The invention discloses a near infrared spectroscopy method for determining the acid value in the process of methyl esterification of biodiesel. The method uses the frequency doubling and frequency combining absorption of COO-H vibration of free fatty acids containing hydrogen group in oil to generate spectrograms, and makes an acid value measurement model by partial least squares regression and factor regression method based on the principle of optimum factor number selection, and indirectly determines the acid value of the tested sample (1). Centrifugal operation was carried out to prepare the samples to be measured; (2) The samples to be measured were put into quartz colorimetric dishes, and the penetrating surface of the colorimetric dishes was wiped clean with mirror paper; (3) According to the original state of the instrument, a pre-established measurement model was selected for reference, and then the colorimetric dishes containing the samples to be measured were put into the sample pool sweep spectrum, and the acid value was measured by near infrared detection. The acid value of the sample was calculated by analytical model software; (4) Samples from the sample pool were taken out and recycled, colorimetric dishes were cleaned, and then soaked in anhydrous ethanol and dried. The invention has the advantages of simple and fast operation, low cost, high accuracy and good applicability.
【技术实现步骤摘要】
生物柴油甲酯化生产过程中酸值的近红外光谱测定方法
本专利技术涉及一种生物柴油(脂肪酸甲酯)酸值的测定方法,具体涉及生物柴油甲酯化生产过程中酸值的近红外光谱测定方法。
技术介绍
酸值[1]是生物柴油产品的一个主要产品指标,是中和1克生物柴油中游离脂肪酸消耗氢氧化钾的毫克数,其值高低代表游离脂肪酸甲酯化的程度。生物柴油调和燃料(B5)[2]对酸值[3]指标提出明确的要求。生物柴油在精细化工有着广泛的应用,尤其是做为替代非环保型增塑剂DOP的一种生物基环保型增塑剂(环氧甲酯、氯化甲酯)的原料而倍受关注,其酸值指标对增塑性能存在较大的影响。酸值做为油脂甲酯化程度的判定依据,在油脂甲酯化生产的过程中对酸值变化的监测,就显得非常的重要。国家标准GB/T264-83《石油产品酸值测定法》分析方法、GB/T5530-2005《动植物油脂酸值和酸度的测定》化学分析方法是目前行业的通用检测分析方法。油脂甲酯化的工业化生产中,酸值检测频率非常高,而现有的检测技术不仅检测工作量非常大,而且还要消耗大量的化学品。因此,建立一种操作简单、成本低廉的准确判定油脂甲酯化进程的酸值测定的方法,已成为油脂甲酯化酸值检测分析中亟需攻克的研究课题,近年来近红外光谱在化工领域的应用[4]给我们提供了条件。参考文献:[1]《石油产品酸值测定法》[S],GB/T264-83。[2]《生物柴油调和燃料(B5)》[S],GB/T25199-2014。[3]《动植物油脂酸值和酸度的测定》[S],GB/T5530-2005。[4]袁洪福,褚小立,陆婉珍,魏东。在线近红外光谱成套分析技术及其在石油化工中的应用[ ...
【技术保护点】
1.一种生物柴油甲酯化生产过程中酸值的近红外光谱测定方法,其特征是:它以近红外光谱分析仪作为测量仪器,利用油脂中游离脂肪酸含氢基团COO-H振动的倍频和合频吸收产生光谱图,以偏最小二乘回归和最佳因子数选取原则因子回归方法制作酸值测量模型,间接确定被测样品的酸值;具体操作步骤如下:第一步:将生产过程中取得的油脂甲酯化进程样进行离心操作,制得待测样品;第二步:将待测样品装填入石英比色皿中,用擦镜纸将比色皿的透色面擦拭干净;第三步:根据仪器原始状态,选定预先制定的测量模型,进行参比,然后将装有待测样品的比色皿放至样品池进行扫谱,经近红外检测后由酸值测量分析模型软件计算样品油脂甲酯化的酸值;第四步:取出样品池试样,回收试样,清洗比色皿,比色皿经无水乙醇浸泡后晾干备用。
【技术特征摘要】
1.一种生物柴油甲酯化生产过程中酸值的近红外光谱测定方法,其特征是:它以近红外光谱分析仪作为测量仪器,利用油脂中游离脂肪酸含氢基团COO-H振动的倍频和合频吸收产生光谱图,以偏最小二乘回归和最佳因子数选取原则因子回归方法制作酸值测量模型,间接确定被测样品的酸值;具体操作步骤如下:第一步:将生产过程中取得的油脂甲酯化进程样进行离心操作,制得待测样品;第二步:将待测样品装填入石英比色皿中,用擦镜纸将比色皿的透色面擦拭干净;第三步:根据仪器原始状态,选定预先制定的测量模型...
【专利技术属性】
技术研发人员:叶活动,杨明聪,
申请(专利权)人:厦门卓越生物质能源有限公司,
类型:发明
国别省市:福建,35
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