CN107573015B - Preparation method of water-resistant and anti-freezing shale ganged brick - Google Patents
Preparation method of water-resistant and anti-freezing shale ganged brick Download PDFInfo
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- CN107573015B CN107573015B CN201710928786.7A CN201710928786A CN107573015B CN 107573015 B CN107573015 B CN 107573015B CN 201710928786 A CN201710928786 A CN 201710928786A CN 107573015 B CN107573015 B CN 107573015B
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Abstract
The invention discloses a preparation method of a water-resistant and freeze-resistant shale ganged brick, and belongs to the technical field of building materials. Crushing shale, soaking in a saturated solution of ferric sulfate at 60 ℃, freezing in liquid nitrogen, then transferring into a microwave for thawing, soaking in the way, performing freeze-thaw cycle for 15-20 times, draining water, sieving to obtain refined shale, fumigating the refined shale under the condition of ammonia gas, drying to constant weight, then performing heating and stirring reaction with tetraethoxysilane under the conditions of sealing, constant temperature and constant pressure, filtering to obtain modified shale, mixing the modified shale with fly ash, adding a small amount of water and a fluxing agent, stirring and mixing, then putting into a granulator for granulation, aging at room temperature to obtain base material particles, pouring the base material particles into a mold, transferring into a press, performing compression molding to obtain a blank, drying the blank, transferring into a sintering furnace for sintering to obtain the water-resistant shale brick. The shale ganged brick prepared by the invention has excellent water resistance and frost resistance, and the compressive strength is improved to a certain degree.
Description
Technical Field
The invention discloses a preparation method of a water-resistant and freeze-resistant shale ganged brick, and belongs to the technical field of building materials.
Background
The dry wall brick is also called as a dry wall brick, has the characteristics of integrated bearing, variable style, simple construction and the like, and is a good building material at present. It includes cuboid standard brick block and matched special-shaped brick, and possesses several decorative effect. The ganged brick is required to have good quality such as heat preservation, heat insulation, sound insulation, water resistance, frost resistance, no color change, durability, environmental protection, no radioactivity and the like, and the product is generally designed into a porous structure form.
The biggest difference between the sintered shale ganged brick and the common sintered shale brick lies in the difference of the production process, and the sintered shale ganged brick is produced by improving the process of sintering the common shale brick. The sintered shale ganged brick is a product obtained by processing a hollow brick blank by pattern decoration, glazing decoration and the like on the basis of a common sintered shale brick, belongs to a stoneware ceramic brick, has small dimensional tolerance, is very beautiful after the surface is processed, and can be directly used as the surface of a wall body without other surface decorations. The sintered shale ganged brick wall has the advantages of attractive appearance, high strength, heat preservation, sound insulation, difficult cracking and water leakage, environmental protection and the like which cannot be achieved by the traditional wall decoration material. The traditional method for improving the sintering of the shale ganged bricks is to use a semi-dry extrusion forming technology in the extrusion forming stage. The semi-dry extrusion molding is a molding method which utilizes a press machine to add a small amount of bonding agent into a dry powder blank and then presses the mixture into a compact blank in a metal mold. Because the formed blank has less moisture, large pressure and compact blank, the green blank with less defects, small shrinkage, accurate size and no need of strengthening and drying can be obtained. The new production process is adopted in the firing process, the performance of the shale ganged brick is improved to a certain extent, but a huge improvement space is still provided.
Because the production process of the sintered shale ganged brick is greatly different from that of the common sintered shale brick, the frost resistance of the brick is different. The damage generated by the freeze-thaw cycle is that the brick body is contacted with water and the brick body is in an environment with alternating positive and negative temperature, so that the moisture contained in the brick body is subjected to the freeze-thaw cycle. The strength and quality of the brick body are influenced after the brick body is damaged by freezing and thawing, and the thermal performance of the brick body is also greatly influenced. Therefore, the water resistance of the shale ganged bricks is also a great factor for evaluating the anti-freezing performance.
Therefore, the water resistance, the freezing resistance and the mechanical property of the shale ganged brick are improved, and the problem to be solved is to be popularized and used in the field of building materials and wider fields.
