CN100491099C - Powder composite modification Method and device - Google Patents

Powder composite modification Method and device Download PDF

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CN100491099C
CN100491099C CNB2005100205021A CN200510020502A CN100491099C CN 100491099 C CN100491099 C CN 100491099C CN B2005100205021 A CNB2005100205021 A CN B2005100205021A CN 200510020502 A CN200510020502 A CN 200510020502A CN 100491099 C CN100491099 C CN 100491099C
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powder
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temperature
modifier
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CN1683138A (en
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毕舒
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Abstract

The powder compounding modification process includes the following steps: pre-mixing powder with metered modifier in a pre-mixer; mixing to modifying powder in the first modifying container at controlled temperature for the modifier to react; and modifying powder in the three-shaft eddy current high speed mixer for the second time to obtain the modified product. The present invention also discloses the apparatus therefor. The present invention has two stage modification apparatus capable of realizing the precise control of the modification process and three-shaft eddy current high speed mixer with excellent dispersing effect.

Description

Powder composition modification method and device
[technical field]
The present invention relates to the dispersing depolymerization that mixes of powder, be specifically related to a kind of composite modifying method and device of powder.
[background technology]
Powder body material must at first be handled through modification in being applied to macromolecular materials such as rubber, plastics the time.The method that modification is handled can be divided into dry method and wet method two big classes, and wherein is most common form with the dry method.Dry method modification is exactly (moisture generally≤0.5%) suitable chemical assistant of adding in the powder of drying, in specific device, handle, under certain process conditions (temperature, time) can obtain modified powder, and the technical indicator of modified powder first is an activation grade, requires〉95%; The secondth, check to have or not the graininess aggregate.The technology of dry method modification mainly is at the common powder below 2500 orders with device at present both at home and abroad, still is not applicable to superfine powder, the particularly modification technology and the device of the above superfine powder of 6000 orders so far.
Common powder is because grain graininess is thick, and the surface can be little, itself dispersed all right, thereby under the mechanical mixture of certain intensity, just can evenly mixing take place with surface modifier, and its powder granule is wrapped up by surface modifier and finishes the modification processing.
Handle common powder-modified used device, have two kinds at present, a kind of is high speed kneader (be also referred to as high mixer, height stirs machine), and this is that the powder dry method modification is the most commonly used both at home and abroad at present, also is the most ripe a kind of.For example: French OMYA company carries out powder-modified with this device exactly.The high speed kneader is a kind of powder dry method modification device of batch (-type) operation, thereby can only be used for the stearic acid parcel to common powder, and is difficult to be applicable to coupling agent modified.Its operation principle is with in powder and the disposable activating apparatus of packing into of modifier, the activating apparatus volume does not wait from several liters to hundreds of liter, the container of activating apparatus axially on two groups of shafts are arranged, rotation at a high speed under driven by motor, stir powder, make that powder and modifier are disposable to feed intake, batch production, output is controlled by vessel volume.Its shortcoming is that mixing intensity is not enough, because in the space of sealing, difficult control of temperature, labour intensity is big, and dust pollution is heavier.For superfine powder, because its surface can be big, thereby the poly-group of powder is difficult to disperse.
Another kind is the nearly 2 years three cylinder high-speed mixers that just occurred, basically form by three activating apparatus that form cylindrical tube outward, its operation principle is that three cylindrical tube axially parallel ground are arranged by serpentine, each inner barrel is upwards arranged in drum shaft rotor and stator, rotation at a high speed makes powder fully mix with modifier under driven by motor.Be characterized in that continuous dosing produces continuously, stirring intensity is big, and shortcoming is owing to there is not heater and the powder time of staying in equipment very short, thereby temperature is difficult to reach coupling agent and reacts needed temperature.For superfine powder, though its stirring intensity is bigger, because the time of staying is short, thereby final stirring and mixing effect is still relatively poor.And,, carry out modification by existing apparatus and be difficult to address this problem because powder tends to constantly occur the particle agglomeration phenomenon in modifying process.
[summary of the invention]
Purpose of the present invention is intended to overcome above-mentioned the deficiencies in the prior art, proposes a kind of dispersion and depolymerization that is particularly conducive to the powder reuniting particle, also is suitable for dissimilar coupling agent modified and modified effects good powder composition modification method and device.
The technical scheme that realizes above-mentioned purpose is: a kind of powder composition modification method comprises the steps:
1) powder is transported in the one-level modification container via pre-mix reservoir, and the metering spray adds modifier in the process that pre-mix reservoir is carried;
2) powder carries out mixed and modifiedly in one-level modification container, in modifying process one-level modification container is carried out temperature control, and it is in the temperature range that is suitable for the modifier reaction;
3) powder conveying that will finish after the one-level modification is carried out the secondary modification in three axial eddy super mixers, obtains finished product after finishing the secondary modification.
