脂肪酸生产中的油脚去杂及其在氧化铝结晶助剂中的应用
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摘要
脂肪酸生产中的油脚(下文简称油脚)植物油经水解、蒸馏等工序加工天然脂肪酸后留在蒸馏塔底的脚料。目前,油脚主要被用于脱膜剂、防水沥青、人工饲料等粗产品的制备,没有实现资源的充分利用。本文目的在于通过脱胶、脱酸、脱色实现对油脚的去杂,并将其应用于氧化铝生产油溶性添加剂中。
首先,合成了用于油脚脱胶用的淀粉接枝聚丙烯酰胺(SPAM)。考察了玉米淀粉的形态和糊化温度、糊化用水量、引发剂量、溶剂量、温度、单体浓度及HLB值等各因素对聚合反应的影响。结果表明淀粉接枝前需要糊化,淀粉糊化温度为80℃,糊化用水量为8%,引发剂浓度为0.070%,溶剂量为50.0mL/g,丙烯酰胺单体浓度为0.55mol/L,反应温度为60℃,乳化剂HLB值为8.5时,淀粉接枝聚丙烯酰胺接枝效果最好。通过红外光谱对淀粉接枝聚丙烯酰胺进行了表征和分析。
其次,通过脱胶、脱色、脱酸的手段对油脚进行了去杂处理。确定了淀粉接枝聚丙烯酰胺(SPAM)絮凝脱胶的最佳工艺,即0.03%的SPAM用量,温度为50℃,油脚的运动粘度可由772.5mm2/s降为370.0mm2/s。发现氨水配合破乳剂乙醇,在80℃和搅拌速率为150r/min下进行脱酸操作,脱酸率为84.7%。研究了以活性白土、活性碳、双氧水为脱色剂的油脚脱色方法。通过多因素正交实验,确定了活性白土用量、活性炭用量、双氧水用量,双氧水脱色温度、活性白土脱色时间等主要因素的最佳值,即当以上各因素分别为8%、3.5%、1.2%、55℃、35min时,脱色率为71.3%。
最后,研究了油脚部分替代氧化铝生产中的油溶性添加剂。发现油溶性添加剂Hb和Hc分别被油脚替代20%和15%后得到的新型添加剂H2和H3,其提高铝酸钠溶液分解率的能力基本上与Hb和Hc相当。通过氧化铝分解实验找到了H2和H3的最佳加入时间和加入量分别为8h时,100mg/L和15h时,75mg/L。
Oil residue is the leavings from the production of fatty acid by hydrolysis and distillation of vegetable oil. At present, it is mainly used in the production of releasing agent, waterproofing asphalt, feeding and so on. All of these haven't achieved the full use of oil residue. This paper focused on using degumming, deacidification, decoloration technology to change some of its qualities and making it a useable component of additive for the production of alumina.
First, the degumming agent SPAM was synthesized by NH4S2O8 and NaHSO3 as initiator. The synthetic conditions of SPAM were researched systematically. The optimal synthetic conditions were as follows:pre-gelatinizing temperature:80℃, pre-gelatinizing water:8%, NH4S2O8/NaHSO3:0.070%, grafting Temperature:60℃, solvent dosage:50.0mL/g, HLB value 8.5. The structure of SPAM was characterized by IR.
Second, oil residue was purified by degumming, deacidification and decoloration. The optimal conditions for degumming:SPAM dosage:0.03%, temperature:50℃. The viscosity of oil residue can be reduced from 772.5mm2/s to 370.0mm2/s. Deacidification rate can reach 84.7% with NH3-H2O as the neutralizing agent and ethanol as demulsifier under the temperature of 80℃and whisking velocity of 150r/min. The decoloration based on actived floridin, actived carbon, H2O2 was studied. Through orthogonal experiment best condiction was found:mass fraction of actived floridin:8%, mass fraction of actived carbon:3.5%, mass fraction of H2O2:1.2%, temperature for the H2O2 racting with oil residue:5℃, time for the actived floridin adsorption:35min. Under this condition the best decoloration rate can reach 71.3%.
