葡聚糖对碳酸饱充和蔗糖成核过程影响机理的研究
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摘要
制糖行业是涉及国计民生的重要行业。污染排放已成为影响我国甘蔗制糖业生存与可持续发展的瓶颈问题。制糖过程产生的葡聚糖，引起加工困难的同时也影响食糖产品的产量和质量，如何消除或减少葡聚糖对制糖工业的影响，是行业非常关注的问题。
本论文以制糖工业中葡聚糖为主线。研究了葡聚糖分子量对模拟烟道气饱充糖液生成的碳酸钙的物化性质及蔗糖成核过程的影响机理。利用超声场辅助饱充蔗糖钙生成碳酸钙过程工艺和分段式饱充技术工艺，可解决采用锅炉烟道气中CO_2存在其纯度低、浓度波动大和吸收率低等共性关键问题，为实现制糖产业的绿色加工和节能减排提供理论和技术依据。
用乙醇沉淀法提取砂糖中葡聚糖，体积排阻色谱法测定的重均分子量范围为：1.04×10~4-2.24×10~6Da。葡聚糖分子量对模拟烟道气饱充石灰乳生成碳酸钙的影响为：碳酸钙颗粒的弦长范围和不加权中位数弦长，都随葡聚糖分子量的增大而增加；葡聚糖的存在，可使生成的方解石型的碳酸钙的晶格发生畸变；葡聚糖与碳酸钙之间存在物理吸附作用。
葡聚糖分子量对模拟烟道气饱充蔗糖钙生成的碳酸钙的影响：随着葡聚糖分子量的增加，碳酸钙颗粒形状，从分叉钟乳石状变为不规则状；碳酸钙颗粒的弦长范围和不加权中位数弦长，都随着葡聚糖分子量的增大而减小；葡聚糖不引起方解石型碳酸钙晶格的变化；糖液中存在分子量T40的葡聚糖时，生成的碳酸钙有利于糖液清净。
超声辅助葡聚糖对烟道气饱充蔗糖钙的影响：随着超声波功率的增加，不规则形状的碳酸钙颗粒数目增加，而颗粒的弦长分布范围和不加权中位数的弦长减小；超声场和葡聚糖的存在，方解石型的碳酸钙的晶格没有发生畸变；在2W/cm~2的超声功率作用下，饱充生成的碳酸钙有利于糖液清净，并可缩短饱充时间。
葡聚糖对碳酸氢钙制备碳酸钙的影响。将Ca(HCO_3)_2加热分解制备碳酸钙：碳酸钙颗粒中有方解石和文石相，其中文石相的质量百分比为67.0±0.5%；碳酸钙颗粒的形状主要是立方体状、柱状和纺锤形等；存在的葡聚糖和蔗糖，碳酸钙不发生晶型变化。通过Ca(HCO_3)_2与Ca(OH)_2反应制备碳酸钙：生成方解石型碳酸钙，形状主要有球状和立方体状等；葡聚糖和蔗糖的存在，能使碳酸钙的晶格发生畸变。用Ca(HCO_3)_2与Ca(OH)_2反应制备的碳酸钙，对糖液澄清的效果较优。
蔗糖在水溶液中的超溶解度，随着葡聚糖分子量的增加而增加。糖液中存在高分子量的葡聚糖时，能抑制蔗糖自发成核，减缓和减少生成蔗糖晶体的颗粒数。随着添加葡聚糖分子量的增加，可显著抑制蔗糖晶体（110）和（110）面的生长。
通过中心组合优化结果分析，表明糖液锤度一次项、添加酶量一次项和糖浆温度一次项对糖浆中葡聚糖酶解率的影响，达极显著水平。通过控制末效蒸发罐的糖浆锤度和添加葡聚糖酶的量，可降低糖浆中葡聚糖的含量。
The Sugar industry was acknowledged crucial importance to the national economy andpeople's livelihood. Emissions and wastes are becoming the bottleneck problem to the sugarindustry with survival and sustainable development. In addition, recent research detailed thepresence of dextran in the sugar factories leads to processing problems like increased ofsucrose loss to molasses, that how to remove or reduce the dextran was urgently concerned inthe sugar industry.
Dextran in the sugar industry was the main research object in this thesis. Effect of themolecular weights of dextran on physicochemical properties of calcium carbonate obtained bycarbonation in the juice and the nucleation process of sucrose in pure sucrose solutions wereinvestigated. With the method of ultrasound to assist carbonation in the juice and sectionalcarbonation to figure out the low concentration, fluctuation and low absorption rate of CO_2inthe boiler flue gas were proposed. Which make foundation for practical application on greenprocessing and energy savings of sugar industry in the future.
The ethanol sedimentary method was used to extract dextran from the sucrose. Theweight-average molecular weight of the dextran was between1.04×10~4and2.24×10~6Da bysize-exclusion chromatography, using a refractive index detector. Then, the effect ofmolecular weights of dextran on the calcium carbonate obtained by carbonation in the milk oflime was investigated. Chord length range and unweighted median chord length of thecalcium carbonate increased with the increase of the molecular weight of dextran. The dextranin the milk of lime can raised lattice distortion in the calcium carbonate. And we found thephysical adsorption was exist between the dextran and the calcium carbonate.