Described step 2) in the temperature of one-level modification container is controlled and can be realized by such process,
2a) heating one-level modification container makes it reach certain temperature;
2b) rotating speed of control one-level modification container changes its temperature, if temperature is lower than setting range, then improves rotating speed and elevates the temperature, if temperature is higher than setting range, then reduces rotating speed temperature is reduced.
The preferred high speed Hot mixer of described one-level modification container, the range of speeds when carrying out the one-level modification is 120~1800 rev/mins.
It is index that the standard that activation grade with powder reaches setting is finished preferably in described one-level modification.
In step 3), powder conveying also measurable spray in the process of three axial eddy super mixers is added and preceding identical modifier or second kind of modifier.
The range of speeds of three axial eddy super mixers is preferably 2400~3000 rev/mins in step 3).
The present invention also provides a kind of powder composition modification device, comprises measuring jet, first conveying device, one-level modification container, premix glassware, second conveying device and three axial eddy super mixers; Described measuring jet is arranged on the premix glassware, can in the process of premix glassware conveying powder partially modified dose be mixed with powder; The premix glassware is connected with one-level modification container by first conveying device, and one-level modification container is connected with three axial eddy super mixers by second conveying device; The housing of described one-level modification container is provided with heater, can powder wherein be heated.
The preferred high speed Hot mixer of described one-level modification container.
Described first, second conveying device all is preferably conveyor screw.
Described heater can be the heating jacket of the double-wall structure on the housing, wherein is filled with conduction oil, can heat the powder in the housing by the heat transmission of conduction oil.
Also can comprise second measuring jet, be arranged on second conveying device, can add modifier to powder spray wherein.
Adopt technique scheme, beneficial technical effects of the present invention is: 1) adopt the structure of two-stage reforming apparatus, be convenient to the accurate control to each stage of modifying process, satisfy required different condition of each stage; Owing to use three axial eddy super mixers as the secondary reforming apparatus, make the present invention have goodish dispersing depolymerization effect, the activation, the modification that are specially adapted to cohesive force is big between the particle powder and organic matter powder (as rubber powder, molding powder, food etc.) are handled; Before powder carries out modification, be provided with the step of premix, make powder more even with mixing of modifier.2) method of employing change rotating speed is carried out temperature control to one-level modification container, and is simple and easy to do, can fully satisfy the reaction condition of powder and modifier, improves modified effect.3) adopt the high speed Hot mixer as one-level modification container,, therefore, feed intake during production, can enhance productivity in inner control time in a big way disposable because the reaction time wherein can be by the people for controlling.4) with the powder activation grade as the index of whether finishing the one-level modification, can better more accurate control technological process, judge the optimum time of carrying out the secondary modification, help improve production efficiency and product quality.5) second nozzle is set, in secondary activation, adds the modifier of identical or different type, overcome the existing equipment once-through operation and can only throw in a kind of modifier and shortcoming that can not increment.
[description of drawings]
Fig. 1 is a kind of powder composition modification apparatus structure schematic diagram.
[specific embodiment]
Below by embodiment also in conjunction with the accompanying drawings, the present invention is described in further detail:
A kind of powder composition modification method comprises the steps:
1) powder is transported in the one-level modification container via pre-mix reservoir, and the metering spray adds modifier in the process that pre-mix reservoir is carried.Powder is realized mixing with the first time of modifier in this process.
2) powder carries out mixed and modifiedly in one-level modification container, in modifying process one-level modification container is carried out temperature control, and it is in the temperature range that is suitable for the modifier reaction.Described temperature control can realize by such process, heating one-level modification container makes it reach certain temperature earlier, the rotating speed of controlling one-level modification container again changes its temperature, if temperature is lower than setting range, then improving rotating speed elevates the temperature, if temperature is higher than setting range, then reduces rotating speed temperature is reduced.The preferred high speed Hot mixer of described one-level modification container, when powder carries out the one-level modification therein, the main shaft of high speed Hot mixer rotates (120~1800 rev/mins) at a high speed, the blade that drives on the axle is implemented strong shear-mixed to powder, and pass through heating and powder from the friction effect, temperature is risen to about 110~195 ℃, when surpassing setting range, temperature changes low speed rotation (120~200 rev/mins) into, when temperature is lower than when setting scope, change rotation (600~1800 rev/mins) at a high speed into, general after about 15 to 30 minutes, promptly finish the one-level modification.Whether this index of available activation grade detects the one-level modification of powder and finishes, and this technology generally requires the activation grade index after the one-level modification〉78%.
