廉价的高半纤维素含量的浆粕纺制Lyocell纤维的研究
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摘要
本论文简要介绍了Lyocell纤维的发展近况，针对目前Lyocell纤维发展缓慢的主要原因，生产成本高，价格贵这一发展瓶颈提出了一种解决方法：即采用廉价的浆粕原料来纺制Lyocell纤维，从而适当地降低Lvocell工艺的生产成本。探讨使用这种低成本的浆粕原料来纺制Lyocell纤维的可行性。
Lyocell纤维工艺一直沿袭传统粘胶纤维工艺，采用高alpha-纤维素含量的浆粕作为原料。高alpha-纤维素含量是为了保证得到高的粘胶纤维得率，但是高alpha-纤维素含量的浆粕，生产成本高。
为此，本论文选择了一种低成本的浆粕原料(高半纤维素浆粕)，这种浆粕，alpha-纤维素含量较低，半纤维素含量高达20％左右。在浆粕生产中，高半纤维素浆粕，一方面能够简化浆粕生产工艺，另一方面浆粕的得率高，因此能够降低浆粕生产成本约1／2。
论文中，首先探讨了高半纤维素浆粕的溶解性、浆液的可纺性和稳定性、以及Lvocell纤维的得率。研究结果表明：高半纤维素浆粕比高alpha-纤维素浆粕更易溶解，所需溶解条件温和、溶解范围较宽、溶解效果良好，更有利于实验操作的控制；高半纤维素浆液，粘流活化能略低，表观粘度、结构粘度及弹性较小。因此浆液的流动性能好，可纺性好，能够在较高浆粕含量下纺制Lyocell纤维，既能提高Lyocell纤维的质量，又能提高Lyocell工艺的生产效率；采用高半纤维素浆粕纺制Lyocell纤维，纤维得率仍然很高，从而降低了Lyocell纤维的成本；高半纤维素浆液比高alpha-纤维素浆液的稳定性略低，在氧化法纯化回收溶液时，需要消耗较多的双氧水，但是双氧水价格便宜，因此仍然能够降低Lyocell纤维的成本。
作为Lyocell纤维的低成本浆粕原料，高半纤维素浆粕的分子质量(MW)及其分布(MWD)信息对Lyocell纤维的加工生产是至关重要的。纤维素的MW和MWD，不仅会影响它在N-甲基吗琳-N-氧化物(NMMO)水溶剂中的溶解性能和纺丝浆液的可纺性能，而且会影响最终纤维的机械性能。因此，必须对浆粕原料进行MW和MWD的测定。
凝胶渗透色谱法(GPC)测定高聚物的MW和MWD，被普遍接受，广泛使用，但是针对纤维素而言，应用受到限制，因为纤维素不能溶解在大多数的有机溶剂中。为此，本论文采用高聚物的动态流变性质测定纤维素的相对MW和MWD，并且讨论了用流变法测定纤维素的相对分子质量及其分布时，纤维素在NMMO·H_2O溶剂中不同浓度的影响。研究结果表明：用流变法测定纤维素的相对分子质量及其分布时，纤维素溶液的浓度对测定结果有影响。但当纤维素溶液浓度足够高时(超过某个临界值后)，浓度对测定结果的影响可以忽略。而且，计算的结果与GPC法测得结果相比大小趋势相一致。此外，流变法测定纤维素的相对分子质量及其分布，经济、简单、快速且方便，所以在纤维工业生产中，用来快速分析纤维素的分子质量及其分布是可行的。
高半纤维素浆粕原料纺制成的Lyocell纤维，在纤维质量上与常规浆粕原料(高alpha-纤维素浆粕)纺制成的Lyocell纤维有什么不同，论文进行了对比研究，结果如下：
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，湿摩擦值增大1／2倍。这是由于高半纤维素Lyocell纤维比高alpha-纤维素Lyocell纤维，原纤聚集束尺寸小，且原纤聚集束结构稳定，从而不易劈裂成细小的原纤，提高了Lyocell纤维的抗原纤化能力。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，染料的吸色率和固色率增加了5-8％。因为前者的结晶度略低，以及原纤聚集束尺寸小，从而可达及原纤的表面增大，增加了纤维素伯醇羟基的可及度和反应性。另外，前者中低分子量的半纤维素含量较高，小分子比大分子易于染色，因而提高了Lyocell纤维的染色性能。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，在同样的纺丝浆液浓度下，前者比后者的强度低。因为前者含有较多低分子量的半纤维素组分，使其力学性能有所下降。另一方面，高半纤维素浆粕的纺丝浆液，流动性能好，可以用较高浓度的纺丝浆液来纺丝，这既提高了Lyocell纤维的机械性能，又提高了Lyocell纤维的生产效率。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，取向度较高，结晶度较低。高半纤维素浆粕的纺丝浆液，流动性能好，在喷头拉伸时易于取向，因而具有较高的取向度；半纤维素是纤维素三级结构的主要调节剂，从而使得纤维素原纤间结合的更加紧密，使得纤维素纤维的结晶度略低。
以上研究结果可见：低成本的高半纤维素浆粕纺制的Lyocell纤维，在纤维质量上，能与高alpha-纤维素浆粕纺制的Lyocell纤维相比。而且某些纤维性能(抗原纤化和染色)有所提高。
