防治煤自燃的凝胶泡沫及特性研究
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摘要
煤炭自燃是煤矿生产中的主要自然灾害之一，它不仅烧毁或冻结大量煤炭资源，而且常会引发重特大瓦斯爆炸灾害事故，造成重大的人员伤亡和经济损失。目前用于矿井煤自燃防治的方法主要有注浆、注惰气、注阻化剂、注凝胶和注泡沫等，这些技术在矿井煤自燃防治中起到了重要的作用，但也还存在一些不足，难以满足矿井持续堵漏控风与惰化降温的防灭火需要。为了高效防治矿井煤自燃，结合矿井注凝胶和注泡沫防灭火方法，提出了凝胶泡沫防灭火技术。为此，论文对凝胶泡沫的形成机理及相关特性进行了系统研究，在聚合物胶凝机制与形成化学动力学过程、发泡剂与聚合物研制、采空区流动特性、成膜特性、防灭火性能与现场应用等方面都取得了系列的成果。
应用界面化学、胶体化学和高分子材料化学等较系统地提出了凝胶泡沫形成化学动力学过程和胶凝机理。凝胶泡沫是一种介于整体凝胶和胶态分散凝胶之间弱凝胶体系，是由低浓度聚合物以分子间交联为主，分子内交联为辅的高分子体系。浆液在表面活性剂的作用下，通过物理机械搅拌方式形成泡沫，泡沫体系内稠化剂和交联剂通过延迟胶凝作用最终形成凝胶泡沫。其胶凝机理是稠化剂溶于水后，分子链间形成螺旋网状聚合体或双螺旋缔合体，聚合体或缔合体结构中的活性基团与交联剂主链结构中的活性基团充分碰撞接触，从而交联形成立体三维网状结构。
针对凝胶泡沫交联特征及发泡工艺对交联聚合物的要求，研制出适合制备凝胶泡沫的稠化剂和交联剂；同时，依据稠化剂和交联剂对表面活性剂的作用特点，复配出一种发泡倍数高的凝胶泡沫发泡剂。对凝胶泡沫的成胶时间以及稳定性进行了实验研究，得出凝胶泡沫成胶时间在10~20min可调，泡沫静置24h仍能稳定存在。在实验室构建了制备凝胶泡沫的系统并确定了其制备的工艺流程，通过大量实验研究，当溶液复配发泡剂质量浓度为4‰、稠化剂和交联剂质量浓度均为3‰，pH值为7~9时，所形成的凝胶泡沫性能最佳。
研究了凝胶泡沫的流变学特性，结果表明凝胶泡沫具有剪切变稀的性质。即随着剪切速率的增大，凝胶泡沫的表观黏度降低；依据表观黏度和屈服应力测定结果，分别得到了剪切应力—剪切速率的曲线和公式模型。在此基础上，研究了凝胶泡沫在多孔介质中的渗透特性，采用Fluent软件对其在不同倾角采空区的流动扩散与堆积特性进行了数值模拟，弄清了凝胶泡沫在采空区的堆积高度、扩散宽度和扩散长度等参数。
研究了凝胶泡沫的成膜特性，包括成膜微观形貌、水蒸气透过性、吸水性、热辐射阻隔性和堵漏性等。利用AFM观测了凝胶泡沫所成膜的微观形貌，探讨了不同聚合物配比对成膜形貌及性能的影响，实验发现有且仅当稠化剂和交联剂按质量比1:1共混使用时才能够充分交联形成致密平坦的薄膜；同时共混聚合物浓度越大，成膜性越好。通过对薄膜水蒸气透过率、吸水性、热辐射阻隔性和封堵性进行了测试，结果表明，凝胶泡沫表面膜的阻水性能优良，在持续一周内水蒸气透过率均为零；膜吸水重量为自身重量的60~70倍；同时膜能够显著降低外界对可燃物的热辐射，使可燃物表面温度下降40℃以上；且表面膜能承受2500Pa以上的风压，对采空区具有一定的封堵漏风能力。
实验研究了凝胶泡沫的防灭火特性，包括抗温性、抗烧性、凝结堵漏性和阻化性等。结果表明凝胶泡沫抗温性较普通两相泡沫显著提高，随稠化剂和交联剂质量浓度的提高，抗温时间增长，随发泡倍数的提高，抗温时间缩短；抗烧时间为347min，是水的13.88倍、两相泡沫的6.20倍；凝结碎煤比重占原煤样的57%~93.8%（1d后），10d后仍高达13.4%~52.6%；加了1%凝胶泡沫的煤样释放CO速率比原始煤样要推迟20~30℃，100℃时阻化率高达68.89%。并对凝胶泡沫扑灭煤火有效性进行了研究，得出扑灭相同大小的煤火，体积使用量仅为普通泡沫的九分之一，灭火时间不到普通泡沫的一半。灭火时间随稠化剂和交联剂质量浓度的提高，先缩短后增长，当质量浓度均为3‰时，灭火时间最短，效率最高。
最后，采用凝胶泡沫防灭火技术对新集二矿采空区、高冒区等隐蔽位置火源进行了治理，现场的工程应用效果表明，凝胶泡沫技术防灭火以及充填高冒区效果显著，优点突出，特别适用于采空区不明位置火源和高冒区煤炭自燃的防治，是一种具有广阔应用前景和推广价值的新型矿用防灭火材料。
Coal spontaneous combustion, one of the natural disasters in coal mineproduction, not only can burn down or freeze a great deal of coal resources, but alsocommonly triggers severe accidents of gas explosion, causing heavy casualties andeconomic loss. At present, the major control technologies at home and abroad aregrouting, insert gas, inhibitor, gel and foam, etc. Although these techniques haveplayed an important role in preventing coal spontaneous combustion, someshortcomings are obviously existed. For instance, it is difficult to meet the needs ofcontinuous plugging and controlling wind in mine and inserting cooling for coal fire.In order to prevent coal spontaneous combustion effectively, combining with the geland foam, the technology of foamed gel is brought out to prevent the spontaneouscombustion of coal. Consequently, the formation mechanism and correlatedcharacteristics of foamed gel have been systematically studied in this thesis and a lotof results in many aspects are achieved, such as in crosslinking mechanism andforming chemical kinetics, development of foaming agent and polymer, flowcharacteristics in goaf, film forming ability, fire extinguishing and preventing propertyand field application, etc.
