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工业骨胶除臭、脱色工艺条件研究

Study on Deodorization and Decolorization of Industrial Bone Glue

【作者】 刘静

【导师】 苏秀霞;

【作者基本信息】 陕西科技大学 , 化学, 2018, 硕士

【摘要】 骨胶是一种天然高分子胶粘剂,具有原料易得、价格低廉和粘结强度高等优点,广泛应用于造纸、印刷、包装和木材等行业。然而骨胶的胶液具有一定程度的不良气味,长期使用会对使用者的身体健康造成危害,同时不利于环保。骨胶本身具有较深的颜色,影响了其感官特性和商品的价值,也限制了其在浅色木材及纸张领域的应用。为了克服这些缺点,本研究主要通过添加β-CD作为除臭剂对其进行除臭,通过添加过硫酸钠和酸化凹凸棒土作为脱色剂对其进行脱色,主要研究内容与结果如下:本文选择β-CD为除臭剂,在m(水):m(干骨胶)为1.3∶1的条件下,以骨胶的气味、粘度和凝固点为指标,通过单因素实验法研究了β-CD用量、反应时间、反应温度及搅拌速率4个因素对指标的影响,探索骨胶除臭的工艺条件。结果表明骨胶除臭的工艺条件:β-CD用量为骨胶用量的5.7%,反应时间为90 min,反应温度为45℃,搅拌速率为200 r/min。除臭后得到一种无味、粘接强度较高和凝固点较低的骨胶胶粘剂。FT-IR和XRD分析说明β-CD与骨胶之间发生了物理吸附作用,同时具有良好的除臭稳定性。在单因素实验的基础上,以骨胶为原料,以β-CD用量、反应时间、反应温度及搅拌速率为自变量,骨胶的气味和粘度为响应值,根据Box-Benhnken试验设计原理,采用四因素三水平的分析法模拟得到二次多项式回归方程的预测模型,优化骨胶的除臭工艺。结果显示骨胶除臭的较优最佳工艺条件为:β-CD用量为骨胶用量的6.3%,反应温度45.7℃,反应时间为90 min,搅拌速率300 r/min。优化后的骨胶气味良好,粘度为2.9 Pa·s。力学性能测试表明β-CD的加入对骨胶胶膜的拉伸剪切强度影响不明显。同时耐水性测试和TGA测试说明除臭剂的加入对骨胶的耐水性和热稳定性的影响也较小。以骨胶为原料,氧化法与物理吸附法相结合,在m(水)m(干骨胶)为1.3∶1时,以骨胶的色泽为指标,研究了过硫酸钠用量、酸化凹凸棒土用量、反应温度和反应时间对骨胶色泽的影响,探索骨胶脱色的工艺条件。结果表明骨胶脱色的工艺条件为:过硫酸钠用量分数为9.3%,酸化凹凸棒土用量分数为8.0%,反应温度为50℃,反应时间为60 min,该工艺条件下骨胶的脱色率为71.13%,稳定性良好,同时骨胶的性能未发生改变。紫外光谱图显示双键发生断裂,双键的数量减少,从而发色团受到一定程度的破坏,使脱色后的骨胶具有良好的色泽。本文选择过硫酸钠和酸化凹凸棒土作为骨胶的脱色剂。通过响应面法(RSM)研究在m(水)∶m(干骨胶)为1.3∶1时,脱色过程中过硫酸钠用量、酸化凹凸棒土用量、反应温度和反应时间对骨胶色泽的影响。结果表明骨胶脱色的较优工艺条件为:过硫酸钠和酸化凹凸棒土用量,反应温度和反应时间分别为9.3%,9.3%,45℃和60 min。在最佳条件下,脱色率达到71.15%。TGA分析可以表明脱色剂的加入对骨胶的热稳定性并无显著影响。FT-IR和XRD分析说明脱色剂与骨胶之间发生了相互作用。以除臭和脱色的较优工艺条件,对骨胶进行综合处理,综合处理后骨胶获得了良好的气味、感官色泽和脱色率,同时并不影响骨胶的基本性能。XRD和FT-IR分析表明骨胶与除臭剂和脱色剂之间存在物理作用和化学作用。

