瓜尔胶衍生物的制备及在造纸法再造烟叶中的应用研究
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摘要
造纸法再造烟叶是利用烟梗、烟末、烟叶碎片、废次烟叶等烟草废料作基本原料通过造纸工艺生产的烟草薄片，具有变废为宝、节省烟叶原料、降低卷烟成本等特点。再造烟叶浆料中含有30%以上包含细小纤维、烟末和填料的细小组分，由于造纸法再造烟叶生产对助剂的特殊要求（无毒无害易生化降解、不影响烟草燃烧气味），目前，造纸法再造烟叶在抄造过程中基本不添加任何助剂，这导致了大量细小组分的流失。瓜尔胶及其衍生物由于其独特的理化特征，在提高造纸法再造烟叶浆料细小组分的留着率和滤水性能，以及改善薄片的物理性能方面具有广阔的应用价值和应用前景。
本文系统研究了阳离子瓜尔胶（CGG）、阳离子瓜尔胶丙烯酰胺接枝共聚物（CGG-g-PAM）在离子液体中的制备、表征及助留助滤性能，分析了造纸法再造烟叶浆料的特性，将CGG、CGG-g-PAM、商品阳离子瓜尔胶和阳离子羟丙基瓜尔胶对烟草浆的助留助滤效果进行了比较，进一步将一元与二元微粒助留助滤体系进行了比较，研发适合于造纸法再造烟叶湿部抄造的一剂多功能瓜尔胶衍生物助留助滤增强剂。
采用微波辐射法合成了氯化1-烯丙基-3-甲基咪唑（[AMIM]Cl）和氯化1-丁基-3-甲基咪唑（[BMIM]Cl）两种离子液体。比较了连续辐射法和间歇辐射法对合成反应时间、产物得率及原料转化率的影响。结果表明微波间歇辐射法合成咪唑类离子液体不仅反应时间更短，咪唑的转化率和得率更加接近，反应效率更高，而且能够减轻反应过程中放热对产物颜色加深的负面影响，得到纯度更高的产品。红外光谱和13C-NMR表征证实了合成反应的发生。
在离子液体中制备了阳离子瓜尔胶，考察了阳离子醚化剂用量、反应温度、碱化时间和反应时间对产物阳离子取代度（氮含量）和粘度的影响，确定了最佳反应条件。通过偏光显微镜的观察发现瓜尔胶在离子液体中反应时处于溶胀状态，是非均相反应。用FT-IR，13C-NMR表征CGG结构，证实了在瓜尔胶分子单元的C6位置发生了醚化反应，用SEM观察CGG的表面形态，TG分析表明CGG的热稳定性能稍好于瓜尔胶原粉。比较了几种不同的阳离子瓜尔胶的氮含量、粘度、流变性能和分子量及分子量分布，结果表明：以CTA为阳离子单体，在离子液体中合成的阳离子瓜尔胶具有较高的阳离子取代度（0.14）和粘度（904mPa·s），抗剪切性能较好，分子量分布较集中。
创新性研究了过硫酸铵引发阳离子瓜尔胶和丙烯酰胺在离子液体中的接枝共聚反应，研究了单体与阳离子瓜尔胶的质量比、引发剂与阳离子瓜尔胶的质量比、反应温度和反应时间对接枝聚合参数的影响，确定了最佳合成条件。FT-IR，13C-NMR表征了CGG-g-PAM的结构，用SEM观察CGG-g-PAM的表面形态。热重分析表明CGG-g-PAM有两个失重峰，耐热性能优于瓜尔胶原粉。CGG-g-PAM水溶液表现出假塑性流体行为，但其粘度下降速率较慢，在相同剪切速率下，粘度较CGG和CPAM大。通过聚合反应动力学研究发现，温度对聚合反应速率有较大影响，在离子液体中反应的表观活化能为(ΔEappa)11.6KJ/mol，聚合反应速率随单体与CGG摩尔比的增加而下降，而聚合物的分子量增加，分子量分布变窄。
通过对造纸法再造烟叶浆料的电荷特性研究发现，Zeta电位随着离子浓度、浆浓和打浆度的提高而增加，随pH的升高而降低；阳离子需求量随着pH、浆浓和打浆度的提高而增加，随离子浓度的升高而降低。阳离子瓜尔胶能够显著降低再造烟叶浆料体系的阳离子需求量并大幅提高Zeta电位。
对烟草浆的纤维性能进行了分析，烟草浆原料经过机械磨浆后含有较多的纤维束、纤维团簇和烟末；显微镜图片显示烟草浆料中存在较多剥落的细小纤维和烟末。比较了在离子液体中合成的四种不同阳离子取代度的CGG对烟草浆细小组分的助留效果，结果表明阳离子取代度为0.14，粘度为904mPa·s的CGG-2对烟草浆的助留效果最好，CGG-2对细小组分单程留着率的效果优于商品CGG和溶剂法合成的CGG，而后两者的效果相当。
阳离子瓜尔胶的DS对接枝共聚物助留性能的影响较小；CHPG对提高烟草浆的FPR有明显效果，CHPG的加入量从0增加到0.08%，FPR从40.1%提高到80.5%，提高了101%。对比了三种瓜尔胶衍生物对造纸法再造烟叶浆的助留助滤效果，结果表明CGG-2的效果稍好于CGG2-g-PAM和CHPG，以离子液体为反应介质合成的CGG-2在造纸法再造烟叶浆中具有最好的应用效果，但如果出于工业化的考虑，阳离子取代度为0.08的阳离子羟丙基瓜尔胶可以作为其替代品。用十八烷基三甲基溴化铵(STAB)对膨润土进行了有机改性，研究了CGG和膨润土组成的二元微粒助留体系对烟草浆的助留助滤效果，考察了剪切速率、pH值和电解质浓度对CGG/膨润土二元微粒助留体系的影响，结果表明膨润土与CGG组成的微粒助留助滤体系具有较好的抗剪切能力、较广的pH使用范围和较好的抗电解质性能。
