CN115594581A - 一种化学法回收废旧纺织品制备再生dmt的方法及其在制备阻燃聚酯切片中的应用 - Google Patents
一种化学法回收废旧纺织品制备再生dmt的方法及其在制备阻燃聚酯切片中的应用 Download PDFInfo
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- CN115594581A CN115594581A CN202211343832.4A CN202211343832A CN115594581A CN 115594581 A CN115594581 A CN 115594581A CN 202211343832 A CN202211343832 A CN 202211343832A CN 115594581 A CN115594581 A CN 115594581A
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Abstract
本发明公开了一种化学法回收废旧纺织品制备再生DMT的方法及其在制备阻燃聚酯切片中的应用。利用废旧聚酯纺织品为原料,采用乙二醇解聚‑甲醇酯交换技术制备再生DMT,并在此过程中采用物理‑化学复合发泡技术制备了多孔、高堆积密度及大比表面积的密实化废旧聚酯原料,提高了废旧纺织品的堆积密度,增大了醇解反应效率及产物收率;采用原位自组装策略制备了高催化活性、优异顺磁性以及易分离回收的非均相醇解催化剂SDS‑BTA‑LDH,克服了传统醇解催化剂易溶于解聚液而导致再生单体提纯困难以及解聚液难处理的问题。利用再生DMT为原料通过共聚合方法合成了阻燃性能优异的共聚酯切片,实现了废旧聚酯纺织品的高值化回收利用。
Description
技术领域
本发明涉及DMT的制备及应用技术领域,特别是涉及一种化学法回收废旧纺织品制备再生DMT的方法及其在制备阻燃聚酯切片中的应用。
背景技术
随着我国聚酯纤维用量的增加,废旧聚酯纺织品的积累量逐年上升,由于聚酯材料难以自然降解,造成了严重的环境污染和资源浪费的问题。化学法回收废旧聚酯不仅原料适用性广,且再生产品具有媲美原生石油基材料的潜质,近年来受到了广泛的关注。其中,乙二醇醇解法反应条件温和、工艺流程简单,利用再生单体BHET(对苯二甲酸乙二醇酯)与甲醇进行酯交换反应能够制备出易于提纯的再生DMT(对苯二甲酸二甲酯),是工业化制备高品质再生聚酯材料最具发展前景的工艺路线。
目前,在工业生产中利用废旧聚酯纺织品的醇解-酯交换技术制备下游再生聚酯材料存在以下关键技术难题:(1)未经处理的废旧纺织品体态蓬松、堆积密度较小,不仅输送效率过低、极易引起管道堵塞,并且液态解聚剂难以与原料有效接触,导致反应转化率降低、产物收率下降。(2)废旧聚酯醇解过程大多使用可溶性金属盐类催化剂,不仅增加了再生单体的纯化难度,还为解聚液的后处理造成极大的阻碍。(3)再生DMT现有下游产品的开发大多局限于普通聚酯及其纤维材料,对于功能化、高值化再生聚酯材料的开发却鲜有报道,醇解-酯交换法回收废旧聚酯纺织品未能发挥真正的潜力。
发明内容
本发明的目的在于克服上述现有技术的不足,提供一种化学法回收废旧纺织品制备再生DMT的方法及其在制备阻燃聚酯切片中的应用。利用废旧聚酯纺织品为原料,创新性地使用物理、化学复合发泡技术制备了具有多孔、高堆积密度及大比表面积的密实化废旧聚酯原料,采用原位组装的策略制得具有高催化活性、易于分离回收的磁性醇解催化剂SDS-BTA-LDH,进而制得高纯度再生DMT;并以高纯度再生DMT为原料,采用共聚合方法合成了高极限氧指数、阻燃性能优异的本征型共聚酯切片,有效解决了醇解-酯交换工艺在工业生产中存在的技术难题,实现了废旧聚酯纺织品的高值化回收利用。
为了实现上述目的,本发明采用如下技术方案:
本发明的有益效果是:
