CN107459672A - 一种废pet的脱色回收方法 - Google Patents

一种废pet的脱色回收方法 Download PDF

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CN107459672A
CN107459672A CN201610388203.1A CN201610388203A CN107459672A CN 107459672 A CN107459672 A CN 107459672A CN 201610388203 A CN201610388203 A CN 201610388203A CN 107459672 A CN107459672 A CN 107459672A
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pet
decolouring
ethylene glycol
useless
recovery
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邢士合
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Tianjin Fragrance Plastic Products Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/04Recovery or working-up of waste materials of polymers
    • C08J11/10Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/18Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
    • C08J11/22Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
    • C08J11/24Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D167/00Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
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  • Polymers & Plastics (AREA)
  • Sustainable Development (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

本发明公开了一种废PET的脱色回收方法,其特征在于,包括如下步骤:(1)废PET的碱酸清洗,制得初步PET片粒;(2)废PET的微波醇解,得到初步溶液和杂质;(3)废PET的脱色回收,制得含有染料、油墨的乙二醇溶液和微黄色的透明渣饼;进一步制得透明晶体,干燥封装保存,即得废PET的脱色回收产品。本发明工艺简单,成本低,效率高,整个处理过程不会产生二次污染。回收的PET材料主要应用于环氧‑聚酯粉末涂料、TPA醋酸酯的制备,能够制备出高性能、高纯度的涂料、TPA,经济效果极佳。

Description

一种废PET的脱色回收方法
技术领域
本发明涉及废PET回收利用技术,特别涉及一种废PET的脱色回收方法。
背景技术
废PET主要来源于废旧PET膜。废旧PET膜,特别是印刷复合膜在生活与工业上应用广泛,其含有大量的油墨、染料,回收处理难度极大,成本高,效率低,几乎没有厂家愿意去进行回收处理,成为废弃PET材料回收利用的一大难题。
发明内容
本发明为弥补现有技术的不足,提供一种废PET的脱色回收方法。本发明具体技术方案步骤如下:
(1)废PET的碱酸清洗
将废弃PET膜粉碎成碎片,先后用0.5mol/L的NaOH溶液、0.5mol/L的HCl溶液浸泡清洗,再用水冲洗干净后,干燥,制得初步PET片粒;所述废弃PET膜粉碎成5~10mm5~10mm0.1mm大小的碎片;所述浸泡清洗时间为5h;所述干燥条件为:温度80~90℃,时间24h;
(2)废PET的微波醇解
称取重量份数100的初步PET片粒,在N2保护下,250~260℃加热熔融,然后加入重量份数50的乙二醇(易结晶且易挥发,是较佳选择,其他二元醇也适用,但效果相去甚远)、重量份数0.5的ZnAc2,于微波条件下充分反应;所述微波条件下的反应时间为1~10min;冷却至150~200℃后,将熔融状态的溶液加入空洞为50~100目的过滤器中进行过滤,得到初步溶液和杂质;
(3)废PET的脱色回收
将初步溶液逐渐降温冷却结晶,将液体部分压榨脱除,制得含有染料、油墨的乙二醇溶液和微黄色的透明渣饼;将含有染料、油墨的乙二醇溶液蒸发后得到纯净的乙二醇,再次回收利用。剩下的染料、油墨也回收利用,可作为油墨厂的初始原料;将微黄色的透明渣饼再熔融,加入乙二醇,冷却结晶并蒸发乙二醇,获得透明晶体,将该透明晶体真空干燥,封装保存,即得废PET的脱色回收产品;
(4)醇解产物的酯化
将100质量分数的醇解产物先加热熔融,然后加入适量的多元酸或酸酐,以及1质量分数的酯化催化剂Sb2O3,充分混合后,在微波条件下反应,反应完成后,得到粉末涂料用聚酯;所述醇解产物加热熔融温度为200℃。
本发明的优点在于:本发明解决了废弃PET膜中油墨含量过高难以回收处理的问题,既回收了PET又回收了油墨,一举两得。而且本发明工艺简单,成本低,效率高,针对性强,整个处理过程不会产生二次污染,而且乙二醇也可以不断地回收再用,非常的科学合理。采用本发明方法回收的PET材料主要应用于环氧-聚酯粉末涂料、TPA醋酸酯的制备,能够制备出高性能、高纯度的涂料、TPA,经济效果极佳。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步描述,以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
本发明提供的一种废PET的脱色回收方法包括以下步骤:
实施例1
(1)废PET的碱酸清洗
将废弃PET膜粉碎成碎片,先后用0.5mol/L的NaOH溶液、0.5mol/L的HCl溶液浸泡清洗,再用水冲洗干净后,干燥,制得初步PET片粒;所述废弃PET膜粉碎成5~10mm5~10mm0.1mm大小的碎片;所述浸泡清洗时间为5h;所述干燥条件为:温度80~90℃,时间24h;
(2)废PET的微波醇解
称取重量份数100的初步PET片粒,在N2保护下,250~260℃加热熔融,然后加入重量份数50的乙二醇(易结晶且易挥发,是较佳选择,其他二元醇也适用,但效果相去甚远)、重量份数0.5的ZnAc2,于微波条件下充分反应;所述微波条件下的反应时间为1~10min;冷却至150~200℃后,将熔融状态的溶液加入空洞为50~100目的过滤器中进行过滤,得到初步溶液和杂质;
(3)废PET的脱色回收
将初步溶液逐渐降温冷却结晶,将液体部分压榨脱除,制得含有染料、油墨的乙二醇溶液和微黄色的透明渣饼;将含有染料、油墨的乙二醇溶液蒸发后得到纯净的乙二醇,再次回收利用。剩下的染料、油墨也回收利用,可作为油墨厂的初始原料;将微黄色的透明渣饼再熔融,加入乙二醇,冷却结晶并蒸发乙二醇,获得透明晶体,将该透明晶体真空干燥,封装保存,即得废PET的脱色回收产品;
(4)醇解产物的酯化
将100质量分数的醇解产物先加热熔融,然后加入适量的多元酸或酸酐,以及1质量分数的酯化催化剂Sb2O3,充分混合后,在微波条件下反应,反应完成后,得到粉末涂料用聚酯;所述醇解产物加热熔融温度为200℃。
本发明的优点在于:本发明解决了废弃PET膜中油墨含量过高难以回收处理的问题,既回收了PET又回收了油墨,一举两得。本发明工艺简单,成本低,效率高,针对性强,整个处理过程不会产生二次污染,而且乙二醇也可以不断地回收再用,非常的科学合理。采用本发明方法回收的PET材料主要应用于环氧-聚酯粉末涂料、TPA醋酸酯的制备,能够制备出高性能、高纯度的涂料、TPA,经济效果极佳。
以上对本发明的一个实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。