Paper-making process reconstituted tobacco is use of tobacco peduncle, dust, brokentobacco pieces and tobacco waste as basic raw materials through paper-making processproduced tobacco sheet. Paper-making process reconstituted tobacco have the characteristicsof recycling waste materials, saving tobacco materials, reducing cigarette cost, etc. Thereconstituted tobacco pulp contains more than30%tiny fibers, tobacco dust and filler. As thereconstituted tobacco process special requires of additives(non-toxic and harmless, easybiochemical degradation, do not affect the tobacco smell of burning), currently, thereconstituted tobacco pulp does not add any additive in the manufacturing process. This leadsto large number of fines loss. Guar gum and its derivatives have broad application value andapplication prospect in increasing the retention and drainage performance of reconstitutedtobacco pulp fines, also it can improve the physical properties of the tobacco sheet because ofits unique physical and chemical characteristics.
This thesis studied the preparation and characterization of cationic guar gum(CGG),cationic guar gum acrylamide graft copolymer(CGG-g-PAM) in ionic liquid. Their retentionand drainage aid performance on paper-making process reconstituted tobacco pulp were alsoresearched. First, analysis the properties of paper-making process reconstituted tobacco pulp;and then comparison the effects of retention and drainage aid of CGG, CGG-g-PAM,commodity cationic guar gum and cationic hydroxypropyl guar gum(CHPG) application onreconstituted tobacco pulp; at last, monobasic and binary of microparticle retention anddrainage aid systems were compared. Research and development multifunctional guar gumderivatives as retention and drainage aid and reinforcing agent suitable for wet end process ofpaper-making process reconstituted tobacco.
Synthesized chlorinated1-allyl-3-methylimidazole([AMIM]Cl) and chlorinated1-butyl-3-methylimidazole([BMIM]Cl) two kinds of ionic liquids using microwave radiationmethod. Compared continuous microwave radiation method and intermittent microwaveradiation method on the influence of synthesis reaction time, product yield and raw materialconversion. The results showed that intermittent microwave radiation method could shortenthe reaction time in synthesis imidazoles ionic liquid. The conversion of imidazole was close to the yield and the reaction efficiency were higher than continuous microwave radiationmethod. It could reduce the negative effect on product color darken because of the reactionexothermic, so we could get high purity product. The infrared spectrum and the13C-NMRrepresentation confirmed the synthetic reaction.
