无机膜制备高品质磷脂研究及工业化生产
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摘要
针对国内在高品质磷脂产品开发及工业化生产中脱杂、脱色、脱溶、脱油等尚未完全解决的问题，本课题以饲料级浓缩磷脂为原料，采用新型高效的无机膜分离技术，通过深入系统的研究，解决了上述技术难点，建立了高品质食品级浓缩磷脂、粉末磷脂产品的生产技术，并进行了工业化生产实践。
首先以饲料级浓缩磷脂为原料，采用无机陶瓷膜微滤技术，制备杂质含量低的浓缩磷脂。在水分含量0.1%，膜孔径0.20μm，溶料比6:1（w/w），过滤温度50°C，物料流速3m/s的条件下，产品中丙酮不溶物含量达到60%以上，乙醚不溶物含量可以稳定地控制在0.05%以下。在考察膜管孔径、压力、溶剂比、温度等工艺参数与膜通量、产品指标的关系的基础上，研究了膜污染的清洗方法以及膜微滤截留物。研究表明：在过滤进行到6h后必须进行清洗，采用2g/dL NaOH溶液在80°C对膜进行2h清洗效果最佳；膜微滤截留物中主要包括蛋白质、糖类以及灰分，其中蛋白质含量为45.64%，糖类33.22%(其中水溶性多糖15.86%)，灰分7.44%。其组成接近于大豆粕，且热稳定性较好，富含无机矿物质元素；研究结果表明上述物质是影响国产大豆浓缩磷脂含杂量、透明度的主要因素。
其次采用食品级双氧水对膜微滤浓缩磷脂进行了化学脱色，研究结果表明：温度、时间和脱色剂添加量是影响脱色的重要条件，在温度40°C，时间60min，脱色剂添加量为2.5%的条件下，脱色磷脂Gardner色泽为9.6，酸值为34.5mgKOH/g油，过氧化值为16.15mmol/kg油；经蒸发预脱溶后，在50°C，残压为0.18kPa下薄膜蒸发，产品丙酮不溶物大于61%，在刮板转速100r/min，进料速率7L/h，预热温度90℃，冷凝水温度25℃，蒸馏温度100℃条件下进一步短程蒸馏，获得产品丙酮不溶物大于62%，乙醚不溶物小于0.05%，过氧化值低于3.5mmol/kg，加德纳色泽低于9+，挥发物小于50mg/kg，产品透明度良好，满足一级浓缩磷脂及ADM食品级浓缩磷脂标准。
基于磷脂在非极性溶剂中形成大尺寸反胶束原理，利用磷脂在正己烷-水体系形成反胶束，采用动态光散射对影响磷脂反胶束尺寸的因素进行了系统研究。研究表明，溶剂比、加水量和温度对反胶束尺寸有重要影响，反胶束尺寸随加水量增加出现先增大后减小，随溶剂比减小和温度降低而增大。经实验可知：浓缩磷脂与正己烷质量比为1:3，加水量9%，温度25°C的条件下，所形成的磷脂反胶束平均粒径为9.8nm，超过98%的粒子尺寸大于5nm。故选用5nm的无机陶瓷膜超滤截留磷脂反胶束，脱除了食品级浓缩磷脂中甘油三酯。食品级浓缩磷脂溶液系统的组分相当复杂，通过生长曲线模型预测了超滤过程中膜污垢热阻和膜通量随膜分离时间的变化规律，为工业化生产中控制膜过滤过程，提高膜分离效率提供了理论指导。
在上述实验室小试研究基础上，对食品级浓缩磷脂、粉末磷脂制备进行了工业化放大，通过中试、生产调试工作，建立了高效膜法生产高品质食品级浓缩磷脂、粉末磷脂的技术，最终产品的各项指标达到甚至超过国外相应产品标准。通过该项目的工业化实践，扭转了我国此类产品完全依赖进口的局面，实现了高品质磷脂产品国产化，打破了国外在此项技术上的长期垄断，增强了我国磷脂加工企业的核心竞争力，作为“大豆磷脂生产关键技术及产业化开发”项目的主要内容获2010年国家科技进步二等奖。
For domestic technical difficulties in high quality lecithin products development and industrialproduction in taking off impurities, decoloring, desolvating and taking off the oil aspects, thefeed-grade lecithin was used as raw material in this research, solving these difficulties using thenew and high efficient inorganic membrane separation technology through deeply systematicresearch, establishing the production technology of high quality food-grade lecithin and powderlecithin, and conducting industrial production practice.