The effect of molecular weights of dextran on the calcium carbonate obtained bycarbonation in the calcium saccharate solution was investigated. The morphology of thecalcite was changed from bifurcation stalactite into irregular shape with the increasing ofdextran molecular weight. In addition, both of chord length range and unweighted medianchord length of the calcite decreased with the increase of the dextran molecular weight. Thedextran in the calcium saccharate solution could not cause lattice distortion in the calciumcarbonate. The calcium carbonate obtained by carbonation with presence of dextran T40waspositively effect to clarify juice.
And also we found the effect of ultrasonic on the calcium carbonate obtained bycarbonation in the calcium saccharate solution with dextran, the number of the calcite with the irregular shape was increased by the increasing of ultrasonic power. Furthermore, both ofchord length range and not weighted median chord length of the calcite decreased with theincrease of ultrasonic power. Both ultrasonic and dextran could not cause lattice distortion inthe calcium carbonate. The calcium carbonate obtained by carbonation with presence ofdextran T40and ultrasonic power2w/cm~2was positively effect to clarify juice.
The effect of dextran on the calcium carbonate obtained by Ca(HCO_3)_2also wasinvestigated. The calcium carbonate which could include calcite and aragonite was producedusing the decomposition of Ca(HCO_3)_2by heat treatment and the percentage of aragonite was67.0±0.5%. The shape of the calcium carbonate was cubic, columnar and fusiform. Thedextran and sucrose in the Ca(HCO_3)_2solution could not cause lattice distortion in thecalcium carbonate. However, the calcium carbonate produced by reacting betweenCa(HCO_3)_2and Ca(OH)_2was calcite. The shape of the calcite was globular, cubic andneedlelike. Both sucrose and dextran could cause lattice distortion in the calcium carbonate.the existence of dextran and sugar could can cause lattice distortion in the calcium carbonate.Clarified juice was better with the calcium carbonate obtained by reacting betweenCa(HCO_3)_2and Ca(OH)_2.
The supersolubility of sucrose in the water solution increased with the increase of thehigher molecular weights of dextran. The spontaneous nucleation of sucrose, mitigation andreducing the counts of sucrose crystal in the syrup could be obviously inhibited by the highermolecular weight of dextran in sugar liquid. The development of the crystals faces of sucrose(110and110) were inhibited by the increasing of molecular weights of dextan.
With the center combination design optimization of the test results, the concentration ofsolid matter in the solution, the dosage of enzyme and the temperature of the soltuion affectedthe dextran in the syrup digestion rate extremely. By controlling the concentration of solidmatter at the end of the effect evaporation tank and the dosage of the dextranase can reducethe content of dextran in the syrup.
本论文以制糖工业中葡聚糖为主线。研究了葡聚糖分子量对模拟烟道气饱充糖液生成的碳酸钙的物化性质及蔗糖成核过程的影响机理。利用超声场辅助饱充蔗糖钙生成碳酸钙过程工艺和分段式饱充技术工艺，可解决采用锅炉烟道气中CO_2存在其纯度低、浓度波动大和吸收率低等共性关键问题，为实现制糖产业的绿色加工和节能减排提供理论和技术依据。
用乙醇沉淀法提取砂糖中葡聚糖，体积排阻色谱法测定的重均分子量范围为：1.04×10~4-2.24×10~6Da。葡聚糖分子量对模拟烟道气饱充石灰乳生成碳酸钙的影响为：碳酸钙颗粒的弦长范围和不加权中位数弦长，都随葡聚糖分子量的增大而增加；葡聚糖的存在，可使生成的方解石型的碳酸钙的晶格发生畸变；葡聚糖与碳酸钙之间存在物理吸附作用。
葡聚糖分子量对模拟烟道气饱充蔗糖钙生成的碳酸钙的影响：随着葡聚糖分子量的增加，碳酸钙颗粒形状，从分叉钟乳石状变为不规则状；碳酸钙颗粒的弦长范围和不加权中位数弦长，都随着葡聚糖分子量的增大而减小；葡聚糖不引起方解石型碳酸钙晶格的变化；糖液中存在分子量T40的葡聚糖时，生成的碳酸钙有利于糖液清净。
超声辅助葡聚糖对烟道气饱充蔗糖钙的影响：随着超声波功率的增加，不规则形状的碳酸钙颗粒数目增加，而颗粒的弦长分布范围和不加权中位数的弦长减小；超声场和葡聚糖的存在，方解石型的碳酸钙的晶格没有发生畸变；在2W/cm~2的超声功率作用下，饱充生成的碳酸钙有利于糖液清净，并可缩短饱充时间。
葡聚糖对碳酸氢钙制备碳酸钙的影响。将Ca(HCO_3)_2加热分解制备碳酸钙：碳酸钙颗粒中有方解石和文石相，其中文石相的质量百分比为67.0±0.5%；碳酸钙颗粒的形状主要是立方体状、柱状和纺锤形等；存在的葡聚糖和蔗糖，碳酸钙不发生晶型变化。通过Ca(HCO_3)_2与Ca(OH)_2反应制备碳酸钙：生成方解石型碳酸钙，形状主要有球状和立方体状等；葡聚糖和蔗糖的存在，能使碳酸钙的晶格发生畸变。用Ca(HCO_3)_2与Ca(OH)_2反应制备的碳酸钙，对糖液澄清的效果较优。
蔗糖在水溶液中的超溶解度，随着葡聚糖分子量的增加而增加。糖液中存在高分子量的葡聚糖时，能抑制蔗糖自发成核，减缓和减少生成蔗糖晶体的颗粒数。随着添加葡聚糖分子量的增加，可显著抑制蔗糖晶体（110）和（110）面的生长。
通过中心组合优化结果分析，表明糖液锤度一次项、添加酶量一次项和糖浆温度一次项对糖浆中葡聚糖酶解率的影响，达极显著水平。通过控制末效蒸发罐的糖浆锤度和添加葡聚糖酶的量，可降低糖浆中葡聚糖的含量。
The Sugar industry was acknowledged crucial importance to the national economy andpeople's livelihood. Emissions and wastes are becoming the bottleneck problem to the sugarindustry with survival and sustainable development. In addition, recent research detailed thepresence of dextran in the sugar factories leads to processing problems like increased ofsucrose loss to molasses, that how to remove or reduce the dextran was urgently concerned inthe sugar industry.
