CN112321771B - Efficient permeation wetting type moisturizing agent for coal seam water injection and preparation method thereof - Google Patents
Efficient permeation wetting type moisturizing agent for coal seam water injection and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of dust suppressants for mine dust prevention, and discloses a high-efficiency permeable wetting agent for coal seam water injection and a preparation method thereof, wherein the high-efficiency permeable wetting agent comprises, by mass, 1.25% of hydroxyethyl cellulose, 2.5% -4.5% of methyl stearoyl acrylate, 1% -3% of acrylamide, 0.1% -0.5% of an initiator, 0.0% -0.5% of a penetrating agent, 0.0% -0.5% of a wetting agent and water. The lubricant greatly improves the self-lipophilicity and the wettability, can improve the wettability of water to a coal bed, and is beneficial to reducing the dust yield in coal exploitation from the source. The penetrating agent is sodium dodecyl sulfate, is an anionic surfactant, the wetting agent is fatty alcohol polyoxyethylene ether, is a nonionic surfactant, and the two surfactants with different ions interact to jointly promote the penetration-wetting of the solution to the coal seam.
Description
Technical Field
The invention belongs to the technical field of dust suppressants for mine dust prevention, and particularly relates to a high-efficiency permeable wetting type moisturizing agent for coal seam water injection and a preparation method thereof.
Background
At present: coal is used as a main energy source in China and has an irreplaceable position. Along with the continuous improvement of the mechanization level in the coal mining process, dust in the operation production process is seriously out of standard, and the physical health of miners is seriously threatened. In the occupational safety and health problems caused by various occupational hazards in the working environment, the number of new cases, the accumulated number of cases and the number of death cases of occupational diseases mainly comprising coal dust and lungs are the first place in the world. By 2018, 97.5 thousands of occupational diseases are reported cumulatively, wherein 87.3 thousands of occupational pneumoconiosis diseases account for about 90% of the total number of reported occupational disease cases; the statistics shows that the deaths of coal mines in China are about 1900 people each year, which is about 6 times as large as the deaths of miners in mining accidents and other industrial accidents, and coal dust pollution becomes a great threat for safe and efficient production of coal. Therefore, the dust concentration in the coal mining process is reduced, and secondary dust emission in the coal mining, storage, loading, unloading and transportation processes is prevented, so that the problem which needs to be solved primarily is solved.
Therefore, in order to reduce the amount of dust generated from the source, the coal seam is usually pre-wetted by adopting a coal seam water injection mode so as to reduce the amount of dust generated in the mining process. However, as coal mining depths increase, low permeability coals increase, making the affinity between water and coal weaker, making it difficult for water to wet the coal bed, and thus, this also results in undesirable dust reduction effects of coal seam water injection.
Through the above analysis, the problems and defects existing in the prior art are as follows: the existing water has poor wetting effect on the coal seam.
The difficulty of solving the problems and the defects is as follows: along with the increase of the exploitation depth, low-permeability coal is increased, so that the affinity between water and coal is weaker, the water is difficult to wet a coal bed, and the dust reducing effect of coal bed water injection is finally affected.
The meaning of solving the problems and the defects is as follows: the method is beneficial to improving the affinity between water and coal, and wetting the coal more effectively, so that the dust yield in coal exploitation is reduced.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an efficient permeable wetting type moisturizing agent for coal seam water injection and a preparation method thereof.
The invention is realized in such a way that the high-efficiency penetration wetting type moisturizing agent for coal seam water injection consists of 1.25% of hydroxyethyl cellulose, 2.5% -4.5% of methyl stearoyl acrylate, 1% -3% of acrylamide, 0.1% -0.5% of an initiator, 0.0% -0.5% of a penetrating agent, 0.0% -0.5% of a wetting agent and water according to mass percentage; the water is filled up to 100%. When the penetrant is 0, in order to examine various performance indexes of the lubricant when the penetrant and the wetting agent are not added, whether the wettability of the lubricant without the penetrant and the wetting agent is better than that of water is judged
Further, the initiator is ceric ammonium nitrate.