值得引起注意的是：Lyocell纤维工艺中，纤维素浆粕原料与溶剂NMMO·H_2O溶液形成纺丝浆液，在经过凝固浴时，大部分的纤维素都能沉淀出来，转化为再生纤维素纤维，但仍有微量的低聚糖(短链的纤维素和半纤维素)留在凝固浴中。工业化大生产中，是常年连续循环生产的，留在凝固浴中的微量低聚糖不断积累后，是否会对纺制Lyocell纤维，纤维质量以及凝固浴的回收工程带来困难，这个问题是Lyocell纤维实现工业化大生产的关键之一。为此，本论文对这一问题进行了探索性的研究。
首先，采用高效液相色谱法(HPLC)分析了Lyocell纤维和浆粕原料中的单糖成分，得知它们的各种单糖组分含量基本一样。然后，根据这个单糖组分含量配比成为混合糖，测得在0~0C下，此混合糖在9％(w／w)的NMMO·H_2O溶液中的饱和值约为32％。从而建立了凝固浴中混和糖总含量的测定方法，为Lyocell纤维的工业化生产提供了技术支持。最后，模拟研究了不断积累在凝固浴中的低聚糖含量对纺制Lyocell纤维的影响。研究发现：低聚糖在凝固浴中不断积累，即使形成饱和溶液(32％)，也不会对纺制Lyocell纤维过程和成品纤维的质量产生明显的影响。至于是否对溶剂NMMO的回收产生影响，这一问题我们将进一步研究。
Lyocell fiber has attracted great attention in the textile field since it was developed in the mid-1970s, because Lyocell fiber technology is a relatively simple and environmentally friendly way to produce regenerated cellulose fiber compared to the conventional viscose process. However, the development of Lyocell fiber is relatively slow due to its high price. Therefore, it is crucial to reduce the cost of Lyocell process for the further development.
It is reported that the pulp material containing more than 90% alpha-cellulose is called high alpha-cellulose pulp and the pulp material containing around 20% hemicellulose is called high hemicellulose pulp. In the conventional viscose process, only high alpha-cellulose pulp can be used as raw material in order to obtain a high yield of viscose fiber. Up to now, Lyocell fiber process still follows the conventional viscose process using this high alpha-cellulose pulp material. However, the cost of high alpha-cellulose pulp is higher than that of high hemicellulose pulp. It is significant in industry if a cheap pulp containing high hemicellulose can be used to produce Lyocell fiber since using a cheap pulp can reduce the cost in certain degree. The aim of this paper is to investigate the feasibility of using the cheap pulp with high hemicellulose content to produce Lyocell fiber.
Firstly, the yield of Lyocell fiber from high hemicellulose pulp and high alpha-cellulose pulp was measured. It was found that the yield of them was approximately equal. That means the yield of Lyocell fiber is not dependent on the alpha-cellulose content in pulp material.