Firstly, the feed-grade lecithin was used as raw material, lecithin concentrate contained lowcontent of impurities was prepared using inorganic ceramic microfiltration membrane. Under thecondition of moisture content0.1%, membrane aperture0.20μm, solvent/material6:1, filtrationtemperature50°C, and the material flow3m/s, acetone insoluble content of products more than60%and ethyl ether insoluble content could be steadily controlled under0.05%. In examining therelationship between process parameters, such as film pipe diameter, pressure, solvent ratio,temperature, membrane flux and the product index, the clean method of membrane pollution andcomposition film microfilter intercept content were studied. After filter6h, the film must becleaned, and the cleaning effect was the best using2g/dL NaOH solution in80°C washed thefilm2h. The composition of intercept mainly include45.64%protein,33.22%carbohydrate(including15.86%water-soluble polysaccharide) and ash. Its component closed to soybean meal,and had good thermal stability, which was rich in inorganic mineral elements. The results showthat the above material is the main factors which affect impurity and transparency of domesticlecithin concentrate.
Secondly, membrane microfilter lecithin concentrate was chemical decolored using the foodgrade hydrogen peroxide. The results of these study show that temperature, time and amount ofdecoloring agents adding are the important conditions influence bleaching. Under the condition of40°C,60min decoloring time,2.5%decoloring agents addition, Gardner colour, acid value andperoxide value of decoloring lecithin was9.6,34.5mgKOH/g oil,16.15mmol/kg, respectively.After prior solvent evaporation, acetone insoluble of product was greater than61%under50°C,0.18kPa pressure using the film evaporation. And after further short-range distillation under thecondition of scraper speed100r/min, feeding rate7L/h, preheat temperature90°C, thecondensed water temperature25°C, temperature100°C, in addition to acetone insoluble morethan62%, other parameters, such as ethyl ether insoluble, peroxide value, Gardner colour, volatilematter were less than0.05%,3.5mmol/kg,9+,50mg/kg, respectively, transparency of productwas good, satisfying the first level standards of lecithin concentrate and ADM food-grade lecithin.
Based on the principle of the lecithins form big size reverse micelle in nonpolar solvent, asystematic study on the factors effect lecithin reverse micelle size in hexane-water system usingdynamic light scattering was conducted. Research showed that, the solvent ratio, water additionand temperature had significant effects on the size of reverse micelle, reverse micelle size firstincreased with water added, then decreased, increased with the decrease of the solvent ratio andtemperature. The experiment indicated that average particle size of lecithin reverse micelle was9.8nm, more than98%of the particle size was greater than5nm. So choosing5nm inorganicceramic membrane intercepted lecithin reverse micelle through the ultrafiltration, removingtriglycerides from the food-grade lecithin. The components of food-grade lecithin solution werevery complex. It could forecast the chang rule of fouling heat resistance and flux of ultrafiltrationmembrane with the ultrafiltration time throughing the growth curve model, which could providethe theoretical guidance in improving the membrane separation efficiency for the industrialproduction controlling film filtration process.
Based on the above laboratory test, food-grade and powder lecithin were produced underindustrialization amplifier, throughing the test and production debugging work, established thetechnology of high efficient membrane production of high quality food-grade and powder lecithin,and the indexes of corresponding products achieved and even exceed corresponding foreignproduct standards. Throughing the project practice of industrialization, reversed the situation ofsuch products of our country completely dependent on imported, realized the high quality lecithinproduct localization, breaked long-term technical monopoly of abroad, and enhanced lecithinprocessing enterprise's core competitiveness of our country. As the main contents of "soybeanlecithin production key technology and industrialization development" project, it was awardedsecond prize in2010National Science and Technology Awards.
