CN117843263B - Array laser ablation phosphogypsum pretreatment method based on synchronous modification of composite carbon materials - Google Patents
Array laser ablation phosphogypsum pretreatment method based on synchronous modification of composite carbon materials Download PDFInfo
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- 238000000608 laser ablation Methods 0.000 title claims abstract description 42
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 22
- 238000002203 pretreatment Methods 0.000 title claims abstract description 10
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- 238000012986 modification Methods 0.000 title claims description 19
- 230000004048 modification Effects 0.000 title claims description 19
- 230000001360 synchronised effect Effects 0.000 title claims description 6
- 239000002994 raw material Substances 0.000 claims abstract description 84
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 27
- 238000009529 body temperature measurement Methods 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 230000010355 oscillation Effects 0.000 claims description 23
- 229910021389 graphene Inorganic materials 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 18
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 16
- 229910003472 fullerene Inorganic materials 0.000 claims description 16
- 238000009423 ventilation Methods 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 13
- 239000011797 cavity material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 6
- 239000000375 suspending agent Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 3
- 230000000750 progressive effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 229910052602 gypsum Inorganic materials 0.000 description 5
- 239000010440 gypsum Substances 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000002679 ablation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 125000003003 spiro group Chemical group 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/362—Laser etching
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/005—Preparing or treating the raw materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/024—Ingredients added before, or during, the calcining process, e.g. calcination modifiers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/028—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/268—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke pelletizing of the material before starting the manufacture
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- Tunnel Furnaces (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The method comprises the steps of ball milling phosphogypsum raw materials based on an array laser ablation phosphogypsum pretreatment method with synchronously modified composite carbon materials, tiling the ball milled raw materials, and feeding the raw materials into an array laser ablation furnace; starting an array laser ablation furnace, moving array laser according to a preset route, ablating the tiled raw materials, ventilating and exhausting the furnace, and determining the moving speed range and the time consumption on the preset route through infrared temperature measurement; according to the determined moving speed and the determined time, the raw materials laid in batches are processed in the array laser ablation furnace, and each time a batch of raw materials laid in batches is processed, a suspending system containing carbon materials is sprayed on the surface of the raw materials, and finally the raw materials are dried to finish pretreatment, so that the pretreatment efficiency and the impurity removal uniformity of phosphogypsum are improved, and the bending resistance of the formed plate is enhanced.
Description
Technical Field
The application relates to a phosphogypsum pretreatment method, in particular to an array laser ablation phosphogypsum pretreatment method for synchronously modifying composite carbon materials.
Background
Phosphogypsum is a general raw material for heat insulation and high temperature resistance, and contains soluble and crystal-form impurities such as phosphorus, fluorine, carboxylic ester, alkane derivatives and the like, and particularly the latter two restrict the possibility of direct use. It is usually required to pretreat it by chemical, physical and biological methods to obtain it.
Wherein the chemical method comprises lime method and acid method. While physical methods have more options including water washing, flotation, ball milling, screening, natural blowing, and heat treatment. The water washing method is easy to lose quality, the floatation standing time is long, the ball milling starts through a modified structure, other methods are usually needed to be combined, screening is easy, screening is not in place, natural wind blowing is easy and appropriate, particulate impurities in other atmospheres are introduced, and the process is prolonged under windless conditions. The heat treatment method generally refers to calcination, but the calcination often adopts batch, the temperature is not uniformly raised, the temperature raising process is long, and the generated gas is difficult to be efficiently discharged for phosphogypsum to be treated, which is accumulated in a furnace and is pressed below. Because phosphogypsum has poor mechanical properties, modification of other materials is usually required to be considered, and the possibility of modification in the pretreatment process is not considered in the prior art, so that the pretreated phosphogypsum is required to be subjected to a secondary modification process. The whole process has low efficiency. And the space for modification is also to be increased.
