CN110698658B - 一种废聚酯链解制备有色聚酯的方法 - Google Patents
一种废聚酯链解制备有色聚酯的方法 Download PDFInfo
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Abstract
本发明属于废聚酯再生技术领域,尤其涉及一种废聚酯链解制备有色聚酯的方法。一种废聚酯链解制备有色聚酯的方法,该方法包括以下的步骤:1)回收的废聚酯进行前处理和配比调色;2)链解催化剂作用下进行链解反应,所述的链解工艺为母液温度190~210℃,反应时间30分钟‑5小时;链解液进行沉淀除杂,多级过滤处理;过滤精度依次提升,初级过滤的精度为50‑100目,最终过滤精度为500~800目;3)除杂后的链解物经补色送至缩聚釜进行预缩聚,最后经终缩聚形成成品。该方法可制备连续稳定高品质的有色再生聚酯,实现废旧聚酯的高值化回收利用。该方法可制备连续稳定高品质的有色再生聚酯,实现废旧聚酯的高值化回收利用。
Description
技术领域
本发明属于废聚酯再生技术领域,尤其涉及一种废聚酯链解制备有色聚酯的方法。
背景技术
聚对苯二甲酸乙二醇酯(PET)是由对苯二甲酸或对苯二甲酸二甲酯与乙二醇聚合而成的饱和聚酯。由于具有良好的物理化学稳定性、可拉伸性能,普遍应用于服装,食品包装等领域。但是由于PET在自然条件下具有极强的化学惰性,难以被生物降解,大量的废弃聚酯给环境造成严重的污染,因此,对废旧聚酯制品进行回收,实现资源的有效循环利用,减少环境污染成为聚酯工业的重要课题。
目前对废旧聚酯制品回收利用主要有物理法和化学法。物理法是通过熔融造粒的方式对聚酯进行再利用,但是由于废聚酯中含有多种染料和添加剂等杂质,一般只能生产常规的短纤产品。化学法主要有水链解法、甲醇链解法,乙二醇链解法等。废聚酯通过化学处理将固态聚酯链解,转化为较小的分子、中间原料,或直接转化为单体,然后再缩聚为高品质的再生聚酯,实现对废聚酯的封闭式循环再生。化学法回收聚酯理论上能达到原生聚酯的水平,而且可以进行化学改性,但实际上由于原料中含有多种杂质,存在再生聚酯性能不稳定,副产物含量不易控制等问题,兼有原料中含有多种染料,造成再生聚酯产品色相较差。
发明内容
为了克服废聚酯链解法再生过程中的问题,并对废聚酯物颜色有效利用,本申请的目的是提供一种废聚酯链解制备有色聚酯的方法,该方法可制备连续稳定高品质的有色再生聚酯,实现废旧聚酯的高值化回收利用。
为了实现上述的目的,本申请采用了以下的技术方案:
一种废聚酯链解制备有色聚酯的方法,该方法包括以下的步骤:
1)回收的废聚酯进行前处理和配比调色;
2)链解催化剂作用下进行链解反应,所述的链解工艺为母液温度190~210℃,反应时间30分钟-5小时;链解液进行沉淀除杂,多级过滤处理;过滤精度依次提升,初级过滤的精度为50-100目,最终过滤精度为500~800目;
3)除杂后的链解物经补色送至缩聚釜进行预缩聚,最后经终缩聚形成成品。
作为优选,废聚酯前处理包括,对于聚酯瓶片、聚酯薄膜,清洗后干燥;对于聚酯纤维制品通过热摩擦成型工艺进行致密化处理,温度150~260℃,压力0.1~10MPa,时间5~15min。
作为优选,所述的配比调色处理包括,经过前处理的回收聚酯纤维由色度的不同进行筛选,按比例进行配比调色处理。
作为优选,所述的链解催化剂采用醋酸钠或醋酸锌等金属醋酸盐等。
作为优选,所述的链解反应,按废聚酯:乙二醇的摩尔百分比1:1~6的比例投入链解釜,其中链解釜中含有占投入废聚酯总量10~30%质量百分比的对苯二甲酸乙二醇酯及齐聚物,并添加链解催化剂;控制链解反应温度190~210℃、反应时间30分钟~5小时,得到含对苯二甲酸乙二醇酯及齐聚物的链解物。
作为优选,所述的沉淀除杂用的沉淀剂包括以下的组分:
纳米氧化钙 4-12份
硅藻土 2-10份
纳米氧化铝 5-15份
氢氧化钾 1-6份
碳酸钙 2-10份
羟乙基纤维素钠1-5份
聚丙烯酰胺 2-10份。
作为再优选,该沉淀剂由以下的组分构成:
纳米氧化钙 6-8份
硅藻土 3-5份
纳米氧化铝 8-10份
氢氧化钾 2-4份