Disclosure of Invention
The invention mainly solves the technical problems that: aiming at the problem that the water resistance, frost resistance and mechanical property of the traditional shale ganged brick are poor, the preparation method of the water-resistant and frost-resistant shale ganged brick is provided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
(1) taking 100-120 parts of shale by weight, crushing the shale in a crusher to obtain crushed shale, soaking the crushed shale in a saturated solution of ferric sulfate at 60 ℃, freezing the crushed shale in liquid nitrogen, then thawing the crushed shale by microwave, soaking the crushed shale in the microwave thawing mode, performing freeze thawing cycle for 15-20 times, draining surface water, and sieving to obtain refined shale;
(2) fumigating the refined shale under the condition of ammonia gas, drying to constant weight to obtain fumigated shale, mixing the fumigated shale with tetraethoxysilane, carrying out constant-temperature and constant-pressure closed reaction, and filtering to obtain modified shale;
(3) mixing the modified shale and the fly ash according to the mass ratio of 2: 1-4: 1, mixing, sequentially adding water with the mass of 0.10-0.15 times of that of the modified shale and a fluxing agent with the mass of 0.05-0.12 times of that of the modified shale, stirring and mixing to obtain a mixture, putting the mixture into a granulator for granulation to obtain a pretreated blank, and aging the pretreated blank for 1-2 days to obtain base material particles;
(4) pouring the base material particles into a mould, moving the mould into a press machine, and performing compression molding to obtain a blank body;
(5) transferring the blank into a drying box, and drying at the temperature of 88-96 ℃ until the moisture content is 3-6% to obtain a pretreated blank;
(6) and (4) transferring the pre-treated green body into a sintering furnace, and firing and forming to obtain the water-resistant and anti-freezing shale ganged brick.
The specific preparation method of the saturated solution of ferric sulfate at 60 ℃ in the step (1) comprises the following steps: and adding ferric sulfate into the water under the conditions that the water temperature is 60 ℃ and the rotating speed is 250-280 r/min until the ferric sulfate is not dissolved any more, and filtering to obtain filtrate, namely obtaining saturated solution of the ferric sulfate at the temperature of 60 ℃.
The fluxing agent in the step (3) is boric acid, calcium oxide and cryolite according to the mass ratio of 1: 1: 1 configuration.
The invention has the beneficial effects that:
(1) when the modified shale is prepared, firstly, the shale is soaked, subjected to freeze thawing cycle and then fumigated by ammonia gas, firstly, after the shale is soaked with ferric sulfate saturated solution and subjected to freeze thawing cycle, the shale can not only reduce the size of the shale, but also more fully disperse ferric sulfate in the shale structure, and secondly, after the shale is fumigated by ammonia gas, the ammonia gas can more fully enter the shale structure to react with ferric sulfate distributed in the shale structure due to the fact that the ammonia gas has stronger fluidity and permeability than liquid, and the ammonia gas is dissolved in water, and the hydrolysis generates hydroxyl ions to precipitate the ferric ions, so that the ferric ions cannot immediately react with the ferric sulfate to block a passage, and the ferric sulfate reacts more fully;
(2) according to the invention, the fumigated shale is reacted with ethyl orthosilicate to prepare the modified shale, on one hand, ferric hydroxide is dehydrated and converted into ferric oxide under a high-temperature condition, the existence of the ferric oxide can be used as a sintering aid to enhance the fluidity of the shale during sintering, so that the generation of pores during sintering is reduced, the porosity of the product is reduced, the density is effectively improved, the waterproofness and the frost resistance are improved, on the other hand, the ferric hydroxide is converted into the ferric oxide to generate water, the ethyl orthosilicate can perform hydrolysis reaction at a certain pressure and temperature to produce silicon dioxide, and the silicon dioxide can be filled in the pore structure of the shale, so that the porosity of the product is reduced, the waterproofness and the frost resistance of the product are further improved, and the compression resistance of the product is improved to a certain extent.
Drawings
FIG. 1 shows the water resistance, freezing resistance and mechanical property test results of the water-resistant and freezing-resistant shale ganged brick.
