CN109135346A - Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof - Google Patents

Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof Download PDF

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CN109135346A
CN109135346A CN201811029638.2A CN201811029638A CN109135346A CN 109135346 A CN109135346 A CN 109135346A CN 201811029638 A CN201811029638 A CN 201811029638A CN 109135346 A CN109135346 A CN 109135346A
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silicon powder
modified
fine
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powder
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李佩悦
吴建新
马立云
陈志强
段树桐
谢恩俊
周新军
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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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
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • 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
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • 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
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3018—Grinding
    • 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
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3027—Drying, calcination
    • 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
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • 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
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • 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
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12

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  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to modified silicon powders of a kind of high pure and ultra-fine and preparation method thereof, it is characterised in that comprises the following raw materials by weight percent: SiO2 99.8‑100%、Al2O3 0‑0.03%、Fe2O30-0.003%, granularity D50=0.5~1 μm, D100≤5 μm, a. dry method ore grinding；B. wet milling obtains silicon powder mixed liquor added with machine aliphatic ester；C. silicon powder mixed liquor is classified with hydrocyclone group, obtains silicon powder；D. silicon powder enters centrifugal dehydrator or plate type pressure filter dehydration, controls water content≤10%；E. it dries, controls water content≤0.3%；F. it is modified with high-speed mixer, adds silane-modified medicament, obtain modified silicon powder；G. it is removed with Horizontal air flow grader and reunites " coarse granule ".The invention has the advantages that 1. obtained silicon powder D100≤5 μm；2. this method effectively avoids powder reuniting, powder secondary pollution problems；3. products application made from has extensive application value in ultrathin copper-clad plate industry.