The formation of chemical kinetics and gelatinization mechanism of foamed gelwere systematically proposed by interface chemistry, colloid chemistry, polymermaterials chemistry, etc. Foamed gel, a weak gel system between bulk gel andcolloidal dispersion gel, is a kind of polymer system formed by polymer with lowconcentration which are intermolecular crosslinking mainly and intramolecularcrosslinking auxiliarily. With the help of surfactant, the foam is formed by physicaland mechanical stirring. After foaming, the thickener and crosslinker react with eachother and form foamed gel by delayed gelation. The gelatinization mechanism is whenthe thickener dissolved in water, the helical mesh polymer or double helix cluster areformed by molecular chains, besides, active group in polymer or cluster fully collidewith that in the main chain structure of crosslinker, thereby the three-dimensionalnetwork structures are formed.
According to crosslinking characteristics of foamed gel and the requirement offoaming process to crosslinking polymer, the thickener and crosslinker which aresuitable to prepare foamed gel are developed. Meanwhile, depends on the functioncharacteristics that the thickener and crosslinker have on the surfactant, a new kind of foaming agent with high foam expansion has been compounded. Experimental studywas conducted on the gelation time and stability of foamed gel. The results show thatthe gelation time of foamed gel is between10to20min, and the foam is still stableafter standing for24h. In the lab, the system used to develop the foamed gel wasestablished and its technological process was confirmed. After massive experimentalstudies, it turns out that when the mass concentration of compounded foaming agent is4‰, the thickener and crosslinking agent are both3‰, and the pH value is7to9, thefoamed gel with best performance can be formed.
The rheological properties of foamed gel had also been researched. The resultsindicate that it has the shear thinning nature. That is, with the increase of shear rate,the apparent viscosity of foamed gel decreases. Depends on the analysis results of theapparent viscosity and yield stress, the curve and formula model of shear stress-shearrate are obtained respectively. On this basis, the permeability characteristic of foamedgel was studied on the porous media. The Fluent software was adopted to numericallysimulate the characteristics of flowing diffusion and accumulation in goaf withdifferent angles. And the parameters are figured out such as stack height, diffusionwidth and diffusion length.
