CN107141842B - A method of improving silicon carbide micro-powder dispersibility - Google Patents
A method of improving silicon carbide micro-powder dispersibility Download PDFInfo
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- CN107141842B CN107141842B CN201710460433.9A CN201710460433A CN107141842B CN 107141842 B CN107141842 B CN 107141842B CN 201710460433 A CN201710460433 A CN 201710460433A CN 107141842 B CN107141842 B CN 107141842B
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- silicon carbide
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- 239000000843 powder Substances 0.000 title claims abstract description 75
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 15
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000010583 slow cooling Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 239000002826 coolant Substances 0.000 claims 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000004537 pulping Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- WLLGXSLBOPFWQV-UHFFFAOYSA-N MGK 264 Chemical compound C1=CC2CC1C1C2C(=O)N(CC(CC)CCCC)C1=O WLLGXSLBOPFWQV-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of methods improving silicon carbide micro-powder dispersibility, include the following steps：(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly heated up；(2) when mixture temperature rises to 366 DEG C~380 DEG C in step (1), 20~50 minutes are kept the temperature, then slow cooling is added diethylenetriamine aqueous solution, 10~20 minutes are stood after mixing to 25 DEG C；(4) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is the silicon carbide micro-powder particle reunited；(5) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene, then dry modified silicon carbide micro-powder；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.The present invention can preferably solve stable problem after dispersion and dispersion in silicon carbide micro-powder pulping process, obtain the silicon carbide micro-powder that high-performance meets practical application.
Description
Technical field
The present invention relates to a kind of method improving silicon carbide micro-powder dispersibility, the side that especially silicon carbide micro-powder surface is modified
Method.
Background technology
Silicon carbide micro-powder is as abrasive material or filler in ceramic microabrasive tools, resin finish grinding wheel and diamond wheel
Etc. have a wide range of applications.Since its excellent properties such as hardness is high, intensity is high, and anti-oxidant and wear-resisting property is very prominent
It is also very extensive Deng the application of, silicon carbide micro-powder in terms of the non-grinding purposes such as refractory material, engineering ceramics, structural material.Mesh
Before, silicon carbide micro-powder have become development modern national defense, modern industry and high and new technology main raw material(s).Due to fine granularity
The silicon carbide micro-powder of (10 μm or less) is in irregular shape, surface energy is larger, easily causes to reunite, and forms offspring, makes superfine powder
The advantage of body is difficult to play.Not only moulded manufacturability is not achieved in dispersibility and mobility in the pouring forming technology of ceramic abrasive tool
Can require, and resin finish grinding wheel production in it is also poor with the compatibility of bonding agent, seriously affected finished product quality and
Excellent properties.
Therefore, surface modification is carried out to silicon carbide micro-powder, makes it have good dispersibility, mobility, eliminates and reunite,
The silicon carbide micro-powder prepared in subsequent mist projection granulating can be configured to disperse evenly and stably and solid concentration is higher, viscosity is relatively low
Slurry.The prior art there are energy consumptions it is big, particle dispersion is bad, the production cycle is long, product stability is poor the shortcomings of.The present invention
Have many advantages, such as that operating procedure is simple, it is high to wrap up uniform, stably dispersing, production efficiency.
Invention content
For deficiency in the prior art, the present invention provides a kind of methods improving silicon carbide micro-powder dispersibility.
The present invention is achieved through the following technical solutions, and its step are as follows：
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly risen
Temperature, the weight of wherein phthalimide are the 0.5%~2.0% of silicon carbide micro-powder weight；
(2) when mixture temperature rises to 366 DEG C~380 DEG C in step (1), 20~50 minutes are kept the temperature, is then slowly dropped
Temperature is added diethylenetriamine aqueous solution, after being stirred stands 10~20 minutes, wherein diethylenetriamine aqueous solution to 25 DEG C
Weight is 1~3 times of silicon carbide micro-powder weight；
(3) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is that the silicon carbide of reunion is micro-
Powder；
(4) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene is then modifiedly dry
Silicon carbide micro-powder afterwards；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.
Wherein the weight concentration of diethylenetriamine is 0.5%~1.0% in the diethylenetriamine aqueous solution.
