites are evenly dispersed in an epoxy resin matrix, and have good compatibility with the matrix resin; and furthermore, the SiO2 coated sisal cellulose crystallites have an obvious toughening modification effect on the epoxy resin.
Description
Technical field
The present invention relates to sisal fibers element crystallite (SFCM) technical field, particularly a kind of SiO
2preparation method and the application thereof of coated sisal fibers element crystallite, this SiO
2coated sisal fibers element crystallite is applied to, in the enhancing modified of epoxy resin, can significantly improve its comprehensive mechanical property and thermal characteristics.
Background technology
Natural plant cellulose is more than 50 % of one of natural organic matter the abundantest on earth ，Ta Zhan vegitabilia carbon content, can synthesize approximately 1.5 * 10 every year by photosynthesis
12t.In recent years, along with the rapidly soaring and Sustainable development of oil, coal equal energy source price in the urgent need to, natural plant cellulose more and more comes into one's own as eco-friendly renewable resources.The natural plant cellulose that is commonly used to research mainly comprises that various agricultural crop straws and some agricultural product castoffs are as (modification technology of natural plant cellulose and progress such as bagasse, cotton stalk, sisal hemp, straw, flax, < < Guangdong chemical industry > >, 2012).And sisal hemp microcrystalline cellulose is the natural fiber the most widely using, have that specific surface area is large, the feature such as compressibility, degradable, the reactivity worth that renewable, water-absorbent is large, good and function, be widely used in the fields such as food-drink, daily-use chemical industry, medical and health and light industry industry.
Epoxy resin, since the later stage forties 20th century starts to obtain application in industrial production, has developed very swift and violent.The molecular structure of epoxy resin is to take in molecular chain to contain active epoxide group as its feature, owing to containing active epoxide group in molecular structure, make it can form with polytype solidifying agent generation crosslinking reaction insoluble, the not molten superpolymer with tridimensional network.Epoxy resin after solidifying has good physical and chemical performance, and it has excellent cohesive strength to the surface of metal and non-metallic material, product size good stability, hardness is high, snappiness is better, to alkali and most of solvent-stable, thereby is widely used in national defence, each department of national economy.
Nano particles of silicon dioxide have chemical stability good, high temperature resistant, do not burn, the feature such as electrical insulating property is good, be rubber, plastics, coating, medicine, agricultural chemicals, papermaking and the important mineral filler of daily-use chemical industry numerous areas.Nano particles of silicon dioxide surfactivity is large, can have an effect with other molecule, thereby have the performances such as good acidproof, alkaline-resisting, absorptivity, dispersiveness, thickening and thixotropy.
SiO
2coated SFCM modified epoxy, casting obtains the curing network of high-sequential, deep-crosslinked after solidifying.It has merged sisal hemp Microcrystalline Cellulose and has met environment friendly trend and the SiO that Materials science develops
2nanoparticle is more stable, the advantage such as high temperature resistant, its cured article has the aspect performances such as excellent machinery, heat, electricity, particularly dimensional stability, thermotolerance, the relative ordinary epoxy resin of shock resistance are greatly improved, and in fields such as aerospace, generator insulating material, military and national defense, have potential application foreground.
Summary of the invention
The object of this invention is to provide a kind of SiO
2preparation method and the application thereof of coated sisal fibers element crystallite.
Thinking of the present invention: take sisal hemp as raw material, prepare sisal fibers element crystallite by pre-treatment, alkaline purification, acid treatment method, adopt hydrothermal method hydrolysis SiO
2sisal fibers element crystallite surface is coated and makes SiO
2coated sisal fibers element crystallite; Get appropriate SiO
2coated sisal fibers element crystallite and epoxy blend, make the good SiO of over-all properties through solidifying
2coated sisal fibers element crystallite modified epoxy hybrid material.
Concrete steps are:
(1) sisal hemp short fibre of 4 millimeters of the length through super-dry being placed in to volume ratio is that the toluene/ethanol mixed solvent of 2:1 boils, and removes surperficial wax, makes the sisal hemp short fibre after paraffin removal.
(2) get the mixed solution that sisal hemp short fibre after the paraffin removal that 8 grams of steps (1) make is placed in the aqueous ethanolic solution that 30 milliliter of 0.1 mol/L NaOH aqueous solution and 200 milliliters of mass percents are 50%, at 45 ℃, constant temperature stirred after 3 hours, filter, dry, make thick product.