Researches had also been made on the film forming ability of foamed gel,including film micro-morphology, vapor penetrability, water absorption, radiationbarrier property and leaking stoppage, etc. AFM was employed to observe the filmmicro-morphology and the effects of different proportions of polymers on filmmorphology and characteristics were discussed. The study finds that only when thethickener and crosslinker blending used as well as their mass ratio is1:1, can theycrosslink into tight and smooth film. At the same time, the higher the concentration ofblending polymer is, the better the property of film forming is. After investigating thevapor penetrability, water absorption, radiation barrier property and leaking stoppageof film, the experimental results state that the surface film has a good performance ofwater blocking, the vapor penetrability is zero within a lasted week. After absorbingwater, the weight of film is60~70times of its own weight. Moreover, the film cansignificantly reduce the radiation from outside on the combustible, and therebydecrease the surface temperature of combustible more than40℃. Furthermore, thesurface film can bear the wind pressure of at least2500Pa, thus it has certain ability ofblock air leakage in goaf.
Comprehensive studies were conducted on the fire extinguishing and preventing property of foamed gel, including temperature resistance, burn resistance, coagulationand leaking stoppage, and inhibitation, etc. The results show that the temperatureresistance of foamed gel is significantly improved comparing to two-phase foam，withthe increase of the mass concentration of thickener and crosslinker, the temperatureresistance time grows, moreover, as the increasing of foaming expansion, the time oftemperature resistance decreases. The burn resistance time is347min, which is13.88times of water’s and6.20times of two-phase foam. The proportion that the foamedgel coagulates slack coal is57%~93.8%(1d later) of the coal sample.10d later still upto13.4%~52.6%. When adding1%foamed gel, the coal sample releases CO prolong20~30℃than the original coal sample, when100℃, the inhibition rate reach up to68.89%. This thesis also carried on a research on the effectiveness of foamed gel toputting out coal fire, and it turns out that if puting out the same size of coal fire, onlyuse one ninth of the amount of common foam, less than half of the fire-extinguishingtime of two-phase foam. The time of preventing fire first decreases then increaseswith the increase of mass concentration of thickener and crosslinker, when the massconcentration is3‰, the time is the least and the fire extinguishing effectiveness isthe highest.
Finally, the foamed gel was adopted to prevent and distinguish fire in goaf,top-coal falling region and other concealed locations in Xinji No.2Coal Mine. Theapplication results show that the technology of foamed gel has a significantly effectand outstanding merits in fire preventing and distinguishing and filling top-coalfalling region, which is especially suitable for unknown fire location and coalspontaneous combustion in top-coal falling region. Furthermore, it is a kind of newtype of fire extinguishing and preventing material which has wide applicationprospect and popularization value.
应用界面化学、胶体化学和高分子材料化学等较系统地提出了凝胶泡沫形成化学动力学过程和胶凝机理。凝胶泡沫是一种介于整体凝胶和胶态分散凝胶之间弱凝胶体系，是由低浓度聚合物以分子间交联为主，分子内交联为辅的高分子体系。浆液在表面活性剂的作用下，通过物理机械搅拌方式形成泡沫，泡沫体系内稠化剂和交联剂通过延迟胶凝作用最终形成凝胶泡沫。其胶凝机理是稠化剂溶于水后，分子链间形成螺旋网状聚合体或双螺旋缔合体，聚合体或缔合体结构中的活性基团与交联剂主链结构中的活性基团充分碰撞接触，从而交联形成立体三维网状结构。