Disclosure of Invention
Based on the above-described problems of the prior art, the present invention provides a feasible method of simultaneous modification and contemplates a more sophisticated laser ablation method. In view of the two aspects, the invention provides an array laser ablation phosphogypsum pretreatment method based on synchronous modification of composite carbon materials, which comprises the following steps:
S1, ball milling is carried out on phosphogypsum raw materials, the raw materials after ball milling are tiled, and the raw materials are sent into an array laser ablation furnace;
S2, starting an array laser ablation furnace, moving an array laser according to a preset route, ablating the tiled raw materials, ventilating and exhausting the furnace, and determining the moving speed range and time consumption on the preset route through infrared temperature measurement;
S3, according to the determined moving speed and the time, the tiled raw materials are processed in batches in the array laser ablation furnace, each batch of the tiled raw materials is processed, a suspension system containing carbon materials is sprayed on the surface of the tiled raw materials, and finally the raw materials are dried and pretreated.
It can be understood that the phosphogypsum is changed into fine particles by adopting a ball milling mode, heat is efficiently collected and volatile gas is removed by laser ablation of a walking array, and the phosphogypsum is taken away by ventilation and exhaust. The walking speed and the time are determined by infrared temperature measurement, so that the ablation temperature is ensured to be within a preset range. When the walking speed is different, the heating condition of heat generation and heating up are different in the unified ablation area due to different reciprocating action frequency, so that the walking speed and the time consumption need to be considered, and the walking speed and the time consumption are related to the tiled size. When the speed is too low, steam smoke is generated locally to take away gypsum components, and when the speed is too high, the heating efficiency is not high. Because the laser ablation has short action time and rapid temperature rise, the heating efficiency is higher than that of the traditional integral heating.
Optionally, the feedstock after ball milling is at a particle size of 40-150 mesh.
Optionally, the ball-milled raw materials are tiled by using a heat-insulating ceramic disc.
Preferably, the ball-milled raw material loaded into the heat-insulating ceramic disk is tiled by shaking of a shaker.
More preferably, the thickness of the tile is 0.3-1cm.
The array laser ablation furnace comprises a furnace body with supporting legs, an inlet and an outlet for a conveyor belt to enter and exit respectively on the furnace body, two sealing doors arranged at the inlet and the outlet, a vent arranged on the side surface where the sealing doors are arranged, and an exhaust port arranged on the other side surface where the sealing doors are arranged, at least two infrared temperature measuring ports arranged on one side surface different from the side surfaces where the vent and the exhaust port are arranged, an infrared temperature measuring gun is inserted to perform multipoint temperature test on the surface of the flat-bed raw material in the furnace, and a movable array laser arranged at the top of the furnace body, wherein the furnace body is provided with an inner cavity, and raw materials which are tiled and ball-milling is completed can be placed, so that laser ablation impurity removal is performed.
Optionally, the portable array laser includes the array laser head, supplies the movable frame that the array laser head set up, the parallel guide rail that furnace body top upper surface both ends set up, with the guide block that the movable frame is connected, at the outer upper surface of furnace body top set up, be used for with parallel guide rail cooperation, and through pass a lead screw of the spiro union portion at guide block top and pass a slide bar or another lead screw of guide block top second connect portion, by at least one motor drive for spiro union portion with second connect portion do first reciprocating motion.
Optionally, a second guide block is disposed on the top of the moving frame and located below the top lower surface of the furnace body, so that the moving frame makes a second reciprocating motion perpendicular to the first reciprocating motion direction with respect to the second guide block.
It will be readily appreciated that at least one embodiment provides for a lead screw structure on the carriage that is threaded through the second guide block to effect reciprocal movement of the carriage relative to the second guide block.
Optionally, the array laser heads are in a square matrix or a single row, and the total number of the laser heads is 3-9.
Preferably, the first reciprocating movement and the second reciprocating movement are performed simultaneously, so that the movement of each light spot shot on the tiled raw material in the array laser head is performed according to the preset route as a zigzag track or a progressive scanning movement track.
Preferably, the laser head is a solid-state laser, and the irradiation spot diameter is 5-11mm.
