CN113817446B - Preparation method of environment-friendly coal dust composite dust suppressant for spraying - Google Patents
Preparation method of environment-friendly coal dust composite dust suppressant for spraying Download PDFInfo
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- CN113817446B CN113817446B CN202111115225.8A CN202111115225A CN113817446B CN 113817446 B CN113817446 B CN 113817446B CN 202111115225 A CN202111115225 A CN 202111115225A CN 113817446 B CN113817446 B CN 113817446B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0033—Xanthan, i.e. D-glucose, D-mannose and D-glucuronic acid units, saubstituted with acetate and pyruvate, with a main chain of (beta-1,4)-D-glucose units; Derivatives thereof
Abstract
The invention discloses a preparation method of an environment-friendly coal dust composite dust suppressant for spraying, which comprises the steps of modifying bentonite to obtain 4 bentonite modifiers of bentonite-itaconic acid-acrylic acid, bentonite-sodium carboxymethylcellulose-sodium dodecyl sulfate, bentonite-polyvinyl alcohol and bentonite-acrylic acid; modifying the xanthan gum to obtain a xanthan gum modifier; preparing porous active carbon by using straws, strongly and uniformly mixing 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of active carbon, 0.02% of triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water, and dissolving and uniformly stirring to obtain the dust settling agent for spraying; the optimal dust removal efficiency of the coal dust composite dust suppressant can reach 84%.
Description
Technical Field
The invention relates to the field of coal bed wetting dust suppressant, in particular to a preparation method of an environment-friendly coal dust composite dust suppressant for spraying.
Background
With the depletion of shallow resources, deep mining has become the main melody of the 21 st century, the ventilation difficulty of coal mines is increased under the condition of deep mining, high-yield and efficient mechanized underground operation often causes high dust concentration on a fully-mechanized excavating surface, reduced visibility of a working surface and high dust explosion risk, and particularly, a large amount of respirable dust inhaled by miners for a long time can cause pneumoconiosis. At present, wet operation (spraying and sprinkling), ventilation and dust removal and the like are commonly used for dust control measures on coal mine sites, but the technologies have higher economic cost, have certain effect on coal dust control, and a plurality of coal dust inhibitors appear along with the development of related technologies, but the dust settling efficiency is not high due to the fact that most of the existing coal dust is difficult to wet due to poor hydrophilicity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an environment-friendly coal dust composite dust suppressant for spraying, so as to at least achieve the purpose of combining the bonding property and the wetting property of the environment-friendly coal dust composite dust suppressant for spraying.
The purpose of the invention is realized by the following technical scheme: a preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
s11, neutralizing 12.5g of acrylic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, simultaneously neutralizing 5g of itaconic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, then mixing the neutralized itaconic acid with the neutralized acrylic acid, stirring at 70 ℃ for 1.5h, adjusting the pH value of the mixed solution to 6-8 by dropwise adding a sodium hydroxide solution with the mass concentration of 30%, then preparing an ammonium persulfate solution with the mass concentration of 0.5%, and adding 0.15g of the prepared ammonium persulfate solution into the mixed solution with the adjusted pH value to obtain an itaconic acid acrylic acid polymer;
s12, dissolving 2g of bentonite in 100ml of distilled water, adding an itaconic acid acrylic acid polymer into a bentonite solution, adding 0.15g of a prepared ammonium persulfate solution, simultaneously adding 0.075g of a cross-linking agent N, N-methylene bisacrylamide with the mass concentration of 0.2%, and stirring at 65 ℃ for 3 hours to obtain a bentonite-itaconic acid-acrylic acid graft copolymer to obtain a bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the dropwise added sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate into 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bis-imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding NaOH solution with the mass concentration of 10 percent to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) sodium bisiminodiphenyl sulfonate (TCS), then dropwise adding NaOH solution with the mass concentration of 10 percent to adjust the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2h, then filtering and washing filter residue with absolute ethyl alcohol for three times to obtain TSGX solid, and obtaining a xanthan gum modifier for later use after cooling and drying;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
