CN1285503C - Process for preparing silicon carbide by using carburized rice husk - Google Patents
Process for preparing silicon carbide by using carburized rice husk Download PDFInfo
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- CN1285503C CN1285503C CN 200410027511 CN200410027511A CN1285503C CN 1285503 C CN1285503 C CN 1285503C CN 200410027511 CN200410027511 CN 200410027511 CN 200410027511 A CN200410027511 A CN 200410027511A CN 1285503 C CN1285503 C CN 1285503C
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Abstract
The present invention discloses a method for preparing silicon carbide by carburized rice hulls, which comprises: carbonized rice hulls and coke are added to sodium hydroxide and water, and the main components of the carbonized rice hulls are silicon oxide; a hydrothermal method is used, temperature of 200 to 300 DEG C is kept for 24(+/-)5 hours, 50 to 1500 of atmospheric pressure is pressurized, and silicon carbide is synthesized by reaction. The present invention has the advantages of low reaction temperature and low cost, and is suitable for industrial mass production.
Description
Technical field
The present invention relates to a kind of method of utilizing carbonization rice husk to make silicon carbide.
Background technology
In Taiwan, annual nearly 400 ten thousand tons rice husk produces, and abandons the pollution that will cause environment.And rice husk can be converted into carbonization rice husk under 700 ℃ of burnings, it is the mixture of a kind of highly porous and bigger serface, wherein contain a large amount of amorphous silicon-dioxide and carbon, silicon-dioxide and carbon can prepare silicon carbide, silicon carbide has high mechanical strength and good high temperature resistant and resistance to chemical attack character, so, utilize rice husk to make silicon carbide, turning waste into wealth, is the mode that meets very much environmental protection.
As far back as 1973, the I.B.Cutler rice husk that just begins one's study transformed silicon carbide, and from then on the research of making silicon carbide by rice husk is that the various countries investigator payes attention to.People such as Milewski study rice husk in the atmosphere of nitrogen, argon, ammonia, when 1300-1500 ℃ of temperature, can change into silicon carbide, if add iron as catalyzer, then more help the conversion of silicon carbide.People such as Lakiza study rice husk when 1000 ℃ of temperature, can change into carbonization rice husk under anaerobic environment, if temperature of reaction is 1650 ℃, keep 15 minutes, and carbonization rice husk can change into silicon carbide fully.People postgraduate's rice husks such as Raju can obtain the silicon carbide whisker product in the atmosphere of nitrogen under 1000-1500 ℃ high temperature, and to having done in-depth analysis by crystalline substance.Some investigator is with the experiment of gas silicon monoxide and carbon monoxide synthesizing silicon carbide the time, and observing on the outer furnace wall of 1500 ℃ of reaction zones that (about 1200 ℃ of temperature) have must brilliant settling.
But, in any case when tradition changed into silicon carbide by rice husk, its temperature of reaction often needed more than 1000 ℃ high temperature, cost height, industrial mass production not as yet so far.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing carbonization rice husk to make silicon carbide, its temperature of reaction is low, and cost is also low, is fit to industrial mass production.
The present invention utilizes the method for carbonization rice husk manufacturing silicon carbide as follows:
With major ingredient is in the carbonization rice husk and coke adding sodium hydroxide and water of silicon-dioxide, utilizes hydrothermal method, holds temperature 24 ± 5 hours at 200-300 ℃, 50-1500 the normal atmosphere that pressurize, reaction synthesizing silicon carbide.
Wherein, above-mentioned carbonization rice husk can be burnt down at 700 ± 50 ℃ by rice husk and be transformed in about 2 hours.
Above-mentioned carbonization rice husk and coke were pulverized earlier before hydro-thermal reaction, so that the two fully reacts.
The product silicon carbide of above-mentioned hydro-thermal reaction under 800 ± 50 ℃, was held temperature about 2 hours, removed unnecessary carbon, obtained silicon carbide.
Like this, the present invention utilizes carbonization rice husk and coke to be raw material, adds sodium hydroxide and water, uses hydrothermal method below 300 ℃, has just synthesized silicon carbide, and sodium hydroxide is catalyzer, and main purpose is to destroy the Si-O bond.Temperature of reaction of the present invention is significantly less than the temperature of reaction of prior art, and the synthetic cost is also low, is fit to industrial mass production, is beneficial to environmental protection.
Description of drawings
Fig. 1 be carbonization rice husk under the deionized water and 0.2ml NaOH solution of 2ml, 300 ℃ of temperature of reaction were held temperature after 24 hours, its product is done X-ray diffractometer atlas analysis;
Fig. 2 be carbonization rice husk under the deionized water and 0.2ml NaOH solution of 2ml, hold the temperature 24 hours, difference is held the X-ray diffractometer collection of illustrative plates under the warm thermotonus, (A) 200 ℃ (B) 250 ℃ of (C) 300 ℃;
Fig. 3 be carbonization rice husk under the deionized water and 0.2ml NaOH solution of 2ml, 300 ℃ of temperature of reaction were held temperature 24 hours, the Fu Shi line outside line far away analyser collection of illustrative plates under the reaction.
