CN112871122A - Reaction kettle for preparing nano silicon modified steel fibers in large batch and preparation method - Google Patents
Reaction kettle for preparing nano silicon modified steel fibers in large batch and preparation method Download PDFInfo
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- CN112871122A CN112871122A CN202011618468.9A CN202011618468A CN112871122A CN 112871122 A CN112871122 A CN 112871122A CN 202011618468 A CN202011618468 A CN 202011618468A CN 112871122 A CN112871122 A CN 112871122A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
A reaction kettle for preparing nano silicon modified steel fibers in a large scale and a preparation method belong to the technical field of concrete preparation. The equipment comprises a plurality of grid plates for placing steel fibers, a plurality of grid plates for supporting the steel fibers and the grid plates, a liquid medicine reaction box and a water bath temperature adjusting box for placing the liquid medicine reaction box; the liquid medicine reaction box is used for accommodating a plurality of grid plates, steel fibers and reaction liquid medicine. The preparation method comprises the following steps: s2, uniformly spreading common steel fibers in each steel fiber throwing area of the grid plate 7; s4, feeding the reaction solution into a liquid medicine reaction box; s5, opening a water bath temperature adjusting box to carry out water bath; s6, adding clear water into the liquid medicine reaction box to rinse the steel fibers; and S7, opening a water bath temperature adjusting box for drying. The invention can effectively avoid the peeling of the nano silicon coating, greatly enhance the bonding stress of the steel fiber-matrix interface and play a role in enhancing and toughening the cement-based material.
Description
Technical Field
The invention belongs to the technical field of concrete preparation, and particularly relates to a reaction kettle for preparing nano silicon modified steel fibers in a large scale and a preparation method.
Background
The traditional concrete material has the defects of low compressive/tensile strength, large brittleness, easy cracking and the like, and in order to make up for the disadvantages of the concrete material, a proper amount of hooks, corrugations, short straight steel fibers and the like are added to meet the toughness requirement in the structural design. However, the traditional concrete material has large water cement ratio, loose microstructure inside the material and limited bonding property of the steel fiber-matrix interface. The ultra-high performance concrete has high pozzolan activity components by reducing the water-cement ratio, greatly adding silica fume, fly ash, slag and the like, consuming excessive calcium hydroxide generated by cement hydration by utilizing the 'secondary hydration effect', effectively improving the interface bonding performance of the steel fiber-matrix, and reaching the interface bonding strength of 3.9-4.8MPa when the water-cement ratio is 0.2. But the strength of the steel fiber is high, the damage of UHPC is mainly expressed as the compression damage of the matrix, the steel fiber is mainly pulled out at the moment, the stress on the steel fiber is small in the pulling-out process, the steel fiber is still in the elastic stress stage, the utilization rate of the strength of the steel fiber is low, and the pulling-out energy consumption is low. The steel fiber is modified by the nano silicon, so that the bonding stress of the steel fiber-matrix interface can be effectively improved, and the strength utilization rate of the steel fiber is improved.
The generation of nano-silicon is completed in a static solution, and the deposition quality, thickness and uniformity of the nano-silicon on the surface of the steel fiber are related to the concentration of the nano-silicon in the solution around the steel fiber. The thickness is different inevitably in the fiber spreading process, which greatly influences the growth of the nano silicon coating on the surface of the steel fiber. And the modified steel fiber nano silicon which is overlapped with each other is peeled off in the cleaning process.
Disclosure of Invention
The invention aims to provide a reaction kettle for preparing nano silicon modified steel fibers in large batch and a preparation method, and aims to solve the technical problems that the thickness of a nano silicon coating on the surface of the steel fiber is not uniform, and the nano silicon coating is peeled off due to the water flow velocity in the rinsing process after modification.
In order to solve the technical problems, the specific technical scheme of the reaction kettle for preparing the nano silicon modified steel fibers in large batch and the preparation method is as follows:
a reaction kettle for preparing nano silicon modified steel fibers in large batch comprises a plurality of grid plates for placing the steel fibers, a plurality of grid plates for supporting the steel fibers and the grid plates, a liquid medicine reaction box and a water bath temperature adjusting box for placing the liquid medicine reaction box; the liquid medicine reaction box is used for accommodating a plurality of grid plates, steel fibers and reaction liquid medicine; and valves are arranged on the water bath temperature regulating box and the liquid medicine reaction box and are respectively used for discharging water and reacting liquid medicine.