针对凝胶泡沫交联特征及发泡工艺对交联聚合物的要求，研制出适合制备凝胶泡沫的稠化剂和交联剂；同时，依据稠化剂和交联剂对表面活性剂的作用特点，复配出一种发泡倍数高的凝胶泡沫发泡剂。对凝胶泡沫的成胶时间以及稳定性进行了实验研究，得出凝胶泡沫成胶时间在10~20min可调，泡沫静置24h仍能稳定存在。在实验室构建了制备凝胶泡沫的系统并确定了其制备的工艺流程，通过大量实验研究，当溶液复配发泡剂质量浓度为4‰、稠化剂和交联剂质量浓度均为3‰，pH值为7~9时，所形成的凝胶泡沫性能最佳。
研究了凝胶泡沫的流变学特性，结果表明凝胶泡沫具有剪切变稀的性质。即随着剪切速率的增大，凝胶泡沫的表观黏度降低；依据表观黏度和屈服应力测定结果，分别得到了剪切应力—剪切速率的曲线和公式模型。在此基础上，研究了凝胶泡沫在多孔介质中的渗透特性，采用Fluent软件对其在不同倾角采空区的流动扩散与堆积特性进行了数值模拟，弄清了凝胶泡沫在采空区的堆积高度、扩散宽度和扩散长度等参数。
研究了凝胶泡沫的成膜特性，包括成膜微观形貌、水蒸气透过性、吸水性、热辐射阻隔性和堵漏性等。利用AFM观测了凝胶泡沫所成膜的微观形貌，探讨了不同聚合物配比对成膜形貌及性能的影响，实验发现有且仅当稠化剂和交联剂按质量比1:1共混使用时才能够充分交联形成致密平坦的薄膜；同时共混聚合物浓度越大，成膜性越好。通过对薄膜水蒸气透过率、吸水性、热辐射阻隔性和封堵性进行了测试，结果表明，凝胶泡沫表面膜的阻水性能优良，在持续一周内水蒸气透过率均为零；膜吸水重量为自身重量的60~70倍；同时膜能够显著降低外界对可燃物的热辐射，使可燃物表面温度下降40℃以上；且表面膜能承受2500Pa以上的风压，对采空区具有一定的封堵漏风能力。
实验研究了凝胶泡沫的防灭火特性，包括抗温性、抗烧性、凝结堵漏性和阻化性等。结果表明凝胶泡沫抗温性较普通两相泡沫显著提高，随稠化剂和交联剂质量浓度的提高，抗温时间增长，随发泡倍数的提高，抗温时间缩短；抗烧时间为347min，是水的13.88倍、两相泡沫的6.20倍；凝结碎煤比重占原煤样的57%~93.8%（1d后），10d后仍高达13.4%~52.6%；加了1%凝胶泡沫的煤样释放CO速率比原始煤样要推迟20~30℃，100℃时阻化率高达68.89%。并对凝胶泡沫扑灭煤火有效性进行了研究，得出扑灭相同大小的煤火，体积使用量仅为普通泡沫的九分之一，灭火时间不到普通泡沫的一半。灭火时间随稠化剂和交联剂质量浓度的提高，先缩短后增长，当质量浓度均为3‰时，灭火时间最短，效率最高。
最后，采用凝胶泡沫防灭火技术对新集二矿采空区、高冒区等隐蔽位置火源进行了治理，现场的工程应用效果表明，凝胶泡沫技术防灭火以及充填高冒区效果显著，优点突出，特别适用于采空区不明位置火源和高冒区煤炭自燃的防治，是一种具有广阔应用前景和推广价值的新型矿用防灭火材料。
Coal spontaneous combustion, one of the natural disasters in coal mineproduction, not only can burn down or freeze a great deal of coal resources, but alsocommonly triggers severe accidents of gas explosion, causing heavy casualties andeconomic loss. At present, the major control technologies at home and abroad aregrouting, insert gas, inhibitor, gel and foam, etc. Although these techniques haveplayed an important role in preventing coal spontaneous combustion, someshortcomings are obviously existed. For instance, it is difficult to meet the needs ofcontinuous plugging and controlling wind in mine and inserting cooling for coal fire.In order to prevent coal spontaneous combustion effectively, combining with the geland foam, the technology of foamed gel is brought out to prevent the spontaneouscombustion of coal. Consequently, the formation mechanism and correlatedcharacteristics of foamed gel have been systematically studied in this thesis and a lotof results in many aspects are achieved, such as in crosslinking mechanism andforming chemical kinetics, development of foaming agent and polymer, flowcharacteristics in goaf, film forming ability, fire extinguishing and preventing propertyand field application, etc.
The formation of chemical kinetics and gelatinization mechanism of foamed gelwere systematically proposed by interface chemistry, colloid chemistry, polymermaterials chemistry, etc. Foamed gel, a weak gel system between bulk gel andcolloidal dispersion gel, is a kind of polymer system formed by polymer with lowconcentration which are intermolecular crosslinking mainly and intramolecularcrosslinking auxiliarily. With the help of surfactant, the foam is formed by physicaland mechanical stirring. After foaming, the thickener and crosslinker react with eachother and form foamed gel by delayed gelation. The gelatinization mechanism is whenthe thickener dissolved in water, the helical mesh polymer or double helix cluster areformed by molecular chains, besides, active group in polymer or cluster fully collidewith that in the main chain structure of crosslinker, thereby the three-dimensionalnetwork structures are formed.
