CN105130443A - Preparation method for silicon carbide ceramic material - Google Patents
Preparation method for silicon carbide ceramic material Download PDFInfo
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- CN105130443A CN105130443A CN201510523940.3A CN201510523940A CN105130443A CN 105130443 A CN105130443 A CN 105130443A CN 201510523940 A CN201510523940 A CN 201510523940A CN 105130443 A CN105130443 A CN 105130443A
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Abstract
The invention discloses a preparation method for a silicon carbide ceramic material. The preparation method comprises: grinding bamboo charcoal to powder by using a ball mill; adding silicon powder and phenolic resin to be uniformly mixed, wherein the molar ratio of bamboo charcoal and silicon powder is 1: (1-1.1) and the ratio of mass of the mixture of the silicon powder and bamboo charcoal and the volume of the phenolic resin is 1: (1-1.1); pre-heating the mixture at 140-150 DEG C to form; and then raising the temperature to 1600-1700 DEG C in a vacuum or argon atmosphere for high-temperature sintering for 30-35 minutes to obtain the silicon carbide ceramic material. The silicon carbide ceramic material prepared by the preparation method disclosed by the invention has good adsorption property, resistivity and corrosion resistant rate and can be used for preparing a conductive material, an adsorption material, a corrosion-resistant material, an antioxidant material and a high-temperature-resistant material.
Description
Technical field
The application relates to a kind of preparation method of thyrite, and this material can be used for electro-conductive material, sorbing material, corrosion resistant material, oxidation-resistant material and high temperature material.
Background technology
Thyrite has high strength, high rigidity, erosion resistance and the advantage such as anti-oxidant because of it and is extensively widely used in multiple fields such as petrochemical complex, metallurgical machinery, microelectronics, automobiles.
In prior art, thyrite cannot realize good conductivity, corrosion-resistant rate and absorption property simultaneously, therefore applies limited.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of thyrite, to overcome deficiency of the prior art.
For achieving the above object, the invention provides following technical scheme:
The embodiment of the present application discloses a kind of preparation method of thyrite, comprise: utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1 ~ 1.1, the quality of the mixture of silica flour and bamboo charcoal is 1:1 ~ 1.1 with the ratio of the volume of resol, preheat shaping at 140 ~ 150 DEG C, then under vacuum or argon gas atmosphere, temperature is increased to 1600 ~ 1700 DEG C and carries out high temperature sintering 30 ~ 35min, obtain thyrite.
Preferably, in the preparation method of above-mentioned thyrite, in described high-temperature sintering process, before 200 DEG C, heat-up rate is 5 DEG C/min, after 200 DEG C, heats up with 15 DEG C/min heat-up rate.
Preferably, in the preparation method of above-mentioned thyrite, the preparation method of described resol is: joining in the reactor of 40 ~ 45 DEG C by dissolving phenol, in whipping process, adding the sodium hydroxide solution of 42%, 10min is reacted at 45 DEG C ~ 60 DEG C, then add formaldehyde, the temperature adding reaction solution in formaldehyde process remains on 65 ~ 80 DEG C, after adding formaldehyde, in 10 ~ 30 minutes, be warming up to 90 ~ 95 DEG C, then cooling obtains resol.
Preferably, in the preparation method of above-mentioned thyrite, the preparation method of described resol is: be first added in reactor by phenol and xylogen by 90 ~ 100:1 mass ratio, stir, catalyzer phosphoric acid is added again in reactor, pH value is regulated to be 2.5 ~ 2.7, then be heated to 140 ~ 160 DEG C and carry out the first reaction, isothermal reaction is after 1 ~ 1.2 hour, obtain the first reaction mixture, then by above-mentioned first reaction mixture cooling, 50 ~ 70 DEG C, add phenol to stir, and mix, be warming up to 85 ~ 90 DEG C again and drip formaldehyde, the mol ratio of formaldehyde and phenol is 0.7:1, need in dropping process to keep temperature to be 88 ~ 90 DEG C, then be warming up to 95 ~ 100 DEG C and continue polycondensation 1 ~ 1.2 hour, the second reaction mixture is obtained after having reacted, after at ambient pressure described second reaction mixture being heated to 110 ~ 120 DEG C of distillation dehydrations, be cooled to 110 DEG C again, add xylene formaldehyde resin, stir and be then warming up to 120 ~ 150 DEG C of continuation air distillation dehydrations, in the vacuum under pressure dephenolize of 0.01MPa after having dewatered, obtain resol.