(1)创新性地采用物理-化学复合发泡技术,利用废旧聚酯纺织品制备了具有多孔、高堆积密度及大比表面积的密实化废旧聚酯原料,有效提高了生产中原料的输送效率,增大了原料的密实化程度,增加了废旧聚酯原料与解聚液的接触效果,提升了醇解效率。
(2)采用原位自组装策略,制备了具有高催化活性、优异顺磁性以及容易分离回收的非均相醇解催化剂SDS-BTA-LDH,有效克服了传统醇解催化剂易溶于解聚液而导致再生单体提纯困难以及解聚液污染的问题。
(3)首次采用化学法回收废旧聚酯纺织品制得的再生DMT为原料,通过共聚合的方式制备了高极限氧指数、阻燃性能优异的功能型再生聚酯,有效实现了废旧聚酯纺织品的高值化回收利用,拓展了再生DMT下游应用领域。
附图说明
图1为实施例1中密实化废旧聚酯原料的形貌图;
图2为实施例1中密实化废旧聚酯原料的刨面图;
图3为实施例1中自组装型SDS-BTA-LDH的形貌图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步描述:
实施例1
(1)密实化废旧聚酯原料的制备:
将洗净的废旧聚酯纺织品破碎后送入泡料机,并依次加入占废旧聚酯纺织品质量0.5%的正戊烷,占废旧聚酯纺织品质量0.65%的偶氮二甲酰胺,开启搅拌开关后将泡料机转速缓慢升至1500r/min,待废旧聚酯原料温度升高至210℃时缓慢降低搅拌转速至200r/min,开启喷淋水开关使原料降温冷却至50℃,随后将成型的粒料通过螺杆挤出机送入干燥箱,在110℃的温度下烘干8h,即可得到密实化废旧聚酯原料。
(2)磁性自组装型醇解催化剂SDS-BTA-LDH的制备
以100质量份的二价金属盐醋酸锌为基准,在5000质量份的蒸馏水中加入醋酸锌(100质量份)、氯化铁(40质量份)、十二烷基苯磺酸钠(20质量份)、2-(2-羟基-5-甲基苯基)苯并三氮唑(30质量份)、尿素(80质量份)。在80℃、PH=8的条件下连续搅拌进行水热反应15h,反应结束后过滤得到产物,并使用大量蒸馏水洗涤,最后通过真空干燥12h后得到自组装型改性剂SDS-BTA-LDH。
(3)高纯度再生DMT的制备:
将密实化废旧聚酯、乙二醇、SDS-BTA-LDH按照1:2:0.004的质量比投入醇解釜,缓慢搅拌升温至195℃,解聚2h,反应结束后从釜顶抽出多余的乙二醇,醇解产物经过滤装置后送入酯交换反应釜,催化剂SDS-BTA-LDH通过磁性过滤器收集,随后将醇解产物、甲醇、NaOH按照1:3:0.003的质量比送入酯交换反应釜,反应进行2h后对酯交换产物进行过滤,并在45℃下采用甲醇重结晶法对酯交换产物进行3次提纯,经干燥后得到纯度大于99%的再生DMT。
(4)再生阻燃聚酯的合成:
将3质量份阻燃改性剂2-羧乙基苯基次膦酸(CEPPA)添加至6质量份的乙二醇溶液中,在缓慢搅拌条件下加热混合溶液至65℃,待CEPPA完全溶解后溶液变至澄清即得到阻燃改性剂;将100质量份再生DMT、94质量份乙二醇和1.4质量份醋酸锰依次送入酯交换反应釜,缓慢提高釜温至200℃进行酯交换反应,,反应过程中持续蒸出甲醇副产物;随后将阻燃改性剂、0.8质量份的酯化催化剂氧化锡以及0.09质量份的稳定剂磷酸三苯酯、0.12质量份的抗氧剂烷基化多酚、1.23质量份的消光剂二氧化钛添加至反应釜中,缓慢升高釜温,将混合液在235℃温度条件下保持30min,反应结束后抽出多余的乙二醇和水得到再生BHET和CEPPA-EG的混合酯化物;将混合酯化物送入共聚合反应釜中,升温至250℃,保持低真空进行预缩聚反应以初步提升其分子量;随后进入终缩聚阶段,控制温度260℃、真空度20pa,反应时间1.5h,然后通过熔体泵出料、过滤、切粒、包装,最终得到的再生阻燃聚酯切片。
实施例2
(1)密实化废旧聚酯原料的制备:
将洗净的废旧聚酯纺织品破碎后送入泡料机,并依次加入占废旧聚酯纺织品质量0.5%的环己烷,占废旧聚酯纺织品质量0.65%的偶氮二甲酸二异丙酯,开启搅拌开关后将泡料机转速缓慢升至1500r/min,待废旧聚酯原料温度升高至200℃时缓慢降低搅拌转速至200r/min,开启喷淋水开关使原料降温冷却至50℃,随后将成型的粒料通过螺杆挤出机送入干燥箱,在110℃的温度下烘干8h,即可得到密实化废旧聚酯原料。
(2)磁性自组装型醇解催化剂SDS-BTA-LDH的制备
以100质量份的二价金属盐为基准,在5000质量份的蒸馏水中加入醋酸锰(100质量份)、硫酸铁(40质量份)、十二烷基苯磺酸钠(20质量份)、2-(2-羟基-5-甲基苯基)苯并三氮唑(30质量份)、尿素(80质量份)。在80℃、PH=8的条件下连续搅拌进行水热反应15h,反应结束后过滤得到产物,并使用大量蒸馏水洗涤,最后通过真空干燥12h后得到自组装型改性剂SDS-BTA-LDH。
(3)高纯度再生DMT的制备:
将密实化废旧聚酯、乙二醇、SDS-BTA-LDH按照1:2:0.006的质量比投入醇解釜,缓慢搅拌升温至195℃,解聚2h,反应结束后从釜顶抽出多余的乙二醇,醇解产物经过滤装置后送入酯交换反应釜,催化剂SDS-BTA-LDH通过磁性过滤器收集,随后将醇解产物、甲醇、NaOH按照1:3:0.003的质量比送入酯交换反应釜,反应进行2h后对酯交换产物进行过滤,并在45℃下采用甲醇重结晶法对酯交换产物进行3次提纯,经干燥后得到纯度大于99%的再生DMT。
(4)阻燃再生聚酯的合成:
将3质量份阻燃改性剂2-羧乙基苯基次膦酸(CEPPA)添加至6质量份的乙二醇溶液中,在缓慢搅拌条件下加热混合溶液至70℃,待CEPPA完全溶解后溶液变至澄清即得到阻燃改性剂;将100质量份再生DMT、94质量份乙二醇和1.4质量份醋酸钠依次送入酯交换反应釜,缓慢提高釜温至205℃进行酯交换反应,,反应过程中持续蒸出甲醇副产物;随后将阻燃改性剂、0.8质量份的酯化催化剂氧化锡以及0.09质量份的稳定剂磷酸三甲酯、0.12质量份的抗氧剂烷基单酚、1.23质量份的消光剂二氧化钛添加至反应釜中,缓慢升高釜温,将混合液在240℃温度条件下保持40min,反应结束后抽出多余的乙二醇和水得到再生BHET和CEPPA-EG的混合酯化物;将混合酯化物送入共聚合反应釜中,升温至255℃,保持低真空进行预缩聚反应以初步提升其分子量;随后进入终缩聚阶段,控制温度265℃、真空度20pa,反应时间2h,然后通过熔体泵出料、过滤、切粒、包装,最终得到的再生阻燃聚酯切片。
实施例3
(1)密实化废旧聚酯原料的制备:
将洗净的废旧聚酯纺织品破碎后送入泡料机,并依次加入占废旧聚酯纺织品质量0.5%的二氯甲烷,占废旧聚酯纺织品质量0.65%的偶氮二异丁腈,开启搅拌开关后将泡料机转速缓慢升至1500r/min,待废旧聚酯原料温度升高至220℃时缓慢降低搅拌转速至200r/min,开启喷淋水开关使原料降温冷却至50℃,随后将成型的粒料通过螺杆挤出机送入干燥箱,在110℃的温度下烘干8h即可得到具有大比表面积、高空隙率的密实化废旧聚酯原料。
(2)磁性自组装型醇解催化剂SDS-BTA-LDH的制备
以100质量份的二价金属盐为基准,在5000质量份的蒸馏水中加入醋酸钴(100质量份)、硫酸铁(40质量份)、十二烷基苯磺酸钠(20质量份)、2-(2-羟基-5-甲基苯基)苯并三氮唑(30质量份)、尿素(80质量份)。在80℃、PH=8的条件下连续搅拌进行水热反应15h,反应结束后过滤得到产物,并使用大量蒸馏水洗涤,最后通过真空干燥12h后得到自组装型改性剂SDS-BTA-LDH。
(3)高纯度再生DMT的制备:
将密实化废旧聚酯、乙二醇、SDS-BTA-LDH按照1:2:0.008的质量比投入醇解釜,缓慢搅拌升温至195℃,解聚2h,反应结束后从釜顶抽出多余的乙二醇,醇解产物经过滤装置后送入酯交换反应釜,催化剂SDS-BTA-LDH通过磁性过滤器收集,随后将醇解产物、甲醇、NaOH按照1:3:0.003的质量比送入酯交换反应釜,反应进行2h后对酯交换产物进行过滤,并在45℃下采用甲醇重结晶法对酯交换产物进行3次提纯,经干燥后得到纯度大于99%的再生DMT。
(4)阻燃再生聚酯的合成:
将3质量份阻燃改性剂2-羧乙基苯基次膦酸(CEPPA)添加至6质量份的乙二醇溶液中,在缓慢搅拌条件下加热混合溶液至75℃,待CEPPA完全溶解后溶液变至澄清即得到阻燃改性剂;将100质量份再生DMT、94质量份乙二醇和1.4质量份醋酸钾依次送入酯交换反应釜,缓慢提高釜温至210℃进行酯交换反应,,反应过程中持续蒸出甲醇副产物;随后将阻燃改性剂、0.8质量份的酯化催化剂三氧化二锑以及0.09质量份的稳定剂磷酸三甲酯、0.12质量份的抗氧剂烷基单酚、1.23质量份的消光剂二氧化钛添加至反应釜中,缓慢升高釜温,将混合液在245℃温度条件下保持45min,反应结束后抽出多余的乙二醇和水得到再生BHET和CEPPA-EG的混合酯化物;将混合酯化物送入共聚合反应釜中,升温至260℃,保持低真空进行预缩聚反应以初步提升其分子量;随后进入终缩聚阶段,控制温度275℃、真空度20pa,反应时间2.5h,然后通过熔体泵出料、过滤、切粒、包装;最终得到的再生阻燃聚酯。
实施例4
(1)密实化废旧聚酯原料的制备:
将废旧聚酯纺织品破碎后送入泡料机,并依次加入占废旧聚酯纺织品质量0.5%的二氯乙烷,占废旧聚酯纺织品质量0.65%的偶氮氨基苯,开启搅拌开关后将泡料机转速缓慢升至1500r/min,待废旧聚酯原料温度升高至220℃时缓慢降低搅拌转速至200r/min,开启喷淋水开关使原料降温冷却至50℃,随后将成型的粒料通过螺杆挤出机送入干燥箱,在110℃的温度下烘干8h即可得到密实化废旧聚酯原料。
(2)磁性自组装型醇解催化剂SDS-BTA-LDH的制备
以100质量份的二价金属盐为基准,在5000质量份的蒸馏水中加入醋酸锌(100质量份)、氯化铁(40质量份)、十二烷基苯磺酸钠(20质量份)、2-(2-羟基-5-甲基苯基)苯并三氮唑(30质量份)、尿素(80质量份)。在80℃、PH=8的条件下连续搅拌进行水热反应15h,反应结束后过滤得到产物,并使用大量蒸馏水洗涤,最后通过真空干燥12h后得到自组装型改性剂SDS-BTA-LDH。
(3)高纯度再生DMT的制备:
将密实化废旧聚酯、乙二醇、醋酸锌按照1:2:0.01的质量比投入醇解釜,缓慢搅拌升温至195℃,解聚2h,反应结束后从釜顶抽出多余的乙二醇,醇解产物经过滤装置后送入酯交换反应釜,催化剂SDS-BTA-LDH通过磁性过滤器收集,随后将醇解产物、甲醇、NaOH按照1:3:0.003的质量比送入酯交换反应釜,反应进行2h后对酯交换产物进行过滤,并在45℃下采用甲醇重结晶法对酯交换产物进行3次提纯,经干燥后得到纯度大于99%的再生DMT。
(4)阻燃再生聚酯的合成:
将5质量份阻燃改性剂2-羧乙基苯基次膦酸(CEPPA)添加至6质量份的乙二醇溶液中,在缓慢搅拌条件下加热混合溶液至85℃,待CEPPA完全溶解后溶液变至澄清即得到阻燃改性剂;将100质量份再生DMT、94质量份乙二醇和1.4质量份醋酸铵依次送入酯交换反应釜,缓慢提高釜温至220℃进行酯交换反应,反应过程中持续蒸出甲醇副产物;随后将阻燃改性剂、0.8质量份的酯化催化剂氧化亚锡以及0.09质量份的稳定剂亚磷酸、0.12质量份的抗氧剂硫代双酚、1.23质量份的消光剂二氧化钛添加至反应釜中,缓慢升高釜温,将混合液在245℃温度条件下保持50min,反应结束后抽出多余的乙二醇和水得到再生BHET和CEPPA-EG的混合酯化物;将混合酯化物送入共聚合反应釜中,升温至260℃,保持低真空进行预缩聚反应以初步提升其分子量;随后进入终缩聚阶段,控制温度275℃、真空度20pa,反应时间2.5h,然后通过熔体泵出料、过滤、切粒、包装;最终得到的再生阻燃聚酯。