A preparation method for preparing nano silicon modified steel fibers in large batch comprises the following steps:
s1, combining a group of grid plates and grate plates and placing the grid plates and the grate plates into a liquid medicine reaction box;
s2, uniformly spreading common steel fibers in each steel fiber throwing area of the grid plate 7;
s3, repeating S1 and S2 for multiple times until the reaction capacity of the liquid medicine reaction box is reached;
s4, feeding the reaction solution into a liquid medicine reaction box;
s5, opening a water bath temperature adjusting box to carry out water bath, and discharging waste liquid from a liquid medicine reaction box after the reaction is finished;
s6, adding clear water into the liquid medicine reaction box to rinse the steel fibers, and removing uncoated residues through circulating water flow;
and S7, opening a water bath temperature regulating box for drying, and taking out the modified steel fibers layer by layer.
The invention has the beneficial effects that:
the reaction kettle realizes loose arrangement of fibers by dividing grids and controlling the throwing quantity of the fibers, the unit reaction volume and the concentration of liquid medicine, reduces mutual adhesion of nano-silicon in the growth and crystallization processes, can effectively avoid the nano-silicon coating from peeling off caused by mutual friction in the fiber cleaning process, obviously improves the thickness of the nano-silicon coating on the surface of steel fibers, greatly enhances the bonding stress of a steel fiber-matrix interface by utilizing the 'secondary hydration effect' of the nano-silicon, and plays a role in enhancing and toughening cement-based materials.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a front cross-sectional view of the present invention;
FIG. 3 is a schematic view of a grid plate of the present invention;
FIG. 4 is a schematic view of a grid plate of the present invention;
FIG. 5 is a top view of the grid and grate combination of the present invention;
FIG. 6 is a schematic view of the stacked multi-layer grate plates of the present invention;
FIG. 7 is a schematic representation of a generic unmodified steel fiber;
FIG. 8 is a microstructure view of unmodified steel fibers;
FIG. 9 is a schematic representation of a steel fiber modified without the use of a reaction vessel;
FIG. 10 is a microstructure of a conventional modified steel fiber;
FIG. 11 is a schematic representation of steel fibers modified using a reaction kettle (surface metallic luster almost completely disappeared);
FIG. 12 is a microscopic morphology of a steel fiber modified by a reaction vessel;
the notation in the figure is: 1. a stainless steel spacer; 2. a grid plate; 3. a steel fiber throwing area; 4. a liquid medicine reaction box; 5. a water bath temperature adjusting box; 6. a valve; 7. and (4) a grid plate.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the following will describe in detail a reaction kettle and a method for preparing nano silicon modified steel fiber in large scale with reference to the accompanying drawings.
The quality, thickness and uniformity of the deposition of nanosilicon on the surface of the steel fibre is related to the concentration of nanosilicon in the solution surrounding the steel fibre. The thickness of the nano silicon coating on the surface of the steel fiber is uneven due to uneven compactness of the steel fiber in the spreading process, and the nano silicon coating is peeled off due to the water flow velocity in the rinsing process after modification. Through the reaction unit grid division, the steel fiber stacking density can be effectively controlled, the nano silicon deposition thickness is improved, the nano silicon peeling in the rinsing process is weakened, the production quality is effectively controlled, and the production efficiency is improved.
A reaction kettle for preparing nano silicon modified steel fiber in large batch comprises a grid plate 7 for placing the steel fiber, a grid plate 2 for supporting the steel fiber and the grid plate 7, a liquid medicine reaction box 4 for containing the grid plate 7, the grid plate 2, the steel fiber and reaction liquid medicine, and a water bath temperature adjusting box 5 for placing the liquid medicine reaction box 4,
as shown in fig. 3, the steel fiber throwing area 3 serving as a grid of the solution reaction unit is obtained on the grid plate 7 by partitioning with the stainless steel spacers 1,
the bonding property of the normal straight steel fiber-matrix interface is weak, the utilization rate of the strength of the steel fiber is low, and the bonding strength of the steel fiber-matrix interface can be obviously improved through the surface modification of the nano silicon to the steel fiber. The modification effect of the existing modification method depends on the fiber throwing uniformity in the early stage, and the modification quality is not easy to control. By grid division, the throwing uniformity of the fibers in the unit grids can be effectively controlled, and the reaction of the liquid medicine in the unit grids is in a synchronous state, so that the thickness of the nanometer silicon coating of the steel fibers in each unit grid tends to be consistent.