3) powder conveying that will finish after the one-level modification is carried out the secondary modification in three axial eddy super mixers.In that powder conveying also measurable spray in the process of three axial eddy super mixers is added and preceding identical modifier or second kind of modifier, can certainly not add, this application and needed modification situation on powder is decided.The powder (2400-3000 rev/min) under the powerful shear-mixed of high speed that enters three axial eddy super mixers is suspended state, fully mix, the superfine powder cluster of grains is torn apart simultaneously, temperature further rises, can remain between 120~220 ℃ according to the actual process condition, this temperature almost is suitable for all modifier.Through this operation, the activation grade of powder will 95%, thoroughly eliminate the agglomeration of particle simultaneously, flowability also is improved, and finally obtains finished product.
Realize the device of above-mentioned powder composition modification method, as shown in Figure 1, comprise measuring jet 2, premix glassware 4, as the conveyor screw 1 of first conveying device, as the hot mixing drum 10 of the high speed of one-level modification container, as conveyor screw 2 13, the three axial eddy super mixers 17 of second conveying device.
Described measuring jet 2 is provided with the weight metering that electronic scale 1 carries out modifier; Premix glassware 4 is provided with premix glassware charging aperture 3 and premix glassware discharging opening 5, and measuring jet 2 is arranged on the premix glassware charging aperture 3, can in the process of premix glassware conveying powder partially modified dose be mixed with powder; Conveyor screw 1 is provided with conveyor screw one discharging opening 7, and premix glassware discharging opening 5 is communicated with conveyor screw 1; The hot mixing drum 10 of high speed is arranged on the hot mixing drum pedestal 21 of high speed, also be provided with the hot mixing drum motor 22 of high speed on this pedestal 21, the hot mixing drum 10 of high speed is provided with hot mixing drum charging aperture 9 of high speed and the hot mixing drum discharging opening 11 of high speed, and conveyor screw one discharging opening 7 is communicated with the hot mixing drum charging aperture 9 of high speed by hookup 1; On the housing of the hot mixing drum 10 of high speed and be provided with heater (not drawing in the drawings), this heater is the heating jacket of the double-wall structure on the housing, wherein is filled with conduction oil, can powder wherein be heated; Conveyor screw 2 13 is provided with conveyor screw two charging apertures 12 and conveyor screw two discharging openings 14, and the hot mixing drum discharging opening 11 of high speed is communicated with conveyor screw two charging apertures 12; Three axial eddy super mixers 17 are arranged on the three axial eddy super mixer pedestals 20, which is provided with three axial eddy super mixer charging apertures 16 and three axial eddy super mixer discharging openings 19, conveyor screw two discharging openings 14 are communicated with three axial eddy super mixer charging apertures 16 by hookup 2 15.The said apparatus overall fixed is on reforming apparatus frame 23.
The concrete course of work:
1. powder is entered by premix glassware charging aperture 3, and modifier is sprayed in the premix glassware 4 by measuring jet 2 meterings after electronic scale 1 weighing, again by conveyor screw 1, realizes that powder mixes (premix) with the first time of modifier.
2. the powder through premix enters the hot mixing drum 10 of high speed by conveyor screw 1, carries out the one-level modification therein.From the friction effect and change self rotating speed and temperature is controlled in the scope that the modifier reaction suited, (for example activation grade) promptly finishes the one-level modification to the hot mixing drum 10 of high speed after reaching the index that sets by heating heat-conducting oil, powder.
3. the powder through the one-level modification enters three axial eddy super mixers 17 by conveyor screw 2 13, its three rotary main shafts 18 fully contact the particle that surface in the powder is not stained with modifier, mix with modifier by high-speed stirred, and carry out dispersing depolymerization completely, finally obtain finished product.
Modification experiment: get the heavy calcium carbonate powder of 6000 orders (2 μ〉90%), 120 kg, moisture≤0.3%, and titanate coupling agent (Nanjing dawn chemical plant ND131 or NDZ-131), addition is 0.25% to carry out the modification experiment.At first equipment is heated up to the heat-conducting oil heating in the heating jacket, when temperature reaches 150 ℃, beginning drops into powder continuously by the charging aperture of feeder and is metered into coupling agent simultaneously and (adds 60% during the feeder charging, the blender front end adds 10%, the middle part adds 25%, and the rear end adds 5%), mixing through three grades of activating apparatus successively, after 7 minutes, modification is finished.By National Standard Method test activation grade is 97%, and hand is touched the imperceptible any particle of powder.
Comparative Examples one: get with modification experiment in employed identical powder and modifier; with SHR-300 type high speed kneader (manufacturing of Zhangjiagang Machinery Plant of Light Industry) modification; stirring 5 minutes temperature rises to 150 ℃ and becomes low speed; high low speed like this alternately; shut down discharging after keeping the fast state cumulative time to reach 20 minutes, amounting to modification time is 63 minutes.By National Standard Method test activation grade is 70%, and hand is touched powder can feel more particle.
Comparative Examples two: get with modification experiment in employed identical powder and modifier, with SYR3 type three cylinder high-speed mixers (four directions, Jiangsu machine-building Co., Ltd makes) modification, to throw in the powder that does not add coupling agent equipment is being heated up certainly under the friction state earlier, temperature reaches 105 ℃ after 50 minutes, beginning drops into powder continuously and is metered into coupling agent simultaneously, and post-modification was finished in 18 minutes.By National Standard Method test activation grade is 52%, and hand is touched powder can feel a little particle.
Contrast above-mentioned example as seen, the present invention is a kind of composite modified machine with function of agglomerated particle depolymerization, is very suitable for ultra-fine and nano-powder.