According to crosslinking characteristics of foamed gel and the requirement offoaming process to crosslinking polymer, the thickener and crosslinker which aresuitable to prepare foamed gel are developed. Meanwhile, depends on the functioncharacteristics that the thickener and crosslinker have on the surfactant, a new kind of foaming agent with high foam expansion has been compounded. Experimental studywas conducted on the gelation time and stability of foamed gel. The results show thatthe gelation time of foamed gel is between10to20min, and the foam is still stableafter standing for24h. In the lab, the system used to develop the foamed gel wasestablished and its technological process was confirmed. After massive experimentalstudies, it turns out that when the mass concentration of compounded foaming agent is4‰, the thickener and crosslinking agent are both3‰, and the pH value is7to9, thefoamed gel with best performance can be formed.
The rheological properties of foamed gel had also been researched. The resultsindicate that it has the shear thinning nature. That is, with the increase of shear rate,the apparent viscosity of foamed gel decreases. Depends on the analysis results of theapparent viscosity and yield stress, the curve and formula model of shear stress-shearrate are obtained respectively. On this basis, the permeability characteristic of foamedgel was studied on the porous media. The Fluent software was adopted to numericallysimulate the characteristics of flowing diffusion and accumulation in goaf withdifferent angles. And the parameters are figured out such as stack height, diffusionwidth and diffusion length.
Researches had also been made on the film forming ability of foamed gel,including film micro-morphology, vapor penetrability, water absorption, radiationbarrier property and leaking stoppage, etc. AFM was employed to observe the filmmicro-morphology and the effects of different proportions of polymers on filmmorphology and characteristics were discussed. The study finds that only when thethickener and crosslinker blending used as well as their mass ratio is1:1, can theycrosslink into tight and smooth film. At the same time, the higher the concentration ofblending polymer is, the better the property of film forming is. After investigating thevapor penetrability, water absorption, radiation barrier property and leaking stoppageof film, the experimental results state that the surface film has a good performance ofwater blocking, the vapor penetrability is zero within a lasted week. After absorbingwater, the weight of film is60~70times of its own weight. Moreover, the film cansignificantly reduce the radiation from outside on the combustible, and therebydecrease the surface temperature of combustible more than40℃. Furthermore, thesurface film can bear the wind pressure of at least2500Pa, thus it has certain ability ofblock air leakage in goaf.
Comprehensive studies were conducted on the fire extinguishing and preventing property of foamed gel, including temperature resistance, burn resistance, coagulationand leaking stoppage, and inhibitation, etc. The results show that the temperatureresistance of foamed gel is significantly improved comparing to two-phase foam，withthe increase of the mass concentration of thickener and crosslinker, the temperatureresistance time grows, moreover, as the increasing of foaming expansion, the time oftemperature resistance decreases. The burn resistance time is347min, which is13.88times of water’s and6.20times of two-phase foam. The proportion that the foamedgel coagulates slack coal is57%~93.8%(1d later) of the coal sample.10d later still upto13.4%~52.6%. When adding1%foamed gel, the coal sample releases CO prolong20~30℃than the original coal sample, when100℃, the inhibition rate reach up to68.89%. This thesis also carried on a research on the effectiveness of foamed gel toputting out coal fire, and it turns out that if puting out the same size of coal fire, onlyuse one ninth of the amount of common foam, less than half of the fire-extinguishingtime of two-phase foam. The time of preventing fire first decreases then increaseswith the increase of mass concentration of thickener and crosslinker, when the massconcentration is3‰, the time is the least and the fire extinguishing effectiveness isthe highest.
Finally, the foamed gel was adopted to prevent and distinguish fire in goaf,top-coal falling region and other concealed locations in Xinji No.2Coal Mine. Theapplication results show that the technology of foamed gel has a significantly effectand outstanding merits in fire preventing and distinguishing and filling top-coalfalling region, which is especially suitable for unknown fire location and coalspontaneous combustion in top-coal falling region. Furthermore, it is a kind of newtype of fire extinguishing and preventing material which has wide applicationprospect and popularization value.
引文
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