CN107141842A - A kind of method for improving silicon carbide micro-powder dispersiveness - Google Patents

A kind of method for improving silicon carbide micro-powder dispersiveness Download PDF

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Publication number
CN107141842A
CN107141842A CN201710460433.9A CN201710460433A CN107141842A CN 107141842 A CN107141842 A CN 107141842A CN 201710460433 A CN201710460433 A CN 201710460433A CN 107141842 A CN107141842 A CN 107141842A
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silicon carbide
powder
carbide micro
micro
weight
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CN107141842B (en
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时松超
吴来根
孙国平
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Zhengzhou Xilikang New Material Co Ltd
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Zhengzhou Xilikang New Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological 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 method for improving silicon carbide micro-powder dispersiveness, comprise the following steps:(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly heat up;(2) when mixture temperature rises to 366 DEG C~380 DEG C in step (1), 20~50 minutes are incubated, then slow cooling adds the diethylenetriamine aqueous solution to 25 DEG C, and 10~20 minutes are stood after mixing;(4) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is the silicon carbide micro-powder particle reunited;(5) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene, then dry modified silicon carbide micro-powder;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.The present invention can preferably solve the scattered and scattered rear stable problem in silicon carbide micro-powder pulping process, obtain the silicon carbide micro-powder that high-performance meets practical application.

Description

A kind of method for improving silicon carbide micro-powder dispersiveness
Technical field
The present invention relates to a kind of method for improving silicon carbide micro-powder dispersiveness, the side that particularly 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 emery wheel and diamond wheel In terms of have a wide range of applications.Because its excellent properties such as hardness is high, intensity is high, and anti-oxidant and anti-wear performance is very prominent Deng the application of, silicon carbide micro-powder in terms of the non-grinding purposes such as refractory material, engineering ceramics, structural material also widely.Mesh Before, silicon carbide micro-powder has become the main raw material(s) of development modern national defense, modern industry and high and new technology.Due to fine granularity The silicon carbide micro-powder of (less than 10 μm) is in irregular shape, surface can it is larger, easily cause reunions, formation offspring makes superfine powder The advantage of body is difficult to play.Not only dispersiveness and mobility do not reach moulded manufacturability in the pouring forming technology of ceramic abrasive tool Can require, and also poor with the compatibility of bonding agent in the production of resin finish emery wheel, had a strong impact on finished product quality and Excellent properties.
Therefore, surface modification is carried out to silicon carbide micro-powder, makes it have good dispersiveness, mobility, eliminates and reunite, The silicon carbide micro-powder prepared in follow-up mist projection granulating can be configured to be uniformly dispersed, and stable and solid concentration is higher, viscosity is relatively low Slurry.There is the shortcomings of energy consumption is big, particle dispersion is bad, production cycle length, product stability are poor in prior art.The present invention Have the advantages that operating procedure is simple, it is high to wrap up uniform, stably dispersing, production efficiency.
The content of the invention
For deficiency of the prior art, the invention provides a kind of method for improving silicon carbide micro-powder dispersiveness.
The present invention is achieved through the following technical solutions, and its step is as follows:
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly rise The weight of temperature, wherein 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 incubated, then slow drop Temperature adds the diethylenetriamine aqueous solution to 25 DEG C, standing 10~20 minutes after stirring mixing, wherein the diethylenetriamine aqueous solution Weight is 1~3 times of silicon carbide micro-powder weight;
(3) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is micro- for the carborundum reunited Powder;
(4) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene, it is then dry must be modified Silicon carbide micro-powder afterwards;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.
The weight concentration of diethylenetriamine is 0.5%~1.0% in the wherein described diethylenetriamine aqueous solution.
Wherein described reactor carries chuck and agitating device.
Wherein described cooling method is situated between to remove heating source and naturally cooling to less than 110 DEG C and be passed through to cool down again in chuck Matter cools.
Beneficial effects of the present invention:
The present invention is heated up simultaneously by the way that silicon carbide micro-powder and phthalimide are stirred into mixing in closed reactor Allow phthalimide distillation to be changed into gaseous state, be 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 reacts the larger band of generation molecular weight with phthalimide There is the organic molecule of amido and carbonyl, in silicon carbide micro-powder space forming surface steric hindrance, hinder the interparticle group of silicon carbide micro-powder It is poly-, improve the dispersiveness 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 it to disperse, therefore is deposited in bottom.The silicon carbide micro-powder particle do not reunited is disperseed well.The present invention The silicon carbide micro-powder surface parcel of processing is uniform, is firmly combined with, silicon carbide micro-powder particle diameter is evenly distributed, and dispersiveness and divides again Scattered property has great raising.
The present invention has the advantages that operating procedure is simple, it is high to wrap up uniform, stably dispersing, production efficiency.
Specific implementation method
With reference to instantiation, the present invention will be described, and implementation below is merely to illustrate the present invention, and without In limitation scope of the present invention.
A kind of embodiment 1, method for improving silicon carbide micro-powder dispersiveness, its step is as follows:
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly rise The weight of temperature, wherein phthalimide is 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 incubated, then slow cooling is extremely 25 DEG C, the diethylenetriamine aqueous solution is added, 10 minutes are stood after stirring mixing, wherein the weight of the diethylenetriamine aqueous solution is carbon 1.5 times of SiClx micropowder weight;
(3) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is micro- for the carborundum reunited Powder;
(4) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene, it is then dry must be modified Silicon carbide micro-powder afterwards;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.
The weight concentration of diethylenetriamine is 0.5% in the wherein described diethylenetriamine aqueous solution.
Wherein described reactor carries chuck and agitating device.
Wherein described cooling method is situated between to remove heating source and naturally cooling to less than 110 DEG C and be passed through to cool down again in chuck Matter cools.
A kind of embodiment 2, method for improving silicon carbide micro-powder dispersiveness, its step is as follows:
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly rise The weight of temperature, wherein phthalimide is 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 incubated, then slow cooling is extremely 25 DEG C, the diethylenetriamine aqueous solution is added, 15 minutes are stood after stirring mixing, wherein the weight of the diethylenetriamine aqueous solution is carbon 2 times of SiClx micropowder weight;
(3) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is micro- for the carborundum reunited Powder;
(4) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene, it is then dry must be modified Silicon carbide micro-powder afterwards;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.
The weight concentration of diethylenetriamine is 0.8% in the wherein described diethylenetriamine aqueous solution.
Wherein described reactor carries chuck and agitating device.
Wherein described cooling method is situated between to remove heating source and naturally cooling to less than 110 DEG C and be passed through to cool down again in chuck Matter cools.
A kind of embodiment 3, method for improving silicon carbide micro-powder dispersiveness, its step is as follows:
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly rise The weight of temperature, wherein phthalimide is 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 incubated, then slow cooling is extremely 25 DEG C, the diethylenetriamine aqueous solution is added, 20 minutes are stood after stirring mixing, wherein the weight of the diethylenetriamine aqueous solution is carbon 3 times of SiClx micropowder weight;
(3) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is micro- for the carborundum reunited Powder;
(4) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene, it is then dry must be modified Silicon carbide micro-powder afterwards;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.
The weight concentration of diethylenetriamine is 1.0% in the wherein described diethylenetriamine aqueous solution.
Wherein described reactor carries chuck and agitating device.
Wherein described cooling method is situated between to remove heating source and naturally cooling to less than 110 DEG C and be passed through to cool down again in chuck Matter cools.