Secondly, the dissolvability, spinnablility and stablity of high hemicellulose pulp in N-methlymorpholine-N-oxide (NMMO) aqueous solution were studied. The results showed that the dissolvability and spinnablity of high hemicellulose dope were better than those of high alpha-cellulose dope. Although the stablity of high hemicellulose dope decreased slightly, it can be solved by using more hydrogen peroxide solution (H_2O_2) to purify and recycle NMMO.
Thirdly, the molecular weight (MW) and molecular weight distribution (MWD) of high hemicellulose pulp was measured since it was important for Lyocell fiber process to choose appropriate pulp material. The gel permeation chromatograghy (GPC) method has been widely used and accepted for measuring the MW and MWD for polymers. However, the method has its limitations. The key of this method is to find the suitable solvents to dissolve the polymer well. But cellulose can not be dissolved in most of the organic solvents because of inter- and intro- hydrogen bonding of the cellulose chains. Lithium chloride / N, N-dimethlylacetamide (LiCl/DMAc) can dissolve cellulose, but the dissolution process is very complicated, which includes pre-activation, solvent exchange, swelling and dissolution. Furthermore, more attention must be paid to each step, and cellulose has to be dissolved for 5-10 days according to the type of cellulose pulp. Therefore, it is necessary to develop a new way to measure MW and MWD. In this work, rheology method was selected to measure MW and MWD of cellulose.
Moreover, during the prediction of MW and MWD of cellulose using rheology method, the influence of cellulose concentration in NMMO·H_2O solution on the measured result was investigated. It is shown that the results of the rheology method and the GPC method are comparable. It is also found the concentration of cellulose in NMMO·H_2O solution affected the calculated results when rheology method was applied. But there is no significant influence of cellulose concentration on the calculated data when the cellulose concentration is high enough. That is to say, when rheology method was applied to prediction of MW and MWD of cellulose, high concentration of cellulose in NMMO·H_2O solution has to be used in order to get a reliable and stable data. In addition, the rheology method is simple and fast. Therefore it is a useful and easy way to analyze the MW and MWD of cellulose in the fiber industry.
Fourthly, the structure and properties of Lyocell fibers from high hemicellulose pulp and high alpha-cellulose pulp were compared in order to investigate the influence of hemicellulose on the quality of Lyocell fiber.
It was found that the mechanical properties of high hemicellulose Lyocell fiber would decrease slightly, but a higher hemicellulose concertration spinning solution could be processed, which would increase the mechanical properties and the efficiency of the fiber process. Meanwhile, the fibrillation resistance and dyeing properties of high hemicellulose Lyocell fiber could also be improved.
In addition, compared to high alpha-cellulose Lyocell fiber, high hemicellulose Lyocell fiber has slightly higher orientation, lower crystallinity, smaller fibril aggregation size and more stable structure.
Those findings showed that the properties of high hemicellulose Lyocell fiber could be comparable to those of high alpha-cellulose Lyocell fiber. Therefore, it is feasible that this cheap pulp containing high hemicellulose could be used to produce Lyocell fiber.
Here, it is well known that Lyocell fiber technology is a close-cycled processing. Cellulose pulp is directly dissolved in NMMO·H_2O solution to form spinning solution. After that, filament (ejected spinning solution) is precipitated from coagulation bath and regenerated into Lyocell fiber. However, during industrial production, some oligosaccharides would be dissolved and accumulated in coagulation bath in this process. It is possible that this phenomenon would influence formation of fiber and affect the properties of obtained fiber and the process of solvent recovery. Therefore, these problems were also investigated in the paper.
The research results showed the monosaccharide composition of Lyocell fibers and their raw material pulps was approximately equal. A sugar mixture was made according to the monosaccharide composition of Lyocell fiber and the method of measuring the total sugar mixture content in coagulation bath was established. It was found that the saturation point of sugar mixture dissolved in coagulation bath (9%, w/w, NMMO aqueous solution) at 0°C was about 32%. Besides, the influence of content of oligosaccharides in coagulation bath on the fiber formation and properties was investigated. Further work is being carried out to study on the influence of accumulated sugar in coagulation bath on solvent recovery.