首先以饲料级浓缩磷脂为原料，采用无机陶瓷膜微滤技术，制备杂质含量低的浓缩磷脂。在水分含量0.1%，膜孔径0.20μm，溶料比6:1（w/w），过滤温度50°C，物料流速3m/s的条件下，产品中丙酮不溶物含量达到60%以上，乙醚不溶物含量可以稳定地控制在0.05%以下。在考察膜管孔径、压力、溶剂比、温度等工艺参数与膜通量、产品指标的关系的基础上，研究了膜污染的清洗方法以及膜微滤截留物。研究表明：在过滤进行到6h后必须进行清洗，采用2g/dL NaOH溶液在80°C对膜进行2h清洗效果最佳；膜微滤截留物中主要包括蛋白质、糖类以及灰分，其中蛋白质含量为45.64%，糖类33.22%(其中水溶性多糖15.86%)，灰分7.44%。其组成接近于大豆粕，且热稳定性较好，富含无机矿物质元素；研究结果表明上述物质是影响国产大豆浓缩磷脂含杂量、透明度的主要因素。
其次采用食品级双氧水对膜微滤浓缩磷脂进行了化学脱色，研究结果表明：温度、时间和脱色剂添加量是影响脱色的重要条件，在温度40°C，时间60min，脱色剂添加量为2.5%的条件下，脱色磷脂Gardner色泽为9.6，酸值为34.5mgKOH/g油，过氧化值为16.15mmol/kg油；经蒸发预脱溶后，在50°C，残压为0.18kPa下薄膜蒸发，产品丙酮不溶物大于61%，在刮板转速100r/min，进料速率7L/h，预热温度90℃，冷凝水温度25℃，蒸馏温度100℃条件下进一步短程蒸馏，获得产品丙酮不溶物大于62%，乙醚不溶物小于0.05%，过氧化值低于3.5mmol/kg，加德纳色泽低于9+，挥发物小于50mg/kg，产品透明度良好，满足一级浓缩磷脂及ADM食品级浓缩磷脂标准。
基于磷脂在非极性溶剂中形成大尺寸反胶束原理，利用磷脂在正己烷-水体系形成反胶束，采用动态光散射对影响磷脂反胶束尺寸的因素进行了系统研究。研究表明，溶剂比、加水量和温度对反胶束尺寸有重要影响，反胶束尺寸随加水量增加出现先增大后减小，随溶剂比减小和温度降低而增大。经实验可知：浓缩磷脂与正己烷质量比为1:3，加水量9%，温度25°C的条件下，所形成的磷脂反胶束平均粒径为9.8nm，超过98%的粒子尺寸大于5nm。故选用5nm的无机陶瓷膜超滤截留磷脂反胶束，脱除了食品级浓缩磷脂中甘油三酯。食品级浓缩磷脂溶液系统的组分相当复杂，通过生长曲线模型预测了超滤过程中膜污垢热阻和膜通量随膜分离时间的变化规律，为工业化生产中控制膜过滤过程，提高膜分离效率提供了理论指导。
在上述实验室小试研究基础上，对食品级浓缩磷脂、粉末磷脂制备进行了工业化放大，通过中试、生产调试工作，建立了高效膜法生产高品质食品级浓缩磷脂、粉末磷脂的技术，最终产品的各项指标达到甚至超过国外相应产品标准。通过该项目的工业化实践，扭转了我国此类产品完全依赖进口的局面，实现了高品质磷脂产品国产化，打破了国外在此项技术上的长期垄断，增强了我国磷脂加工企业的核心竞争力，作为“大豆磷脂生产关键技术及产业化开发”项目的主要内容获2010年国家科技进步二等奖。
For domestic technical difficulties in high quality lecithin products development and industrialproduction in taking off impurities, decoloring, desolvating and taking off the oil aspects, thefeed-grade lecithin was used as raw material in this research, solving these difficulties using thenew and high efficient inorganic membrane separation technology through deeply systematicresearch, establishing the production technology of high quality food-grade lecithin and powderlecithin, and conducting industrial production practice.