Detailed Description
The method comprises the steps of taking 100-120 parts by weight of shale, transferring the shale into a pulverizer to be pulverized for 1-2 hours to obtain pulverized shale, mixing the pulverized shale with a saturated solution of ferric sulfate at 60 ℃ according to a mass ratio of 1: 5-1: 10, soaking for 4-6 hours at 60 ℃, filtering to obtain soaked shale, transferring the soaked shale into liquid nitrogen to be frozen for 4-6 minutes to obtain frozen pulverized shale, thawing the frozen pulverized shale for 3-5 minutes by microwave, soaking, filtering, performing freeze-thaw cycle for 15-20 times to obtain pretreated shale, draining the surface water of the pretreated shale, sieving with a 100-120 mesh sieve to obtain refined shale, transferring the refined shale into a reaction kettle, introducing ammonia gas into the reaction kettle at a speed of 15-20 m L/min, transferring the materials in the reaction kettle after 2-4 hours under the condition, transferring the materials in the reaction kettle into a drying box at a temperature of 80-95 ℃, drying to obtain a weight of the fumigated silicic acid shale, transferring the material into a constant-temperature silica gel, transferring the shale and ethyl ester to a constant-temperature modification reaction kettle, transferring the shale into a constant-temperature, transferring the slurry of a slurry, transferring the slurry into a slurry, transferring the slurry into a slurry, transferring the slurry, a slurry, transferring the slurry, a slurry, transferring the slurry, a drying process, a slurry, a drying process, a slurry, a drying process, a slurry, a drying process, a slurry, a drying process, a.
Example 1
The method comprises the steps of taking 120 parts by weight of shale, transferring the shale into a pulverizer to be pulverized for 2 hours to obtain pulverized shale, transferring the pulverized shale and a saturated solution of ferric sulfate at 60 ℃ to be mixed according to a mass ratio of 1: 10, soaking for 6 hours at 60 ℃, filtering to obtain soaked shale, transferring the soaked shale into liquid nitrogen to be frozen for 6 minutes to obtain frozen pulverized shale, performing microwave thawing on the frozen pulverized shale for 5 minutes, soaking in the above manner, filtering, performing freeze-thaw cycle for 20 times to obtain pretreated shale, draining water on the surface of the pretreated shale, sieving with a 120-mesh sieve to obtain refined shale, transferring the refined shale into a reaction kettle, introducing ammonia gas into the reaction kettle at a speed of 20m L/min, transferring materials in the reaction kettle to a drying box after fumigation for 4 hours, drying to constant weight at a temperature of 95 ℃ to obtain fumigation, transferring the fumigated shale into a reaction kettle according to a mass ratio of 1: 12, transferring the mixture of the pretreated ferric sulfate into a drying box, transferring the mixture into a constant-temperature modification-water-cement-coal ash-containing coal ash-fly ash-containing coal ash-containing material, transferring the mixture into a reaction-containing coal ash-forming material, transferring the mixture into a reaction-forming furnace, transferring the coal-ash-forming furnace, transferring the coal-forming furnace, transferring the coal-ash-coal-ash-coal-ash-coal-.
Example 2
Taking 120 parts of shale by weight, transferring the shale into a pulverizer to be pulverized for 2 hours to obtain pulverized shale, transferring the pulverized shale and a saturated solution of ferric sulfate at 60 ℃ to be mixed according to a mass ratio of 1: 10, soaking for 6 hours at 60 ℃, filtering to obtain soaked shale, transferring the soaked shale into liquid nitrogen to be frozen for 6 minutes to obtain frozen pulverized shale, microwave thawing the frozen pulverized shale for 5 minutes, soaking in the above manner, filtering, performing freeze-thaw cycle for 20 times to obtain pretreated shale, draining the surface water of the pretreated shale, sieving with a 120-mesh sieve to obtain refined shale, transferring the refined shale into a reaction kettle, introducing ammonia gas into the reaction kettle at a rate of 20m L/min, transferring the materials in the reaction kettle into a drying box after fumigating for 4 hours, drying to constant weight at a temperature of 95 ℃ to obtain fumigating, adding the fumigated shale into the reaction kettle, sealing the reaction kettle, reacting at a pressure of 3.1MPa, at a temperature of 500 ℃, reacting at a constant temperature of 280r/min, reacting for 4 minutes, filtering at a constant temperature, transferring the mixture of the filtrate until the mixture of ferric sulfate is dried, transferring the mixture into a slurry into a mold with a constant temperature of 1.1.1.1.1.1.1 ℃, drying, transferring the slurry of a slurry, drying furnace, transferring the slurry coal ash, drying furnace, transferring the slurry into a slurry, transferring the slurry of a slurry to obtain a slurry, transferring the slurry into a slurry, transferring the slurry, transferring a slurry into a slurry, transferring the slurry into a slurry, transferring the slurry, transferring a slurry into a slurry, transferring a slurry into a slurry, transferring a mold, transferring the slurry into a slurry, transferring a slurry into a mold, transferring the slurry, transferring a slurry, transferring the slurry, transferring a.