碳酸钙 4-6份
羟乙基纤维素钠2-3份
聚丙烯酰胺 3-4份。
本申请还公开了上述的沉淀剂的制备方法,将纳米氧化钙、硅藻土、纳米氧化铝、碳酸钙、羟乙基纤维素钠、聚丙烯酰胺加入研磨机研磨,过100筛后加入氢氧化钾,混合后加入搅拌釜中进行充分搅拌,搅拌速率600转/分钟,时间50分钟,得到其沉淀剂。
作为进一步改进,除杂方法还包括磁流体吸附除杂,沉淀除杂后继续将滤液投入至磁流体除杂器中,使FeO磁流体与滤液在除杂器中旋转混合,然后断开除杂器的磁座使之变成永恒磁场,10-20分钟后,磁性颗粒向下沉淀分层,将其过滤除去尼龙、氨纶、消光剂、二氧化钛等;优选,采用醇水共热法制备FeO磁流体,按Fe3+和Fe2+摩尔比1-3:1比例的Fe2(SO4)3溶液和FeSO4溶液混匀,加热至60-70℃保持恒温,滴加NaOH溶液充分搅拌使混合均匀,调节PH值为10-12,继续搅拌并加入无水乙醇,静止20-30分钟,调节PH值,继续升高温度,迅速搅拌并加入0.4-0.8倍Fe2+用量的表面活性剂油酸钠进行包裹,随后即可看到黑色的磁性颗粒生成。
作为优选,所述的过滤设置为三级,链解后完成一次过滤,经沉淀除杂处理后完成一次过滤,预缩聚后完成三次过滤,从一次过滤到三次过滤,过滤精度依次提高。
作为优选,所述的预缩聚设置两道,分别为预缩聚一和预缩聚二,预缩聚一的反应温度为230~250℃,真空度5~30KPa,停留时间1~3小时,预缩聚二的反应温度为250~280℃,真空度1~5 KPa,停留时间1~3小时;所述的终缩聚反应温度为275~290℃,真空度0.05~1 KPa,反应时长1~5小时。
作为优选,所述的补色处理为添加一点量的色母粒对链解物进行补色。
本申请还公开了所述的方法制备得到的有色聚酯熔体纺丝获得的再生聚酯短纤维。有色聚酯熔体的成品特性黏度值0.6~0.73dl/g,熔点210~230℃,黏度波动值≤±0.025,灰分含量≤0.15%,B值波动值≤±5,凝集粒子≤6个/mg。
本发明的有益效果为:1)在醇解釜中保留一定量的母液,可提高链解效率、稳定链解产物质量;2)由于废聚酯原料颜色的不确定性,对链解产物色值波动较大,通过在链解之前进行配比调色处理,保证了链解产物颜色的连续稳定;3)由于废聚酯原料来源复杂,内含不可链解的棉、麻和可链解的锦纶、氨纶,对链解液进行沉淀处理,有效减少链解产物中的杂质;4)废聚酯物经链解后,颜色会有一定的缺失,通过添加色母粒进行补色处理,可制备不同色值的再生产品。5)从链解到酯化、再到缩聚,采用较低的反应温度,能有效减少可链解高聚物的产生。
具体实施方法
下面结合具体实施方式,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
一种用于链解废聚酯品溶液中除杂的沉淀剂,该沉淀剂由以下的组分构成:
纳米氧化钙 6份
硅藻土 4份
纳米氧化铝 10份
氢氧化钾 3份
碳酸钙 4份
羟乙基纤维素钠2份
聚丙烯酰胺 4份;
将纳米氧化钙、硅藻土、纳米氧化铝、碳酸钙、羟乙基纤维素钠、聚丙烯酰胺加入研磨机研磨,过100筛后加入氢氧化钾,混合后加入搅拌釜中进行充分搅拌,搅拌速率600转/分钟,时间50分钟,得到其沉淀剂。
实施例5
一种用于链解废聚酯品溶液中除杂的沉淀剂,该沉淀剂由以下的组分构成:
纳米氧化钙 9份
硅藻土 2份
纳米氧化铝 8份
氢氧化钾 2份
碳酸钙 5份
羟乙基纤维素钠3份
聚丙烯酰胺 3份;
将纳米氧化钙、硅藻土、纳米氧化铝、碳酸钙、羟乙基纤维素钠、聚丙烯酰胺加入研磨机研磨,过100筛后加入氢氧化钾,混合后加入搅拌釜中进行充分搅拌,搅拌速率600转/分钟,时间50分钟,得到其沉淀剂。
实施例3
采用醇水共热法制备FeO磁流体,按Fe3+和Fe2+摩尔比1:1比例的Fe2(SO4)3溶液和FeSO4溶液混匀,加热至65℃保持恒温,滴加NaOH溶液充分搅拌使混合均匀,调节PH值为11左右,继续搅拌并加入无水乙醇,静止20-30分钟,调节PH值,继续升高温度,迅速搅拌并加入0.5倍Fe2+用量的表面活性剂油酸钠进行包裹,随后即可看到黑色的磁性颗粒生成。
实施例4