We prepared cationic guar gum in ionic liquids. Studied the effects of the cationicetherification agent dosage, reaction temperature, alkalization time and reaction time ondegree of substitution(nitrogen content) and the viscosity of CGG, then the optimum reactionconditions were determined. Through the polarizing microscope we found that guar gum wasin a swelling state when reacting in ionic liquids, obviously it was a homogeneous reaction.FT-IR and13C-NMR characterized CGG’s structure. It confirmed the etherification reactionhappened on C6position of guar gum molecular unit. SEM analysed the CGG surface formand TG analysis showed that the CGG performance slightly better than guar gum on thermalstability. Compared different kinds of cationic guar gum of nitrogen content, viscosity,rheological properties, molecular weight and molecular weight distribution, the resultsshowed that the cationic guar gum had higher cationic degree of substitution(0.14) andviscosity(904mpa·s) as CTA cationic monomer. The shear performance was better and themolecular weight distribution was more concentrated.
Innovative studied ammonium persulfate initiated cationic guar gum and acrylamidegraft copolymerization in ionic liquid. Researched the effect of monomers and cationic guargum mass ratio, initiator and cationic guar gum mass ratio, reaction temperature and reactiontime on graft polymerization parameters, to determine the optimum synthesis conditions.FT-IR and13C-NMR characterized the structure of CGG-g-PAM. Surface morphology wasobserved by SEM. Thermal analysis showed that CGG-g-PAM had two peaks, so theheat-resistant property was better than guar gum. CGG-g-PAM aqueous solution showedpseudoplastic fluid behavior, but the viscosity decreased slower, and at the same shear rate,viscosity was higher than that of CGG and CPAM. Polymerization kinetics showed thattemperature had great influence on polymerization rate. The apparent activationenergy(ΔEapp
a) was11.6KJ/mol in ionic liquids. The reaction rate of polymerizationdecreased with monomer and CGG mole ratio increasing. The polymer molecular weightincreased and the molecular weight distribution became narrow.
The charge characteristics of paper-making process reconstituted tobacco pulp showedthat Zeta potential raised with the ion concentration, pulp consistency and beating degreeincreasing, while reduced with pH increasing. Cationic demand raised with pH, pulpconsistency and beating degree increasing, while reduced with ion concentration raising.Cationic guar gum could significantly reduce cationic demand of reconstituted tobacco pulpsystem and sharp increase Zeta potential.
Analysis on fiber performance of tobacco pulp showed that tobacco pulp raw materialscontained many fiber, fiber clusters and tobacco powder after mechanical grind. Microscopyimage showed that tobacco slurry had many peeling fine and tobacco powder. Comparison offour different kinds of cation substitution degree of CGG synthesed in ionic liquid applicatedon tobacco pulp fines. The effect of retention aid showed that the CGG-2of cationsubstitution degree0.14, viscosity904mPa·s had best application effect on paper-makingprocess reconstituted tobacco pulp. The effect of fines first-pass retention which CGG-2applicated on paper-making process reconstituted tobacco pulp was better than merchandiseCGG and CGG synthesed in solvent, while the latter two had effect of considerable.
The DS of cationic guar gum had small effect on retention aid properties of graftcopolymer. CHPG had obvious effect on improving FPR of tobacco pulp. With the CHPGcontent increasing from0to0.08%, FPR increased from40.1%to80.5%, improving101%.Comparison of three kinds of guar gum derivatives retention and drainage aid effects onpaper-making reconstituted tobacco pulp, the results showed that CGG-2had better effectthan CGG2-g-PAM and CHPG. CGG-2which synthesed in ionic liquid application onpaper-making reconstituted tobacco pulp had best effect, but if on the industrializationconsideration, cationic hydroxypropyl guar gum which cationic substituted degree was0.08could be used as its replacement.