Disclosed herein as well is a kind of preparation method of thyrite, comprising:
First phenol and xylogen are added in reactor by 90 ~ 100:1 mass ratio, stir, catalyzer phosphoric acid is added again in reactor, pH value is regulated to be 2.5 ~ 2.7, then be heated to 140 ~ 160 DEG C and carry out the first reaction, isothermal reaction is after 1 ~ 1.2 hour, obtain the first reaction mixture, then by above-mentioned first reaction mixture cooling, 50 ~ 70 DEG C, add phenol to stir, and mix, be warming up to 85 ~ 90 DEG C again and drip formaldehyde, the mol ratio of formaldehyde and phenol is 0.7:1, need in dropping process to keep temperature to be 88 ~ 90 DEG C, then be warming up to 95 ~ 100 DEG C and continue polycondensation 1 ~ 1.2 hour, the second reaction mixture is obtained after having reacted, after at ambient pressure described second reaction mixture being heated to 110 ~ 120 DEG C of distillation dehydrations, be cooled to 110 DEG C again, add xylene formaldehyde resin, stir and be then warming up to 120 ~ 150 DEG C of continuation air distillation dehydrations, in the vacuum under pressure dephenolize of 0.01MPa after having dewatered, obtain resol,
Utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1, the quality of the mixture of silica flour and bamboo charcoal is 1:1 with the ratio of the volume of resol, preheat shaping at 140 ~ 150 DEG C, then under vacuum or argon gas atmosphere, temperature is increased to 1650 DEG C and carries out high temperature sintering 30 ~ 35min, obtain thyrite.
Compared with prior art, the invention has the advantages that:
Thyrite prepared by the present invention has good absorption property, resistivity and corrosion-resistant rate, can be prepared into electro-conductive material, sorbing material, corrosion resistant material, oxidation-resistant material and high temperature material.
This case take bamboo charcoal as raw material, environmental protection, pollution-free.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present application or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the application, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Figure 1 shows that the SEM figure of thyrite in the specific embodiment of the invention 1.
Embodiment
The present invention is described further by the following example: according to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material ratio, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
In order to understand the present invention further, below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
Join in the reactor of 40 ~ 45 DEG C by dissolving phenol, in whipping process, add the sodium hydroxide solution of 42%, 10min is reacted at 45 DEG C ~ 60 DEG C, then add formaldehyde, the temperature adding reaction solution in formaldehyde process remains on 65 ~ 80 DEG C, after adding formaldehyde, in 10 ~ 30 minutes, be warming up to 90 ~ 95 DEG C, then cooling obtains resol.
Utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1, the quality of the mixture of silica flour and bamboo charcoal is 1:1 with the ratio of the volume of resol, preheat shaping at 140 DEG C, then under an argon atmosphere, temperature is increased to 1650 DEG C and carries out high temperature sintering 30min, wherein, before 200 DEG C, heat-up rate is 5 DEG C/min, after 200 DEG C, with 15 DEG C/min heat-up rate, obtain thyrite.
In above-mentioned preparation method, before 200 DEG C, heat-up rate is 5 DEG C/min, and object is to discharge oxygen, and after 200 DEG C, with 15 DEG C/min heat-up rate, object is to promote that reaction occurs, and prevents rate of heating too fast simultaneously.
Shown in SEM figure ginseng Fig. 1 of thyrite prepared by the present embodiment.
By test, prepared thyrite has good absorption property to benzene and TVOC, reaches 5.43% and 2.41% respectively; The resistivity of thyrite is 15.1 Ω .cm; The corrosion-resistant rate of thyrite is more than 99%.
Embodiment 2
Join in the reactor of 40 ~ 45 DEG C by dissolving phenol, in whipping process, add the sodium hydroxide solution of 42%, 10min is reacted at 45 DEG C ~ 60 DEG C, then add formaldehyde, the temperature adding reaction solution in formaldehyde process remains on 65 ~ 80 DEG C, after adding formaldehyde, in 10 ~ 30 minutes, be warming up to 90 ~ 95 DEG C, then cooling obtains resol.
Utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1.05, the quality of the mixture of silica flour and bamboo charcoal is 1:1.2 with the ratio of the volume of resol, preheat shaping at 140 DEG C, then under vacuum, temperature is increased to 1600 DEG C and carries out high temperature sintering 30min, wherein, before 200 DEG C, heat-up rate is 5 DEG C/min, after 200 DEG C, with 15 DEG C/min heat-up rate, obtain thyrite.