Further, the penetrating agent is sodium dodecyl sulfate; the wetting agent is fatty alcohol polyoxyethylene ether.
Further, the optimal proportion of the high-efficiency penetration wetting type moisturizing agent for coal seam water injection in 400ml of water is hydroxyethyl cellulose: stearoyl methyl acrylate: acrylamide=1:1:1, ceric ammonium nitrate: water = 1:500, sodium dodecyl sulfate: fatty alcohol polyoxyethylene ether=3:1.
The invention also aims to provide a preparation method for preparing the high-efficiency permeable wetting type moisturizing agent for coal seam water injection, which comprises the following steps of:
step one, loading hydroxyethyl cellulose into a three-neck flask with distilled water, and introducing nitrogen to perform gelatinization to obtain a first solution;
step two, cooling after the first solution is gelatinized, respectively adding methyl stearoyl acrylate and acrylamide, after the methyl stearoyl acrylate and acrylamide are completely dissolved, adding ceric ammonium nitrate, and keeping the water bath for heating;
step three, adding N-N methylene bisacrylamide, mixing, stirring and dissolving to obtain a second solution; cooling the second solution; adding sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether, and continuing to heat in a water bath;
and fourthly, synthesizing and extracting a product by adopting microwave vibration, and obtaining the efficient permeable wetting type moisturizing agent for coal seam water injection.
Further, in the first step, the gelatinization temperature is 80 ℃.
Further, in the second step, cooling after the first solution is gelatinized includes: cooling the first solution to 30-70 ℃ after gelatinization; wherein the optimum cooling temperature is 60 ℃.
Further, in the third step, the mixing and stirring dissolution time is 1h.
Further, in the third step, the cooling the second solution includes: the second solution was cooled to room temperature.
Further, in the third step, the water bath heating time is 1h.
By combining all the technical schemes, the invention has the advantages and positive effects that: the process parameters of the invention are all optimal data obtained through a large number of experimental operations. The permeability enhancer prepared by the parameters has optimal reverse osmosis height, optimal weight gain rate and the like. The wetting agent disclosed by the invention has excellent wettability, can improve the wettability of water to a coal bed, and is beneficial to reducing the dust yield in coal exploitation.
TABLE 5 comparison of Water with the inventive moisturizing Agents
The invention adopts the hydroxyethyl cellulose as the raw material, the hydroxyethyl cellulose is a modified biological base material, and the material has a high molecular structure, and has wide sources and simple synthesis; the initiator of the invention has strong oxidizing property. The penetrating agent is sodium dodecyl sulfate, is an anionic surfactant, the wetting agent is fatty alcohol polyoxyethylene ether, is a nonionic surfactant, and has good synergistic effect by interaction of two surfactants with different ions, so that the penetrating-wetting of the solution to the coal seam is promoted.
According to the invention, a free radical polymerization method is adopted to modify hydroxyethyl cellulose, methyl stearoyl acrylate and acrylamide are grafted to the hydroxyethyl cellulose, and then a penetrating agent and a wetting agent are compounded to further improve the performance of the product, so that the moisturizing agent with excellent wettability is finally generated. The lubricant greatly improves the self-lipophilicity and can better wet the coal seam. When the coal seam is injected with water, the solution pulls more water to permeate into the deep part of the coal seam under the synergistic effect of the penetrating agent and the wetting agent, so that the aim of wetting the coal seam and reducing dust production is fulfilled. In addition, the modified hydroxyethyl cellulose has certain low viscosity and is also beneficial to capturing scattered dust.