Fig. 4 be carbonization rice husk under the deionized water and 0.2ml NaOH solution of 2ml, 300 ℃ of temperature of reaction were held temperature after 24 hours, the electron micrograph of product.
Specific embodiment
Present embodiment elder generation under 750 ℃, burns rice husk 2 hours, makes it to finish as far as possible changing into carbonization rice husk, and major ingredient is a silicon-dioxide.
Get 1 gram carbonization rice husk and 0.5 gram coke, utilize mortar to grind the back thorough mixing, and accurately measure the ready powder of scale, grinding powder is in order to be beneficial to reaction, the two fully to be reacted.
The powder that scale is good is put into the pincers pot, adds the 2ml deionized water, then adds the sodium hydroxide of 0.2ml, 1mol.
Temperature of reaction is set at 200 ℃, 250 ℃ and 300 ℃, 24 hours time, be forced into 85.9 normal atmosphere for best, reach as high as 1500 normal atmosphere, through after the hydro-thermal reaction, held temperature 2 to 4 hours for 800 ℃ with the process furnace heating, purpose removes the surplus carbon in the powder product, obtains purer silicon carbide.
At last, being the adult respectively with X-ray diffractometer, electron microscope and Fu Shi line outside line far away analyser analyzes and the character discussion.
As seen from Figure 1, in NaOH solution, temperature of reaction is held temperature after 24 hours for 300 ℃, has the diffraction peak of silicon carbide to produce.As seen from Figure 2, along with the reaction times increases, the diffraction peak grow of silicon carbide.As seen from Figure 3, in NaOH solution, hold temperature 24 hours for 300 ℃, just produce the bond of Si-C.As seen from Figure 4, in NaOH solution, held temperature 24 hours for 300 ℃, observed crystalline and produced, and the product crystallization of gained is the needle-like coccoid that Fibre diameter may reach nano level.
Like this, temperature of reaction of the present invention is significantly less than the temperature of reaction of prior art, and the synthetic cost is also low, is fit to industrial mass production, and variable rice husk refuse is precious, is beneficial to environmental protection.
Claims (4)
1, a kind of method of utilizing carbonization rice husk to make silicon carbide is characterized in that:
With major ingredient is in the carbonization rice husk and coke adding sodium hydroxide and water of silicon-dioxide, utilizes hydrothermal method, holds temperature 24 ± 5 hours at 200-300 ℃, 50-1500 the normal atmosphere that pressurize, reaction synthesizing silicon carbide.
2, a kind of method of utilizing carbonization rice husk to make silicon carbide according to claim 1 is characterized in that: carbonization rice husk is burnt down at 700 ± 50 ℃ by rice husk and was transformed in about 2 hours.
3, a kind of method of utilizing carbonization rice husk to make silicon carbide according to claim 1, it is characterized in that: carbonization rice husk and coke were pulverized earlier before hydro-thermal reaction, so that the two fully reacts.
4, a kind of method of utilizing carbonization rice husk to make silicon carbide according to claim 1 is characterized in that: the product silicon carbide of hydro-thermal reaction, under 800 ± 50 ℃, held temperature about 2 hours, and remove unnecessary carbon, obtain silicon carbide.
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CN1285503C true CN1285503C (en) | 2006-11-22 |
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Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100348547C (en) * | 2005-12-26 | 2007-11-14 | 西北工业大学 | Process for preparing silicon carbide coating on surface of carbon/carbon composite material |
CN102212219B (en) * | 2011-04-06 | 2013-05-08 | 江南大学 | Rice-husk-based carbon/silicon composite used as rubber filler and preparation method thereof |
CN103382030A (en) * | 2012-05-04 | 2013-11-06 | 江苏瑞力新材料科技有限公司 | Preparation method and use of nano-SiC whisker |
CN104692387B (en) * | 2015-02-11 | 2018-03-06 | 武汉佰迈思新材料有限公司 | A kind of method using silicon containing biomass as raw material low temperature preparation nanometer silicon carbide and preparation-obtained nanometer silicon carbide |
CN107237007B (en) * | 2017-04-27 | 2019-07-05 | 广东石油化工学院 | A kind of abrasion resistant fibrous preparation method and abrasion resistant fibrous |
CN108247553B (en) * | 2017-12-30 | 2020-11-17 | 义乌市安航科技有限公司 | Preparation method of wear-resistant artificial oilstone |
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