含氟丙烯酸酯树脂的合成及在油水分离材料中的应用
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摘要
随着航空、汽车工业的发展,人们对飞机、汽车发动机的要求越来越高,而作为发动机的“血液”-燃油和液压油,它们的品质直接影响着发动机的性能。油液含水量是油液品质的一项重要指标,是导致发动机故障的主要原因之一。燃油中水的危害可以归纳为:腐蚀和堵塞空隙。燃油中的水常常析出硫化物使之转变成酸,增加了对发动机喷油系统和发动机本身的腐蚀。水也促使了形成积渣的微生物的滋长,它很容易使有微孔的零部件堵塞例如喷嘴、滤清器等。上述现象即使在水的含量很低的情况下也会发生。因此除去油液中的少量含水显得非常的重要和有意义。本论文制备具有良好疏水和机械性能的含氟丙烯酸酯树脂,并对其进行亲油性的改善,制备了具有油水分离功能的滤网涂层,应用在油液滤清器上取得了较好的油水分离效率。
论文首先合成了含氟丙烯酸酯树脂,确定了单体的种类、加入量、反应温度、引发剂种类等。采用甲基丙烯酸甲酯MMA、丙烯酸丁酯BA、甲基丙烯酸羟基乙酯HEMA、甲基丙烯酸全氟烷基酯FMA为反应单体,偶氮二异丁腈AIBN为引发剂加入量1.5%(w/w)分两次添加、反应温度85℃、MMA与BA的配比为4:6(w/w),HEMA的加入量为15%(w/w),氟单体FMA采用后期一次性添加的方式加入量为3%制得了具有低粘度,低分子量的共聚物,对树脂的涂装工艺进行了探索,确定了树脂的涂装工艺条件:固化剂中NCO含量与羟基含量比值为1.1:1(摩尔比),树脂固化温度110℃,固化时间2h,以及在不锈钢滤网涂膜时的上胶浓度为3%(w/w)。
固化后涂膜具有良好的附着力划格法0级,较好的耐溶剂性、耐油性,涂膜在10%(w/w) HCl和10%(w/w) NaOH溶液中浸泡7天后表面无明显变化;涂膜在煤油、液压油中浸泡1个月无明显变化。耐高低温性能良好在-55℃到200℃范围内性质无变化,基本满足树脂在滤清器油水分离环境中需要达到的要求。
对含氟丙烯酸酯树脂进行亲油改善,通过引入长链烷烃高级丙烯酸酯,讨论了长链烷烃高级丙烯酸酯的烷烃链长,添加方式、与氟单体的配比以及氟单体链长对亲油性效果的影响。确定了最优的亲油改善工艺配方,即以甲基丙烯酸十八烷基酯SMA作为亲油改性单体,氟单体选用甲基丙烯酸全氟烷基酯FMA,两者按照3:7(w/w)的比例,用量占单体总量的15%的条件下,在反应后期一次性加入。改性后的树脂对煤油的亲油性提高较为明显;对液压油亲油性的提高效果不明显。同时,树脂能在提高亲油性的同时进一步提高树脂的疏水效果。
最后通过油水分离实验,对树脂的油水分离效率进行测试,结果表明分离效率与油液的初始含水量成正比关系;要获得好的分离效率在亲油改善过程中一定要保证树脂好的疏水效果。通过与成熟的商品样进行比较,得出自制的亲油改善的含氟丙烯酸酯树脂具有较好的油水分离效率,与商品样的分离效率较为接近。
With the development of aviation and automobile industry, people’s demand for the engines of car and aircraft have become increasingly high, and as the "blood" of engine - oil and hydraulic oil plays an important role in the efficiency of engine.the risk of water in the oil can be summarized: corrosion and block holes .The water in oil offen make the precipitate becoming into acid.which will increase the corrosion of the fuel injection system and the engine.and the water promote the growth of microorganisms.which is the resion to produce precipitates. It's worth noting that the above-mentioned phenomenon offen taken place when the water is very less in the oil.so,it is very important to separate water from oil. my paper provided the fluorine-containing acrylic resin with good hydro-oil-phobicity and adhesion, mechanical properties, and then improved the oilphilic of resion and prepared the filter coating with oil and water separation function which applied to the oil filter achieved a better water separation efficiency.
Firstly synthesized fluorinated acrylic resin and determined the choice of monomer, used MMA BA HEMA and FMA as the monomers. The ratio MMA/BA:4:6(w/w),AIBN as the initiator and the dosage is 1.5%(w/w).and add in two times.rection temperature is 85℃,the dosage of HEMA is 15%(w/w).and the dosage of FMA is 3%(w/w),add in one time at the later period. received copolymer with low viscosity, low molecular weight. explored the coating technique of the resin and determine the conditions of coating procedure: the ratio of curing agent content- NCO and hydroxyl content is 1.1:1(mol/mol), curing temperature:110℃, curing time:2h and the coating concentration when coating on stainless steel filter is 3%(w/w).
the cured film has good adhesion:0 grade , good solvent resistance :there is no change under the condition of Immersing in 10%(w/w) HCl和10%(w/w) NaOH for 7 days.and it is als o that Immerse in oil and hydraulic oil for 1 month. and good resistance to high and low temperature performance:there is no change at the temperature between -55℃and 300℃. The resion can meet the mechanical properties required which is used in the oil and water separation industries .
Improve the oilphilic of the fluorinated acrylic resin through the introduction of long-chain alkanes acrylate. discussed the length of long-chain alkanes acrylate, add methods, and the ratio of fluorine monomers and long-chain alkanes acrylate,the length of fluorine monomer chain to the oilphilic .and determined to use SMA and FMA at the ratio of 7:3 (w/w),and the adding volume:15%(w/w).the contact angele with coal oil decreased obviously. and the contact angele with hydraulic oil decrease only a little.