The material-hydroxyethyl cellulose selected by the invention is a modified biological base material, has a high molecular structure, is wide in source and simple to synthesize, has excellent biodegradability, is a good environment-friendly biological material, is used as a main carrier for graft copolymerization due to the good performances, can generate bond breaking capacity under the initiation of an initiator by using methyl stearoyl acrylate and acrylamide, has unstable active sites, and can actively separate active electrons from molecules to form unsaturated bond breaking under the initiation of the initiator. By using these unsaturated broken bonds, the unsaturated bonds are combined with each other under microwave vibration to form new bonds, thereby obtaining a new product. In order to further increase the viscosity of the product, a small amount of surfactant and calcium chloride are added in the reaction process to enhance and improve the generated wetting agent, so that the wetting agent has low viscosity, the self low viscosity is utilized to promote the gap-increasing permeation, in addition, the wetting agent has excellent wettability, the coal seam can be further wetted, and contains a large amount of carboxyl, hydroxyl and amino groups which are all hydrophilic functional groups and can attract water molecules to promote the adsorption of the water molecules and coal bodies, and when the coal is mined, the wetting agent wrapping dust can adsorb the dust under the synergistic effect of the self cohesiveness and intermolecular acting force, thereby being beneficial to promoting the deposition of the dust.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following description will briefly explain the drawings needed in the embodiments of the present application, and it is obvious that the drawings described below are only some embodiments of the present application, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of a preparation method of a high-efficiency permeable wetting type moisturizing agent for coal seam water injection according to an embodiment of the present invention.
Fig. 2 is a molecular synthesis diagram of the high-efficiency penetration wetting type moisturizing agent for coal seam water injection according to the embodiment of the invention.
Fig. 3 is a flowchart of a preparation method of an efficient permeable wetting agent for coal seam water injection according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Aiming at the problems existing in the prior art, the invention provides an efficient permeable wetting type moisturizing agent for coal seam water injection and a preparation method thereof, and the invention is described in detail below with reference to the accompanying drawings.
The efficient penetrating and wetting type moisturizing agent for coal seam water injection provided by the embodiment of the invention comprises, by mass, 1.25% of hydroxyethyl cellulose, 2.5% -4.5% of methyl stearoyl acrylate, 1% -3% of acrylamide, 0.1% -0.5% of an initiator, 0.0% -0.5% of a penetrating agent, and 0.0% -0.5% of a wetting agent and water; the water is filled up to 100%.
The initiator provided by the embodiment of the invention is ceric ammonium nitrate.
The penetrating agent provided by the embodiment of the invention is sodium dodecyl sulfate; the wetting agent is fatty alcohol polyoxyethylene ether.
The optimal proportion of the high-efficiency permeable wetting type moisturizing agent for coal seam water injection in 400ml of water provided by the embodiment of the invention is hydroxyethyl cellulose: stearoyl methyl acrylate: acrylamide=1:1:1, ceric ammonium nitrate: water = 1:500, sodium dodecyl sulfate: fatty alcohol polyoxyethylene ether=3:1.
As shown in fig. 1 to 3, the preparation method of the efficient permeable wetting agent for coal seam water injection provided by the embodiment of the invention comprises the following steps:
s101, placing hydroxyethyl cellulose into a three-neck flask with distilled water, introducing nitrogen, and gelatinizing at 80 ℃ to obtain a first solution;
s102, cooling to 30-70 ℃ after gelatinizing the first solution, respectively adding methyl stearoyl acrylate and acrylamide, adding ceric ammonium nitrate after the methyl stearoyl acrylate and acrylamide are completely dissolved, and keeping the water bath for heating;
s103, adding N-N methylene bisacrylamide, mixing, stirring and dissolving for 1h to obtain a second solution; cooling the second solution to room temperature; adding sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether, and continuing to heat in water bath for 1h;
s104, synthesizing and extracting a product by adopting microwave vibration, and obtaining the efficient permeable wetting type moisturizing agent for coal seam water injection.
In step S102, the optimal cooling temperature provided in the embodiment of the present invention is 60 ℃.
The preparation method of the efficient permeable wetting agent for coal seam water injection comprises the following steps:
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained.
