CN103360797A - Preparation method for dry-process ultrafine modified hydrated white carbon black - Google Patents

Preparation method for dry-process ultrafine modified hydrated white carbon black Download PDF

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CN103360797A
CN103360797A CN2013103054634A CN201310305463A CN103360797A CN 103360797 A CN103360797 A CN 103360797A CN 2013103054634 A CN2013103054634 A CN 2013103054634A CN 201310305463 A CN201310305463 A CN 201310305463A CN 103360797 A CN103360797 A CN 103360797A
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carbon black
white carbon
particle diameter
ball milling
preparation
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CN2013103054634A
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CN103360797B (en
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胡鹏华
徐明星
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NINGBO CREATE NEW MATERIAL CO Ltd
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NINGBO CREATE NEW MATERIAL CO Ltd
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Abstract

The invention discloses a preparation method for dry-process ultrafine modified hydrated white carbon black. The preparation method comprises a formula and a process method. The dry-process ultrafine modification method comprising ball milling, calcining dehydration and mixing of auxiliary agents is employed, fine processing of an initial product of hydrated white carbon black is carried out once again, and the cost performance of the hydrated white carbon black is improved by reducing the particle size and the water content, namely, by improving the dispersing activity of the hydrated white carbon black. Through the above technology schemes, the problem of relatively low cost performance of the hydrated white carbon black in the prior art is overcome; and the initial product is processed into the ultrafine product, so the cost performance of the hydrated white carbon black is improved.