Organic modified bentonite with STAB, SEM, FT-IR, TG and XRD shown that theorganic modifier had been got into the layer of bentonite. We could decide the betterconditions of organic modifying by orthogonal experiment. Binary of microparticle retentionand drainage aid system which contained CGG and bentonite application on paper-makingreconstituted tobacco pulp was researched. We studied the effect of shear rate, pH and theconsistency of electrolyte on binary of microparticle retention and drainage aid system. The results indicated the binary of microparticle retention and drainage aid system had betterresisting shear capacity, wide-ranging of pH application scope and better resisting electrolyteresistance.
本文系统研究了阳离子瓜尔胶（CGG）、阳离子瓜尔胶丙烯酰胺接枝共聚物（CGG-g-PAM）在离子液体中的制备、表征及助留助滤性能，分析了造纸法再造烟叶浆料的特性，将CGG、CGG-g-PAM、商品阳离子瓜尔胶和阳离子羟丙基瓜尔胶对烟草浆的助留助滤效果进行了比较，进一步将一元与二元微粒助留助滤体系进行了比较，研发适合于造纸法再造烟叶湿部抄造的一剂多功能瓜尔胶衍生物助留助滤增强剂。
采用微波辐射法合成了氯化1-烯丙基-3-甲基咪唑（[AMIM]Cl）和氯化1-丁基-3-甲基咪唑（[BMIM]Cl）两种离子液体。比较了连续辐射法和间歇辐射法对合成反应时间、产物得率及原料转化率的影响。结果表明微波间歇辐射法合成咪唑类离子液体不仅反应时间更短，咪唑的转化率和得率更加接近，反应效率更高，而且能够减轻反应过程中放热对产物颜色加深的负面影响，得到纯度更高的产品。红外光谱和13C-NMR表征证实了合成反应的发生。
在离子液体中制备了阳离子瓜尔胶，考察了阳离子醚化剂用量、反应温度、碱化时间和反应时间对产物阳离子取代度（氮含量）和粘度的影响，确定了最佳反应条件。通过偏光显微镜的观察发现瓜尔胶在离子液体中反应时处于溶胀状态，是非均相反应。用FT-IR，13C-NMR表征CGG结构，证实了在瓜尔胶分子单元的C6位置发生了醚化反应，用SEM观察CGG的表面形态，TG分析表明CGG的热稳定性能稍好于瓜尔胶原粉。比较了几种不同的阳离子瓜尔胶的氮含量、粘度、流变性能和分子量及分子量分布，结果表明：以CTA为阳离子单体，在离子液体中合成的阳离子瓜尔胶具有较高的阳离子取代度（0.14）和粘度（904mPa·s），抗剪切性能较好，分子量分布较集中。
创新性研究了过硫酸铵引发阳离子瓜尔胶和丙烯酰胺在离子液体中的接枝共聚反应，研究了单体与阳离子瓜尔胶的质量比、引发剂与阳离子瓜尔胶的质量比、反应温度和反应时间对接枝聚合参数的影响，确定了最佳合成条件。FT-IR，13C-NMR表征了CGG-g-PAM的结构，用SEM观察CGG-g-PAM的表面形态。热重分析表明CGG-g-PAM有两个失重峰，耐热性能优于瓜尔胶原粉。CGG-g-PAM水溶液表现出假塑性流体行为，但其粘度下降速率较慢，在相同剪切速率下，粘度较CGG和CPAM大。通过聚合反应动力学研究发现，温度对聚合反应速率有较大影响，在离子液体中反应的表观活化能为(ΔEappa)11.6KJ/mol，聚合反应速率随单体与CGG摩尔比的增加而下降，而聚合物的分子量增加，分子量分布变窄。
通过对造纸法再造烟叶浆料的电荷特性研究发现，Zeta电位随着离子浓度、浆浓和打浆度的提高而增加，随pH的升高而降低；阳离子需求量随着pH、浆浓和打浆度的提高而增加，随离子浓度的升高而降低。阳离子瓜尔胶能够显著降低再造烟叶浆料体系的阳离子需求量并大幅提高Zeta电位。
对烟草浆的纤维性能进行了分析，烟草浆原料经过机械磨浆后含有较多的纤维束、纤维团簇和烟末；显微镜图片显示烟草浆料中存在较多剥落的细小纤维和烟末。比较了在离子液体中合成的四种不同阳离子取代度的CGG对烟草浆细小组分的助留效果，结果表明阳离子取代度为0.14，粘度为904mPa·s的CGG-2对烟草浆的助留效果最好，CGG-2对细小组分单程留着率的效果优于商品CGG和溶剂法合成的CGG，而后两者的效果相当。
阳离子瓜尔胶的DS对接枝共聚物助留性能的影响较小；CHPG对提高烟草浆的FPR有明显效果，CHPG的加入量从0增加到0.08%，FPR从40.1%提高到80.5%，提高了101%。对比了三种瓜尔胶衍生物对造纸法再造烟叶浆的助留助滤效果，结果表明CGG-2的效果稍好于CGG2-g-PAM和CHPG，以离子液体为反应介质合成的CGG-2在造纸法再造烟叶浆中具有最好的应用效果，但如果出于工业化的考虑，阳离子取代度为0.08的阳离子羟丙基瓜尔胶可以作为其替代品。用十八烷基三甲基溴化铵(STAB)对膨润土进行了有机改性，研究了CGG和膨润土组成的二元微粒助留体系对烟草浆的助留助滤效果，考察了剪切速率、pH值和电解质浓度对CGG/膨润土二元微粒助留体系的影响，结果表明膨润土与CGG组成的微粒助留助滤体系具有较好的抗剪切能力、较广的pH使用范围和较好的抗电解质性能。