Example 3
Taking 120 parts of shale by weight, transferring the shale into a pulverizer to be pulverized for 2 hours to obtain pulverized shale, and mixing the pulverized shale with water according to a mass ratio of 1: 10, mixing, soaking for 6 hours at the temperature of 60 ℃, filtering to obtain soaked shale, transferring the soaked shale into liquid nitrogen for freezing for 6 minutes to obtain frozen crushed shale, unfreezing the frozen crushed shale by microwaves for 5 minutes, soaking in the above way, filtering, performing freeze-thaw cycling for 20 times to obtain pretreated shale, draining the surface water of the pretreated shale, and sieving by a 120-mesh sieve to obtain refined shale; refining shale and tetraethoxysilane according to the mass ratio of 1: 12, mixing the materials in the reaction furnace into a reaction kettle, sealing the reaction kettle, carrying out constant-temperature and constant-pressure sealed reaction for 4 hours under the conditions that the pressure is 3.1MPa, the temperature is 500 ℃ and the rotating speed is 280r/min, naturally cooling the materials in the reaction furnace to room temperature, discharging, and filtering to obtain a filter cake, namely the modified shale; mixing the modified shale and the fly ash according to a mass ratio of 4: 1, mixing, sequentially adding water with the mass being 0.15 time of that of the modified shale and a fluxing agent with the mass being 0.12 time of that of the modified shale into a mixture of the modified shale and the fly ash, stirring and mixing at the temperature of 45 ℃ and the rotating speed of 300r/min to obtain a mixture, putting the mixture into a granulator for granulation to obtain a pretreated blank, and aging the pretreated blank at room temperature for 2 days to obtain base material particles; pouring the base material particles into a mould, moving the mould into a press machine, pressing and forming under the condition that the pressure is 2.5MPa to obtain a blank body, moving the blank body into a drying box, and drying at the temperature of 96 ℃ until the moisture content of the blank body is 6 percent to obtain a pretreated blank body; and (3) transferring the pre-treated green body into a sintering furnace, sintering at the constant temperature of 1300 ℃ for 70h, cooling to room temperature along with the furnace, and discharging to obtain the water-resistant and anti-freezing shale ganged brick. The fluxing agent is boric acid, calcium oxide and cryolite according to the mass ratio of 1: 1: 1 configuration.
Comparative example: shale ganged bricks produced by a certain shale brick product company Limited in Tianjin.
The water-resistant and freeze-resistant shale ganged bricks obtained in examples 1 to 3 and comparative products are subjected to performance detection, and the specific detection method is as follows:
1. water resistance: cleaning the surface of the brick body of the test piece by using a brush respectively, putting the brick body into a drying oven at 100 ℃ for drying for 24 hours, and then weighing the brick body as m0. And then the dried brick body is put into a water tank with the temperature of 20 ℃. After 24h of soaking, the surface water is wiped off by a towel, and the weight is immediately weighed as m24Water absorption (W) of the fired shale ganged brick24) The calculation is performed according to equation (1):
W24=（（m24-m0）/m0）×100% （1）；
2. freezing resistance: the test is carried out according to GB/T2542 strictly. A test piece brick body with a complete surface and no crack is selected to carry out the test, the surface of the brick body is cleaned by a rag, and the brick is put into a drying oven at 100 ℃ to be dried to constant weight. And then the brick bodies are placed in a freeze-thaw box, the freeze-thaw box is selected to be in a heating state, so that water at the bottom of the freeze-thaw box is pumped by a water pump to soak the brick bodies, the freeze-thaw box is closed after 24 hours, and after the water surface descends, the water on the surfaces of the brick bodies is wiped off by using a cleaning cloth and then is placed back into the freeze-thaw box. The minimum temperature was set at-15 ℃ and the temperature of the melt water was set at 15 ℃. After 50 times of freeze-thaw cycles, the mass loss rate and the strength loss rate were measured and calculated.
