CN112938981A - Preparation method of modified high-dispersion silicon carbide powder - Google Patents
Preparation method of modified high-dispersion silicon carbide powder Download PDFInfo
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- CN112938981A CN112938981A CN201911268649.0A CN201911268649A CN112938981A CN 112938981 A CN112938981 A CN 112938981A CN 201911268649 A CN201911268649 A CN 201911268649A CN 112938981 A CN112938981 A CN 112938981A
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Abstract
The preparation process of the modified high-dispersion silicon carbide powder is to simply mix, stir and heat the silicon carbide powder and the modifier. The invention uses disperse dye as main modifier, sodium alginate as auxiliary stabilizer, and silicon carbide powder is modified jointly. Adding disperse dye and sodium alginate into an aqueous medium, heating to 50-90 ℃, uniformly stirring, adding silicon carbide powder, continuously stirring for 1-4 h, and centrifugally drying the slurry to obtain the modified high-dispersion silicon carbide powder. The slurry prepared by adopting the high-dispersion silicon carbide powder realizes high solid content and low viscosity, namely the lowest viscosity is only 0.170 Pa.s when the volume solid content is 47 percent, and the maximum volume solid content is 60 percent.
Description
Technical Field
The invention relates to a preparation method of silicon carbide modified powder, which is used for preparing a biscuit of recrystallized silicon carbide.
Background
Silicon carbide, one of the ceramic materials, has been widely used in the chemical industry due to its excellent properties, such as high hardness, low thermal expansion, good heat resistance, excellent oxidation resistance, and corrosion resistance. The advantages of the grouting forming are simple and convenient in process, high in efficiency, low in cost and the like, and the grouting forming is widely applied to the manufacturing process of ceramic parts, so that the defect of low ceramic processability is effectively overcome.
For the slip casting process, the solid content and viscosity index of the slurry are very important. China can independently prepare the silicon carbide micro powder. However, the modification of micro powder to increase its solid content and reduce its viscosity is still far from foreign countries, so the modified silicon carbide powder for slip casting mainly depends on import. At present, the maximum volume solid content of slurry prepared from modified silicon carbide powder produced by Saint gobain, France can reach 60%, the modified powder is weakly acidic, and has good fluidity when the volume solid content is 50%, and no slurry layering and network structure exist under the solid content.
Compared with the foreign weakly acidic modified silicon carbide powder, the modified silicon carbide powder prepared at home shows weak alkalinity or even strong alkalinity. Although the properties of the ultrafine silicon carbide powder are close to those of Shenggoban modified silicon carbide powder in appearance, for example, Shenchun et al use polyvinylpyrrolidone, polyethyleneimine and polyethylene glycol modified silicon carbide powder to obtain the ultrafine silicon carbide powder high-performance slurry, the volume solid content is 51-55%, and the apparent viscosity is 0.01-0.5 Pa.s at a shear rate of 400s < -1 >. And the slurry prepared by the silicon carbide micro powder with lower viscosity and higher stability is obtained after the silane coupling agent and the dispersing agent are used for modification such as Tao Neo et al. However, the slip casting process needs to be carried out under a weakly alkaline condition, and the viscosity and the solid content of the silicon carbide powder are greatly changed along with the change of the pH value, namely, the viscosity is obviously reduced along with the increase of the pH value, and the solid content is increased. Therefore, in practical application, the performance of the foreign weakly acidic powder in a weakly alkaline environment is greatly improved, so that the performance of the silicon carbide powder prepared at home still cannot meet the production requirement. Especially, the viscosity of the slurry is increased gradually in the process of mixing and stirring the coarse powder and the fine powder in the subsequent forming process, and the slurry can not be used for forming. The preparation process of the weakly acidic modified powder is rarely reported in China.
Disclosure of Invention
The invention aims to realize the preparation of weakly acidic modified silicon carbide slurry with high solid content and low viscosity. In order to realize the purpose, the silicon carbide powder is modified by using the disperse dye and the sodium alginate composite. In the heating and stirring process, the modifiers are connected through chemical action and simultaneously form hydrogen bond action with the surface of the silicon carbide powder. The modified silicon carbide powder is effectively dispersed in an aqueous medium through steric hindrance and electrostatic repulsion. The preparation process is simple, and only the silicon carbide powder and the medicines are mixed in the aqueous solution and heated and stirred for 1-4 hours at 50-90 ℃. The invention has simple process and easy control of the process, and the obtained modified silicon carbide slurry has high solid content and low viscosity.