Description

Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof
Technical field
The invention belongs to nonmetallic mineral deep process technology fields, are related to a kind of copper-clad plate (CCL) production field, and in particular to Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof.
Background technique
Copper-clad plate (CCL) is the foundation stone of hyundai electronics industry development, as the basic material in printed circuit board (pcb) manufacture Material, the fundamental characteristics and processing performance of copper-clad plate largely affect the quality and reliably and with long-term of printed circuit board (pcb) Property, performance, weight and the manufacturing cost of printed circuit board (pcb) are heavily dependent on copper-clad plate (CCL).Print both at home and abroad Circuit board (PCB) processed is to high density, high-precision, fine pore, thin wire, thin space, and light weight, slim direction are developed, in production Simultaneously to productivity is improved, cost is reduced, reduces pollution, adapts to multi items, the development of small lot production mode reform.
In order to improve the heat resistance of copper-clad plate (CCL), increase anti-flammability, modified dimensional stability reduces thermal expansion coefficient, Inorganic particle filler is added in copper-clad plate (CCL), such as silicon powder, aluminium hydroxide, three two magnesium of oxidation, talcum powder are inevitable Selection.Currently, apply super-fine silicon micro-powder average grain diameter (D50) on copper-clad plate (CCL) at 2~3 μm, with baseplate material to Ultrathin direction is developed, and filler will be required to have smaller granularity, better thermal diffusivity.
Summary of the invention
It is inadequate applied to the super-fine silicon micro-powder average particle size on copper-clad plate (CCL) that the purpose of the present invention is to solve existing Carefully the problem of (average grain diameter D50 is mostly 2~3 μm), modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof is provided.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of modified silicon powder of high pure and ultra-fine, it is characterised in that comprise the following raw materials by weight percent:
Chemical analysis: SiO2 99.8-100%、Al2O3 0-0.03%、Fe2O30-0.003%, granularmetric composition: granularity D50=0.5~ 1μm、D100≤5μm。
Further, the granularmetric composition is 0.6 ~ 0.1mm >=95%
Further, the modified silicon powder of a kind of high pure and ultra-fine, product whiteness >=92%, water content≤0.3%, the μ of conductivity EC≤5 S/cm, pH value 6-8, hydrophobicity >=120min.
A kind of preparation method of the modified silicon powder of high pure and ultra-fine, it is characterised in that the following steps are included:
A. dry method ore grinding: silicon powder raw material (SiO2 >=99.8%, D50 is 2~3 μm) ore grinding, ball mill are carried out using ball mill Draw ratio is 1:2 ~ 2:1, and liner is aluminium oxide liner plate, and control product granularity is D75≤10 μm, D100≤25 μm；
B. wet milling: the silicon powder raw material after step a ore grinding is subjected to ore grinding in sand mill, sand mill liner material is oxidation The grinding-aid dispersant organic fatty acid esters of silicon powder raw material weight 0.5~5 ‰ is added in grinding process, obtains silicon for aluminium or zirconium oxide Micro mist mixed liquor；
C. it is classified: the silicon powder mixed liquor after step b ore grinding is used into hydrocyclone group (aluminium oxide or zirconium oxide material, φ The series connection of 50/25/10 cyclone) it is classified, the silicon powder of granularity D50 >=5 μm is back to sand mill, obtains granularity D50=0.5~1 μm, the silicon powders of D100≤5 μm；
D. cleaning-dehydration: the silicon powder that step c is obtained, it is de- into centrifugation using deionized water (conductivity≤2 μ S/cm) Water dispenser or plate type pressure filter are dehydrated, and are controlled water content≤10%, are obtained the silicon powder of the μ of conductivity EC≤5 S/cm；
E. it dries: the obtained silicon powder of step d being entered into spray drying or microwave dryer is dried, control water content≤ 0.3%, obtain dry silicon powder；
F. it is modified: using liner to be modified to aoxidize the high-speed mixer of aluminium material the drying silicon powder obtained through step e The silane-modified medicament of dring silicon micropowder weight 0.5~3 ‰ is added in processing, and control modification time is 30~60min, and temperature is 100~150 DEG C, obtain modified silicon powder；
G. it goes thick: the modification silicon powder that step f is obtained is removed into the reunion generated in modifying process by Horizontal air flow grader " coarse granule ", the grading wheel of Horizontal air flow grader are Al2O3Material, modified silicon powder coarse granule return to mixed at high speed after collecting Machine, obtaining modified silicon powder fine powder is a kind of modified silicon powder of high pure and ultra-fine produced by the present invention.
Further, silane-modified medicament is preferably in the step f, by silane coupling agent KH560 and silane coupling agent KH570 is mixed by weight for 1-2:1-2.