3. Mechanical properties: and (5) detecting the compressive strength of the single brick of the test piece according to GB/T2542. And selecting a test piece with a flat surface and no obvious defects or cracks, and testing the compressive strength of the single brick.
The concrete detection results are shown in the accompanying drawing, and the detection results shown in the accompanying drawing description and shown in fig. 1 show that the water-resistant and anti-freezing shale ganged brick prepared by the technical scheme of the invention has the advantages that the water resistance and the freezing resistance are improved, the mechanical property is also obviously improved, and the water-resistant and anti-freezing shale ganged brick has a wide prospect in the development of the technical field of building materials.
Claims (3)
1. A preparation method of a water-resistant and freeze-resistant shale ganged brick is characterized by comprising the following specific preparation steps:
(1) taking 100-120 parts of shale by weight, crushing the shale in a crusher to obtain crushed shale, soaking the crushed shale in a saturated solution of ferric sulfate at 60 ℃, freezing the crushed shale in liquid nitrogen, then thawing the crushed shale by microwave, soaking the crushed shale in the microwave thawing mode, performing freeze thawing cycle for 15-20 times, draining surface water, and sieving to obtain refined shale;
(2) fumigating the refined shale under the condition of ammonia gas, drying to constant weight to obtain fumigated shale, mixing the fumigated shale with tetraethoxysilane, carrying out constant-temperature and constant-pressure closed reaction, and filtering to obtain modified shale;
(3) mixing the modified shale and the fly ash according to the mass ratio of 2: 1-4: 1, mixing, sequentially adding water with the mass of 0.10-0.15 times of that of the modified shale and a fluxing agent with the mass of 0.05-0.12 times of that of the modified shale, stirring and mixing to obtain a mixture, putting the mixture into a granulator for granulation to obtain a pretreated blank, and aging the pretreated blank for 1-2 days to obtain base material particles;
(4) pouring the base material particles into a mould, moving the mould into a press machine, and performing compression molding to obtain a blank body;
(5) transferring the blank into a drying box, and drying at the temperature of 88-96 ℃ until the moisture content is 3-6% to obtain a pretreated blank;
(6) and (4) transferring the pre-treated green body into a sintering furnace, and firing and forming to obtain the water-resistant and anti-freezing shale ganged brick.
2. The preparation method of the water-resistant and freeze-resistant shale ganged brick according to claim 1, characterized by comprising the following steps: the specific preparation method of the saturated solution of ferric sulfate at 60 ℃ in the step (1) comprises the following steps: and adding ferric sulfate into the water under the conditions that the water temperature is 60 ℃ and the rotating speed is 250-280 r/min until the ferric sulfate is not dissolved any more, and filtering to obtain filtrate, namely obtaining saturated solution of the ferric sulfate at the temperature of 60 ℃.
3. The preparation method of the water-resistant and freeze-resistant shale clear water brick according to claim 1, which is characterized by comprising the following steps: the fluxing agent in the step (3) is boric acid, calcium oxide and cryolite according to the mass ratio of 1: 1: 1 configuration.
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| CN111228562B (en) * | 2020-03-26 | 2022-03-15 | 江苏德威兰医疗器械股份有限公司 | Starch hemostatic sponge and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629093A (en) * | 2003-12-16 | 2005-06-22 | 许长洪 | Shale hollow brick and its preparing method |
| CN105906368A (en) * | 2016-04-28 | 2016-08-31 | 浏阳新源建材有限责任公司 | Environment-friendly shale brick and production process thereof |
| CN106278173A (en) * | 2016-08-25 | 2017-01-04 | 董晓 | A kind of method utilizing discarded concrete to prepare freeze proof environmental protection brick |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629093A (en) * | 2003-12-16 | 2005-06-22 | 许长洪 | Shale hollow brick and its preparing method |
| CN105906368A (en) * | 2016-04-28 | 2016-08-31 | 浏阳新源建材有限责任公司 | Environment-friendly shale brick and production process thereof |
| CN106278173A (en) * | 2016-08-25 | 2017-01-04 | 董晓 | A kind of method utilizing discarded concrete to prepare freeze proof environmental protection brick |
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