(3) thick product step (2) being made is placed in the nitric acid mixing solutions that 150 ml volumes are 68% than the acetic acid that is 80% for the mass percent of 10:1 and mass percent, in 120 ℃, process 15 minutes, filter, the ethanol that is 95% with mass percent and distilled water repetitive scrubbing are to neutral, after dry, obtain white powder, be sisal fibers element crystallite.
(4) in autoclave, add sisal fibers element crystallite that 5 ~ 10 grams of steps (3) make, 10 ~ 20 milliliters of tetraethoxys, 10 ~ 40 milliliters of ethanol and 20 ~ 80 ml deionized water, drip again 0.2 ~ 0.5 milliliter of concentrated hydrochloric acid, 150 ℃ are reacted 2 ~ 6 hours, cooled and filtered, washing, the dry SiO that makes
2coated sisal fibers element crystallite.
SiO prepared by the present invention
2coated sisal fibers element crystallite is applied to epoxy resin modification.
Concrete steps are:
Get SiO prepared by 0.2 ~ 2 gram of the present invention
2coated sisal fibers element crystallite joins in 20 ~ 60 grams of epoxy resin, decompression is bled, adding 2 ~ 16 grams of DDS solidifying agent is 4 again, 4 '-diaminodiphenylsulfone(DDS), after heating and melting, pour in the steel die that scribbles silicone grease, curing molding under the condition of 120 ℃/2 hours+160 ℃/2 hours+180 ℃/2 hours, makes SiO
2coated sisal fibers element crystallite modified epoxy hybrid material.
The present invention has the following advantages:
(1) prepare that the raw material sources of sisal fibers element crystallite extensively, cheap are easy to get, processing ease, technique be simple.
(2) by hydrothermal method, prepare SiO
2coated sisal fibers element crystallite, has realized sisal fibers element crystallite and SiO
2synergistic effect, the surface coated one deck SiO of sisal fibers element crystallite
2improved the thermotolerance of sisal hemp Microcrystalline Cellulose.
(3) SiO
2coated sisal fibers element crystallite is dispersed in epoxy resin-base, has good consistency with matrix resin, and epoxy resin is had to obvious toughening modifying effect.
(4) through SiO
2the epoxy resin of coated sisal fibers element crystallite modification, its impact property is 1.27 ~ 1.70 times of pure epoxy resin system, and tensile strength improves 37 ~ 37%, and flexural strength improves 1.11 ~ 1.41 times, and thermolysis starting temperature improves 18 ~ 35 ℃, SiO
2coating efficiency be 40 ~ 60%.
(5) SiO
2the preparation technology of coated sisal fibers element crystallite modified epoxy hybrid material is simple, with low cost, is conducive to industrial scale and produces and practical application.
Embodiment
In the main raw material that following examples are used, sisal hemp short fibre is industrial goods, and epoxy resin E-44 is technical grade, and the mass percent concentration of concentrated hydrochloric acid is 37%, and toluene is chemical pure, and other are analytical pure.
embodiment 1:
(1) sisal hemp short fibre of 4 millimeters of the length through super-dry being placed in to volume ratio is that the toluene/ethanol mixed solvent of 2:1 boils, and removes surperficial wax, makes the sisal hemp short fibre after paraffin removal.
(2) get the mixed solution that sisal hemp short fibre after the paraffin removal that 8 grams of steps (1) make is placed in the aqueous ethanolic solution that 30 milliliter of 0.1 mol/L NaOH aqueous solution and 200 milliliters of mass percents are 50%, at 45 ℃, constant temperature stirred after 3 hours, filter, dry, make thick product.
(3) thick product step (2) being made is placed in the nitric acid mixing solutions that 150 ml volumes are 68% than the acetic acid that is 80% for the mass percent of 10:1 and mass percent, in 120 ℃, process 15 minutes, filter, the ethanol that is 95% with mass percent and distilled water repetitive scrubbing are to neutral, after dry, obtain white powder, be sisal fibers element crystallite.
(4) in autoclave, add sisal fibers element crystallite that 5 grams of steps (3) make, 10 milliliters of tetraethoxys, 32 milliliters of ethanol and 40 ml deionized water, drip again 0.2 milliliter of concentrated hydrochloric acid, 150 ℃ are reacted 4 hours, cooled and filtered, washing, the dry SiO that makes
2coated sisal fibers element crystallite.
SiO prepared by the present embodiment
2coated sisal fibers element crystallite is applied to epoxy resin modification.