adding 0.5g of sodium carboxymethylcellulose into 100ml of distilled water at 70 ℃, and stirring for 10min at the rotating speed of 200 r/min; then 3g of bentonite is added under the stirring condition of 400r/min of rotation speed, and the reaction is carried out for 20min at 70 ℃; then adding 10mL of lauryl sodium sulfate with the mass concentration of 0.5 percent, stirring at the rotating speed of 400r/min (10 min, then placing the mixture into a microwave oven for microwave radiation for 2min by medium fire, and then drying and crushing the mixture to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotation speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the mixture, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bis-imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding 10 mass percent NaOH solution to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) sodium bisiminodiphenyl sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
adding 190mL of deionized water into 14.00g of polyvinyl alcohol, heating to 90 ℃, stirring for 60min to completely dissolve the polyvinyl alcohol, stopping heating and stirring, adding 10mL of ammonium persulfate solution with the mass concentration of 0.5% when the temperature is reduced to 60 ℃, stirring for 10min, adding 6g of bentonite, stirring uniformly, adding 10mL of N, N-methylene bisacrylamide solution with the mass concentration of 0.2%, stopping stirring when the temperature is increased to 75 ℃, keeping the temperature for 30min, and cooling to room temperature to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chlorine-1,3,5-triazine-2,4-) double imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
neutralizing 12g of acrylic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, then adding 5g of bentonite, then sequentially adding 0.3g of ammonium persulfate solution with the mass concentration of 0.5% and 5mL of N, N-methylene bisacrylamide crosslinking agent with the mass concentration of 0.2%, then introducing nitrogen to remove oxygen, then magnetically stirring and reacting at the temperature of 50 ℃ at the rotating speed of 400r/min for 2.5h, then transferring to a microwave oven for microwave irradiation with medium fire for 3min, then taking out, drying at the temperature of 60 ℃ to constant weight, and then crushing and sieving to obtain a bentonite modifier for later use;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the mixture, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bis-imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
According to the invention, bentonite is modified, the binding force on water molecules is increased, the evaporation rate of the water molecules is reduced, the wettability and the water retention performance are improved, especially when the bentonite is grafted with acrylic acid, a lightly crosslinked macromolecule containing strong hydrophilic groups is formed, and the crosslinking structure and the hydrogen bonding of the groups form a three-dimensional network structure, so that the binding force on the water molecules is stronger, the water evaporation rate is slower, and the water retention time is longer; meanwhile, the xanthan gum is modified into xanthan gum triazine bisimino diphenyl sodium sulfonate, and a hydrophobic benzene ring is introduced into the structure of the modified derivative, so that the adsorption energy (pi-pi effect) of the modified derivative and an aromatic ring in a coal dust component substance can be increased; meanwhile, a proper amount of hydrophilic groups such as sodium sulfonate, hydroxyl and ether bond (hydrogen bond effect) are connected on the aromatic ring structure of the derivative to enhance the effect with water molecules, so that the derivative is used as a wetting adhesive, the wetting performance of the derivative on a coal dust structure with aromatic ring, hydroxyl and ether bond functional groups is improved, the system viscosity is also improved, the adhesion efficiency of the coal dust composite dust suppressant on dust is improved, and the derivative has the advantages of cohesiveness, moisture retention and wettability and improves the efficiency of the coal dust composite dust suppressant; the waste straws are modified to prepare porous activated carbon which is used as a dispersing agent of the coal dust composite dust suppressant, so that the porous activated carbon has the characteristics of large surface area and good stability, a porous hollow structure in the porous activated carbon can be compositely dispersed with a natural surfactant, the contact surface of the dust suppressant and dust is increased, the surface tension of the dust suppressant is further reduced, the surface viscosity of the dust suppressant is increased, more active sites are provided for dust adsorption, and the dust suppression efficiency is further improved; the triton X-100 is used as a micromolecular surfactant, has emulsification, wetting and permeation effects, and can accelerate the dust capture speed; the diethylenetriamine penta (methylene phosphonic acid) is added into the coal dust composite dust suppressant to prevent the coal dust composite dust suppressant from corroding a spray pipeline.