Technical effects
The invention has the advantages that the invention realizes high solid content and low viscosity of the silicon carbide slurry, namely the lowest viscosity is 0.170 Pa.s when the volume solid content is 47 percent, and the maximum volume solid content is 60 percent. The powder obtained by the invention is weakly acidic, and the slurry property is further improved in the subsequent grouting forming process in an alkaline environment. The invention has simple process, low cost and short period, and is suitable for mass production.
Description of the drawings:
FIG. 1 is a flow chart of a preparation process for preparing modified silicon carbide powder by the method of the present invention.
Detailed Description
The method comprises the following concrete implementation steps:
1. the disperse dye was ultrasonically stirred in deionized water for 5 minutes.
2. Adding sodium alginate into the mixed solution obtained in step 1, mixing, and continuing to stir for 5 minutes by ultrasound
3. Adding a certain mass of silicon carbide powder into the mixed liquid obtained in step 2, wherein the mass ratio of the water to the silicon carbide powder is 1: 1.
4. And (3) placing the mixture obtained in the step (3) into a three-neck flask, heating, and stirring at 50-90 ℃ for 1-4 hours.
5. And (4) centrifuging the silicon carbide slurry obtained in the step (4) for 5 minutes to remove supernatant and retain a filter cake in a centrifugal tube.
6. And (4) adding deionized water into the filter cake obtained in the step (5), and fully dispersing for 10 minutes by ultrasonic to obtain slurry.
7. The slurry obtained in 6 was centrifuged for 5 minutes and the supernatant was decanted.
8. And 6-7 are repeated to obtain the silicon carbide filter cake.
9. And (3) drying the filter cake in the step (8) for 48 hours at 85 ℃ to obtain a dried filter cake.
10. The silicon carbide filter cake obtained in 9 was broken up, and a slurry was prepared at a ratio of 1:1 of the material to the water to test a pH of 5.2, even at which the minimum viscosity was 0.170 Pa.s and the maximum volume solid content was 60% at a volume solid content of 47%.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1:
1. 50ml of deionized water, 0.5g of disperse Red and 0.5g of disperse blue were placed in a beaker and mixed with ultrasonic agitation for 5 minutes.
2. 0.2g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was poured into a three-necked flask and heated and stirred at 50 ℃ for 4 hours.
5. The obtained silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours to obtain a dried cake.
6. The dried filter cake was ground to a powder to prepare a slurry with a volume solids content of 47%, and the apparent viscosity was found to be 0.506 pa.s, with a maximum volume solids content of 54.28%.
Example 2:
1. 50ml of deionized water, 0.7g of disperse orange and 0.5g of disperse blue were placed in a beaker and mixed with ultrasonic agitation for 5 minutes.
2. 0.1g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 60 ℃ for 4 hours.
5. The obtained silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours to obtain a dried cake.
6. Grinding the filter cake obtained by drying into powder to prepare slurry with the volume solid content of 47%, and measuring that the apparent viscosity is 0.315 Pa.s and the maximum volume solid content is 55.56%.
Example 3:
1. 50ml of deionized water and 1g of disperse red were put into a beaker and mixed and stirred ultrasonically for 5 minutes.
2. 0.1g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 70 ℃ for 4 hours.
5. The obtained silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours to obtain a dried cake.
6. Grinding the dried filter cake into powder to prepare slurry with volume solid content of 47%, wherein the apparent viscosity is 0.289 Pa.s, and the maximum volume solid content is 57.28%.
Example 4:
1. 50ml of deionized water, 0.5g of disperse black and 0.5g of disperse red were placed in a beaker and mixed with ultrasonic agitation for 5 minutes.
2. 0.1g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 50 ℃ for 2 hours.
5. The obtained silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours to obtain a dried cake.
6. Grinding the dried filter cake into powder to prepare slurry with the volume solid content of 47%, wherein the apparent viscosity is 0.206 Pa.s, and the maximum volume solid content is 57.28%.
Example 5:
1. 50ml of deionized water, 0.5g of disperse black and 0.5g of disperse blue were placed in a beaker and mixed with ultrasonic agitation for 5 minutes.
2. 0.1g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 50 ℃ for 4 hours.
5. The resulting silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours.
6. The dried powder was formulated into a slurry with a volume solid content of 47%, and the apparent viscosity was found to be 0.256 pa.s, with a maximum volume solid content of 57.28%.