Third, the purified oil residue was used in the substitution of alumina crystal additive. The primary aditive Hb and Hc can be replaced by the purified oil residue with the content of 20%(H2) and 15%(H3) respectively. The best adding time and quantity for H2 and H3 were 8h, 100mg/L and 15h,75mg/L respectively。
首先,合成了用于油脚脱胶用的淀粉接枝聚丙烯酰胺(SPAM)。考察了玉米淀粉的形态和糊化温度、糊化用水量、引发剂量、溶剂量、温度、单体浓度及HLB值等各因素对聚合反应的影响。结果表明淀粉接枝前需要糊化,淀粉糊化温度为80℃,糊化用水量为8%,引发剂浓度为0.070%,溶剂量为50.0mL/g,丙烯酰胺单体浓度为0.55mol/L,反应温度为60℃,乳化剂HLB值为8.5时,淀粉接枝聚丙烯酰胺接枝效果最好。通过红外光谱对淀粉接枝聚丙烯酰胺进行了表征和分析。
其次,通过脱胶、脱色、脱酸的手段对油脚进行了去杂处理。确定了淀粉接枝聚丙烯酰胺(SPAM)絮凝脱胶的最佳工艺,即0.03%的SPAM用量,温度为50℃,油脚的运动粘度可由772.5mm2/s降为370.0mm2/s。发现氨水配合破乳剂乙醇,在80℃和搅拌速率为150r/min下进行脱酸操作,脱酸率为84.7%。研究了以活性白土、活性碳、双氧水为脱色剂的油脚脱色方法。通过多因素正交实验,确定了活性白土用量、活性炭用量、双氧水用量,双氧水脱色温度、活性白土脱色时间等主要因素的最佳值,即当以上各因素分别为8%、3.5%、1.2%、55℃、35min时,脱色率为71.3%。
最后,研究了油脚部分替代氧化铝生产中的油溶性添加剂。发现油溶性添加剂Hb和Hc分别被油脚替代20%和15%后得到的新型添加剂H2和H3,其提高铝酸钠溶液分解率的能力基本上与Hb和Hc相当。通过氧化铝分解实验找到了H2和H3的最佳加入时间和加入量分别为8h时,100mg/L和15h时,75mg/L。
Oil residue is the leavings from the production of fatty acid by hydrolysis and distillation of vegetable oil. At present, it is mainly used in the production of releasing agent, waterproofing asphalt, feeding and so on. All of these haven't achieved the full use of oil residue. This paper focused on using degumming, deacidification, decoloration technology to change some of its qualities and making it a useable component of additive for the production of alumina.
First, the degumming agent SPAM was synthesized by NH4S2O8 and NaHSO3 as initiator. The synthetic conditions of SPAM were researched systematically. The optimal synthetic conditions were as follows:pre-gelatinizing temperature:80℃, pre-gelatinizing water:8%, NH4S2O8/NaHSO3:0.070%, grafting Temperature:60℃, solvent dosage:50.0mL/g, HLB value 8.5. The structure of SPAM was characterized by IR.
Second, oil residue was purified by degumming, deacidification and decoloration. The optimal conditions for degumming:SPAM dosage:0.03%, temperature:50℃. The viscosity of oil residue can be reduced from 772.5mm2/s to 370.0mm2/s. Deacidification rate can reach 84.7% with NH3-H2O as the neutralizing agent and ethanol as demulsifier under the temperature of 80℃and whisking velocity of 150r/min. The decoloration based on actived floridin, actived carbon, H2O2 was studied. Through orthogonal experiment best condiction was found:mass fraction of actived floridin:8%, mass fraction of actived carbon:3.5%, mass fraction of H2O2:1.2%, temperature for the H2O2 racting with oil residue:5℃, time for the actived floridin adsorption:35min. Under this condition the best decoloration rate can reach 71.3%.
Third, the purified oil residue was used in the substitution of alumina crystal additive. The primary aditive Hb and Hc can be replaced by the purified oil residue with the content of 20%(H2) and 15%(H3) respectively. The best adding time and quantity for H2 and H3 were 8h, 100mg/L and 15h,75mg/L respectively。
引文
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