Firstly, the feed-grade lecithin was used as raw material, lecithin concentrate contained lowcontent of impurities was prepared using inorganic ceramic microfiltration membrane. Under thecondition of moisture content0.1%, membrane aperture0.20μm, solvent/material6:1, filtrationtemperature50°C, and the material flow3m/s, acetone insoluble content of products more than60%and ethyl ether insoluble content could be steadily controlled under0.05%. In examining therelationship between process parameters, such as film pipe diameter, pressure, solvent ratio,temperature, membrane flux and the product index, the clean method of membrane pollution andcomposition film microfilter intercept content were studied. After filter6h, the film must becleaned, and the cleaning effect was the best using2g/dL NaOH solution in80°C washed thefilm2h. The composition of intercept mainly include45.64%protein,33.22%carbohydrate(including15.86%water-soluble polysaccharide) and ash. Its component closed to soybean meal,and had good thermal stability, which was rich in inorganic mineral elements. The results showthat the above material is the main factors which affect impurity and transparency of domesticlecithin concentrate.
Secondly, membrane microfilter lecithin concentrate was chemical decolored using the foodgrade hydrogen peroxide. The results of these study show that temperature, time and amount ofdecoloring agents adding are the important conditions influence bleaching. Under the condition of40°C,60min decoloring time,2.5%decoloring agents addition, Gardner colour, acid value andperoxide value of decoloring lecithin was9.6,34.5mgKOH/g oil,16.15mmol/kg, respectively.After prior solvent evaporation, acetone insoluble of product was greater than61%under50°C,0.18kPa pressure using the film evaporation. And after further short-range distillation under thecondition of scraper speed100r/min, feeding rate7L/h, preheat temperature90°C, thecondensed water temperature25°C, temperature100°C, in addition to acetone insoluble morethan62%, other parameters, such as ethyl ether insoluble, peroxide value, Gardner colour, volatilematter were less than0.05%,3.5mmol/kg,9+,50mg/kg, respectively, transparency of productwas good, satisfying the first level standards of lecithin concentrate and ADM food-grade lecithin.
Based on the principle of the lecithins form big size reverse micelle in nonpolar solvent, asystematic study on the factors effect lecithin reverse micelle size in hexane-water system usingdynamic light scattering was conducted. Research showed that, the solvent ratio, water additionand temperature had significant effects on the size of reverse micelle, reverse micelle size firstincreased with water added, then decreased, increased with the decrease of the solvent ratio andtemperature. The experiment indicated that average particle size of lecithin reverse micelle was9.8nm, more than98%of the particle size was greater than5nm. So choosing5nm inorganicceramic membrane intercepted lecithin reverse micelle through the ultrafiltration, removingtriglycerides from the food-grade lecithin. The components of food-grade lecithin solution werevery complex. It could forecast the chang rule of fouling heat resistance and flux of ultrafiltrationmembrane with the ultrafiltration time throughing the growth curve model, which could providethe theoretical guidance in improving the membrane separation efficiency for the industrialproduction controlling film filtration process.
Based on the above laboratory test, food-grade and powder lecithin were produced underindustrialization amplifier, throughing the test and production debugging work, established thetechnology of high efficient membrane production of high quality food-grade and powder lecithin,and the indexes of corresponding products achieved and even exceed corresponding foreignproduct standards. Throughing the project practice of industrialization, reversed the situation ofsuch products of our country completely dependent on imported, realized the high quality lecithinproduct localization, breaked long-term technical monopoly of abroad, and enhanced lecithinprocessing enterprise's core competitiveness of our country. As the main contents of "soybeanlecithin production key technology and industrialization development" project, it was awardedsecond prize in2010National Science and Technology Awards.
引文
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