The invention has the beneficial effects that:
(1) The bentonite is modified into a three-dimensional network structure, so that the surface tension of the solution is reduced, and the dust collection efficiency of water is improved.
(2) The xanthan gum is modified to contain hydrophilic sodium sulfonate, the hydrophobic end of the xanthan gum is provided with three benzene rings, the wettability and the adsorption performance of the xanthan gum with the hydrophobic end (mainly containing aromatic rings) of coal dust are improved, and the xanthan gum serving as a binder can increase the system viscosity and improve the dust adhesion efficiency of the dust settling agent.
(3) Porous active carbon obtained after hydrothermal carbonization of straws is used as a dispersing agent of the dust suppression agent, and the porous active carbon has the characteristics of large surface area and good stability, so that an internal porous hollow structure can be compounded and dispersed with a natural surfactant, the contact surface of the dust suppression agent and dust is increased, the surface tension of the dust suppression agent is further reduced, the surface viscosity of the dust suppression agent is increased, more active sites are provided for dust adsorption, and the dust suppression efficiency is further improved.
(4) Triton X-100 is used as a micromolecular surfactant, has the functions of emulsification, wetting and permeation, and accelerates the dust capture speed.
(5) The environment-friendly coal dust composite dust suppressant for spraying has the advantages of both adhesive property, wettability and moisture retention property, and the optimal dust removal efficiency can reach 84%.
Drawings
FIG. 1 is a flow chart of the preparation of a coal dust composite dust suppressant;
FIG. 2 is a flow chart of xanthan gum modification;
FIG. 3 is a graph of the moisture retention performance of the coal dust composite dust suppressant.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following.
Example 1
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
s11, neutralizing 12.5g of acrylic acid by using a 30% sodium hydroxide solution to a neutralization degree of 70%, simultaneously neutralizing 5g of itaconic acid by using a 30% sodium hydroxide solution to a neutralization degree of 70%, mixing the neutralized itaconic acid with the neutralized acrylic acid in a three-neck flask, placing the three-neck flask in a constant-temperature magnetic heating pot, heating and stirring the three-neck flask at 70 ℃, stirring the three-neck flask at a rotating speed of 400r/min for 1.5h, adjusting the pH value of the mixed solution to 6-8 by using a 30% sodium hydroxide solution, preparing a 0.5% ammonium persulfate solution, and adding 0.15g of the prepared ammonium persulfate solution into the mixed solution with the adjusted pH value to obtain an itaconic acid acrylic polymer;
s12, dissolving 2g of bentonite in 100ml of distilled water, adding an itaconic acid acrylic acid polymer into a bentonite solution, adding 0.15g of a prepared ammonium persulfate solution with the mass concentration of 0.5%, simultaneously adding 0.075g of a cross-linking agent N, N-methylene bisacrylamide with the mass concentration of 0.2%, and stirring at 65 ℃ for 3 hours to obtain a bentonite-itaconic acid-acrylic acid graft copolymer to obtain a bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, adding 1.84g of cyanuric chloride into a three-neck flask, then adding 10ml of acetone to dissolve the cyanuric chloride, then adding 3-4g of ice, putting the three-neck flask into a constant-temperature magnetic heating pot, and simultaneously stirring for 5min at the rotation speed of 400r/min at the temperature of 0 ℃; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out by an SHZ-D (III) circulating water type multipurpose vacuum pump, and then filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bis-imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a 10-mass-concentration NaOH solution to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate (TCS), then dropwise adding a 10-mass-concentration NaOH solution to adjust the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours (performing ice bath if no solid is precipitated), then filtering, washing filter residue with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, cooling and taking out to obtain active carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
Example 2
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