Embodiment 3
First by 100g phenol and 1g xylogen in reactor, stir, then add catalyzer phosphoric acid in reactor, regulate pH value to be 2.5, be then heated to 140 DEG C and carry out the first reaction, isothermal reaction, after 1 hour, obtains the first reaction mixture.Then above-mentioned first reaction mixture is cooled to 70 DEG C, adds 3g phenol and stir, and mix.Be warming up to 90 DEG C again and drip formaldehyde, the mol ratio of formaldehyde and phenol is 0.7:1, needs to keep temperature to be 88 DEG C in dropping process.Then be warming up to 95 DEG C and continue polycondensation 1 hour, after having reacted, obtain the second reaction mixture.After at ambient pressure above-mentioned second reaction mixture being heated to 120 DEG C of distillation dehydrations, then be cooled to 110 DEG C, add 6g xylene formaldehyde resin, stir and be then warming up to 150 DEG C of continuation air distillation dehydrations.In the vacuum under pressure dephenolize of 0.01MPa after having dewatered, when the mass content of the free phenol in said mixture equals 1%, finally obtain resol.
Utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1.1, the quality of the mixture of silica flour and bamboo charcoal is 1:1.1 with the ratio of the volume of resol, preheat shaping at 140 DEG C, then under an argon atmosphere, temperature is increased to 1700 DEG C and carries out high temperature sintering 30min, wherein, before 200 DEG C, heat-up rate is 5 DEG C/min, after 200 DEG C, with 15 DEG C/min heat-up rate, obtain thyrite.
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.The example of these preferred implementations illustrates in the accompanying drawings.Shown in accompanying drawing and the embodiments of the present invention described with reference to the accompanying drawings be only exemplary, and the present invention is not limited to these embodiments.
At this, also it should be noted that, in order to avoid the present invention fuzzy because of unnecessary details, illustrate only in the accompanying drawings with according to the closely-related structure of the solution of the present invention and/or treatment step, and eliminate other details little with relation of the present invention.
Finally, also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
Claims (5)
1. the preparation method of a thyrite, it is characterized in that, comprise: utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1 ~ 1.1, the quality of the mixture of silica flour and bamboo charcoal is 1:1 ~ 1.1 with the ratio of the volume of resol, preheat shaping at 140 ~ 150 DEG C, then under vacuum or argon gas atmosphere, temperature is increased to 1600 ~ 1700 DEG C and carries out high temperature sintering 30 ~ 35min, obtain thyrite.
2. the preparation method of thyrite according to claim 1, is characterized in that: in described high-temperature sintering process, and before 200 DEG C, heat-up rate is 5 DEG C/min, after 200 DEG C, heats up with 15 DEG C/min heat-up rate.
3. the preparation method of thyrite according to claim 1, it is characterized in that: the preparation method of described resol is: join in the reactor of 40 ~ 45 DEG C by dissolving phenol, in whipping process, add the sodium hydroxide solution of 42%, at 45 DEG C ~ 60 DEG C, react 10min, then add formaldehyde, the temperature adding reaction solution in formaldehyde process remains on 65 ~ 80 DEG C, after adding formaldehyde, be warming up to 90 ~ 95 DEG C in 10 ~ 30 minutes, then cooling obtains resol.
4. the preparation method of thyrite according to claim 1, it is characterized in that: the preparation method of described resol is: first phenol and xylogen are added in reactor by 90 ~ 100:1 mass ratio, stir, catalyzer phosphoric acid is added again in reactor, pH value is regulated to be 2.5 ~ 2.7, then be heated to 140 ~ 160 DEG C and carry out the first reaction, isothermal reaction is after 1 ~ 1.2 hour, obtain the first reaction mixture, then by above-mentioned first reaction mixture cooling, 50 ~ 70 DEG C, add phenol to stir, and mix, be warming up to 85 ~ 90 DEG C again and drip formaldehyde, the mol ratio of formaldehyde and phenol is 0.7:1, need in dropping process to keep temperature to be 88 ~ 90 DEG C, then be warming up to 95 ~ 100 DEG C and continue polycondensation 1 ~ 1.2 hour, the second reaction mixture is obtained after having reacted, after at ambient pressure described second reaction mixture being heated to 110 ~ 120 DEG C of distillation dehydrations, be cooled to 110 DEG C again, add xylene formaldehyde resin, stir and be then warming up to 120 ~ 150 DEG C of continuation air distillation dehydrations, in the vacuum under pressure dephenolize of 0.01MPa after having dewatered, obtain resol.