Description

The preparation method of the superfine modified hydration White Carbon black of a kind of dry method
Technical field
The present invention relates to a kind of preparation method of White Carbon black goods, specifically refer to for the further retrofit of initial product with the hydration White Carbon black to be the preparation method of the superfine modified hydration White Carbon black of a kind of dry method of the ultrafine hydrous White Carbon black goods of ultra-fine highly disperse active.
Background technology
White Carbon black is as the strengthening agent of rubber-plastics material, and the less then dispersed activity of its granularity is higher, and the prior art White Carbon black is divided into hydration precipitator method White Carbon black (precipitated silica) by the preparation method, is also referred to as the hydration White Carbon black; Fumed silica (aerosil) is also referred to as the gas phase White Carbon black; Hydration White Carbon black particle is larger, and median size is 70~90 μ m, water ratio 6~9%; Gas phase White Carbon black particle is less, and median size is 10~15nm; Gas phase White Carbon black particle diameter is little, and dispersed activity is high, and cost is high, and price is also high, and namely cost performance is low; Hydration White Carbon black particle diameter is large, dispersed activity is low than the gas phase White Carbon black, but cost is low, price is also low, and namely cost performance is also low; No matter gas phase White Carbon black or the cost performance of hydration White Carbon black are all on the low side, in actual applications, rubber and plastic enterprise usually can be used for the higher product of rubber and plastic of cost performance with the gas phase White Carbon black, and the hydration White Carbon black is used for the lower product of rubber and plastic of cost performance for the consideration to the product of rubber and plastic cost performance; Therefore, there are cost performance problems and shortcomings on the low side in the hydration White Carbon black of prior art.
Summary of the invention
Problems and shortcomings for above-mentioned prior art existence, the present invention adopts the superfine modified method of the dry method of ball milling, calcined dehydration, mixed aid, initial product to the hydration White Carbon black carry out again retrofit, by reducing particle diameter, reducing water ratio, namely improve the technical scheme that its dispersed activity improves hydration White Carbon black goods cost performance, the preparation method of the superfine modified hydration White Carbon black of a kind of dry method is provided, be intended to be processed into the super-refinement product by the initial product with the hydration White Carbon black, make the hydration White Carbon black reach the purpose that improves cost performance.
The object of the present invention is achieved like this: the preparation method of the superfine modified hydration White Carbon black of a kind of dry method, comprise the composition and engineering method, wherein:
Described prescription is,
White Carbon black raw material: precipitated silica, particle diameter 70~90 μ m, water ratio 6~9%, 97%;
Auxiliary agent raw material: polyethylene wax, molecular weight 2000~3000,1%; Two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, CAS40372-72-3, molecular weight 539.0,1%; γ-mercaptopropyl trimethoxysilane, CAS4420-74-0, molecular weight 196.34,1%;
The prescription unit is weight percentage;
Described preparation technology is, ball milling, calcined dehydration, mixed aid,
Step 1, the White Carbon black raw material in will filling a prescription drop into planetary ball mill, and ball milling is carried out in start, 200~220 rev/mins of rotational speed of ball-mill, and 150~200 ℃ of ball milling temperature, 25 minutes ball milling times spent, shut down, obtaining particle diameter is the fines of 10~12 μ m;
Step 2, with the A suction conveyor described fines is moved to from the closed ball milling machine and to carry out calcined dehydration in the indirect type calcination rotary kiln, calcining temperature 550-600 ℃, 60 minutes calcining temperature times spent, afterwards, be cooled to room temperature, obtaining particle diameter is the dried fines of 10~12 μ m, water ratio 1~2%;
Step 3, with the B suction conveyor described dried fines is moved in the high-speed mixer from the indirect type calcination rotary kiln, auxiliary agent raw material in will filling a prescription again drops in the mixing machine, start mixes, mix 3000 rev/mins of rotating speeds, 140 ℃ of mixing temperatures, mix 15 minutes times spent, shut down, obtaining particle diameter is that 10~12 μ m, water ratio are 1~2% modification fine fodder;
Step 4, with the C suction conveyor described modification fine fodder is moved to from high-speed mixer in the storage tank, again through metering packing, making particle diameter is that 10~12 μ m, water ratio are 1~2% superfine modified hydration White Carbon black goods.
The proportioning of auxiliary agent raw material in the present invention prescription, according to user's actual demand widenable to polyethylene wax, 1~5%; Two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, 0.5~3%; γ-mercaptopropyl trimethoxysilane, 0.5~3%: stearic acid, 0.5~1%; Aluminate, 0.5~1%; Titanic acid ester, 0.5~2%; Amine hydroxybenzene, 0.5~2%; Clorafin, 1~5%; Fatty acid ester, 1~3%.
Beneficial effect
The superfine modified hydration White Carbon black goods that make with the present invention, median size reaches 10~12 μ m, water ratio reaches 1~2%, improved widely the dispersed activity of hydration White Carbon black, the cost that the added value that increases after the ultra-fine deep processing increases greater than deep processing, therefore, the present invention has improved the cost performance of hydration White Carbon black goods.
Above-mentioned, the present invention adopts the superfine modified method of the dry method of ball milling, calcined dehydration, mixed aid, initial product to the hydration White Carbon black carry out again retrofit, by reducing particle diameter, reducing water ratio, namely improve the technical scheme that its dispersed activity improves hydration White Carbon black goods cost performance, there are cost performance problems and shortcomings on the low side in the hydration White Carbon black that has overcome prior art, the preparation method of the superfine modified hydration White Carbon black of a kind of dry method that provides, by initial product are processed into the super-refinement product, make the hydration White Carbon black reach the purpose that improves cost performance.
The embodiment explanation
Below be described in further detail by the preparation method of specific embodiment to the superfine modified hydration White Carbon black of a kind of dry method of the present invention, the those skilled in the art can make superfine modified hydration White Carbon black goods with reference to prescription and the processing method of embodiment, but should not be construed as any limitation of the invention.
Embodiment
Embodiment
The name of an article: superfine modified hydration White Carbon black, median size 10~12 μ m, water ratio 1~2%;
Prescription: the prescription unit is weight percentage;
White Carbon black raw material: precipitated silica, particle diameter 70~90 μ m, water ratio 6~9%, 97%;
Auxiliary agent raw material: polyethylene wax, molecular weight 2000~3000,1%; Two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, CAS40372-72-3, molecular weight 539.0,1%; γ-mercaptopropyl trimethoxysilane, CAS4420-74-0, molecular weight 196.34,1%;
Preparation:
Preparation condition, equipment
Ambient pressure a: normal atmosphere; Envrionment temperature: room temperature;
Preparation equipment: planetary ball mill (abrading-ball: alumina balls, 8 millimeters of sphere diameter and quantitative proportion: φ, 30%; 12 millimeters of φ, 40%; 15 millimeters of φ, 30%), A suction conveyor, indirect type calcination rotary kiln, B suction conveyor, high-speed mixer, C suction conveyor, storage tank, powder metering wrapping machine;
Preparation technology: ball milling, calcined dehydration, mixed aid;
Step 1, the White Carbon black raw material in will filling a prescription drop into planetary ball mill, and ball milling is carried out in start, 200~220 rev/mins of rotational speed of ball-mill, and 150~200 ℃ of ball milling temperature, 25 minutes ball milling times spent, shut down, obtaining particle diameter is the fines of 10~12 μ m;
Step 2, with the A suction conveyor described fines is moved to from the closed ball milling machine and to carry out calcined dehydration in the indirect type calcination rotary kiln, calcining temperature 550-600 ℃, 60 minutes calcining temperature times spent, afterwards, be cooled to room temperature, obtaining particle diameter is the dried fines of 10~12 μ m, water ratio 1~2%;
Step 3, with the B suction conveyor described dried fines is moved in the high-speed mixer from the indirect type calcination rotary kiln, auxiliary agent raw material in will filling a prescription again drops in the mixing machine, start mixes, mix 3000 rev/mins of rotating speeds, 140 ℃ of mixing temperatures, mix 15 minutes times spent, shut down, obtaining particle diameter is that 10~12 μ m, water ratio are 1~2% modification fine fodder;
Step 4, with the C suction conveyor described modification fine fodder is moved to from high-speed mixer in the storage tank, again through metering packing, making particle diameter is that 10~12 μ m, water ratio are 1~2% superfine modified hydration White Carbon black goods.