It will be appreciated that by appropriate adjustment of the reciprocation amplitude and timing of the first and second reciprocations, the tiled material can be illuminated in full coverage by progressive scanning movement with no or little overlap between the multiple illumination ranges of the spots of adjacent laser heads formed by the second reciprocations. The impurities in the ablated material are heated and gasified, so that the ablated material is conveyed away from the inner cavity of the furnace body through ventilation and exhaust.
Alternatively, the movement speed is in the range of 1-10cm/s and the laser power density is 500-1500W/cm 2. The total time of use is determined according to the length and width of the heat insulation ceramic disc and the detection of the impurity removal effect. According to 1500W/cm 2, calculating according to specific heat capacity of gypsum 1.1 kJ/(kg. DEG C), carrying out one-time treatment on the volume of phosphogypsum tiled and ball-milled at 60cm multiplied by 40cm multiplied by 1cm, wherein the fixed point can be heated to about 800 ℃ only by about 0.1-0.2s under a light spot of 1cm 2, so that the impurity removal can be finished by a single row of laser heads in 60cm dimension according to the first reciprocating direction, and in an ideal state, only about 6 s. The time production is about 0.3 ton of impurity removing gypsum, if a square matrix laser head is additionally arranged, the time consumption can be reduced by at least half, and the number of the array laser ablation furnaces, such as 2-3, can meet the time production 2-3 ton order of magnitude requirement.
Preferably, a through groove is formed in the center of the top of the furnace body, the second guide block penetrates through the through groove to be connected with the guide block, rubber pairs are arranged on two sides of the through groove, so that in the first reciprocating motion, all through grooves on all places where the second guide block is not located are masked by the rubber pairs, and when the second guide block moves to a place where the second guide block is located, the portion, located at the place where the second guide block is located, of the rubber pairs is only spread.
Optionally, the wire harness led out by each laser head is formed and the rubber pair is spread to pass through the through groove and led out of the furnace body.
Preferably, the vent is configured as a space with the lowest end positioned above the plane of the top of the heat insulation ceramic disc, the exhaust port is configured as a space with the lowest end higher than the highest end of the vent, and the axes of the vent and the exhaust port are respectively configured to be close to the inner walls of two opposite sides of the furnace body. Therefore, the rotary air flow is easier to form in the inner cavity of the furnace body, and the air flow is easier to guide and carry out ablated air.
Preferably, the ventilation flow is equal to the air draft flow and is 500-10000sccm.
Preferably, the carbon material in the suspension system sprayed with the carbon material is graphene or Graphene Oxide (GO) loaded with fullerene spheres (fullerers), and the suspending agent is pure water.
Preferably, the shaking table is carried out on the heat-insulating ceramic disk loaded with the raw materials after the impurity removal at the same time of spraying. Thereby uniformly covering the surface of the raw material particles.
Optionally, the drying temperature is 60-100 ℃.
And further, S4, adding the dried modified material into lime slurry and water, and stirring to prepare slurry.
Optionally, the processing method is performed by a pretreatment pipeline, and the pretreatment pipeline sequentially comprises the following steps according to the process flow sequence: the ball milling area is used for ball milling phosphogypsum raw materials, the feeding area is used for feeding a proper amount of ball-milled raw materials into the heat insulation ceramic disc in the shaking table oscillation tiling area, the shaking table oscillation tiling area is used for tiling the ball-milled raw materials fed into the heat insulation ceramic disc through shaking table oscillation, the impurity removal area is used for carrying out laser ablation impurity removal on the tiled ball-milled raw materials by adopting the array laser ablation furnace, the modification area is used for shaking table oscillation and applying a suspension system containing carbon materials to the surface of the impurity-removed raw materials, the drying area is used for drying the modified raw materials, the discharging area is used for collecting the dried raw materials, and the vacated heat insulation ceramic disc is continuously conveyed back into the shaking table oscillation tiling area through the conveying belt to continue feeding, so that the circulation is continued.