The division of the unit grids can enable the steel fibers to be in a loose accumulation state in the grids, can effectively ensure that the steel fibers and the nano silicon generated by hydrolysis of ethyl orthosilicate have enough contact area, improves the coating thickness of the nano silicon on the surface of the steel fibers, and can greatly reduce uneven distribution of the nano silicon coating caused by adhesion of the nano silicon of adjacent steel fibers.
As shown in fig. 4, the grid plate 2 plays a role of supporting the steel fibers and the grid plate 7, and prevents the grid plate 7 and the scattered steel fibers from falling into the next layer, the round shape of the grid plate is an opening, the function is to fill the whole reaction kettle with pumped liquid medicine, and in addition, the function of stabilizing the water impact force on each layer of steel fibers is played in the rinsing process, so that the impact stripping effect of the water flow on the nano silicon coating is weakened.
The grid plate 2 can prevent the steel fiber in the unit grid from falling, the uniform holes on the grid plate can effectively penetrate liquid, not only can the reaction units (grid plate 7) be separated, the concentration of the solution in the unit grid is maintained, but also the liquid scouring force of the nano silicon modified steel fiber in each layer of reaction units (grid plate 7) is ensured to be the same in the rinsing process, the difference of the falling degree of nano silicon on the surface of each layer of modified fiber caused by the flow rate change of different layers of rinsing water flow is avoided, and the coating uniformity and the modification effect of the nano silicon layer are reduced.
The advantages are that: performance, quality, precision and efficiency are improved; energy consumption, raw materials and working procedures are saved; simple and convenient processing, operation, control and use, etc.
As shown in fig. 5, each grid plate 7 is matched with one grid plate 2, the grid plate 7 is embedded in the grid plate 2,
as shown in fig. 6, a plurality of grid plates 2 are sequentially stacked,
as shown in fig. 1, the chemical reaction tank 4 is made of stainless steel, and contains a grid plate 7, a grid plate 2, steel fibers and a reaction chemical; the liquid medicine reaction box 4 is placed in the water bath temperature adjusting box 5, water is injected into the water bath temperature adjusting box 5 in the reaction process, water bath addition is carried out, water and the reaction liquid medicine are discharged after the reaction is finished, and the drying operation is carried out by adjusting the temperature. The water bath temperature regulating box 5 is a purchased part in the prior art.
As shown in fig. 2, the water bath temperature adjusting tank 5 and the chemical reaction tank 4 are provided with valves 6 for discharging water and the reaction chemical, respectively.
A method for preparing nano silicon modified steel fiber in large batch,
the method comprises the following steps: combining a group of grid plates 7 and grate plates 2 and placing the grid plates and grate plates into a liquid medicine reaction box 4;
the method specifically comprises the following steps: the grid plate 2 is placed at the bottom layer of a liquid medicine reaction box 4 of the reaction kettle, and a reaction grid plate 7 is buckled on the grid plate.
Step two: the ordinary steel fibers are uniformly scattered in each reaction unit grid of the grid plate 7, and the tail ends of the steel fibers are ensured not to exceed the top surface of the grid plate 7.
Step three: repeating the two steps for many times, buckling the reaction grid plate 2 and the grid plate 7, and spreading the fibers to be as high as the liquid medicine reaction box 4.
Step four: the reaction solution is sent into a liquid medicine reaction box 4;
the method specifically comprises the following steps: the reaction solution (nano silicon) is prepared by a specific preparation method (see patent No. CN108314391B or other existing preparation methods), the prepared solution is pumped into a reaction kettle, and the grid plate 7, the grid plate 2 and the steel fibers in the reaction kettle play a role in buffering, so that the liquid flow velocity can be effectively slowed down.
Step five: starting a water bath temperature adjusting box 5 to carry out water bath, and discharging waste liquid from a liquid medicine reaction box 4 after the reaction is finished;
the method specifically comprises the following steps: reacting for 6-9h under the condition of 50-80 ℃ water bath, then aging for 1-5 days at room temperature, and discharging the reacted waste liquid through a liquid discharge port after the reaction is finished.