对上述实施例1-4制备产品进行测试,测试结果如图1、2及表1、2所示。
由图1、2可知,本发明制备的密实化废旧聚酯原料表面呈明显粗糙、高低不平的不规则型态,通过观察原料刨面形貌图可以看出,经过物理-化学复合发泡的原料内部具有丰富的空隙结构。
由图3可知,通过原位组装的策略成功合成了具有六方片状形貌的SDS-BTA-LDH。
由表1可知,相较于采用单一发泡技术或未采用发泡技术得到的密实化原料,物理协同化学发泡技术制备的废旧原料在相同的反应条件下,具有更快的解聚效率以及更高的BHET及DMT的收率,这归因于具有大比表面积及丰富空隙的废弃聚酯原料在反应过程中能够充分地和乙二醇进行接触,从而实现更高的解聚率以及产物的收率。
表1
由表2可知,利用废旧聚酯聚酯纺织品为原料制备的再生DMT能够成成功合成极限氧指数较高、垂直燃烧性能优异的本征型阻燃再生聚酯切片;在合成过程中,通过提高酯化反应的温度、增加酯交换以及酯化反应的时间能够有效提高阻燃聚酯切片的极限氧指数以及垂直燃烧性能;随着阻燃剂CEPPA添加量的上升,聚酯缩聚时间以及缩聚温度也随之上升,聚酯的缩聚过程逐渐变得困难,聚酯大分子链上引入阻燃单体后,增加了聚合反应难度,阻燃聚酯侧链上苯环的出现,增大了分子链的间距,导致聚酯链段本身的高对称性被破坏,最终产生缩聚反应时间的增加,聚酯的熔点下降;随着聚酯阻燃性能的上升,切片二甘醇的含量呈现出先增加后降低的趋势,这是由于这是因为阻燃剂CEPPA酯化时与一部分EG发生了反应,残留的EG较少,聚合反应时副反应变少,但反应温度过高时乙二醇发生副反应增多,二甘醇的含量上升;此外,随着CEPPA含量的增大,切片逐渐出现了发灰的现象,由此可见加入CEPPA后会对聚酯的色值产生影响。
表2
(1)极限氧指数测试方法为:
据《塑料燃烧性能试验方法氧指数法》(GB/T2406-93),采用平板硫化仪对三种阻燃聚酯切片进行加热融化压片,将其放置在临界氧指数分析仪上,调整氧浓度后进行燃烧测试,多次实验减少误差后,得到试样的极限氧指数。
(2)垂直燃烧性能分析方法为:
根据《阻燃性能实验方法-垂直燃烧法》(GB2409-84),采用微型注塑机将两组阻燃聚酯压制成样条,样条尺寸长100mm,宽6.5mm,厚3mm,将样条固定在离底座30.0cm的位置,底座处放置0.5cm厚的脱脂棉。用火源连续作用于样条下方10s,等待样条熄灭后再作用10s,记录下实验现象及数据后与垂直燃烧级别参考标准对照。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,包括以下步骤:
(1)密实化废旧聚酯原料的制备:
将废旧聚酯纺织品破碎后送入泡料机,加入物理发泡剂及化学发泡剂,将泡料机转速缓慢升至1500r/min,待废旧聚酯原料温度升高至200-220℃时缓慢降低搅拌转速,开启喷淋使原料降温冷却,随后将成型的粒料通过螺杆挤出机送入干燥箱中进行干燥,即可得到具有大比表面积、高空隙率的密实化废旧聚酯原料;
(2)磁性自组装型醇解催化剂SDS-BTA-LDH的制备:
将定量的可溶性二价、三价金属盐溶液缓慢加入到十二烷基硫酸钠和2-(2-羟基-5-甲基苯基)苯并三氮唑的混合溶液中,在混合溶液中加入适量的尿素溶液,在连续搅拌的条件下进行水热反应,反应结束后过滤得到产物,并使用大量蒸馏水洗涤,最后通过真空干燥得到磁性自组装型醇解催化剂SDS-BTA-LDH;
(3)高纯度再生DMT的制备:
将密实化废旧聚酯原料、乙二醇、SDS-BTA-LDH按照1:2:0.004-0.01的质量比投入醇解釜,缓慢搅拌升温至195℃进行解聚;反应结束后从釜顶抽出多余的乙二醇,醇解产物经过滤装置后送入酯交换反应釜,催化剂SDS-BTA-LDH通过磁性过滤器收集,随后将醇解产物、甲醇、NaOH按照1:3:0.003的质量比送入酯交换反应釜中进行反应,反应后对酯交换产物进行过滤,并在45℃下采用甲醇重结晶法对酯交换产物进行提纯,经干燥后得到纯度大于99%的再生DMT。
