CN116905105A - 一种纤维、其制备方法及应用 - Google Patents
一种纤维、其制备方法及应用 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229920000742 Cotton Polymers 0.000 claims abstract description 45
- 239000002608 ionic liquid Substances 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
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- 230000007935 neutral effect Effects 0.000 claims abstract description 5
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
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- 238000007710 freezing Methods 0.000 claims description 10
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- PBIDWHVVZCGMAR-UHFFFAOYSA-N 1-methyl-3-prop-2-enyl-2h-imidazole Chemical compound CN1CN(CC=C)C=C1 PBIDWHVVZCGMAR-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 13
- 239000003921 oil Substances 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 5
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- 239000000975 dye Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 125000000129 anionic group Chemical group 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- XULSCZPZVQIMFM-IPZQJPLYSA-N odevixibat Chemical compound C12=CC(SC)=C(OCC(=O)N[C@@H](C(=O)N[C@@H](CC)C(O)=O)C=3C=CC(O)=CC=3)C=C2S(=O)(=O)NC(CCCC)(CCCC)CN1C1=CC=CC=C1 XULSCZPZVQIMFM-IPZQJPLYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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Abstract
本发明涉及纤维制备技术领域,尤其涉及纤维、其制备方法及应用。包括:将棉短纤维浸入氢氧化钠溶液中进行活化、超声处理、洗涤至中性、烘干,得到活化棉;将离子液体和所述活化棉放入烧瓶中,向所述烧瓶中并加入DMSO,氮气保护下,在油浴中加热直至所述活化棉完全溶解,得到溶解液。本发明利用离子液体溶解成功并制备该纤维,该制备方法具有简单高效的特点,由其制备得到的纤维可作为良好的吸附剂而得到广泛应用。
Description
技术领域
本发明涉及纤维制备技术领域,尤其涉及一种纤维、其制备方法及应用。
背景技术
近来,绿色低成本的吸附剂受到越来越多的关注。以生物质为基础的吸附剂,如纤维、淀粉和几丁质的吸附剂已经被广泛研究。纤维是一种天然聚合物,其不溶于水,结构中含有大量活性羟基,可用于为染料引入更多官能团吸附。通过化学反应对纤维进行改性,可使其吸附能力大大提升,如在纤维中引入阳离子基团,由于静电引力的作用可使其吸附阴离子染料。
纤维是一种高度丰富的可再生材料,但是却不易被溶解,加上部分溶剂系统存在热不稳定的缺点,因而研发了新的溶剂体系—离子液体。离子液体又叫做低温熔融盐,它在室温下是呈现液态的,它是由阴阳离子组成的盐。离子液体作为离子化合物,因其结构中某些取代基的不对称性使离子不能规则地堆积成晶体,因而熔点较低。在各种各样类型的离子液体中,咪唑离子液体对纤维的溶解引起了研究人员的注意。在研究纤维的溶解机理中,许多离子液体被设计合成,诸如[AMIM]Cl和[EMIM]Ac。然而,对于天然棉纤维,室温离子液体只能将它达到溶胀状态。
发明内容
针对上述现有技术存在的不足,本发明提供一种纤维、其制备方法及应用,利用离子液体溶解成功并制备该纤维,该制备方法具有简单高效的特点,由其制备得到的纤维可作为良好的吸附剂而得到广泛应用。
为了达到上述目的,本发明一方面提供一种纤维的制备方法,包括活化棉制备步骤、活化棉溶解步骤、以及纤维合成步骤;