Compared with traditional handicraft, the present invention has the advantage that 1. utilize superfine sand mill wet milling, dry method is reached The granularity limit that grinding process is unable to reach, makes D100≤5 μm of superfine powder；2. can be effective using spray drying or microwave drying Avoid powder reuniting；3. carrying out bulk processing using grading technology；4. carrying out powder surface using ceramic-lined high mixer to change Property, it can avoid the secondary pollution of powder；5. the modified silicon powder of the high pure and ultra-fine of D50=0.5~1 μm of preparation, D100≤5 μm is Raw material necessary to slim copper-clad plate has extensive application value.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
In conjunction with Fig. 1, modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof, specific implementation step is as follows:
Embodiment 1
A. dry method ore grinding: silicon powder raw material (SiO2 >=99.8%, D50 is 2~3 μm) ore grinding, ball mill are carried out using ball mill Draw ratio is 1:1.5, and liner is aluminium oxide liner plate, and control product granularity is D75≤10 μm, D100≤25 μm；
B. wet milling: the silicon powder raw material after step a ore grinding is subjected to ore grinding in sand mill, sand mill liner material is oxidation 2.0 ‰ grinding-aid dispersant organic fatty acid esters is added in grinding process, obtains silicon powder mixed liquor for aluminium；
C. it is classified: by the silicon powder mixed liquor after step b ore grinding using hydrocyclone group (oxidation aluminium material, φ 50/25/10 Cyclone series connection) it is classified, the silicon powder of granularity D50 >=5 μm is back to sand mill, obtains granularity D50=0.5~1 μm, D100 ≤ 5 μm of silicon powder；
D. cleaning-dehydration: the silicon powder that step c is obtained, it is de- into centrifugation using deionized water (conductivity≤2 μ S/cm) Water dispenser or plate type pressure filter are dehydrated, and are controlled water content≤10%, are obtained the silicon powder of the μ of conductivity EC≤5 S/cm；
E. it dries: the obtained silicon powder of step d being entered into spray drying or microwave dryer is dried, control water content≤ 0.3%, obtain dry silicon powder；
F. it is modified: using liner to be modified place to aoxidize the high-speed mixer of aluminium material the drying silicon powder that step e is obtained Reason is separately added into dring silicon micropowder weight 2 ‰ silane coupling agent KH560 and 1 ‰ silane coupling agent KH570, controls modification time For 45min, temperature is 120 DEG C, obtains modified silicon powder；
G. it goes thick: the modification silicon powder that step f is obtained is removed into the reunion generated in modifying process by Horizontal air flow grader " coarse granule ", the grading wheel of Horizontal air flow grader are Al2O3Material, modified silicon powder coarse granule return to mixed at high speed after collecting Machine, obtaining modified silicon powder fine powder is a kind of modified silicon powder of high pure and ultra-fine produced by the present invention.
Embodiment 2
A. dry method ore grinding: silicon powder raw material (SiO2 >=99.8%, D50 is 2~3 μm) ore grinding, ball mill are carried out using ball mill Draw ratio is 1:1, and liner is aluminium oxide liner plate, and control product granularity is D75≤10 μm, D100≤25 μm；
B. wet milling: the silicon powder raw material after step a ore grinding is subjected to ore grinding in sand mill, sand mill liner material is oxidation 1.5 ‰ grinding-aid dispersant organic fatty acid esters is added in grinding process, obtains silicon powder mixed liquor for zirconium；
C. it is classified: the silicon powder mixed liquor after step b ore grinding is used into hydrocyclone group (zirconium oxide material, φ 50/25/10 Cyclone series connection) it is classified, the silicon powder of granularity D50 >=5 μm is back to sand mill, obtains granularity D50=0.5~1 μm, D100 ≤ 5 μm of silicon powder；
D. cleaning-dehydration: the silicon powder that step c is obtained, it is de- into centrifugation using deionized water (conductivity≤2 μ S/cm) Water dispenser or plate type pressure filter are dehydrated, and are controlled water content≤10%, are obtained the silicon powder of the μ of conductivity EC≤5 S/cm；
E. it dries: the obtained silicon powder of step d being entered into spray drying or microwave dryer is dried, control water content≤ 0.3%, obtain dry silicon powder；
F. it is modified: the drying silicon powder that step e is obtained being modified processing using the high-speed mixer of alumina liner, is added Dring silicon micropowder weight 1.5 ‰ silane coupling agent KH560 and 1.5 ‰ silane coupling agent KH570, control modification time are 60min, Temperature is 130 DEG C；
G. it goes thick: the modification silicon powder that step e is obtained is removed into the reunion generated in modifying process by Horizontal air flow grader " coarse granule ", the grading wheel of Horizontal air flow grader are Al2O3Material, modified silicon powder coarse granule return to mixed at high speed after collecting Machine, obtaining modified silicon powder fine powder is a kind of modified silicon powder of high pure and ultra-fine produced by the present invention.
If the following table 1 is the modified silicon powder key technical index of high pure and ultra-fine:
Above embodiments are only that preferred embodiment of the invention is described, and are not defined to the scope of the present invention, not Under the premise of being detached from the principle of the invention, the change of form of ownership should be fallen into claims of the present invention protection scope.