2.如权利要求1所述一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,步骤(1)中,所述物理发泡剂为正戊烷、环己烷、正庚烷、二氯甲烷、二氯乙烷、三氯甲烷中的一种;化学发泡剂为偶氮二甲酰胺、偶氮二异丁腈、偶氮二甲酸二异丙酯、偶氮氨基苯中的一种;所加物理发泡剂为废旧聚酯纺织品质量的0.5%,所加化学发泡剂为废旧聚酯纺织品质量的0.65%。
3.如权利要求1所述一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,步骤(1)中,喷淋降温冷却至50℃;干燥温度为110℃,干燥时间为8h。
4.如权利要求1所述一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,步骤(2)中,所述可溶性二价金属盐为醋酸锌、醋酸锰、醋酸钴中的一种;所述可溶性三价金属盐为氯化铁、硫酸铁、硝酸铁中的一种。
5.如权利要求1所述一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,步骤(2)中,在SDS-BTA-LDH的制备过程中,以100质量份的二价金属盐为基准,其余各原料的投料量为:三价金属盐40质量份、十二烷基苯磺酸钠20质量份、2-(2-羟基-5-甲基苯基)苯并三氮唑30质量份、尿素80质量份;所述水热反应的温度为80℃,时间为15h,反应体系的pH为8。
6.如权利要求1所述一种化学法回收废旧纺织品制备再生DMT的方法,其特征在于,步骤(3)中,解聚时间为2h;酯交换反应时间为2h;提纯次数为3次。
7.一种根据权利要求1-6中任意一项所述方法制备的再生DMT在制备阻燃聚酯切片中的应用,其特征在于,将阻燃改性剂2-羧乙基苯基次膦酸添加至乙二醇溶液中,在缓慢搅拌条件下加热混合溶液至65-85℃,待CEPPA完全溶解后溶液变至澄清即得到阻燃改性剂;将再生DMT、乙二醇和酯交换催化剂依次送入酯交换反应釜,缓慢提高釜温至200-220℃进行酯交换反应,反应过程中持续蒸出甲醇副产物;随后将阻燃改性剂、酯化催化剂以及定量的稳定剂、抗氧剂、消光剂添加至反应釜中,缓慢升高釜温进行酯化反应,将混合液在235-245℃温度条件下保持30-50min,反应结束后抽出多余的乙二醇和水得到再生BHET和CEPPA-EG的混合酯化物;将混合酯化物送入共聚合反应釜中,升温至250-260℃,保持低真空进行预缩聚反应以初步提升其分子量;随后进入终缩聚阶段,控制温度260-275℃、真空度20pa,反应时间1.5-2.5h,然后通过熔体泵出料、过滤、切粒、包装,最终得到再生阻燃聚酯切片。
8.如权利要求7所述一种再生DMT在制备阻燃聚酯切片中的应用,其特征在于,阻燃聚酯切片合成过程中,2-羧乙基苯基次膦酸、制备阻燃改性剂时所用乙二醇、再生DMT、酯交换反应中所用乙二醇、酯交换催化剂、酯化催化剂、稳定剂、抗氧剂、消光剂的质量比为3-5:6:100:94:1.4:0.8:0.09:0.12:1.23;制备阻燃改性剂时,2-羧乙基苯基次膦酸与乙二醇的质量为3:6。
9.如权利要求7所述一种再生DMT在制备阻燃聚酯切片中的应用,其特征在于,所述酯交换催化剂为醋酸锰、醋酸钠、醋酸铵、醋酸钾中的一种;酯化催化剂为氧化锌、氧化锡、氧化亚锡和三氧化二锑中的一种;稳定剂为磷酸三甲酯、磷酸三苯酯、亚磷酸中的一种;抗氧剂为烷基单酚、烷基化多酚、硫代双酚中的一种;消光剂为二氧化钛。
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