Finally, through the experiment of oil-water separation, the efficiency of resin oil and water separation been tested , discussed the initial water content in oil .the two different processes on improve oilphilic. Compare our sample with mature product in oil-water separation efficiency. The results showed that the fluorinated acrylic resin which been treated by oilphilic has good water separation efficiency, but there still some distance compare with merchandise .
论文首先合成了含氟丙烯酸酯树脂,确定了单体的种类、加入量、反应温度、引发剂种类等。采用甲基丙烯酸甲酯MMA、丙烯酸丁酯BA、甲基丙烯酸羟基乙酯HEMA、甲基丙烯酸全氟烷基酯FMA为反应单体,偶氮二异丁腈AIBN为引发剂加入量1.5%(w/w)分两次添加、反应温度85℃、MMA与BA的配比为4:6(w/w),HEMA的加入量为15%(w/w),氟单体FMA采用后期一次性添加的方式加入量为3%制得了具有低粘度,低分子量的共聚物,对树脂的涂装工艺进行了探索,确定了树脂的涂装工艺条件:固化剂中NCO含量与羟基含量比值为1.1:1(摩尔比),树脂固化温度110℃,固化时间2h,以及在不锈钢滤网涂膜时的上胶浓度为3%(w/w)。
固化后涂膜具有良好的附着力划格法0级,较好的耐溶剂性、耐油性,涂膜在10%(w/w) HCl和10%(w/w) NaOH溶液中浸泡7天后表面无明显变化;涂膜在煤油、液压油中浸泡1个月无明显变化。耐高低温性能良好在-55℃到200℃范围内性质无变化,基本满足树脂在滤清器油水分离环境中需要达到的要求。
对含氟丙烯酸酯树脂进行亲油改善,通过引入长链烷烃高级丙烯酸酯,讨论了长链烷烃高级丙烯酸酯的烷烃链长,添加方式、与氟单体的配比以及氟单体链长对亲油性效果的影响。确定了最优的亲油改善工艺配方,即以甲基丙烯酸十八烷基酯SMA作为亲油改性单体,氟单体选用甲基丙烯酸全氟烷基酯FMA,两者按照3:7(w/w)的比例,用量占单体总量的15%的条件下,在反应后期一次性加入。改性后的树脂对煤油的亲油性提高较为明显;对液压油亲油性的提高效果不明显。同时,树脂能在提高亲油性的同时进一步提高树脂的疏水效果。
最后通过油水分离实验,对树脂的油水分离效率进行测试,结果表明分离效率与油液的初始含水量成正比关系;要获得好的分离效率在亲油改善过程中一定要保证树脂好的疏水效果。通过与成熟的商品样进行比较,得出自制的亲油改善的含氟丙烯酸酯树脂具有较好的油水分离效率,与商品样的分离效率较为接近。
With the development of aviation and automobile industry, people’s demand for the engines of car and aircraft have become increasingly high, and as the "blood" of engine - oil and hydraulic oil plays an important role in the efficiency of engine.the risk of water in the oil can be summarized: corrosion and block holes .The water in oil offen make the precipitate becoming into acid.which will increase the corrosion of the fuel injection system and the engine.and the water promote the growth of microorganisms.which is the resion to produce precipitates. It's worth noting that the above-mentioned phenomenon offen taken place when the water is very less in the oil.so,it is very important to separate water from oil. my paper provided the fluorine-containing acrylic resin with good hydro-oil-phobicity and adhesion, mechanical properties, and then improved the oilphilic of resion and prepared the filter coating with oil and water separation function which applied to the oil filter achieved a better water separation efficiency.
Firstly synthesized fluorinated acrylic resin and determined the choice of monomer, used MMA BA HEMA and FMA as the monomers. The ratio MMA/BA:4:6(w/w),AIBN as the initiator and the dosage is 1.5%(w/w).and add in two times.rection temperature is 85℃,the dosage of HEMA is 15%(w/w).and the dosage of FMA is 3%(w/w),add in one time at the later period. received copolymer with low viscosity, low molecular weight. explored the coating technique of the resin and determine the conditions of coating procedure: the ratio of curing agent content- NCO and hydroxyl content is 1.1:1(mol/mol), curing temperature:110℃, curing time:2h and the coating concentration when coating on stainless steel filter is 3%(w/w).
the cured film has good adhesion:0 grade , good solvent resistance :there is no change under the condition of Immersing in 10%(w/w) HCl和10%(w/w) NaOH for 7 days.and it is als o that Immerse in oil and hydraulic oil for 1 month. and good resistance to high and low temperature performance:there is no change at the temperature between -55℃and 300℃. The resion can meet the mechanical properties required which is used in the oil and water separation industries .
Improve the oilphilic of the fluorinated acrylic resin through the introduction of long-chain alkanes acrylate. discussed the length of long-chain alkanes acrylate, add methods, and the ratio of fluorine monomers and long-chain alkanes acrylate,the length of fluorine monomer chain to the oilphilic .and determined to use SMA and FMA at the ratio of 7:3 (w/w),and the adding volume:15%(w/w).the contact angele with coal oil decreased obviously. and the contact angele with hydraulic oil decrease only a little.
Finally, through the experiment of oil-water separation, the efficiency of resin oil and water separation been tested , discussed the initial water content in oil .the two different processes on improve oilphilic. Compare our sample with mature product in oil-water separation efficiency. The results showed that the fluorinated acrylic resin which been treated by oilphilic has good water separation efficiency, but there still some distance compare with merchandise .
引文
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