Claims (8)

1, a kind of powder composition modification method is characterized in that, comprises the steps:
1) powder is transported in the one-level modification container via pre-mix reservoir, and the metering spray adds modifier in the process that pre-mix reservoir is carried;
2) powder carries out mixed and modified in one-level modification container, described one-level modification container is the high speed Hot mixer, the range of speeds when carrying out the one-level modification is 120~1800 rev/mins, and in modifying process, one-level modification container is carried out temperature control, it is in the temperature range that is suitable for the modifier reaction;
3) powder conveying that will finish after the one-level modification is carried out the secondary modification in three axial eddy super mixers, obtains finished product after finishing the secondary modification.
2, powder composition modification method according to claim 1 is characterized in that: control realizes by such process to the temperature of one-level modification container described step 2),
2a) heating one-level modification container makes it reach certain temperature;
2b) rotating speed of control one-level modification container changes its temperature, if temperature is lower than setting range, then improves rotating speed and elevates the temperature, if temperature is higher than setting range, then reduces rotating speed temperature is reduced.
3, powder composition modification method according to claim 1 is characterized in that: the activation grade index that is meant powder is finished in described one-level modification〉78%.
4, according to any described powder composition modification method of claim 1~3, it is characterized in that: in step 3) with powder conveying in the process of three axial eddy super mixers also the metering spray add and preceding identical modifier or second kind of modifier.
5, a kind of powder composition modification device comprises measuring jet, first conveying device, one-level modification container, it is characterized in that: also comprise premix glassware, second conveying device and three axial eddy super mixers; Described measuring jet is arranged on the premix glassware, can in the process of premix glassware conveying powder partially modified dose be mixed with powder; Described one-level modification container is the high speed Hot mixer, and the premix glassware is connected with the high speed Hot mixer by first conveying device, and the high speed Hot mixer is connected with three axial eddy super mixers by second conveying device; The housing of described high speed Hot mixer is provided with heater, can powder wherein be heated.
6, powder composition modification device according to claim 5 is characterized in that: described first, second conveying device is conveyor screw.
7, powder composition modification device according to claim 5 is characterized in that: described heater is the heating jacket of the double-wall structure on the housing, wherein is filled with conduction oil, can heat the powder in the housing by the heat transmission of conduction oil.
8, according to any described powder composition modification device of claim 5~7, it is characterized in that: also comprise second measuring jet, be arranged on second conveying device, can add modifier to powder spray wherein.
CNB2005100205021A 2005-03-07 2005-03-07 Powder composite modification Method and device Active CN100491099C (en)

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CN101293186B (en) * 2007-04-29 2012-01-25 东莞市金盛阻燃材料有限公司 Equipment for tiny nano-powder body blending and surface modifying
CN101502768B (en) * 2009-03-16 2011-03-16 浙江大学 Device for preparing composite absorption agent for semidry flue gas purification
CN101905131B (en) * 2010-07-27 2012-07-25 广州市合诚化学有限公司 Variable frequency low speed mixer and method for mixing materials with different stacking densities
CN102643566B (en) * 2012-05-11 2014-03-19 郑州市中岳涂料助剂有限公司 Composite titanium dioxide and preparation process thereof
CN105435719B (en) * 2015-11-26 2018-01-26 长沙高新开发区万华粉体设备有限公司 Powder surface modification depolymerizer and its method of modifying
CN105536628A (en) * 2016-01-25 2016-05-04 徐州徐工筑路机械有限公司 Efficient multi-stage agitator kettle
CN108610660A (en) * 2018-06-08 2018-10-02 桂林市标地新材料科技有限公司 A kind of modified osmanthus ink mountain flour body and its production technology
CN112191211B (en) * 2020-11-30 2021-03-16 北京艾科美特新材料开发有限公司 Preparation system for inorganic-organic composite material

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