Paper-making process reconstituted tobacco is use of tobacco peduncle, dust, brokentobacco pieces and tobacco waste as basic raw materials through paper-making processproduced tobacco sheet. Paper-making process reconstituted tobacco have the characteristicsof recycling waste materials, saving tobacco materials, reducing cigarette cost, etc. Thereconstituted tobacco pulp contains more than30%tiny fibers, tobacco dust and filler. As thereconstituted tobacco process special requires of additives(non-toxic and harmless, easybiochemical degradation, do not affect the tobacco smell of burning), currently, thereconstituted tobacco pulp does not add any additive in the manufacturing process. This leadsto large number of fines loss. Guar gum and its derivatives have broad application value andapplication prospect in increasing the retention and drainage performance of reconstitutedtobacco pulp fines, also it can improve the physical properties of the tobacco sheet because ofits unique physical and chemical characteristics.
This thesis studied the preparation and characterization of cationic guar gum(CGG),cationic guar gum acrylamide graft copolymer(CGG-g-PAM) in ionic liquid. Their retentionand drainage aid performance on paper-making process reconstituted tobacco pulp were alsoresearched. First, analysis the properties of paper-making process reconstituted tobacco pulp;and then comparison the effects of retention and drainage aid of CGG, CGG-g-PAM,commodity cationic guar gum and cationic hydroxypropyl guar gum(CHPG) application onreconstituted tobacco pulp; at last, monobasic and binary of microparticle retention anddrainage aid systems were compared. Research and development multifunctional guar gumderivatives as retention and drainage aid and reinforcing agent suitable for wet end process ofpaper-making process reconstituted tobacco.
Synthesized chlorinated1-allyl-3-methylimidazole([AMIM]Cl) and chlorinated1-butyl-3-methylimidazole([BMIM]Cl) two kinds of ionic liquids using microwave radiationmethod. Compared continuous microwave radiation method and intermittent microwaveradiation method on the influence of synthesis reaction time, product yield and raw materialconversion. The results showed that intermittent microwave radiation method could shortenthe reaction time in synthesis imidazoles ionic liquid. The conversion of imidazole was close to the yield and the reaction efficiency were higher than continuous microwave radiationmethod. It could reduce the negative effect on product color darken because of the reactionexothermic, so we could get high purity product. The infrared spectrum and the13C-NMRrepresentation confirmed the synthetic reaction.