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1:
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 2
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 30 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 3
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃, 8g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, added sequentially 5 minutes apart, and after complete dissolution, 0.4g of ceric ammonium nitrate was added again, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 4
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 6g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 5
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.8g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 6
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 2.0g of sodium dodecyl sulfate and 0.5g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
Example 7
4g of hydroxyethylcellulose was weighed into a three-necked flask containing 400ml of distilled water, and was purged with nitrogen gas to carry out gelatinization at 80 ℃. After gelatinization, the temperature was adjusted to 60 ℃,4g of methyl stearoyl acrylate, 4g of acrylamide were weighed separately, and added sequentially 5 minutes apart, after which 0.4g of ceric ammonium nitrate was added again after complete dissolution, and the mixture was heated in a water bath for 1 hour. After the mixture is cooled to room temperature, 1.5g of sodium dodecyl sulfate and 1.0g of fatty alcohol polyoxyethylene ether are added, and the product is synthesized and extracted by a microwave vibration method. The high-efficiency penetration wetting type moisturizing agent for coal seam water injection is obtained. And finally testing the relevant performance.
1 reverse osmosis height
The osmotic wetting effect of the moisturizing agent is detected. The glass tubes were filled with coal fines, then the bottom ends were contacted with different solutions, left to stand for one day, and each tube was tested for reverse osmosis height and weight gain for different times for each 4 hours. As shown in table 1.
Reverse osmosis height as in Table 1
Weight gain rate as in Table 2
Shear viscosity
The prepared solutions with different proportions are placed in an NDJ-1 rotary viscometer for testing and shearing viscosity.
Shear viscosity as in Table 3
Dust yield
Crushing the soaked coal blocks, and placing the crushed coal blocks at a wind speed of 6m/s to test the front and rear mass change of the coal blocks so as to obtain the dust yield of the coal blocks.
The dust yield as in Table 4
| Experimental sample | Dust yield (%) |
| Experimental example 1 | 8 |
| Experimental example 2 | 26 |
| Experimental example 3 | 34 |
| Experimental example 4 | 29 |
| Experimental example 5 | 31 |
| Experimental example 6 | 36 |
| Experimental example 7 | 34 |
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (7)
1. The efficient penetration wetting type moisturizing agent for coal seam water injection is characterized in that the efficient penetration wetting type moisturizing agent for coal seam water injection comprises 4g of hydroxyethyl cellulose in 400ml of water, and the ratio of the hydroxyethyl cellulose in 400ml of water is as follows: stearoyl methyl acrylate: acrylamide=1:1:1, penetrant 1.5g, wetting agent 0.5g; and (3) an initiator: water = 1:500 or 1:1000;
the initiator is ceric ammonium nitrate;
the penetrating agent is sodium dodecyl sulfate; the wetting agent is fatty alcohol polyoxyethylene ether; sodium dodecyl sulfate: fatty alcohol polyoxyethylene ether=3:1.
2. A method of preparing the high-efficiency penetration wetting enhancer for coal seam injection of claim 1, comprising:
step one, loading hydroxyethyl cellulose into a three-neck flask with distilled water, and introducing nitrogen to perform gelatinization to obtain a first solution;
step two, cooling after the first solution is gelatinized, respectively adding methyl stearoyl acrylate and acrylamide, after the methyl stearoyl acrylate and acrylamide are completely dissolved, adding ceric ammonium nitrate, and keeping the water bath for heating;
step three, adding N-N methylene bisacrylamide, mixing, stirring and dissolving to obtain a second solution; cooling the second solution; adding sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether, and continuing to heat in a water bath;
and fourthly, synthesizing and extracting a product by adopting microwave vibration to obtain the efficient permeable wetting type moisturizing agent for coal seam water injection.
3. The method of claim 2, wherein in step one, the gelatinization temperature is 80 ℃.
4. The method of claim 2, wherein in step two, the cooling after gelatinization of the first solution comprises: cooling the first solution to 30-70 ℃ after gelatinization; wherein the cooling temperature was 60 ℃.
5. The method of claim 2, wherein in step three, the mixing and stirring dissolution time is 1h.
6. The method of claim 2, wherein in step three, the cooling the second solution comprises: the second solution was cooled to room temperature.
7. The method of claim 2, wherein in step three, the water bath heating time is 1h.
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