【Abstract】 Bone glue is a kind of natural polymer adhesive,which has the advantages of non-toxicity,easy availability of raw materials,low cost and high bond strength.It is widely used in papermaking,printing,packaging,wood industries,et al.However,bone glue has a certain degree of bad odor and long time use will harm the health of users,while not conducive to environmental protection.Bone glue adhesive has a deep color,which affects its sensory properties and the value of its mommodity,and also limits its application in the light-colored wood and paper fields.In order to overcome these shortcomings,this study mainly deodorizes by adding β-cyclodextrin as a deodorant and sodium persulfate and acidified attapulgite as decolorizer.The main contents and results are as follows:This study mainly deodorized β-cyclodextrin as a deodorant,It was a bone glue adhesive which had low freezing point,high viscosity and good smell by study on deodorization conditions of industrial bone glue with β-cyclodextrin.The effects of β-cyclodextrin content,reaction time,reaction temperature and stirring rate on the odor,viscosity and freezing point were studied by single factor experiment,at m(water)to m(dry bone glue)was 1.3:1.The conditions shown as follows:β-cyclodextrin content was 6.3% of bone glue content,reaction time was 90 min,reaction temperature was 45 ℃,stirring rate was 200 r/min.After deodorization,we got a tasteless,higher bonding strength and lower freezing point bone glue adhesive.The results of FT-IR and XRD showed that physical adsorption between β-cyclodextrin and bone glue.At the same time,bone glue had good deodorization stability.The objective of this study was to optimize deodorization conditions for industrial bone glue with β-cyclodextrin.On the basis of single-factor test,at m(water)to m(dry bone glue)was 1.3:1,theresponse surface methodology was utilized to investigate the effects ofβ-cyclodextrin content,reaction time,reaction temperature and stirring rate.The odor and viscosity of the bone glue were chosen as response value.The regression model had a high significance level,and the established regression equations fit with experimental results well and showed good prediction for the odor and viscosity value of bone glue.The influences of each factor on the smell and viscosity were obtained.The results showed that the optimal conditions for deodorization ofβ-cyclodextrin content was 6.3% of bone glue content,reaction temperature of 45.7 ℃,reaction time of 90 min,stirring rate of 300r/min.The bone glue after optimized deodorization process had a good smell and a viscosity of 2.9 Pa.s.The test of mechanical properties showed that the addition of β-cyclodextrin had no obvious effect on the tensile shear strength of the bone glue adhesive.At the same time,the water resistance test and the TGA test showed that the addition of deodorant had less effect on the water resistance and the stability of the bone glue.Using bone glue as raw material,the combination of oxidation method and physical adsorption method,with sodium persulfate and acidified attapulgite as decolorizer,got light-colored bone glue adhesive.The effects of sodium persulfate content,acidified attapulgite content,reaction temperature and reaction time on the color of bone glue were studied,when the ratio of m(water)to m(dry bone glue)was1.3:1.On the basis of single factor experiment,the technological conditions were as follows: the content of sodium persulfate was 9.3%,the content of acidified attapulgite was 8.0%,the reaction temperature was 50 ℃,the reaction time was 60 min,the decolorization rate was71.13%,the stability was good,while the performance of bone glue did not change.The Ultravoilet spectrum showed that the double bond breaks,the number of double bonds decreases and the chromophore were damaged to a certain extent,so that the decolorized bone glue had a good color.In this paper,sodium persulfate and acidified attapulgite were selected as decolorizer for bone glue.The factors,including sodiumpersulfate content,acidified attapulgite content,reaction temperature and reaction time,were studied through response surface methodology(RSM)in the decolorization process.Experiments were carried out by Box-Behnken design(BBD).At m(water)to m(dry bone glue)was 1.3:1,the maximum decolorization rate was obtained as sodium persulfate content,acidified attapulgite content,reaction temperature and reaction time were 9.3%,9.3%,45 ℃ and 60 min,respectively.Under optimization condition,decolorization rate was achieved to be 71.15%.The color of bone glue after decolorization was stable and not easy to back color.Decolorization process did not change the basic properties of bone glue.TGA test showed that the addition of decolorizer had little effect on the thermal stability of bone glue.FT-IR and XRD analysis demonstrated that there was an interaction between the decolorizer and the bone glue.Comprehensive treatment of bone glue with optimum process conditions for deodorization and decolorization,comprehensive treatment let the bone glue obtain a good odor,sensory color and decolorization rate,while not affecting the basic properties of bone glue.XRD and FT-IR analysis showed that there was physical and chemical interaction between bone glue and deodorant and decolorizer.

【关键词】 骨胶除臭脱色响应面
【Key words】 bone gluedeodorizationdecolorizationresponse surface
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