Wherein the reactor carries chuck and agitating device.
The wherein described cooling method is to remove heating source and naturally cool to 110 DEG C or less to be passed through cooling Jie in chuck again
Matter cools down.
Beneficial effects of the present invention：
The present invention is heated up simultaneously by the way that silicon carbide micro-powder and phthalimide to be stirred in closed reactor
It allows phthalimide distillation to become gaseous state, is evenly distributed on around silicon carbide micro-powder, then slow cooling makes adjacent benzene two again
Carboximide is set in silicon carbide micro-powder surface, and diethylenetriamine is reacted with phthalimide generates the larger band of molecular weight
The organic molecule for having amido and carbonyl hinders the interparticle group of silicon carbide micro-powder in silicon carbide micro-powder space forming surface steric hindrance
It is poly-, improve the dispersibility of silicon carbide micro-powder.The particle diameter reunited in silicon carbide micro-powder is larger, surface coated modification point
Son is insufficient to allow its dispersion, therefore is deposited in bottom.The silicon carbide micro-powder particle that do not reunite is disperseed well.The present invention
The silicon carbide micro-powder surface package of processing is uniform, is firmly combined with, and silicon carbide micro-powder particle diameter is evenly distributed, and dispersibility and divides again
Scattered property has great raising.
The present invention has many advantages, such as that operating procedure is simple, it is high to wrap up uniform, stably dispersing, production efficiency.
Specific implementation method
With reference to specific example, the present invention will be described, and following implementation is merely to illustrate the present invention, and does not have to
In limitation scope of the present invention.
Embodiment 1, a method of silicon carbide micro-powder dispersibility being improved, its step are as follows：
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly risen
Temperature, the weight of wherein phthalimide are the 0.5% of silicon carbide micro-powder weight；
(2) when mixture temperature rises to 366 DEG C~368 DEG C in step (1), 20 minutes are kept the temperature, then slow cooling is extremely
25 DEG C, diethylenetriamine aqueous solution is added, 10 minutes are stood after being stirred, wherein the weight of diethylenetriamine aqueous solution is carbon
1.5 times of SiClx micropowder weight；
(3) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is that the silicon carbide of reunion is micro-
Powder；
(4) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene is then modifiedly dry
Silicon carbide micro-powder afterwards；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.
Wherein the weight concentration of diethylenetriamine is 0.5% in the diethylenetriamine aqueous solution.
Wherein the reactor carries chuck and agitating device.
The wherein described cooling method is to remove heating source and naturally cool to 110 DEG C or less to be passed through cooling Jie in chuck again
Matter cools down.
Embodiment 2, a method of silicon carbide micro-powder dispersibility being improved, its step are as follows：
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly risen
Temperature, the weight of wherein phthalimide are the 1.5% of silicon carbide micro-powder weight；
(2) when mixture temperature rises to 368 DEG C~370 DEG C in step (1), 25 minutes are kept the temperature, then slow cooling is extremely
25 DEG C, diethylenetriamine aqueous solution is added, 15 minutes are stood after being stirred, wherein the weight of diethylenetriamine aqueous solution is carbon
2 times of SiClx micropowder weight；
(3) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is that the silicon carbide of reunion is micro-
Powder；
(4) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene is then modifiedly dry
Silicon carbide micro-powder afterwards；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.
Wherein the weight concentration of diethylenetriamine is 0.8% in the diethylenetriamine aqueous solution.
Wherein the reactor carries chuck and agitating device.
The wherein described cooling method is to remove heating source and naturally cool to 110 DEG C or less to be passed through cooling Jie in chuck again
Matter cools down.
Embodiment 3, a method of silicon carbide micro-powder dispersibility being improved, its step are as follows：
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly risen
Temperature, the weight of wherein phthalimide are the 2.0% of silicon carbide micro-powder weight；
(2) when mixture temperature rises to 375 DEG C~380 DEG C in step (1), 35 minutes are kept the temperature, then slow cooling is extremely
25 DEG C, diethylenetriamine aqueous solution is added, 20 minutes are stood after being stirred, wherein the weight of diethylenetriamine aqueous solution is carbon
3 times of SiClx micropowder weight；
(3) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is that the silicon carbide of reunion is micro-
Powder；
(4) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene is then modifiedly dry
Silicon carbide micro-powder afterwards；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.