Claims (1)

1. the preparation method of the superfine modified hydration White Carbon black of dry method comprises the composition and engineering method, it is characterized in that:
Described prescription is,
White Carbon black raw material: precipitated silica, particle diameter 70~90 μ m, water ratio 6~9%, 97%;
Auxiliary agent raw material: polyethylene wax, molecular weight 2000~3000,1%; Two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, CAS40372-72-3, molecular weight 539.0,1%; γ-mercaptopropyl trimethoxysilane, CAS4420-74-0, molecular weight 196.34,1%;
The prescription unit is weight percentage;
Described preparation technology is, ball milling, calcined dehydration, mixed aid,
Step 1, the White Carbon black raw material in will filling a prescription drop into planetary ball mill, and ball milling is carried out in start, 200~220 rev/mins of rotational speed of ball-mill, and 150~200 ℃ of ball milling temperature, 25 minutes ball milling times spent, shut down, obtaining particle diameter is the fines of 10~12 μ m;
Step 2, with the A suction conveyor described fines is moved to from the closed ball milling machine and to carry out calcined dehydration in the indirect type calcination rotary kiln, calcining temperature 550-600 ℃, 60 minutes calcining temperature times spent, afterwards, be cooled to room temperature, obtaining particle diameter is the dried fines of 10~12 μ m, water ratio 1~2%;
Step 3, with the B suction conveyor described dried fines is moved in the high-speed mixer from the indirect type calcination rotary kiln, auxiliary agent raw material in will filling a prescription again drops in the mixing machine, start mixes, mix 3000 rev/mins of rotating speeds, 140 ℃ of mixing temperatures, mix 15 minutes times spent, shut down, obtaining particle diameter is that 10~12 μ m, water ratio are 1~2% modification fine fodder;
Step 4, with the C suction conveyor described modification fine fodder is moved to from high-speed mixer in the storage tank, again through metering packing, making particle diameter is that 10~12 μ m, water ratio are 1~2% superfine modified hydration White Carbon black goods.
CN201310305463.4A 2013-07-09 2013-07-09 Preparation method for dry-process ultrafine modified hydrated white carbon black Expired - Fee Related CN103360797B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613956A (en) * 2013-11-25 2014-03-05 连云港东海硅微粉有限责任公司 Preparation method of mechanochemical modified silica micropowder
CN105713420A (en) * 2014-12-03 2016-06-29 中国石油天然气股份有限公司 Preparation methods of modified white carbon black

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010235783A (en) * 2009-03-31 2010-10-21 Dic Corp Surface-modified silica particle and active energy ray-curable resin composition using the same
CN101979443A (en) * 2010-10-12 2011-02-23 四川久大制盐有限责任公司 Method for producing modified white carbon black

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010235783A (en) * 2009-03-31 2010-10-21 Dic Corp Surface-modified silica particle and active energy ray-curable resin composition using the same
CN101979443A (en) * 2010-10-12 2011-02-23 四川久大制盐有限责任公司 Method for producing modified white carbon black

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613956A (en) * 2013-11-25 2014-03-05 连云港东海硅微粉有限责任公司 Preparation method of mechanochemical modified silica micropowder
CN103613956B (en) * 2013-11-25 2016-02-03 江苏联瑞新材料股份有限公司 The preparation method of mechanical-chemical modification silicon powder
CN105713420A (en) * 2014-12-03 2016-06-29 中国石油天然气股份有限公司 Preparation methods of modified white carbon black
CN105713420B (en) * 2014-12-03 2018-02-02 中国石油天然气股份有限公司 The preparation method of modified white carbon black

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