Dextran in the sugar industry was the main research object in this thesis. Effect of themolecular weights of dextran on physicochemical properties of calcium carbonate obtained bycarbonation in the juice and the nucleation process of sucrose in pure sucrose solutions wereinvestigated. With the method of ultrasound to assist carbonation in the juice and sectionalcarbonation to figure out the low concentration, fluctuation and low absorption rate of CO_2inthe boiler flue gas were proposed. Which make foundation for practical application on greenprocessing and energy savings of sugar industry in the future.
The ethanol sedimentary method was used to extract dextran from the sucrose. Theweight-average molecular weight of the dextran was between1.04×10~4and2.24×10~6Da bysize-exclusion chromatography, using a refractive index detector. Then, the effect ofmolecular weights of dextran on the calcium carbonate obtained by carbonation in the milk oflime was investigated. Chord length range and unweighted median chord length of thecalcium carbonate increased with the increase of the molecular weight of dextran. The dextranin the milk of lime can raised lattice distortion in the calcium carbonate. And we found thephysical adsorption was exist between the dextran and the calcium carbonate.
The effect of molecular weights of dextran on the calcium carbonate obtained bycarbonation in the calcium saccharate solution was investigated. The morphology of thecalcite was changed from bifurcation stalactite into irregular shape with the increasing ofdextran molecular weight. In addition, both of chord length range and unweighted medianchord length of the calcite decreased with the increase of the dextran molecular weight. Thedextran in the calcium saccharate solution could not cause lattice distortion in the calciumcarbonate. The calcium carbonate obtained by carbonation with presence of dextran T40waspositively effect to clarify juice.
And also we found the effect of ultrasonic on the calcium carbonate obtained bycarbonation in the calcium saccharate solution with dextran, the number of the calcite with the irregular shape was increased by the increasing of ultrasonic power. Furthermore, both ofchord length range and not weighted median chord length of the calcite decreased with theincrease of ultrasonic power. Both ultrasonic and dextran could not cause lattice distortion inthe calcium carbonate. The calcium carbonate obtained by carbonation with presence ofdextran T40and ultrasonic power2w/cm~2was positively effect to clarify juice.
The effect of dextran on the calcium carbonate obtained by Ca(HCO_3)_2also wasinvestigated. The calcium carbonate which could include calcite and aragonite was producedusing the decomposition of Ca(HCO_3)_2by heat treatment and the percentage of aragonite was67.0±0.5%. The shape of the calcium carbonate was cubic, columnar and fusiform. Thedextran and sucrose in the Ca(HCO_3)_2solution could not cause lattice distortion in thecalcium carbonate. However, the calcium carbonate produced by reacting betweenCa(HCO_3)_2and Ca(OH)_2was calcite. The shape of the calcite was globular, cubic andneedlelike. Both sucrose and dextran could cause lattice distortion in the calcium carbonate.the existence of dextran and sugar could can cause lattice distortion in the calcium carbonate.Clarified juice was better with the calcium carbonate obtained by reacting betweenCa(HCO_3)_2and Ca(OH)_2.
The supersolubility of sucrose in the water solution increased with the increase of thehigher molecular weights of dextran. The spontaneous nucleation of sucrose, mitigation andreducing the counts of sucrose crystal in the syrup could be obviously inhibited by the highermolecular weight of dextran in sugar liquid. The development of the crystals faces of sucrose(110and110) were inhibited by the increasing of molecular weights of dextan.
With the center combination design optimization of the test results, the concentration ofsolid matter in the solution, the dosage of enzyme and the temperature of the soltuion affectedthe dextran in the syrup digestion rate extremely. By controlling the concentration of solidmatter at the end of the effect evaporation tank and the dosage of the dextranase can reducethe content of dextran in the syrup.
引文
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