It will be readily appreciated that when recycled, the modified pretreated gypsum is also obtained on a 2-3 ton scale.
Optionally, graphene or Graphene Oxide (GO) loaded with fullerene spheres (fullerers), and the suspending agent is pure water.
Optionally, a pedestrian passageway is arranged between the drying area and the blanking area, and the same side of the shaking table oscillation tiling area, the impurity removing area and the modifying area is surrounded by the conveyer belt to define a working area.
It will be readily appreciated that the host machine of the laser head, the pump used for spraying the retrofit area, and the reagent containers may all be placed in the work area where personnel may perform inspection and maintenance of the various placed instruments and appliances. The heat-insulating ceramic trays can be taken out of the drying area at the pedestrian passageway by manpower and collected in the blanking area.
In addition, there may be at least one embodiment in which a conveyor belt is arranged between the drying zone and the blanking zone, in which case the staff may enter the working zone through the space between the conveyor belt bottom brackets. A slide plate which can be turned up can be arranged between the drying area and the blanking area, and the slide plate can be turned up when the work area needs to be entered.
Preferably, the mass ratio of the carbon material in the raw material subjected to impurity removal is 0.02-0.04%.
More preferably, the mass ratio is 0.03%.
Advantageous effects
1. The method for tiling raw materials after ball milling is realized by adopting high-power array laser ablation, so that the heating time is shortened, and phosphogypsum is rapidly and uniformly decontaminated by stable ventilation and air exhaust.
2. After impurity removal, graphene oxide loaded by fullerene balls is sprayed on the surface of the raw material for modification by oscillation, so that the bending resistance of the gypsum board is improved,
3. And the improved step is added into the phosphogypsum pretreatment step by adopting pipeline operation, so that the overall process efficiency is improved.
Drawings
Figure 1a flow chart of a method for pretreating phosphogypsum by array laser ablation based on synchronous modification of composite carbon material in embodiment 1 of the invention,
FIG. 2 is a schematic diagram of a pretreatment pipeline layout on which the phosphogypsum pretreatment method of the embodiment 1 of the present invention is based, wherein the broken line chamfering box is a key flow link related to the present invention and distinguished from the existing phosphogypsum pretreatment,
FIG. 3 is a schematic front view of an array laser ablation furnace according to step S1 of the phosphogypsum pretreatment method in the embodiment 1 of the present invention, showing the position states of a heat insulation ceramic disk C in the inner cavity of the furnace body, a conveyor belt D, a laser head 3 in the movable array laser, an air inlet, an air outlet and an infrared temperature measuring port 1,
Fig. 4 is a schematic side view of the array laser ablation furnace from the inlet side, also showing the position states of the heat insulation ceramic disk C, the conveyor belt D, the air inlet, the air outlet and the infrared temperature measuring port 1, and showing the position state of the door seal,
Fig. 5 shows the raw material S spread on the moving rack and the array laser head 3 after ball milling carried in the insulating ceramic disk C in the view of fig. 4,
Figure 6 is a schematic view of a partial oblique view of the top of the body of the array laser ablation furnace,
FIG. 7 is a schematic view of the composition of fullerene sphere-supported graphene oxide 4, and a schematic view of the state of raw material particles after the fullerene sphere-supported graphene oxide 4 in water suspension is sprayed onto the raw material after the impurity removal,
FIG. 8 shows a comparison of bending resistance at the point of the maximum 0.03% doping ratio (mass ratio) for a carbon nanotube, pure graphene, and fullerene sphere-supported graphene oxide 4 of the present example,
Fig. 9 shows the state of fullerene sphere-supported graphene oxide 4 in the gaps before and after formation in a slurry, in which direction indications of the lateral and longitudinal movement between the agglomerated particles 5 after formation are given.
The ball mill comprises a reference numeral 1, an infrared temperature measuring port 2, a rubber sheet with a cross opening, 3, an array laser head 4, graphene oxide loaded by fullerene balls, 5, agglomerated particles, C, a heat insulation ceramic disc, D, a conveyor belt, S and raw materials which are tiled after ball milling.