adding 100ml of distilled water into a beaker, placing the beaker into a constant-temperature magnetic heating pot, setting the temperature at 70 ℃ and the stirring speed at 200r/min, then adding 0.5g of sodium carboxymethylcellulose, and stirring for 10min; then adjusting the stirring speed to 400r/min, adding 3g of bentonite, and reacting for 20min at 70 ℃; then adding 10mL of lauryl sodium sulfate with the mass concentration of 0.5%, stirring at the rotation speed of 400r/min for 10min, then placing the mixture into a microwave oven for microwave radiation for 2min on medium fire, and then drying and crushing the mixture to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, adding 1.84g of cyanuric chloride into a three-neck flask, then adding 10ml of acetone to dissolve the cyanuric chloride, then adding 3-4g of ice, putting the three-neck flask into a constant-temperature magnetic heating pot, and simultaneously stirring for 5min at the rotation speed of 400r/min at the temperature of 0 ℃; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out by an SHZ-D (III) circulating water type multi-purpose vacuum pump, and then filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) double imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10 percent to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) sodium bisiminodiphenyl sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours (performing ice bath if no solid is precipitated), then filtering, washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
Example 3
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
adding 190mL of deionized water into a three-neck flask, then placing the three-neck flask into a constant-temperature water bath, then adding 14.00g of polyvinyl alcohol, then heating to 90 ℃, starting a stirrer to stir for 60min to completely dissolve the polyvinyl alcohol, then stopping heating and stirring, then adding 10mL of ammonium persulfate solution with the mass concentration of 0.5% when the temperature is reduced to 60 ℃, stirring for 10min, then adding 6g of bentonite, uniformly stirring, then adding 10mL of cross-linking agent N, N-methylene bisacrylamide solution with the mass concentration of 0.2%, simultaneously stopping stirring when heating to 75 ℃, then preserving heat for 30min, and then cooling to room temperature to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, adding 1.84g of cyanuric chloride into a three-neck flask, then adding 10ml of acetone to dissolve the cyanuric chloride, then adding 3-4g of ice, putting the three-neck flask into a constant-temperature magnetic heating pot, and simultaneously stirring for 5min at the rotation speed of 400r/min at the temperature of 0 ℃; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out by an SHZ-D (III) circulating water type multi-purpose vacuum pump, and then filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) double imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10 percent to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) sodium bisiminodiphenyl sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours (performing ice bath if no solid is precipitated), then filtering, washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
Example 4
A preparation method of an environment-friendly coal dust composite dust suppressant for spraying comprises the following steps:
s1, preparing a bentonite modifier:
neutralizing 12g of acrylic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, then adding 5g of bentonite, then sequentially adding 0.3g of ammonium persulfate solution with the mass concentration of 0.5% and 5mL of N, N-methylene bisacrylamide crosslinking agent with the mass concentration of 0.2%, then introducing nitrogen to remove oxygen, then magnetically stirring and reacting for 2.5h at the temperature of 50 ℃ at the rotating speed of 400r/min, then transferring to a microwave oven for medium fire microwave irradiation for 3min, then taking out, drying to the constant weight at the temperature of 60 ℃, and then crushing and sieving to obtain a bentonite modifier for later use;
s2, preparing a xanthan gum modifier:
s21, adding 1.84g of cyanuric chloride into a three-neck flask, then adding 10ml of acetone to dissolve the cyanuric chloride, then adding 3-4g of ice, putting the three-neck flask into a constant-temperature magnetic heating pot, and simultaneously stirring for 5min at the rotation speed of 400r/min at the temperature of 0 ℃; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out by an SHZ-D (III) circulating water type multi-purpose vacuum pump, and then filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) double imino sodium diphenylsulfonate (TCS) for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate (TCS), then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours (performing ice bath if no solid is precipitated), then filtering, washing filter residue with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, and taking out the straws after cooling to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
The sedimentation rate, the coal dust contact angle, the viscosity and the moisture retention performance of the coal dust composite dust suppressant prepared in examples 1 to 4 were measured according to the prior art, and the results of the sedimentation rate test are shown in table 1, the results of the coal dust contact angle test are shown in table 2, the results of the moisture retention performance test are shown in fig. 2, and the results of the viscosity test of the coal dust composite dust suppressant prepared in examples 1 to 4 are shown in table 3.