Concrete steps are:
Get SiO prepared by 0.52 gram of the present embodiment
2coated sisal fibers element crystallite joins in 26 grams of epoxy resin E-44s, decompression is bled, then adds 7.8 grams of DDS solidifying agent, pours in the steel die that scribbles silicone grease after heating and melting, curing molding under the condition of 120 ℃/2 hours+160 ℃/2 hours+180 ℃/2 hours, makes SiO
2coated sisal fibers element crystallite modified epoxy hybrid material.
SiO prepared by the present embodiment
2coated sisal fibers element crystallite modified epoxy hybrid material, its shock strength is by original 17.5kJ/m
2bring up to 22.3kJ/m
2, thermolysis starting temperature improves 19 ℃.
embodiment 2:
(1) sisal hemp short fibre of 4 millimeters of the length through super-dry being placed in to volume ratio is that the toluene/ethanol mixed solvent of 2:1 boils, and removes surperficial wax, makes the sisal hemp short fibre after paraffin removal.
(2) get the mixed solution that sisal hemp short fibre after the paraffin removal that 8 grams of steps (1) make is placed in the aqueous ethanolic solution that 30 milliliter of 0.1 mol/L NaOH aqueous solution and 200 milliliters of mass percents are 50%, at 45 ℃, constant temperature stirred after 3 hours, filter, dry, make thick product.
(3) thick product step (2) being made is placed in the nitric acid mixing solutions that 150 ml volumes are 68% than the acetic acid that is 80% for the mass percent of 10:1 and mass percent, in 120 ℃, process 15 minutes, filter, the ethanol that is 95% with mass percent and distilled water repetitive scrubbing are to neutral, after dry, obtain white powder, be sisal fibers element crystallite.
(4) in autoclave, add sisal fibers element crystallite that 5 grams of steps (3) make, 10 milliliters of tetraethoxys, 32 milliliters of ethanol and 40 ml deionized water, drip again 0.2 milliliter of concentrated hydrochloric acid, 150 ℃ are reacted 4 hours, cooled and filtered, washing, the dry SiO that makes
2coated sisal fibers element crystallite.
SiO prepared by the present embodiment
2coated sisal fibers element crystallite is applied to epoxy resin modification.
Concrete steps are:
Get SiO prepared by 0.78 gram of the present embodiment
2coated sisal fibers element crystallite joins in 26 grams of epoxy resin E-44s, decompression is bled, then adds 7.8 grams of DDS solidifying agent, pours in the steel die that scribbles silicone grease after heating and melting, curing molding under the condition of 120 ℃/2 hours+160 ℃/2 hours+180 ℃/2 hours, makes SiO
2coated sisal fibers element crystallite modified epoxy hybrid material.
SiO prepared by the present embodiment
2coated sisal fibers element crystallite modified epoxy hybrid material, its shock strength is by original 17.5kJ/m
2bring up to 29.8kJ/m
2, thermolysis starting temperature improves 28 ℃.
Claims (2)
1. a SiO
2the preparation method of coated sisal fibers element crystallite, is characterized in that concrete steps are:
(1) sisal hemp short fibre of 4 millimeters of the length through super-dry being placed in to volume ratio is that the toluene/ethanol mixed solvent of 2:1 boils, and removes surperficial wax, makes the sisal hemp short fibre after paraffin removal;
(2) get the mixed solution that sisal hemp short fibre after the paraffin removal that 8 grams of steps (1) make is placed in the aqueous ethanolic solution that 30 milliliter of 0.1 mol/L NaOH aqueous solution and 200 milliliters of mass percents are 50%, at 45 ℃, constant temperature stirred after 3 hours, filter, dry, make thick product;
(3) thick product step (2) being made is placed in the nitric acid mixing solutions that 150 ml volumes are 68% than the acetic acid that is 80% for the mass percent of 10:1 and mass percent, in 120 ℃, process 15 minutes, filter, the ethanol that is 95% with mass percent and distilled water repetitive scrubbing are to neutral, after dry, obtain white powder, be sisal fibers element crystallite;
(4) in autoclave, add sisal fibers element crystallite that 5 ~ 10 grams of steps (3) make, 10 ~ 20 milliliters of tetraethoxys, 10 ~ 40 milliliters of ethanol and 20 ~ 80 ml deionized water, drip again 0.2 ~ 0.5 milliliter of concentrated hydrochloric acid, 150 ℃ are reacted 2 ~ 6 hours, cooled and filtered, washing, the dry SiO that makes
2coated sisal fibers element crystallite.