Detailed Description
Example 1
The embodiment describes an array laser ablation phosphogypsum pretreatment method based on composite carbon material synchronous modification, and as shown in fig. 1, the method comprises the following steps:
S1, ball milling is carried out on phosphogypsum raw materials, the raw materials after ball milling are tiled, and the raw materials are sent into an array laser ablation furnace;
S2, starting an array laser ablation furnace, moving an array laser according to a preset route, ablating the raw materials laid flat, ventilating and exhausting the furnace, and determining the optimal moving speed and time consumption on the preset route through infrared temperature measurement;
S3, according to the determined moving speed and the time, batch processing the tiled raw materials in the array laser ablation furnace, spraying a suspension system containing carbon materials on the surface of each batch of the tiled raw materials after processing, and finally drying to finish pretreatment;
s4, adding the dried modified material into lime slurry and water, and stirring to prepare slurry.
Wherein, the ball milling requirement is 100 meshes, and shaking tables are adopted for shaking during tiling and modification. In particular as shown in fig. 2. The pretreatment assembly line sequentially comprises the following steps according to the process flow sequence: the ball milling area is used for ball milling phosphogypsum raw materials, the feeding area is used for feeding a proper amount of ball-milled raw materials into the heat insulation ceramic disc in the shaking table oscillation tiling area, the shaking table oscillation tiling area is used for tiling the ball-milled raw materials fed into the heat insulation ceramic disc through shaking table oscillation, the impurity removal area is used for carrying out laser ablation impurity removal on the tiled ball-milled raw materials by adopting the array laser ablation furnace, the modification area is used for shaking table oscillation and applying a suspension system containing carbon materials to the surface of the impurity-removed raw materials, the drying area is used for drying the modified raw materials, the discharging area is used for collecting the dried raw materials, and the vacated heat insulation ceramic disc is continuously conveyed back into the shaking table oscillation tiling area through the conveying belt to continue feeding, so that the circulation is continued.
The heat-insulating ceramic plate can be sleeved with a collision-resistant high-temperature-resistant collision-resistant sleeve, so that the heat-insulating ceramic plate can be buffered when being transported on a conveyor belt, especially in the process of being discharged from a drying area to a discharging area. The size of the heat-insulating ceramic plate is 50-60cm multiplied by 30-40cm.
As shown in fig. 3 and 4, the array laser ablation furnace comprises a furnace body with supporting legs, an inlet and an outlet for feeding in and out a conveyor belt at the left side and the right side on the furnace body, two sealing doors (which can be electric doors) arranged at the inlet and the outlet, a ventilation opening arranged at the side where the sealing doors are arranged, and an exhaust opening arranged at the other side where the sealing doors are arranged, three infrared temperature measuring openings 1 with cross-shaped opening rubber 2 arranged on the side where the ventilation opening and the exhaust opening are arranged on the furnace body, wherein the infrared temperature measuring guns are inserted into the surfaces of raw materials S which are subjected to ball milling in the furnace for three-point temperature test, and movable array laser arranged at the top of the furnace body, wherein the furnace body is provided with an inner cavity, and the raw materials S which are subjected to ball milling and tiling can be placed for laser ablation impurity removal. When the temperature measuring gun is taken out from the infrared temperature measuring port, the cross-shaped opening rubber sheet 2 masks the infrared temperature measuring port 1.
As shown in fig. 3, 5 and 6, the movable array laser comprises an array laser head 3 composed of 6 solid-state lasers (1.5 kW/cm 2, with a spot diameter of 10 mm) in a single row, a movable frame for arranging the array laser head 3, parallel guide rails arranged at two ends of the upper surface of the top of the furnace body, a guide block connected with the movable frame and arranged on the upper surface of the top of the furnace body, and used for matching with the parallel guide rails, and the movable array laser is driven by two motors (one of which is blocked due to view angle in fig. 3) through one screw rod passing through a screw joint part at the top of the guide block and the other screw rod passing through a second joint part at the top of the guide block, so that the screw joint part and the second joint part perform a first reciprocating movement (indicated by a double-headed arrow in fig. 6) along the conveying direction of the conveyor belt (from right to left in fig. 3).