Step six: clean water is pumped into the reactor to rinse the steel fibers and the uncoated residues are removed by the circulating water flow.
Step seven: opening a water bath temperature adjusting box 5 for drying, and taking out the modified steel fibers layer by layer;
the method specifically comprises the following steps: and (3) adjusting the temperature to 85 ℃ for drying, sequentially taking out the grid plates 7 after drying is finished, collecting the modified steel fibers, and finally taking out the grid plates 2 for sequential circulation operation until the modified steel fibers are completely taken out.
The interface bonding stress and the extraction energy are greatly improved
Steel fiber modified interface bonding stress and pulling energy consumption
Description of the drawings: c-1 used common steel fiber, C-2 unused reaction kettle modified steel fiber, C-3 used reaction kettle modified steel fiber
The steel fiber modification greatly improves the bonding stress of the interface, and the pulling energy consumption, and especially the early improvement effect is more obvious.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (9)
1. The utility model provides a preparation nanometer silicon modified steel fiber's reation kettle in batches which characterized in that: comprises a plurality of grid plates (7) for placing steel fibers, a plurality of grid plates (2) for bearing the steel fibers and the grid plates (7), a liquid medicine reaction box (4) and a water bath temperature adjusting box (5) for placing the liquid medicine reaction box (4); the liquid medicine reaction box (4) is used for accommodating a plurality of grid plates (7), a plurality of grid plates (2), steel fibers and reaction liquid medicine; and valves (6) are respectively arranged on the water bath temperature regulating box (5) and the liquid medicine reaction box (4) and are respectively used for discharging water and reacting liquid medicine.
2. The reaction kettle for mass production of nano silicon modified steel fiber according to claim 1, wherein: the grid plate (7) is separated by a stainless steel spacer (1) to obtain a steel fiber throwing area (3) used as a solution reaction unit grid.
3. The reaction kettle for mass production of nano silicon modified steel fiber according to claim 2, wherein: the grid plate (2) is uniformly perforated.
4. The reaction kettle for mass production of nano silicon modified steel fiber according to claim 3, wherein: each grid plate (7) is matched with one grid plate (2), and each grid plate (7) is embedded into the corresponding grid plate (2).
5. The reaction kettle for mass production of nano silicon modified steel fiber according to claim 1, wherein: the liquid medicine reaction box (4) is made of stainless steel.
6. A method for preparing nano silicon modified steel fibers in large scale by using any one of claims 1 to 5, comprising the following steps:
s1, combining a group of grid plates (7) and grate plates (2) and placing the grid plates and the grate plates into a liquid medicine reaction box (4);
s2, uniformly spreading common steel fibers in each steel fiber throwing area (3) of the grid plate 7;
s3, repeating S1 and S2 for multiple times until the reaction capacity of the liquid medicine reaction box (4) is reached;
s4, feeding the reaction solution into a liquid medicine reaction box (4);
s5, opening a water bath temperature adjusting box (5) to carry out water bath, and discharging waste liquid from a liquid medicine reaction box (4) after the reaction is finished;
s6, adding clear water into the liquid medicine reaction box (4) to rinse the steel fibers, and removing uncoated residues through circulating water flow;
and S7, opening the water bath temperature adjusting box (5) for drying, and taking out the modified steel fibers layer by layer.
7. The method for preparing nano silicon modified steel fiber in large batch according to claim 6, wherein the method comprises the following steps: in S1, the grid plate (2) is firstly placed at the bottom layer of the liquid medicine reaction box (4) of the reaction kettle, and a reaction grid plate (7) is buckled on the grid plate.
8. The method for preparing nano silicon modified steel fiber in large batch according to claim 6, wherein the method comprises the following steps: in S5, the reaction was carried out in a water bath at 45 ℃ for a predetermined time.
9. The method for preparing nano silicon modified steel fiber in large batch according to claim 6, wherein the method comprises the following steps: and in S7, the temperature is increased to 85 ℃ for drying, after the drying is finished, the grid plates (7) are taken out in sequence, the modified steel fibers are collected, and finally the grid plates (2) are taken out for sequential circulation operation until the modified steel fibers are completely taken out.
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