Claims (1)

1.一种废PET的脱色回收方法,其特征在于,本发明具体技术方案步骤如下:
(1)废PET的碱酸清洗
将废弃PET膜粉碎成碎片,先后用0.5mol/L的NaOH溶液、0.5mol/L的HCl溶液浸泡清洗,再用水冲洗干净后,干燥,制得初步PET片粒;所述废弃PET膜粉碎成5~10mm5~10mm0.1mm大小的碎片;所述浸泡清洗时间为5h;所述干燥条件为:温度80~90℃,时间24h;
(2)废PET的微波醇解
称取重量份数100的初步PET片粒,在N2保护下,250~260℃加热熔融,然后加入重量份数50的乙二醇(易结晶且易挥发,是较佳选择,其他二元醇也适用,但效果相去甚远)、重量份数0.5的ZnAc2,于微波条件下充分反应;所述微波条件下的反应时间为1~10min;冷却至150~200℃后,将熔融状态的溶液加入空洞为50~100目的过滤器中进行过滤,得到初步溶液和杂质;
(3)废PET的脱色回收
将初步溶液逐渐降温冷却结晶,将液体部分压榨脱除,制得含有染料、油墨的乙二醇溶液和微黄色的透明渣饼;将含有染料、油墨的乙二醇溶液蒸发后得到纯净的乙二醇,再次回收利用。剩下的染料、油墨也回收利用,可作为油墨厂的初始原料;将微黄色的透明渣饼再熔融,加入乙二醇,冷却结晶并蒸发乙二醇,获得透明晶体,将该透明晶体真空干燥,封装保存,即得废PET的脱色回收产品;
(4)醇解产物的酯化
将100质量分数的醇解产物先加热熔融,然后加入适量的多元酸或酸酐,以及1质量分数的酯化催化剂Sb2O3,充分混合后,在微波条件下反应,反应完成后,得到粉末涂料用聚酯;所述醇解产物加热熔融温度为200℃。
CN201610388203.1A 2016-06-06 2016-06-06 一种废pet的脱色回收方法 Pending CN107459672A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110172140A (zh) * 2019-05-19 2019-08-27 福建师范大学 一种用微波水解废弃涤纶纺织物制备不饱和聚酯树脂的方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110172140A (zh) * 2019-05-19 2019-08-27 福建师范大学 一种用微波水解废弃涤纶纺织物制备不饱和聚酯树脂的方法
CN110172140B (zh) * 2019-05-19 2023-11-24 福建师范大学 一种用微波水解废弃涤纶纺织物制备不饱和聚酯树脂的方法

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