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PETG Pellets: Dimethyl Terephthalate with Ethylene Glycol and CHDM
PETG is PET in which part of the ethylene glycol is replaced by CHDM, which keeps the plastic clear and amorphous. Eastman's patent US 7,026,027 describes PETG 6763 as terephthalate with about 69 mol % ethylene glycol and 31 mol % CHDM, but gives no recipe for it. This blueprint is our own combination: that composition, made by the same patent's pilot-plant process (Example 12, written for a CHDM/neopentyl glycol copolyester), with ethylene glycol in place of neopentyl glycol as in Kibler's 1959 Eastman patent. The charge weights are our arithmetic.
The picture: our diagram.
高级
About 5 hours
说明
1
1
Charge the reactor
Charge the reactor
Our charge for 31 mol % CHDM: 10.669 kg dimethyl terephthalate (54.9 mol, as in the patent's example), 2.456 kg CHDM (31 % of those moles) and 4.058 kg ethylene glycol, so the glycols total 1.5 times the ester moles as in the example. Add 53.4 g of catalyst solution (15 g titanium isopropoxide in 250 ml n-butanol). The patent's reactor held 18 gallons and had spiral agitators and a distillation column.
此步骤所需材料:
对苯二甲酸二甲酯10.669 公斤
1,4-环己烷二甲醇2.456 公斤
乙二醇4.058 公斤所需工具:
异丙醇钛
正丁醇
等臂天平
夹套聚合反应釜
分馏蒸馏器
化学防溅护目镜2
2
Ester interchange at 200 °C
Ester interchange at 200 °C
Stir (forward 50 minutes, then reverse 10), heat to 200 °C and hold 2 hours. Methanol distils off through the column.
所需工具:
夹套聚合反应釜
分馏蒸馏器
带读数的热电偶3
3
260 °C, then 280 °C
260 °C, then 280 °C
Raise to 260 °C for 30 minutes and weigh the distillate, then raise to 280 °C and weigh it again. The surplus ethylene glycol is driven off; Kibler found the CHDM stays in the polymer.
所需工具:
夹套聚合反应釜
带读数的热电偶
等臂天平4
4
Polymerise under vacuum
Polymerise under vacuum
Switch the agitator direction every 6 minutes and pull vacuum at 13 Torr a minute down to 0.5 Torr. Hold full vacuum for 45 minutes at 25 rpm.
所需工具:
夹套聚合反应釜
真空泵
真空表
冷阱5
5
Extrude and chop into pellets
Extrude and chop into pellets
Let nitrogen in, extrude the polymer at once and chop it into pellets. Check the composition: in the patent's example the polymer kept slightly less CHDM than was charged (38.1 % for 40.7 %).
所需工具:
氮气瓶
造粒机
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