一种链解废聚酯制备有色聚酯的方法,该方法包括以下的步骤:
前处理:回收的废聚酯进行前处理和配比调色,于聚酯(PET)瓶片、聚酯(PET)薄膜,清洗后干燥;对于聚酯(PET)纤维制品(服装边角料、窗帘、地毯等):通过热摩擦成型工艺进行致密化处理(温度150~260℃,压力0.1~10MPa,时间5~15min);经过前处理的回收聚酯(PET)纤维由色度的不同进行筛选,按比例进行配比调色处理。
链解反应:将回收的聚酯(PET)经过致密化处理后,以废聚酯:乙二醇的摩尔百分比1:3的比例进入链解反应釜进行链解反应制备含对苯二甲酸乙二醇酯的链解物。其中链解釜中含有占投入废聚酯总量20%质量百分比的对苯二甲酸乙二醇酯及齐聚物,并添加链解催化剂;控制链解反应温度200℃、反应时间2小时,得到含对苯二甲酸乙二醇酯及齐聚物的链解物。链解催化剂:醋酸锌,催化剂含量:0.2%w。
除杂处理:将链解物先进行第一次过滤,除去不可链解的棉、麻等杂质,过滤规格为100目。然后将滤液投入至含有实施例1所示的沉淀剂的混合沉淀器中,充分搅拌混合后进行再次过滤,主要过滤出链解液中的氨纶、尼龙、消光剂等组份。
磁流体吸附除杂:继续将滤液投入至磁流体除杂器中,使FeO磁流体与滤液在除杂器中旋转混合,然后断开除杂器的磁座使之变成永恒磁场,12分钟后,磁性颗粒向下沉淀分层,将其过滤除去尼龙、氨纶、消光剂、二氧化钛等。
缩聚反应:在催化剂和稳定剂的作用下,在负压的条件下开始低真空阶段的预缩聚反应;预缩聚分为第一预缩聚和第二预缩聚两次缩聚;第一预缩聚压力由常压平稳抽至绝对压强24Kpa左右,温度控制在240℃,反应时间为1小时;在第一预缩聚后用规格为100目的滤网进行过滤;滤液继续抽真空,进行第二预缩聚反应,使反应压力降至绝对压强4Kpa,反应温度控制在275℃,反应时间为2分钟;预缩聚后完成三次过滤,从一次过滤到三次过滤,过滤精度依次提高,最终过滤精度为600目;然后继续抽真空,进行高真空阶段的缩聚反应,使反应压强降至绝对压强0.2Kpa,反应温度控制在285℃,反应时间4小时,制得高品质的有色再生聚酯。
制备的有色聚酯特性黏度值为0.7dl/g,熔点225℃,黏度波动值≤±0.025,灰分含量0.10%,B值波动值≤±5,凝集粒子5个/mg。
实施例5
一种链解废聚酯制备有色聚酯的方法该方法包括以下的步骤:
前处理:回收的废聚酯进行前处理和配比调色,于聚酯(PET)瓶片、聚酯(PET)薄膜,清洗后干燥;对于聚酯(PET)纤维制品(服装边角料、窗帘、地毯等):通过热摩擦成型工艺进行致密化处理(温度150~260℃,压力0.1~10MPa,时间5~15min);经过前处理的回收聚酯(PET)纤维由色度的不同进行筛选,按比例进行配比调色处理。
链解反应:将回收的聚酯(PET)经过致密化处理后,以废聚酯:乙二醇的摩尔百分比1:3的比例进入链解反应釜进行链解反应制备含对苯二甲酸乙二醇酯的链解物。其中链解釜中含有占投入废聚酯总量20%质量百分比的对苯二甲酸乙二醇酯及齐聚物,并添加链解催化剂;控制链解反应温度200℃、反应时间2小时,得到含对苯二甲酸乙二醇酯及齐聚物的链解物。链解催化剂:醋酸锌,催化剂含量:0.2%w。
除杂处理:将链解物先进行第一次过滤,除去不可链解的棉、麻等杂质,过滤规格为100目。然后将滤液投入至含有沉淀剂的混合沉淀器中,充分搅拌混合后进行再次过滤,主要过滤出链解液中的氨纶、尼龙、消光剂等组份。沉淀剂如实施例1所示。
缩聚反应:在催化剂和稳定剂的作用下,在负压的条件下开始低真空阶段的预缩聚反应;预缩聚分为第一预缩聚和第二预缩聚两次缩聚;第一预缩聚压力由常压平稳抽至绝对压强24Kpa左右,温度控制在240℃,反应时间为1小时;在第一预缩聚后用规格为100目的滤网进行过滤;滤液继续抽真空,进行第二预缩聚反应,使反应压力降至绝对压强4Kpa,反应温度控制在275℃,反应时间为2分钟;预缩聚后完成三次过滤,从一次过滤到三次过滤,过滤精度依次提高,最终过滤精度为600目;然后继续抽真空,进行高真空阶段的缩聚反应,使反应压强降至绝对压强0.2Kpa,反应温度控制在285℃,反应时间4小时,制得高品质的有色再生聚酯。