Example 6:
1. 50ml of deionized water, 0.6g of disperse black and 0.5g of disperse blue were mixed and stirred ultrasonically for 5 minutes.
2. 0.1g of sodium alginate is added into the beaker to be mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 65 ℃ for 1 hour.
5. The resulting silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours.
6. Grinding the filter cake obtained by drying into powder to prepare slurry with the volume solid content of 47%, and measuring that the apparent viscosity is 0.335 Pa.s and the maximum volume solid content is 55.56%.
Example 7:
1. 50ml of deionized water, 0.6g of disperse black were mixed and stirred ultrasonically for 5 minutes.
2. 0.05g of sodium alginate is added into the beaker continuously, mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 50 ℃ for 4 hours.
5. The resulting silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours.
6. Grinding the dried filter cake into powder to prepare slurry with volume solid content of 47%, and measuring that the apparent viscosity is 0.230 Pa.s and the maximum volume solid content is 57.28%.
Example 8:
1. 50ml of deionized water, 0.6g of disperse black were mixed in a beaker and stirred ultrasonically for 5 minutes.
2. 0.025g of sodium alginate is added into the beaker and mixed and stirred for 5 minutes by ultrasound.
3. The addition of 50g of silicon carbide powder was continued and the mixture was magnetically stirred in the beaker until homogeneous.
4. The mixture solution was placed in a three-necked flask and heated and stirred at 95 ℃ for 3 hours.
5. The resulting silicon carbide slurry was centrifuged and dried at 80 ℃ for 48 hours.
6. Grinding the dried filter cake into powder to prepare slurry with the volume solid content of 47%, wherein the apparent viscosity is 0.170 Pa.s, and the maximum volume solid content is 60%.
Claims (6)
1. The preparation method of the modified high-dispersion silicon carbide powder is characterized by comprising the following steps: taking silicon carbide raw powder as a raw material, taking a disperse dye as a modifier and taking sodium alginate as an auxiliary stabilizer to modify the silicon carbide raw powder, wherein the use amounts of the modifier and the stabilizer are 0.5-5 wt.% and 0.05-2 wt.% of the mass fraction of the silicon carbide raw powder respectively, firstly mixing the disperse dye and the sodium alginate, stirring uniformly, continuously heating to 50-90 ℃, stirring for 1-4 h, taking out, centrifuging and drying to obtain the modified silicon carbide powder.
2. The method for preparing modified highly dispersed silicon carbide powder according to claim 1, wherein: the modifier is disperse dye.
3. The method for preparing modified highly dispersed silicon carbide powder according to claim 1, wherein: the auxiliary stabilizer is sodium alginate.
4. The method for preparing modified highly dispersed silicon carbide powder according to claim 1, wherein: the addition amount of the disperse dye is 0.5-5 wt.%.
5. The method for preparing modified highly dispersed silicon carbide powder according to claim 1, wherein: the addition amount of the auxiliary stabilizer sodium alginate is 0.05-2 wt.%.
6. The method according to claim 1, wherein the heating and stirring are performed by stirring the mixed slurry at 50-90 ℃ for 1-4 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429209A (en) * | 2021-06-16 | 2021-09-24 | 咸阳陶瓷研究设计院有限公司 | Preparation method of high solid-phase content barren grouting material for desulfurization nozzle |
| CN114932727A (en) * | 2022-05-27 | 2022-08-23 | 江苏耀鸿电子有限公司 | Heat-resistant hydrocarbon resin-based copper-clad plate and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264049A (en) * | 2017-12-30 | 2018-07-10 | 凤阳力拓新型材料有限公司 | A kind of modification process of silicon carbide micro-powder |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264049A (en) * | 2017-12-30 | 2018-07-10 | 凤阳力拓新型材料有限公司 | A kind of modification process of silicon carbide micro-powder |
Non-Patent Citations (1)
| Title |
|---|
| SHICHAO SUN ET AL.: "A novel strategy to obtain superfine modified SiC powder with binary modifier-disperse black/sodium alginate and its mechanism study", 《MATER. RES. EXPRESS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429209A (en) * | 2021-06-16 | 2021-09-24 | 咸阳陶瓷研究设计院有限公司 | Preparation method of high solid-phase content barren grouting material for desulfurization nozzle |
| CN114932727A (en) * | 2022-05-27 | 2022-08-23 | 江苏耀鸿电子有限公司 | Heat-resistant hydrocarbon resin-based copper-clad plate and preparation method thereof |
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