Lyocell纤维工艺一直沿袭传统粘胶纤维工艺，采用高alpha-纤维素含量的浆粕作为原料。高alpha-纤维素含量是为了保证得到高的粘胶纤维得率，但是高alpha-纤维素含量的浆粕，生产成本高。
为此，本论文选择了一种低成本的浆粕原料(高半纤维素浆粕)，这种浆粕，alpha-纤维素含量较低，半纤维素含量高达20％左右。在浆粕生产中，高半纤维素浆粕，一方面能够简化浆粕生产工艺，另一方面浆粕的得率高，因此能够降低浆粕生产成本约1／2。
论文中，首先探讨了高半纤维素浆粕的溶解性、浆液的可纺性和稳定性、以及Lvocell纤维的得率。研究结果表明：高半纤维素浆粕比高alpha-纤维素浆粕更易溶解，所需溶解条件温和、溶解范围较宽、溶解效果良好，更有利于实验操作的控制；高半纤维素浆液，粘流活化能略低，表观粘度、结构粘度及弹性较小。因此浆液的流动性能好，可纺性好，能够在较高浆粕含量下纺制Lyocell纤维，既能提高Lyocell纤维的质量，又能提高Lyocell工艺的生产效率；采用高半纤维素浆粕纺制Lyocell纤维，纤维得率仍然很高，从而降低了Lyocell纤维的成本；高半纤维素浆液比高alpha-纤维素浆液的稳定性略低，在氧化法纯化回收溶液时，需要消耗较多的双氧水，但是双氧水价格便宜，因此仍然能够降低Lyocell纤维的成本。
作为Lyocell纤维的低成本浆粕原料，高半纤维素浆粕的分子质量(MW)及其分布(MWD)信息对Lyocell纤维的加工生产是至关重要的。纤维素的MW和MWD，不仅会影响它在N-甲基吗琳-N-氧化物(NMMO)水溶剂中的溶解性能和纺丝浆液的可纺性能，而且会影响最终纤维的机械性能。因此，必须对浆粕原料进行MW和MWD的测定。
凝胶渗透色谱法(GPC)测定高聚物的MW和MWD，被普遍接受，广泛使用，但是针对纤维素而言，应用受到限制，因为纤维素不能溶解在大多数的有机溶剂中。为此，本论文采用高聚物的动态流变性质测定纤维素的相对MW和MWD，并且讨论了用流变法测定纤维素的相对分子质量及其分布时，纤维素在NMMO·H_2O溶剂中不同浓度的影响。研究结果表明：用流变法测定纤维素的相对分子质量及其分布时，纤维素溶液的浓度对测定结果有影响。但当纤维素溶液浓度足够高时(超过某个临界值后)，浓度对测定结果的影响可以忽略。而且，计算的结果与GPC法测得结果相比大小趋势相一致。此外，流变法测定纤维素的相对分子质量及其分布，经济、简单、快速且方便，所以在纤维工业生产中，用来快速分析纤维素的分子质量及其分布是可行的。
高半纤维素浆粕原料纺制成的Lyocell纤维，在纤维质量上与常规浆粕原料(高alpha-纤维素浆粕)纺制成的Lyocell纤维有什么不同，论文进行了对比研究，结果如下：
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，湿摩擦值增大1／2倍。这是由于高半纤维素Lyocell纤维比高alpha-纤维素Lyocell纤维，原纤聚集束尺寸小，且原纤聚集束结构稳定，从而不易劈裂成细小的原纤，提高了Lyocell纤维的抗原纤化能力。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，染料的吸色率和固色率增加了5-8％。因为前者的结晶度略低，以及原纤聚集束尺寸小，从而可达及原纤的表面增大，增加了纤维素伯醇羟基的可及度和反应性。另外，前者中低分子量的半纤维素含量较高，小分子比大分子易于染色，因而提高了Lyocell纤维的染色性能。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，在同样的纺丝浆液浓度下，前者比后者的强度低。因为前者含有较多低分子量的半纤维素组分，使其力学性能有所下降。另一方面，高半纤维素浆粕的纺丝浆液，流动性能好，可以用较高浓度的纺丝浆液来纺丝，这既提高了Lyocell纤维的机械性能，又提高了Lyocell纤维的生产效率。
高半纤维素浆粕纺制的Lyocell纤维比高alpha-纤维素浆粕纺制的Lyocell纤维，取向度较高，结晶度较低。高半纤维素浆粕的纺丝浆液，流动性能好，在喷头拉伸时易于取向，因而具有较高的取向度；半纤维素是纤维素三级结构的主要调节剂，从而使得纤维素原纤间结合的更加紧密，使得纤维素纤维的结晶度略低。
以上研究结果可见：低成本的高半纤维素浆粕纺制的Lyocell纤维，在纤维质量上，能与高alpha-纤维素浆粕纺制的Lyocell纤维相比。而且某些纤维性能(抗原纤化和染色)有所提高。
值得引起注意的是：Lyocell纤维工艺中，纤维素浆粕原料与溶剂NMMO·H_2O溶液形成纺丝浆液，在经过凝固浴时，大部分的纤维素都能沉淀出来，转化为再生纤维素纤维，但仍有微量的低聚糖(短链的纤维素和半纤维素)留在凝固浴中。工业化大生产中，是常年连续循环生产的，留在凝固浴中的微量低聚糖不断积累后，是否会对纺制Lyocell纤维，纤维质量以及凝固浴的回收工程带来困难，这个问题是Lyocell纤维实现工业化大生产的关键之一。为此，本论文对这一问题进行了探索性的研究。