制备的有色聚酯特性黏度值为0.69dl/g,熔点223℃,黏度波动值≤±0.02,灰分含量0.12%,B值波动值≤±5,凝集粒子4个/mg。
以上为对本发明实施例的描述,通过对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的。本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施列,而是要符合与本文所公开的原理和新颖点相一致的最宽的范围。
Claims (8)
1.一种废聚酯链解制备有色聚酯的方法,其特征在于,该方法包括以下的步骤:
1)回收的废聚酯进行前处理和配比调色;
2)链解催化剂作用下进行链解反应,所述的链解工艺为母液温度190~210℃,反应时间30分钟-5小时;链解液进行沉淀除杂,多级过滤处理;过滤精度依次提升,初级过滤的精度为50-100目,最终过滤精度为500~800目;
3)除杂后的链解物经补色送至缩聚釜进行预缩聚,最后经终缩聚形成成品;
所述的沉淀除杂用的沉淀剂包括以下的组分:
纳米氧化钙 4-12份
硅藻土 2-10份
纳米氧化铝 5-15份
氢氧化钾 1-6份
碳酸钙 2-10份
羟乙基纤维素钠1-5份
聚丙烯酰胺 2-10份;
除杂方法还包括磁流体吸附除杂,沉淀除杂后继续将滤液投入至磁流体除杂器中,使磁流体与滤液在除杂器中旋转混合,然后断开除杂器的磁座使之变成永恒磁场,10-20分钟后,磁性颗粒向下沉淀分层,将其过滤除去尼龙、氨纶、消光剂和二氧化钛;
所述磁流体采用醇水共热法制备,按Fe3+和Fe2+摩尔比1-3:1比例的Fe2(SO4)3溶液和FeSO4溶液混匀,加热至60-70℃保持恒温,滴加NaOH溶液充分搅拌使混合均匀,调节pH值为10-12,继续搅拌并加入无水乙醇,静置20-30分钟,调节pH值,继续升高温度,迅速搅拌并加入0.4-0.8倍Fe2+用量的表面活性剂油酸钠进行包裹,随后即可看到黑色的磁性颗粒生成。
2.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,废聚酯前处理包括,对于聚酯瓶片、聚酯薄膜,清洗后干燥;对于聚酯纤维制品通过热摩擦成型工艺进行致密化处理,温度150~260℃,压力0.1~10MPa,时间5~15min。
3.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,所述的配比调色处理包括,经过前处理的回收聚酯纤维根据色度的不同进行筛选,按比例进行配比调色处理。
4.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,所述的链解催化剂采用醋酸锌。
5.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,所述的链解反应,按废聚酯:乙二醇的摩尔百分比1:1~6的比例投入链解釜,其中链解釜中含有占投入废聚酯总量10~30%质量百分比的对苯二甲酸乙二醇酯及齐聚物,并添加链解催化剂;控制链解反应温度190~210℃、反应时间30分钟~5小时,得到含对苯二甲酸乙二醇酯及齐聚物的链解物。
6.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,所述的过滤设置为三级,链解后完成一次过滤,经沉淀除杂处理后完成一次过滤,预缩聚后完成三次过滤,从一次过滤到三次过滤,过滤精度依次提高。
7.根据权利要求1所述的一种废聚酯链解制备有色聚酯的方法,其特征在于,所述的预缩聚设置两道,分别为预缩聚一和预缩聚二,预缩聚一的反应温度为230~250℃,真空度5~30KPa,停留时间1~3小时,预缩聚二的反应温度为250~280℃,真空度1~5 KPa,停留时间1~3小时;所述的终缩聚反应温度为275~290℃,真空度0.05~1 KPa,反应时长1~5小时。
8.权利要求1-7任意一项权利要求所述的方法制备得到的有色聚酯熔体纺丝获得的再生聚酯短纤维。
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