5. a preparation method for thyrite, is characterized in that, comprising:
First phenol and xylogen are added in reactor by 90 ~ 100:1 mass ratio, stir, catalyzer phosphoric acid is added again in reactor, pH value is regulated to be 2.5 ~ 2.7, then be heated to 140 ~ 160 DEG C and carry out the first reaction, isothermal reaction is after 1 ~ 1.2 hour, obtain the first reaction mixture, then by above-mentioned first reaction mixture cooling, 50 ~ 70 DEG C, add phenol to stir, and mix, be warming up to 85 ~ 90 DEG C again and drip formaldehyde, the mol ratio of formaldehyde and phenol is 0.7:1, need in dropping process to keep temperature to be 88 ~ 90 DEG C, then be warming up to 95 ~ 100 DEG C and continue polycondensation 1 ~ 1.2 hour, the second reaction mixture is obtained after having reacted, after at ambient pressure described second reaction mixture being heated to 110 ~ 120 DEG C of distillation dehydrations, be cooled to 110 DEG C again, add xylene formaldehyde resin, stir and be then warming up to 120 ~ 150 DEG C of continuation air distillation dehydrations, in the vacuum under pressure dephenolize of 0.01MPa after having dewatered, obtain resol,
Utilize ball mill by bamboo charcoal grind into powder, add silica flour and resol mixes, bamboo charcoal powder and silica flour mol ratio are 1:1, the quality of the mixture of silica flour and bamboo charcoal is 1:1 with the ratio of the volume of resol, preheat shaping at 140 ~ 150 DEG C, then under vacuum or argon gas atmosphere, temperature is increased to 1650 DEG C and carries out high temperature sintering 30 ~ 35min, obtain thyrite.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105543519A (en) * | 2015-12-30 | 2016-05-04 | 淮北师范大学 | Preparation method of SiC-(Al-Si) alloy composite material |
| CN107188183A (en) * | 2017-06-23 | 2017-09-22 | 郑州西利康新材料有限公司 | A kind of preparation method of silicon carbide micro-powder |
| CN108610051A (en) * | 2018-07-18 | 2018-10-02 | 东北林业大学 | A kind of preparation method being modified wooden base silicon carbide ceramic material |
| CN108706979A (en) * | 2018-07-18 | 2018-10-26 | 东北林业大学 | A kind of Silica hydrogel is modified the preparation method of wooden base silicon carbide ceramic material |
| CN116854477A (en) * | 2023-07-04 | 2023-10-10 | 北京亦盛精密半导体有限公司 | Silicon carbide ceramic with anisotropic resistivity, preparation method thereof and silicon carbide sheet product |
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| CN101514105A (en) * | 2009-04-02 | 2009-08-26 | 浙江大学 | Method for preparing silicon carbide micropowder |
| CN103641967A (en) * | 2013-12-27 | 2014-03-19 | 山东圣泉化工股份有限公司 | Modified phenolic resin |
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| CN101514105A (en) * | 2009-04-02 | 2009-08-26 | 浙江大学 | Method for preparing silicon carbide micropowder |
| CN103641967A (en) * | 2013-12-27 | 2014-03-19 | 山东圣泉化工股份有限公司 | Modified phenolic resin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543519A (en) * | 2015-12-30 | 2016-05-04 | 淮北师范大学 | Preparation method of SiC-(Al-Si) alloy composite material |
| CN107188183A (en) * | 2017-06-23 | 2017-09-22 | 郑州西利康新材料有限公司 | A kind of preparation method of silicon carbide micro-powder |
| CN107188183B (en) * | 2017-06-23 | 2019-04-12 | 郑州西利康新材料有限公司 | A kind of preparation method of silicon carbide micro-powder |
| CN108610051A (en) * | 2018-07-18 | 2018-10-02 | 东北林业大学 | A kind of preparation method being modified wooden base silicon carbide ceramic material |
| CN108706979A (en) * | 2018-07-18 | 2018-10-26 | 东北林业大学 | A kind of Silica hydrogel is modified the preparation method of wooden base silicon carbide ceramic material |
| CN108706979B (en) * | 2018-07-18 | 2021-03-23 | 东北林业大学 | Preparation method of silica gel modified wood-based silicon carbide ceramic material |
| CN116854477A (en) * | 2023-07-04 | 2023-10-10 | 北京亦盛精密半导体有限公司 | Silicon carbide ceramic with anisotropic resistivity, preparation method thereof and silicon carbide sheet product |
| CN116854477B (en) * | 2023-07-04 | 2024-05-24 | 北京亦盛精密半导体有限公司 | Silicon carbide ceramic with anisotropic resistivity, preparation method thereof and silicon carbide sheet product |
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Application publication date: 20151209 |