首先，采用高效液相色谱法(HPLC)分析了Lyocell纤维和浆粕原料中的单糖成分，得知它们的各种单糖组分含量基本一样。然后，根据这个单糖组分含量配比成为混合糖，测得在0~0C下，此混合糖在9％(w／w)的NMMO·H_2O溶液中的饱和值约为32％。从而建立了凝固浴中混和糖总含量的测定方法，为Lyocell纤维的工业化生产提供了技术支持。最后，模拟研究了不断积累在凝固浴中的低聚糖含量对纺制Lyocell纤维的影响。研究发现：低聚糖在凝固浴中不断积累，即使形成饱和溶液(32％)，也不会对纺制Lyocell纤维过程和成品纤维的质量产生明显的影响。至于是否对溶剂NMMO的回收产生影响，这一问题我们将进一步研究。
Lyocell fiber has attracted great attention in the textile field since it was developed in the mid-1970s, because Lyocell fiber technology is a relatively simple and environmentally friendly way to produce regenerated cellulose fiber compared to the conventional viscose process. However, the development of Lyocell fiber is relatively slow due to its high price. Therefore, it is crucial to reduce the cost of Lyocell process for the further development.
It is reported that the pulp material containing more than 90% alpha-cellulose is called high alpha-cellulose pulp and the pulp material containing around 20% hemicellulose is called high hemicellulose pulp. In the conventional viscose process, only high alpha-cellulose pulp can be used as raw material in order to obtain a high yield of viscose fiber. Up to now, Lyocell fiber process still follows the conventional viscose process using this high alpha-cellulose pulp material. However, the cost of high alpha-cellulose pulp is higher than that of high hemicellulose pulp. It is significant in industry if a cheap pulp containing high hemicellulose can be used to produce Lyocell fiber since using a cheap pulp can reduce the cost in certain degree. The aim of this paper is to investigate the feasibility of using the cheap pulp with high hemicellulose content to produce Lyocell fiber.
Firstly, the yield of Lyocell fiber from high hemicellulose pulp and high alpha-cellulose pulp was measured. It was found that the yield of them was approximately equal. That means the yield of Lyocell fiber is not dependent on the alpha-cellulose content in pulp material.