Claims (5)

1. a kind of modified silicon powder of high pure and ultra-fine, it is characterised in that comprise the following raw materials by weight percent:
Chemical analysis: SiO2 99.8-100%、Al2O3 0-0.03%、Fe2O30-0.003%, granularmetric composition: granularity D50=0.5~ 1μm、D100≤5μm。
2. the modified silicon powder of a kind of high pure and ultra-fine according to claim 1, it is characterised in that: the granularmetric composition is 0.6 ~ 0.1mm≥95%。
3. the modified silicon powder of a kind of high pure and ultra-fine according to claim 1, it is characterised in that: product whiteness >=92%, water content ≤ 0.3%, conductivity EC≤5 μ S/cm, pH value 6-8, hydrophobicity >=120min.
4. a kind of preparation method of the modified silicon powder of high pure and ultra-fine, it is characterised in that the following steps are included:
A. dry method ore grinding: silicon powder raw material carries out ore grinding using ball mill, and ball mill draw ratio is 1:2 ~ 2:1, and liner is oxidation Aluminium liner plate, control product granularity are D75≤10 μm, D100≤25 μm；
B. wet milling: the silicon powder raw material after step a ore grinding is subjected to ore grinding in sand mill, sand mill liner material is oxidation The grinding-aid dispersant organic fatty acid esters of silicon powder raw material weight 0.5~5 ‰ is added in grinding process, obtains silicon for aluminium or zirconium oxide Micro mist mixed liquor；
C. it is classified: the silicon powder mixed liquor after step b ore grinding is classified using hydrocyclone group, granularity D50 >=5 μm Silicon powder is back to sand mill, obtains the silicon powder of granularity D50=0.5~1 μm, D100≤5 μm；
D. cleaning-dehydration: the silicon powder that step c is obtained, using deionized water, into centrifugal dehydrator or plate type pressure filter It is dehydrated, controls water content≤10%, obtain the silicon powder of the μ of conductivity EC≤5 S/cm；
E. it dries: the obtained silicon powder of step d being entered into spray drying or microwave dryer is dried, control water content≤ 0.3%, obtain dry silicon powder；
F. it is modified: using liner to be modified to aoxidize the high-speed mixer of aluminium material the drying silicon powder obtained through step e The silane-modified medicament of dring silicon micropowder weight 0.5~3 ‰ is added in processing, and control modification time is 30~60min, and temperature is 100~150 DEG C, obtain modified silicon powder；
G. it goes thick: the modification silicon powder that step f is obtained is removed into the reunion generated in modifying process by Horizontal air flow grader " coarse granule ", the grading wheel of Horizontal air flow grader are Al2O3Material, modified silicon powder coarse granule return to mixed at high speed after collecting Machine, obtaining modified silicon powder fine powder is a kind of modified silicon powder of high pure and ultra-fine produced by the present invention.
5. the preparation method of the modified silicon powder of a kind of high pure and ultra-fine according to claim 4, it is characterised in that: the step f In silane-modified medicament be preferably, by silane coupling agent KH560 and silane coupling agent KH570 be by weight 1-2:1-2 mixing It forms.
CN201811029638.2A 2018-09-05 2018-09-05 Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof Pending CN109135346A (en)

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CN110079128A (en) * 2019-04-29 2019-08-02 江苏辉迈粉体科技有限公司 A kind of Submicron spherical silica micropowder organic dispersions and preparation method thereof
CN110408237A (en) * 2019-08-07 2019-11-05 江苏联瑞新材料股份有限公司 A kind of woodcare paint clear finish silicon powder and preparation method thereof
CN110913588A (en) * 2019-11-30 2020-03-24 江苏联瑞新材料股份有限公司 Application of crystalline silicon micro powder
CN111073350A (en) * 2019-12-25 2020-04-28 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of submicron active silica micropowder
CN111545157A (en) * 2020-05-29 2020-08-18 山东埃尔派粉体科技股份有限公司 Silicon micropowder modification device and production process thereof
CN112500608A (en) * 2020-11-20 2021-03-16 江苏联瑞新材料股份有限公司 Preparation method of fused silica micropowder for high-frequency high-speed copper-clad plate
CN113149024A (en) * 2021-04-25 2021-07-23 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of ultra-pure submicron silicon micro-powder through foaming
CN113462196A (en) * 2021-06-29 2021-10-01 江苏联瑞新材料股份有限公司 Preparation method of narrow-distribution superfine silicon powder
CN113621254A (en) * 2021-08-05 2021-11-09 江苏联瑞新材料股份有限公司 Preparation method of low-impurity silicon micropowder for high-reliability vehicle-mounted copper-clad plate
CN114308851A (en) * 2021-12-10 2022-04-12 连云港锐智新材料有限公司 Production method of high-purity silicon micro powder for electronic instrument
CN114618646A (en) * 2022-02-07 2022-06-14 中铝山东新材料有限公司 Preparation method of superfine aluminum hydroxide micro powder

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