As shown in fig. 5, a second guide block provided at the top of the moving frame below the top lower surface of the furnace body is connected so that the moving frame makes a second reciprocating motion perpendicular to the first reciprocating motion direction with respect to the second guide block. Specifically, the second reciprocating motion is achieved on the moving frame by a high-frequency reciprocating cylinder.
As shown in fig. 6, the center of the top end of the furnace body is provided with a through groove provided with a rubber pair, and the second guide block is connected with the guide block by stretching the rubber pair, so that the motor drives the screw rod to rotate, the screw joint part and the second joint part do first reciprocating motion, the second guide block stretches the rubber pair to the place where the rubber pair does not reach, and the rubber pair masks the inner cavity of the furnace body. The outgoing lines of the solid-state laser are formed into a wire bundle, and the wire bundle also stretches the rubber pair to be led out of the furnace cavity. The width of the through slots is preferably at least the range of the amplitude of the second reciprocation so that the beam of a single row of solid state lasers can follow the wobble while reducing the blocking effect of the through slots.
The ventilation opening is configured as a space of which the lowest end is positioned above the plane of the top of the heat insulation ceramic disc, the ventilation opening is configured as a space of which the lowest end is higher than the uppermost end of the ventilation opening, and the axes of the ventilation opening and the ventilation opening are respectively configured to be close to the inner walls of two opposite sides of the furnace body. Therefore, the rotary air flow is easier to form in the inner cavity of the furnace body, and the air flow is easier to guide and carry out ablated air. The ventilation flow is equal to the air draft flow and is 1000sccm.
As shown in fig. 3, ventilation and air suction are started, when the conveyor belt D passes through the opened inlet sealing door (i.e., right sealing door) to the heat-insulating ceramic disk C carrying the raw material S spread after ball milling, the inlet sealing door is closed, and the outlet sealing door (left side) is also closed. At this time, the single-row solid-state laser is in the state of returning to the initial position, and the second reciprocating motion driven by the high-frequency reciprocating electric cylinder is increased in frequency (when more frequency increasing is needed if starting from rest at first), and the scanning motion is started. The first reciprocating motion goes back and forth once, returns to the initial position state, closes the laser, takes 8s, and the second reciprocating motion frequency-reduces, opens two seals at this time, and the conveyor belt D sends out the heat-insulating ceramic plate C to the modification area.
As shown in fig. 2, the processing method is performed by a pretreatment pipeline, and the pretreatment pipeline sequentially comprises the following steps according to the process flow sequence: the ball milling area is used for ball milling phosphogypsum raw materials, the feeding area is used for feeding a proper amount of ball-milled raw materials into the heat insulation ceramic disc C in the shaking table oscillation tiling area, the shaking table oscillation tiling area is used for tiling the ball-milled raw materials fed into the heat insulation ceramic disc C through shaking table oscillation, the impurity removal area is used for carrying out laser ablation impurity removal on the tiled ball-milled raw materials by adopting the array laser ablation furnace, the modification area is used for shaking table oscillation and applying a suspension system containing carbon materials to the surface of the impurity-removed raw materials, the drying area is used for drying the modified raw materials, the discharging area is used for collecting the dried raw materials, and the vacated heat insulation ceramic disc C is continuously conveyed into the shaking table oscillation tiling area through a conveying belt by a production line, so that the continuous circulation is realized. A pedestrian passageway is arranged between the drying area and the blanking area, and the same side of the shaking table oscillating tiling area, the impurity removing area and the modifying area is surrounded by the conveyer belt to define a working area.
Example 2
In the modification zone, as shown in fig. 7, the graphene oxide 4 loaded by the fullerene spheres suspended in water is sprayed onto the raw material after the impurity removal, and the heat-insulating ceramic disc C is oscillated by using a concentrating table, so that the spraying is uniform.