所述活化棉制备步骤包括:将棉短纤维浸入氢氧化钠溶液中进行活化、超声处理、洗涤至中性、烘干,得到活化棉;
所述活化棉溶解步骤包括:将离子液体和所述活化棉放入烧瓶中,向所述烧瓶中并加入DMSO,氮气保护下,在油浴中加热直至所述活化棉完全溶解,得到溶解液。
在其中一些实施例中,所述活化棉溶解步骤中所述离子液体与所述DMSO的质量:体积为1:0.24,所述活化棉与所述离子液体的质量比为0.1-0.4:1。
在其中一些实施例中,所述离子液体选自1-乙基-3-甲基咪唑乙酸酯或1-烯丙基-3-甲基咪唑氯化物。
在其中一些实施例中,所述纤维合成步骤包括:将所述溶解液趁热倒入烧杯中,并加入预热的氯化钠固体,搅拌以均匀分布在溶液中,自然冷却至室温并置于冰箱中冷冻,取出、洗净、冷冻,用无水乙醇浸泡,然后晾干,得到纤维。
在其中一些实施例中,所述活化棉制备步骤具体包括:将10g棉短纤维浸入30wt%的氢氧化钠溶液中进行活化,然后将溶液超声处理1小时,洗涤至中性,烘干,得到所述活化棉。
在其中一些实施例中,所述活化棉溶解步骤具体包括:将30g离子液体、0.03-0.12g活化棉放入三颈烧瓶并加入DMSO,氮气保护下,并在110℃的油浴中加热直至其完全溶解,继续磁力搅拌,得到所述溶解液;所述离子液体与所述DMSO的质量:体积为1:0.24。
在其中一些实施例中,所述纤维合成步骤具体包括:将所述溶解液趁热倒入烧杯中,并加入预热的氯化钠固体,所述溶解液与所述氯化钠固体的质量比为1:1,并搅拌以均匀分布在溶液中,然后自然冷却至室温并置于-20℃冰箱中24小时,取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干,得到所述纤维。
在其中一些实施例中,还包括:取2.5mg2,2,6,6-四甲基哌啶-1-氧基(TEMPO)和25mgNaBr加入70ml去离子水中,然后将1g纤维置于上述溶液体系中,并添加相当于一定量纤维的NaClO溶液;调节pH在一定范围内,一定温度下反应一定时间后;加入乙醇淬灭氧化;用乙醇浸泡脱除钠离子48h,室温下干燥。
本发明另一方面提供一种纤维,由上述任一技术方案所述的纤维的制备方法制备得到。
本发明还提供一种上述纤维作为吸附剂的应用。
与现有技术相比,本发明具有如下优点:
本发明提供一种纤维的制备方法,首先对棉短纤维进行活化,利用离子液体结合DMSO实现了对活化棉的成功溶解,一方面可以为理论研究纤维对阳离子染料、油和水吸附性能提供材料基础,对进一步研究纤维的结构具有重要的意义;另一方面,为特棉短绒纤维的制备提供了一种简单高效的合成方法。
附图说明
为了更清楚地说明本发明实施例中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1为实施例2制得的[EMIM]Ac-1%的SEM图;
图2为实施例3制得的[EMIM]Ac-2%的SEM图;
图3为实施例4制得的[EMIM]Ac-3%的SEM图;
图4为实施例5制得的[EMIM]Ac-4%的SEM图;
图5为实施例6的SEM图;
图6为实施例2,实施例3,实施例4,实施例5和实施例6的FTIR图;
图7为实施例2,实施例3,实施例4,实施例5和实施例6的XRD图;
图8为实施例2,实施例3,实施例4,实施例5和实施例6的TG图。
具体实施方式
下面结合附图和具体实施例对本发明技术方案进行详细的描述,以更进一步了解本发明的目的、方案及功效,但并非作为本发明所附权利要求保护范围的限制。
实施例1
将10g棉短纤维浸入氢氧化钠溶液(30wt%)中进行活化,然后将溶液超声处理1小时,并取出,洗涤至中性,烘干。
实施例2
将30g离子液体[EMIM]Ac(1-乙基-3-甲基咪唑乙酸酯),0.03g活化棉放入三颈烧瓶并加入DMSO(离子液体:DMSO=1:0.24(w:v))。用氮气保护该装置并在110℃的油浴中加热直至其完全溶解。在此过程中,继续磁力搅拌。将溶解的溶液趁热倒入烧杯中,并加入预热的氯化钠固体(1:1(w:w))并搅拌以均匀分布在溶液中。然后自然冷却至室温并置于冰箱(-20℃)中24小时。取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干以备后用,标记为[EMIM]Ac-1%。
实施例3
将30g离子液体[EMIM]Ac,0.06g活化棉放入三颈烧瓶并加入DMSO(离子液体:DMSO=1:0.24(w:v))。用氮气保护该装置并在110℃的油浴中加热直至其完全溶解。在此过程中,继续磁力搅拌。将溶解的溶液趁热倒入烧杯中,并加入预热的氯化钠固体(1:1(w:w))并搅拌以均匀分布在溶液中。然后自然冷却至室温并置于冰箱(-20℃)中24小时。取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干以备后用,标记为[EMIM]Ac-2%。
实施例4
将30g离子液体[EMIM]Ac,0.09g活化棉放入三颈烧瓶并加入DMSO(离子液体:DMSO=1:0.24(w:v))。用氮气保护该装置并在110℃的油浴中加热直至其完全溶解。在此过程中,继续磁力搅拌。将溶解的溶液趁热倒入烧杯中,并加入预热的氯化钠固体(1:1(w:w))并搅拌以均匀分布在溶液中。然后自然冷却至室温并置于冰箱(-20℃)中24小时。取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干以备后用,标记为[EMIM]Ac-3%。