We prepared cationic guar gum in ionic liquids. Studied the effects of the cationicetherification agent dosage, reaction temperature, alkalization time and reaction time ondegree of substitution(nitrogen content) and the viscosity of CGG, then the optimum reactionconditions were determined. Through the polarizing microscope we found that guar gum wasin a swelling state when reacting in ionic liquids, obviously it was a homogeneous reaction.FT-IR and13C-NMR characterized CGG’s structure. It confirmed the etherification reactionhappened on C6position of guar gum molecular unit. SEM analysed the CGG surface formand TG analysis showed that the CGG performance slightly better than guar gum on thermalstability. Compared different kinds of cationic guar gum of nitrogen content, viscosity,rheological properties, molecular weight and molecular weight distribution, the resultsshowed that the cationic guar gum had higher cationic degree of substitution(0.14) andviscosity(904mpa·s) as CTA cationic monomer. The shear performance was better and themolecular weight distribution was more concentrated.
Innovative studied ammonium persulfate initiated cationic guar gum and acrylamidegraft copolymerization in ionic liquid. Researched the effect of monomers and cationic guargum mass ratio, initiator and cationic guar gum mass ratio, reaction temperature and reactiontime on graft polymerization parameters, to determine the optimum synthesis conditions.FT-IR and13C-NMR characterized the structure of CGG-g-PAM. Surface morphology wasobserved by SEM. Thermal analysis showed that CGG-g-PAM had two peaks, so theheat-resistant property was better than guar gum. CGG-g-PAM aqueous solution showedpseudoplastic fluid behavior, but the viscosity decreased slower, and at the same shear rate,viscosity was higher than that of CGG and CPAM. Polymerization kinetics showed thattemperature had great influence on polymerization rate. The apparent activationenergy(ΔEapp
a) was11.6KJ/mol in ionic liquids. The reaction rate of polymerizationdecreased with monomer and CGG mole ratio increasing. The polymer molecular weightincreased and the molecular weight distribution became narrow.
The charge characteristics of paper-making process reconstituted tobacco pulp showedthat Zeta potential raised with the ion concentration, pulp consistency and beating degreeincreasing, while reduced with pH increasing. Cationic demand raised with pH, pulpconsistency and beating degree increasing, while reduced with ion concentration raising.Cationic guar gum could significantly reduce cationic demand of reconstituted tobacco pulpsystem and sharp increase Zeta potential.
Analysis on fiber performance of tobacco pulp showed that tobacco pulp raw materialscontained many fiber, fiber clusters and tobacco powder after mechanical grind. Microscopyimage showed that tobacco slurry had many peeling fine and tobacco powder. Comparison offour different kinds of cation substitution degree of CGG synthesed in ionic liquid applicatedon tobacco pulp fines. The effect of retention aid showed that the CGG-2of cationsubstitution degree0.14, viscosity904mPa·s had best application effect on paper-makingprocess reconstituted tobacco pulp. The effect of fines first-pass retention which CGG-2applicated on paper-making process reconstituted tobacco pulp was better than merchandiseCGG and CGG synthesed in solvent, while the latter two had effect of considerable.
The DS of cationic guar gum had small effect on retention aid properties of graftcopolymer. CHPG had obvious effect on improving FPR of tobacco pulp. With the CHPGcontent increasing from0to0.08%, FPR increased from40.1%to80.5%, improving101%.Comparison of three kinds of guar gum derivatives retention and drainage aid effects onpaper-making reconstituted tobacco pulp, the results showed that CGG-2had better effectthan CGG2-g-PAM and CHPG. CGG-2which synthesed in ionic liquid application onpaper-making reconstituted tobacco pulp had best effect, but if on the industrializationconsideration, cationic hydroxypropyl guar gum which cationic substituted degree was0.08could be used as its replacement.
Organic modified bentonite with STAB, SEM, FT-IR, TG and XRD shown that theorganic modifier had been got into the layer of bentonite. We could decide the betterconditions of organic modifying by orthogonal experiment. Binary of microparticle retentionand drainage aid system which contained CGG and bentonite application on paper-makingreconstituted tobacco pulp was researched. We studied the effect of shear rate, pH and theconsistency of electrolyte on binary of microparticle retention and drainage aid system. The results indicated the binary of microparticle retention and drainage aid system had betterresisting shear capacity, wide-ranging of pH application scope and better resisting electrolyteresistance.
引文
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