Claims (4)

1. a kind of method for improving silicon carbide micro-powder dispersiveness, it is characterised in that:Comprise the following steps:
(1) silicon carbide micro-powder and phthalimide are mixed to join in closed reactor, stir and slowly heat up, its 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 incubated, then slow cooling is extremely 25 DEG C, the diethylenetriamine aqueous solution is added, 10~20 minutes are stood after stirring mixing, wherein the weight of the diethylenetriamine aqueous solution For 1~3 times of silicon carbide micro-powder weight;
(3) mixed liquor is divided into two layers:Upper strata is modified silicon carbide micro-powder suspension, and lower floor is the silicon carbide micro-powder grain reunited Son;
(4) the modified silicon carbide micro-powder suspension in upper strata is extracted out and filtered, precipitate washed with benzene is then modifiedly dry Silicon carbide micro-powder;Modification is used the silicon carbide micro-powder particle that lower floor reunites again after de-agglomerated.
2. a kind of method for improving silicon carbide micro-powder dispersiveness according to claim 1, it is characterised in that:Described diethyl The mass concentration of diethylenetriamine is 0.5%~1.0% in the amine aqueous solution of alkene three.
3. a kind of method for improving silicon carbide micro-powder dispersiveness according to claim 1, it is characterised in that:Described reaction Device carries chuck and agitating device.
4. a kind of method of raising silicon carbide micro-powder dispersiveness according to claim 1 or 3, it is characterised in that:Described Cooling method for remove heating source naturally cool to less than 110 DEG C be passed through again in chuck cooling medium cool.
CN201710460433.9A 2017-06-17 2017-06-17 A method of improving silicon carbide micro-powder dispersibility Active CN107141842B (en)

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Citations (10)

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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
CN101948317A (en) * 2010-09-17 2011-01-19 青州宇信陶瓷材料有限公司 Method for preparing silicon carbide micro-powder modifying agent
CN102923706A (en) * 2012-11-29 2013-02-13 江苏乐园新材料集团有限公司 Preparation method of silicon carbide micro powder capable of improving dispersity
CN103833378A (en) * 2014-01-27 2014-06-04 连云港海蓝研磨材料有限公司 Surface modification method of silicon carbide micropowder
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CN105645968A (en) * 2016-03-03 2016-06-08 南京工业大学 Preparation method of ultramicro silicon carbide powder high-performance size
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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
CN101948317A (en) * 2010-09-17 2011-01-19 青州宇信陶瓷材料有限公司 Method for preparing silicon carbide micro-powder modifying agent
CN102923706A (en) * 2012-11-29 2013-02-13 江苏乐园新材料集团有限公司 Preparation method of silicon carbide micro powder capable of improving dispersity
CN103833378A (en) * 2014-01-27 2014-06-04 连云港海蓝研磨材料有限公司 Surface modification method of silicon carbide micropowder
CN105884377A (en) * 2014-12-09 2016-08-24 任海涛 Method for carrying out surface modification on silicon carbide powder by silane coupling agent
CN104610780A (en) * 2015-01-12 2015-05-13 中国科学院宁波材料技术与工程研究所 Modification method for silicon carbide particles
CN105645968A (en) * 2016-03-03 2016-06-08 南京工业大学 Preparation method of ultramicro silicon carbide powder high-performance size

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Denomination of invention: A Method for Improving the Dispersion of Silicon Carbide Powders

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