2. the SiO that prepared by method according to claim 1
2the application of coated sisal fibers element crystallite, is characterized in that this SiO
2coated sisal fibers element crystallite is applied to epoxy resin modification, and concrete steps are:
Get SiO prepared by 0.2 ~ 2 gram of the present invention
2coated sisal fibers element crystallite joins in 20 ~ 60 grams of epoxy resin, decompression is bled, adding 2 ~ 16 grams of DDS solidifying agent is 4 again, 4 '-diaminodiphenylsulfone(DDS), after heating and melting, pour in the steel die that scribbles silicone grease, curing molding under the condition of 120 ℃/2 hours+160 ℃/2 hours+180 ℃/2 hours, makes SiO
2coated sisal fibers element crystallite modified epoxy hybrid material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103628307A (en) * | 2013-12-11 | 2014-03-12 | 山东科技大学 | Method for improving heat resistance of sisal fibers |
| CN104987654A (en) * | 2015-06-05 | 2015-10-21 | 苏州珍展科技材料有限公司 | Preparation method of phenolic resin composite material for storage tank |
| CN106519173A (en) * | 2016-11-29 | 2017-03-22 | 桂林理工大学 | Method for preparing shape memory polyurethane from hyperbranched modified sisal microcrystals |
| CN107287979A (en) * | 2016-03-30 | 2017-10-24 | 新材料与产业技术北京研究院 | A kind of nano silicon compound pulp and preparation method thereof and page |
| CN108976825A (en) * | 2018-06-26 | 2018-12-11 | 武汉中智德远科技开发有限公司 | A kind of high heat resistance modified resin and preparation method thereof |
| CN110028702A (en) * | 2019-04-29 | 2019-07-19 | 济南圣泉集团股份有限公司 | A kind of nano silica dopen Nano cellulosic material and its preparation method and application |
| CN110938284A (en) * | 2018-09-21 | 2020-03-31 | 广西大学 | Preparation method of bagasse fiber epoxy resin composite material coated with nanoparticles |
| CN110983846A (en) * | 2019-12-19 | 2020-04-10 | 蚌埠产品质量监督检验研究院 | Preparation method of sisal cellulose whisker, non-woven fabric for filter and preparation method |
| CN111454488A (en) * | 2019-01-22 | 2020-07-28 | 南京理工大学 | Bacterial cellulose-based composite protective material and preparation method thereof |
| CN112593436A (en) * | 2020-12-19 | 2021-04-02 | 桂林理工大学 | Preparation method of sisal fiber paper-based friction nano-generator |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103628307A (en) * | 2013-12-11 | 2014-03-12 | 山东科技大学 | Method for improving heat resistance of sisal fibers |
| CN104987654A (en) * | 2015-06-05 | 2015-10-21 | 苏州珍展科技材料有限公司 | Preparation method of phenolic resin composite material for storage tank |
| CN107287979A (en) * | 2016-03-30 | 2017-10-24 | 新材料与产业技术北京研究院 | A kind of nano silicon compound pulp and preparation method thereof and page |
| CN106519173A (en) * | 2016-11-29 | 2017-03-22 | 桂林理工大学 | Method for preparing shape memory polyurethane from hyperbranched modified sisal microcrystals |
| CN108976825A (en) * | 2018-06-26 | 2018-12-11 | 武汉中智德远科技开发有限公司 | A kind of high heat resistance modified resin and preparation method thereof |
| CN110938284A (en) * | 2018-09-21 | 2020-03-31 | 广西大学 | Preparation method of bagasse fiber epoxy resin composite material coated with nanoparticles |
| CN111454488A (en) * | 2019-01-22 | 2020-07-28 | 南京理工大学 | Bacterial cellulose-based composite protective material and preparation method thereof |
| CN111454488B (en) * | 2019-01-22 | 2022-03-18 | 南京理工大学 | Bacterial cellulose-based composite protective material and preparation method thereof |
| CN110028702A (en) * | 2019-04-29 | 2019-07-19 | 济南圣泉集团股份有限公司 | A kind of nano silica dopen Nano cellulosic material and its preparation method and application |
| CN110983846A (en) * | 2019-12-19 | 2020-04-10 | 蚌埠产品质量监督检验研究院 | Preparation method of sisal cellulose whisker, non-woven fabric for filter and preparation method |
| CN112593436A (en) * | 2020-12-19 | 2021-04-02 | 桂林理工大学 | Preparation method of sisal fiber paper-based friction nano-generator |
| CN112593436B (en) * | 2020-12-19 | 2022-12-06 | 桂林理工大学 | Preparation method of sisal fiber paper-based friction nano-generator |
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