Secondly, the dissolvability, spinnablility and stablity of high hemicellulose pulp in N-methlymorpholine-N-oxide (NMMO) aqueous solution were studied. The results showed that the dissolvability and spinnablity of high hemicellulose dope were better than those of high alpha-cellulose dope. Although the stablity of high hemicellulose dope decreased slightly, it can be solved by using more hydrogen peroxide solution (H_2O_2) to purify and recycle NMMO.
Thirdly, the molecular weight (MW) and molecular weight distribution (MWD) of high hemicellulose pulp was measured since it was important for Lyocell fiber process to choose appropriate pulp material. The gel permeation chromatograghy (GPC) method has been widely used and accepted for measuring the MW and MWD for polymers. However, the method has its limitations. The key of this method is to find the suitable solvents to dissolve the polymer well. But cellulose can not be dissolved in most of the organic solvents because of inter- and intro- hydrogen bonding of the cellulose chains. Lithium chloride / N, N-dimethlylacetamide (LiCl/DMAc) can dissolve cellulose, but the dissolution process is very complicated, which includes pre-activation, solvent exchange, swelling and dissolution. Furthermore, more attention must be paid to each step, and cellulose has to be dissolved for 5-10 days according to the type of cellulose pulp. Therefore, it is necessary to develop a new way to measure MW and MWD. In this work, rheology method was selected to measure MW and MWD of cellulose.
Moreover, during the prediction of MW and MWD of cellulose using rheology method, the influence of cellulose concentration in NMMO·H_2O solution on the measured result was investigated. It is shown that the results of the rheology method and the GPC method are comparable. It is also found the concentration of cellulose in NMMO·H_2O solution affected the calculated results when rheology method was applied. But there is no significant influence of cellulose concentration on the calculated data when the cellulose concentration is high enough. That is to say, when rheology method was applied to prediction of MW and MWD of cellulose, high concentration of cellulose in NMMO·H_2O solution has to be used in order to get a reliable and stable data. In addition, the rheology method is simple and fast. Therefore it is a useful and easy way to analyze the MW and MWD of cellulose in the fiber industry.
Fourthly, the structure and properties of Lyocell fibers from high hemicellulose pulp and high alpha-cellulose pulp were compared in order to investigate the influence of hemicellulose on the quality of Lyocell fiber.
It was found that the mechanical properties of high hemicellulose Lyocell fiber would decrease slightly, but a higher hemicellulose concertration spinning solution could be processed, which would increase the mechanical properties and the efficiency of the fiber process. Meanwhile, the fibrillation resistance and dyeing properties of high hemicellulose Lyocell fiber could also be improved.
In addition, compared to high alpha-cellulose Lyocell fiber, high hemicellulose Lyocell fiber has slightly higher orientation, lower crystallinity, smaller fibril aggregation size and more stable structure.
Those findings showed that the properties of high hemicellulose Lyocell fiber could be comparable to those of high alpha-cellulose Lyocell fiber. Therefore, it is feasible that this cheap pulp containing high hemicellulose could be used to produce Lyocell fiber.
Here, it is well known that Lyocell fiber technology is a close-cycled processing. Cellulose pulp is directly dissolved in NMMO·H_2O solution to form spinning solution. After that, filament (ejected spinning solution) is precipitated from coagulation bath and regenerated into Lyocell fiber. However, during industrial production, some oligosaccharides would be dissolved and accumulated in coagulation bath in this process. It is possible that this phenomenon would influence formation of fiber and affect the properties of obtained fiber and the process of solvent recovery. Therefore, these problems were also investigated in the paper.
The research results showed the monosaccharide composition of Lyocell fibers and their raw material pulps was approximately equal. A sugar mixture was made according to the monosaccharide composition of Lyocell fiber and the method of measuring the total sugar mixture content in coagulation bath was established. It was found that the saturation point of sugar mixture dissolved in coagulation bath (9%, w/w, NMMO aqueous solution) at 0°C was about 32%. Besides, the influence of content of oligosaccharides in coagulation bath on the fiber formation and properties was investigated. Further work is being carried out to study on the influence of accumulated sugar in coagulation bath on solvent recovery.
引文
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