Table 1: results of sedimentation Rate test
| Sample numbering | Example 1 | Example 2 | Example 3 | Example 4 |
| |
5 minutes 23 seconds | 1 hour 8 minutes 02 |
14 minutes 44 seconds | 1 minute 02 second |
As shown in table 1, the settling rate of the coal dust composite dust suppressant prepared in example 2 is the slowest, and the settling rate of the coal dust composite dust suppressant prepared in example 4 is the fastest and can reach 1 minute 02 seconds, which indicates that the permeability and wetting effect are the best.
Table 2: test results of coal powder contact angle
| Sample numbering | Example 1 | Example 2 | Example 3 | Example 4 |
| Contact angle | 74.9° | 73.3° | 75.5° | 63.1° |
As shown in table 2, the contact angle of the composite dust suppressant prepared in example 4 is the smallest, which indicates that the composite dust suppressant has the best wetting effect and the best dust wetting ability, thus indicating that the composite dust suppressant has the best dust suppression effect and the dust removal efficiency can reach 84%.
TABLE 3 dust suppressant viscosity test Table
| Numbering | Example 1 | Example 2 | Example 3 | Example 4 |
| Size of viscosity (mPa.s) | 9.0 | 18.0 | 11.5 | 8.0 |
The viscosity of unmodified 1% bentonite was 2mpa.s, as shown in table 3, the viscosity after modification was higher than 2mpa.s, indicating that the viscosity after modification was increased, which is more favorable for dust removal of respirable dust.
Table 4: experimental medicine and experimental instrument table
The foregoing is illustrative of the preferred embodiments of the present invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and is not to be construed as limited to the exclusion of other embodiments, and that various other combinations, modifications, and environments may be used and modifications may be made within the scope of the concepts described herein, either by the above teachings or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. A preparation method of an environment-friendly coal dust composite dust suppressant for spraying is characterized by comprising the following steps:
s1, preparing a bentonite modifier:
s11, neutralizing 12.5g of acrylic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, simultaneously neutralizing 5g of itaconic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, then mixing the neutralized itaconic acid with the neutralized acrylic acid, stirring at 70 ℃ for 1.5h, adjusting the pH value of the mixed solution to 6-8 by dropwise adding a sodium hydroxide solution with the mass concentration of 30%, then preparing an ammonium persulfate solution with the mass concentration of 0.5%, and adding 0.15g of the prepared ammonium persulfate solution into the mixed solution with the adjusted pH value to obtain an itaconic acid acrylic acid polymer;
s12, dissolving 2g of bentonite in 100ml of distilled water, adding an itaconic acid acrylic acid polymer into a bentonite solution, adding 0.15g of a prepared ammonium persulfate solution, simultaneously adding 0.075g of a cross-linking agent N, N-methylene bisacrylamide with the mass concentration of 0.2%, and stirring at 65 ℃ for 3 hours to obtain a bentonite-itaconic acid-acrylic acid graft copolymer to obtain a bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then dropwise adding a prepared sodium sulfanilate solution into the solution, wherein the dropwise added sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate into 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenyl sodium sulfonate for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, cooling, and taking out to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
2. A preparation method of an environment-friendly coal dust composite dust suppressant for spraying is characterized by comprising the following steps:
s1, preparing a bentonite modifier:
adding 0.5g of sodium carboxymethylcellulose into 100ml of distilled water at 70 ℃, and stirring for 10min at the rotating speed of 200 r/min; then 3g of bentonite is added under the stirring condition with the rotating speed of 400r/min, and the reaction is carried out for 20min at the temperature of 70 ℃; then adding 10mL of lauryl sodium sulfate with the mass concentration of 0.5%, stirring at the rotation speed of 400r/min for 10min, then placing the mixture into a microwave oven for microwave radiation for 2min on medium fire, and then drying and crushing the mixture to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenyl sodium sulfonate for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding NaOH solution with the mass concentration of 10 percent to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) sodium bisiminodiphenyl sulfonate, then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, cooling, and taking out to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