As shown in fig. 8, compared to the carbon nanotube, the pure graphene, and the fullerene sphere-supported graphene oxide 4 of the present example, the fullerene sphere-supported graphene oxide 4 has a better bending resistance than the carbon nanotube doping at the point of the maximum 0.03% doping ratio (mass ratio).
As shown in fig. 9, the fullerene sphere-supported graphene oxide 4 is attached to the raw material particles. After the treatment of step S4 in example 1, graphene oxide 4 was present in the slurry in the interstitial liquid phase between the agglomerate grains 5, and after the sheet was formed, these interstitial liquid phases were formed into gaps by drying, and at this time, the fullerene-supported graphene oxide 4 remained in the gaps. When the movement between the agglomerated particles 5 in the direction of the arrow in the figure is generated, the interface generates larger transverse friction or longitudinal gap-closing movement due to the existence of the fullerene balls, and the position of the graphene oxide 4 loaded by the fullerene balls is more difficult to be longitudinally torn due to the transverse friction contribution of the graphene oxide 4. Because the carbon nano tube surface is axially smooth and has small area, larger transverse friction is not provided, so that the transverse sliding among the agglomerated particles is easier, and the agglomerated particles are easily influenced by shearing force. Therefore, based on the above-mentioned mechanical analysis in the transverse and longitudinal directions, the fullerene sphere-supported graphene oxide 4 improves the bending resistance as a whole.
Claims (7)
1. The array laser ablation phosphogypsum pretreatment method based on the synchronous modification of the composite carbon material is characterized by comprising the following steps of: s1, ball milling is carried out on phosphogypsum raw materials, the raw materials after ball milling are tiled, and the raw materials are sent into an array laser ablation furnace;
s2, starting an array laser ablation furnace, moving an array laser according to a preset route, ablating the tiled raw materials, ventilating and exhausting the furnace, and determining the moving speed range and time consumption on the preset route through infrared temperature measurement;
s3, according to the determined moving speed and the time, batch processing the tiled raw materials in the array laser ablation furnace, spraying a suspending agent containing carbon materials on the surface of each batch of the tiled raw materials after processing, and finally drying to finish pretreatment; the carbon material in the suspending agent sprayed with the carbon material is graphene oxide loaded with fullerene spheres;
The array laser ablation furnace comprises a furnace body with supporting legs, an inlet and an outlet for a conveyor belt to enter and exit respectively, and two sealing doors arranged at the inlet and the outlet; a ventilation opening arranged on the side surface of the sealing door and an exhaust opening arranged on the side surface of the other sealing door; at least two infrared temperature measuring ports arranged on one side surface different from the side surfaces of the ventilation opening and the exhaust opening, and used for inserting an infrared temperature measuring gun to perform multipoint temperature test on the surface of the raw material laid in the furnace and a movable array laser arranged at the top of the furnace body; wherein, the furnace body is provided with an inner cavity, and raw materials which are tiled and ball-milled can be placed for laser ablation impurity removal; the movable array laser comprises an array laser head and a movable frame arranged for the array laser head;
The parallel guide rails are arranged at two ends of the upper surface of the top of the furnace body, and the guide blocks are connected with the moving frame and are arranged on the outer upper surface of the top of the furnace body, are used for being matched with the parallel guide rails, and are driven by at least one motor through one screw rod passing through a screw joint part at the top of the guide blocks and one slide rod or the other screw rod passing through a second joint part at the top of the guide blocks, so that the screw joint part and the second joint part do first reciprocating movement;
A second guide block arranged at the top of the movable frame and positioned below the lower surface of the top of the furnace body is connected, so that the movable frame makes a second reciprocating motion perpendicular to the first reciprocating motion direction relative to the second guide block;
The array laser heads are in a square matrix or a single row, and the total number of the included laser heads is 3-9;
The first reciprocating movement and the second reciprocating movement are performed simultaneously, so that the movement of each light spot shot on the tiled raw material in the array laser head is performed according to the preset route as a zigzag track or a progressive scanning movement track, the laser head is a solid-state laser, the irradiation light spot diameter is 5-11mm, the movement speed range is 1-10cm/s, and the laser power density is 500-1500W/cm 2.