实施例5
将30g离子液体[EMIM]Ac,0.12g活化棉放入三颈烧瓶并加入DMSO(离子液体:DMSO=1:0.24(w:v))。用氮气保护该装置并在110℃的油浴中加热直至其完全溶解。在此过程中,继续磁力搅拌。将溶解的溶液趁热倒入烧杯中,并加入预热的氯化钠固体(1:1(w:w))并搅拌以均匀分布在溶液中。然后自然冷却至室温并置于冰箱(-20℃)中24小时。取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干以备后用,标记为[EMIM]Ac-4%。
实施例6
制备方法同实施例2-5,制备[AMIM]Cl-1%,[AMIM]Cl-2%,[AMIM]Cl-3%,[AMIM]Cl-4%(1-烯丙基-3-甲基咪唑氯化物)。
实施例7
将实施例2,实施例3,实施例4,实施例5和实施例6得到的纤维进行吸附测试,用亚甲基蓝和甲基紫进行染料吸附的实验,分别取一定浓度的亚甲基蓝溶液和甲基紫溶液置于25mL的玻璃瓶中,分别用0.1mol·L-1的氢氧化钠和盐酸溶液分别调节溶液的pH为2、4、5、6、7、8、10。然后加入一定量的TEMPO-[AMIM]Cl-1%、TEMPO-[AMIM]Cl-2%、TEMPO-[AMIM]Cl-3%、TEMPO-[AMIM]Cl-4%,用锡纸避光处理,迅速放于恒温振荡器中,在一定的条件下,振荡,取液。进行过滤,稀释到一定倍数后测量其在不同pH下的吸光度,确定最适宜的pH值。用移液管分别移取10mL一定浓度的甲基紫和亚甲基蓝溶液放于25mL的透明反应瓶中,调节pH,分别加入等量的A-T-1%、A-T-2%、A-T-3%、A-T-4%,用锡纸全部包上避光。快速置于30℃、100r/min的恒温震荡器中,每隔一定时间取液,稀释到一定倍数后用分光光度计测量吸光度。移取10mL不同浓度的甲基紫和亚甲基蓝溶液分别放于25mL的透明反应瓶中,保持pH值为7,加入10mg的TEMPO-[AMIM]Cl-4%,盖上瓶盖,用锡纸避光,快速置于30℃,100r/min的恒温震荡器中,反应190min,取液,稀释到一定倍数后用分光光度计测量吸光度。将约0.05g纤维样品称入100mL烧杯中,加入20mL蒸馏水,并加入磁体,在室温下以100r/min搅拌24小时。再计算纤维的吸水率。
对实施例2-6制备得到的纤维进行FTIR,XRD,TG,SEM分析,结果如图1-8所示。
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例应用于其它领域,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (9)
1.一种纤维的制备方法,其特征在于,包括活化棉制备步骤、活化棉溶解步骤、以及纤维合成步骤;
所述活化棉制备步骤包括:将棉短纤维浸入氢氧化钠溶液中进行活化、超声处理、洗涤至中性、烘干,得到活化棉;
所述活化棉溶解步骤包括:将离子液体和所述活化棉放入烧瓶中,向所述烧瓶中并加入DMSO,氮气保护下,在油浴中加热直至所述活化棉完全溶解,得到溶解液。
2.根据权利要求1所述的纤维的制备方法,其特征在于,所述活化棉溶解步骤中所述离子液体与所述DMSO的质量:体积为1:0.24,所述活化棉与所述离子液体的质量比为0.1-0.4:1。
3.根据权利要求1所述的纤维的制备方法,其特征在于,所述离子液体选自1-乙基-3-甲基咪唑乙酸酯或1-烯丙基-3-甲基咪唑氯化物。
4.根据权利要求1所述的纤维的制备方法,其特征在于,所述纤维合成步骤包括:将所述溶解液趁热倒入烧杯中,并加入预热的氯化钠固体,搅拌以均匀分布在溶液中,自然冷却至室温并置于冰箱中冷冻,取出、洗净、冷冻,用无水乙醇浸泡,然后晾干,得到纤维。
5.根据权利要求1所述的纤维的制备方法,其特征在于,所述活化棉制备步骤具体包括:将10g棉短纤维浸入30wt%的氢氧化钠溶液中进行活化,然后将溶液超声处理1小时,洗涤至中性,烘干,得到所述活化棉。
6.根据权利要求5所述的纤维的制备方法,其特征在于,所述活化棉溶解步骤具体包括:将30g离子液体、0.03-0.12g活化棉放入三颈烧瓶并加入DMSO,氮气保护下,并在110℃的油浴中加热直至其完全溶解,继续磁力搅拌,得到所述溶解液;所述离子液体与所述DMSO的质量:体积为1:0.24。
7.根据权利要求6所述的纤维的制备方法,其特征在于,所述纤维合成步骤具体包括:将所述溶解液趁热倒入烧杯中,并加入预热的氯化钠固体,所述溶解液与所述氯化钠固体的质量比为1:1,并搅拌以均匀分布在溶液中,然后自然冷却至室温并置于-20℃冰箱中24小时,取出,洗净,冷冻保存24小时,用无水乙醇浸泡,然后晾干,得到所述纤维。
8.一种纤维,其特征在于,由权利要求1-7任一项所述的纤维的制备方法制备得到。
9.根据权利要求8所述的纤维作为吸附剂的应用。
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