Wherein the weight concentration of diethylenetriamine is 1.0% in the diethylenetriamine aqueous solution.
Wherein the reactor carries chuck and agitating device.
The wherein described cooling method is to remove heating source and naturally cool to 110 DEG C or less to be passed through cooling Jie in chuck again
Matter cools down.
Claims (4)
1. a kind of method improving silicon carbide micro-powder dispersibility, it is characterised in that：Include the following steps：
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stirred and slowly heated up,
The weight of middle phthalimide is the 0.5%~2.0% of silicon carbide micro-powder weight；
(2) when mixture temperature rises to 366 DEG C~380 DEG C in step (1), 20~50 minutes are kept the temperature, then slow cooling is extremely
25 DEG C, diethylenetriamine aqueous solution is added, 10~20 minutes, the wherein weight of diethylenetriamine aqueous solution are stood after being stirred
It is 1~3 times of silicon carbide micro-powder weight；
(3) mixed liquor is divided into two layers：Upper layer is modified silicon carbide micro-powder suspension, and lower layer is the silicon carbide micro-powder grain reunited
Son；
(4) the modified silicon carbide micro-powder suspension in upper layer is extracted out filtering, precipitate washed with benzene is then modifiedly dry
Silicon carbide micro-powder；The silicon carbide micro-powder particle that lower layer reunites is modified again after de-agglomerated to be used.
2. a kind of method improving silicon carbide micro-powder dispersibility according to claim 1, it is characterised in that：The diethyl
The mass concentration of diethylenetriamine is 0.5%~1.0% in three amine aqueous solution of alkene.
3. a kind of method improving silicon carbide micro-powder dispersibility according to claim 1, it is characterised in that：The reaction
Device carries chuck and agitating device.
4. a kind of method improving silicon carbide micro-powder dispersibility according to claim 1 or 3, it is characterised in that：Described
Cooling method is to remove heating source and naturally cool to 110 DEG C or less to be passed through cooling medium cooling in chuck again.
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| CN201710460433.9A CN107141842B (en) | 2017-06-17 | 2017-06-17 | A method of improving silicon carbide micro-powder dispersibility |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710460433.9A CN107141842B (en) | 2017-06-17 | 2017-06-17 | A method of improving silicon carbide micro-powder dispersibility |
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| Publication Number | Publication Date |
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| CN107141842A CN107141842A (en) | 2017-09-08 |
| CN107141842B true CN107141842B (en) | 2018-11-06 |
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|---|---|---|---|---|
| US3914312A (en) * | 1973-02-07 | 1975-10-21 | Centre Etd Ind Pharma | Process for the preparation of propargylamine |
| SU1142473A1 (en) * | 1983-03-03 | 1985-02-28 | Физико-химический институт АН УССР | Method of obtaining 2,2'-diphthalimidoethylamine |
| CN101230211A (en) * | 2007-12-27 | 2008-07-30 | 同济大学 | Method for preparing small-molecule imide modified carbon nano-tube |
| CN101531373A (en) * | 2009-04-13 | 2009-09-16 | 四川大学 | Active organo montmorillonite and preparation method thereof |
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-
2017
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| SU1142473A1 (en) * | 1983-03-03 | 1985-02-28 | Физико-химический институт АН УССР | Method of obtaining 2,2'-diphthalimidoethylamine |
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Denomination of invention: A Method for Improving the Dispersion of Silicon Carbide Powders Effective date of registration: 20230320 Granted publication date: 20181106 Pledgee: Bank of China Limited by Share Ltd. Zhengzhou high tech Development Zone Branch Pledgor: ZHENGZHOU XILIKANG NEW MATERIAL Co.,Ltd. Registration number: Y2023980035478 |
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Denomination of invention: A method to improve the dispersibility of silicon carbide micro powder Granted publication date: 20181106 Pledgee: Bank of China Limited by Share Ltd. Xinzheng branch Pledgor: ZHENGZHOU XILIKANG NEW MATERIAL Co.,Ltd. Registration number: Y2024980012327 |