3. A preparation method of an environment-friendly coal dust composite dust suppressant for spraying is characterized by comprising the following steps:
s1, preparing a bentonite modifier:
adding 190mL of deionized water into 14.00g of polyvinyl alcohol, heating to 90 ℃, stirring for 60min to completely dissolve the polyvinyl alcohol, stopping heating and stirring, adding 10mL of ammonium persulfate solution with the mass concentration of 0.5% when the temperature is reduced to 60 ℃, stirring for 10min, adding 6g of bentonite, stirring uniformly, adding 10mL of N, N-methylene bisacrylamide solution with the mass concentration of 0.2%, heating to 75 ℃, stopping stirring, preserving heat for 30min, and cooling to room temperature to obtain the bentonite modifier;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotating speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the solution, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then the filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenyl sodium sulfonate for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate, then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, cooling, and taking out to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
4. The preparation method of the environment-friendly coal dust composite dust suppressant for spraying is characterized by comprising the following steps of:
s1, preparing a bentonite modifier:
neutralizing 12g of acrylic acid by using a sodium hydroxide solution with the mass concentration of 30% until the neutralization degree is 70%, then adding 5g of bentonite, then sequentially adding 0.3g of ammonium persulfate solution with the mass concentration of 0.5% and 5mL of N, N-methylene bisacrylamide crosslinking agent with the mass concentration of 0.2%, then introducing nitrogen to remove oxygen, then magnetically stirring and reacting at the temperature of 50 ℃ at the rotating speed of 400r/min for 2.5h, then transferring to a microwave oven for microwave irradiation with medium fire for 3min, then taking out, drying at the temperature of 60 ℃ to constant weight, and then crushing and sieving to obtain a bentonite modifier for later use;
s2, preparing a xanthan gum modifier:
s21, dissolving 1.84g of cyanuric chloride in 10ml of acetone, adding 3-4g of ice, and stirring at 0 ℃ at a rotation speed of 400r/min for 5min; then, dropwise adding a sodium sulfanilate solution into the mixture, wherein the sodium sulfanilate solution is prepared by dissolving 3.92g of sodium sulfanilate in 20ml of deionized water; then, dropwise adding saturated sodium bicarbonate solution to keep the pH value of the solution at 6-7 all the time, and stirring for 1h at 40 ℃; then ice-bath is carried out for 10min, then filtration is carried out, and then filter residue is washed by acetone for 3 times to obtain 4,4' - (6-chlorine-1,3,5-triazine-2,4-) double imino sodium diphenylsulfonate for standby;
s22, dissolving 7.5214g of xanthan gum in 20ml of isopropanol, then dropwise adding a NaOH solution with the mass concentration of 10% to adjust the pH to 8-9, then heating to 40 ℃, adding 1.841g4,4' - (6-chloro-1,3,5-triazine-2,4-) bisiminodiphenylsodium sulfonate, then adjusting the pH to 8-9, continuously heating to 60 ℃, simultaneously stirring for 2 hours, then filtering and washing filter residues with absolute ethyl alcohol for three times to obtain TSGX solid, and cooling and drying to obtain a xanthan gum modifier for later use;
s3, preparing activated carbon:
crushing 6g of straws, adding potassium hydroxide with equal mass, mixing and crushing the straws by a crusher, putting the straws into a muffle furnace, introducing argon, heating to 700 ℃ at the speed of 2 ℃/min, roasting for 6h, cooling, and taking out to obtain activated carbon for later use;
s4, preparing a dust settling agent for spraying:
according to the mass fraction, 1% of bentonite modifier, 0.01% of xanthan gum modifier, 0.1% of activated carbon, 0.02% of Triton X-100, 0.01% of diethylenetriamine pentamethylene phosphonic acid and 98.86% of water are dissolved and stirred uniformly to obtain the coal dust composite dust suppressant.
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