2. The method according to claim 1, wherein the ball-milled raw material is tiled by using a heat-insulating ceramic disc, the ball-milled raw material is tiled by using a shaking table to oscillate at a granularity of 40-150 meshes, and the thickness of the tiled raw material is 0.3-1cm.
3. The method according to claim 1, wherein the furnace body has a through slot in the center of the top for the second guide block to pass through for connecting the guide blocks, and rubber pairs are provided on both sides of the through slot, so that in the first reciprocating motion, the through slot on all places where the second guide block is not located is masked by the rubber pair, and when the second guide block moves to the place where the rubber pair is located and the vicinity thereof is spread, wire harnesses led out by the laser heads are formed and spread the rubber pair to be led out of the furnace body through the through slot.
4. The method of claim 1, wherein the vent is configured as a space above the plane of the top of the insulating ceramic disk at its lowermost end, the suction port is configured with its lowermost end higher than the uppermost end of the vent, and the axes of the vent and suction port are respectively configured to be adjacent to opposite side inner walls of the furnace body.
5. The method according to claim 1, wherein the suspending agent is pure water, the mass ratio of the carbon material in the raw material after impurity removal is 0.02-0.04%, and the insulating ceramic disc carrying the raw material after impurity removal is subjected to shaking table oscillation while spraying.
6. The method of claim 1, further comprising S4 adding the dried modified stock to lime slurry and water after S3, and stirring to form a slurry.
7. The method of claim 1, wherein the processing is performed using a pre-processing pipeline comprising, in process flow order: the ball milling area is used for ball milling phosphogypsum raw materials, the feeding area is used for feeding a proper amount of ball-milled raw materials into the heat insulation ceramic disc in the shaking table oscillation tiling area, the shaking table oscillation tiling area is used for tiling the ball-milled raw materials fed into the heat insulation ceramic disc through shaking table oscillation, the impurity removal area is used for carrying out laser ablation impurity removal on the tiled ball-milled raw materials by adopting the array laser ablation furnace, the modification area is used for shaking table oscillation and applying a suspending agent containing carbon materials to the surface of the impurity-removed raw materials, the drying area is used for drying the modified raw materials, the discharging area is used for collecting the dried raw materials, and the vacated heat insulation ceramic disc is continuously conveyed back into the shaking table oscillation tiling area through the conveying belt to continue feeding, so that the circulation is continued.
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| CN115744960A (en) * | 2022-12-13 | 2023-03-07 | 中国科学院过程工程研究所 | System device and method for removing impurities of phosphogypsum and low-impurity phosphogypsum obtained by system device and method |
| CN116375376A (en) * | 2023-04-18 | 2023-07-04 | 湖北省地质科学研究院(湖北省富硒产业研究院) | Method for preparing short columnar alpha-type semi-hydrated gypsum by using calcium carbide slag ball-milling modified phosphogypsum through hydrothermal process |
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| CA2852385C (en) * | 2008-07-31 | 2017-07-11 | Yoshino Gypsum Co., Ltd. | Process for continuous modification of dihydrate gypsum and modified dihydrate gypsum obtained by the process |
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| CN115744960A (en) * | 2022-12-13 | 2023-03-07 | 中国科学院过程工程研究所 | System device and method for removing impurities of phosphogypsum and low-impurity phosphogypsum obtained by system device and method |
| CN116375376A (en) * | 2023-04-18 | 2023-07-04 | 湖北省地质科学研究院(湖北省富硒产业研究院) | Method for preparing short columnar alpha-type semi-hydrated gypsum by using calcium carbide slag ball-milling modified phosphogypsum through hydrothermal process |
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