Method for preparing catalyst and dihydroxyl-terminated polyether polyol
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A catalyst and polyol technology, applied in the field of polyether polyol synthesis, can solve problems such as irritating odor and abnormal chromaticity of polyether polyol, and achieve suppression of side reactions, simple polymerization method and system, and good molecular weight and molecular weight distribution. control effect
Pending Publication Date: 2022-07-08
QINGDAO UNIV OF SCI & TECH
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These two methods have their own advantages, but most of the crude polyether polyols obtained by polymerization contain metal ions (such as K + , Zn 2+ 、Co 2+ etc.), aldehydes produced by side reactions, low molecular weight polymers, and unreacted oxyalkylenes, etc., make polyether polyols have problems such as abnormal chromaticity or irritating odors, so post-treatment of polyether polyols is required , in addition, the reaction temperature of the above polymerization technique is relatively high 100-150°C
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Embodiment 1～31
[0050] Examples 1-31 Ring-opening polymerization of propylene oxide
[0051] Set in a glove box, weigh the initiator, sodium hydride, phosphorus salt, propylene oxide, and weigh into a 10 mL pressure-resistant bottle vial equipped with a magnetic stirrer that has been flame-dried in advance. Seal the vial and take out the heating reaction. Set -20~45℃ as the reaction temperature, the molar ratio of propylene oxide, initiator, phosphorus salt and sodium is 10000:1:0.1:0.1-100:1:0.01:0.01, and the reaction time is controlled at 0.3~72h. The specific operations of Examples 1 to 31 are as follows, and the key data are arranged in Table 1.
Embodiment 1
[0053] In a 100mL pressure bottle, add H 2 O (0.1 mmol, 1.8 μL, 1 equiv), sodium hydride (10 μmol, 0.24 mg, 0.1 equiv), phosphorus salt (10 μmol, 5.9 mg, 0.1 equiv), followed by propylene oxide (1 mol, 67.6 mL, 10000 equiv) , the reaction mixture was stirred for 48h, the reaction temperature was 0°C, the number-average molecular weight Mn measured by GPC was 390,000 g / mol, and the molecular weight distribution is 1.12.
Embodiment 2
[0055] In a 100mL pressure bottle, add H 2 O (0.1 mmol, 1.8 μL, 1 equiv), sodium hydride (10 μmol, 0.24 mg, 0.1 equiv), phosphorus salt (10 μmol, 5.9 mg, 0.1 equiv), followed by propylene oxide (0.5 mol, 33.8 mL, 5000 equiv) ), the reaction mixture was stirred for 24 h, the reaction temperature was 0 °C, the number-average molecular weight Mn measured by GPC was 189000 g / mol, and the molecular weight distribution is 1.13.
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Abstract
The invention relates to the field of polyether polyol synthesis. Aiming at the problems that most of crude polyether polyol obtained by the existing polymerization reaction contains metal ions, aldehyde generated by side reaction, low-molecular-weight polymer, unreacted oxyalkylene and other substances, the polyether polyol has abnormal chromaticity or easily generates pungent smell, and the reaction temperature is relatively high, the invention provides a preparation method of the polyether polyol. The invention provides a method for preparing a catalyst and dihydroxyl-terminated polyether polyol, which comprises the following steps: mixing onium salt, sodium hydride or potassium hydride and an initiator to obtain a catalytic system, controlling the molar ratio of alkylene oxide to the initiator to phosphorus salt to sodium hydride or potassium hydride to be (100-10000): (1-10): (0.01-1): (0.01-1), controlling the temperature at-20-45 DEG C, and reacting for 0.3-72 hours. Middle molecular weight and controllable molecular weight distribution can be obtained under mild conditions, side reaction of polymerization reaction and the like can be inhibited, and the method is very suitable for industrial production of terminal dihydroxyl polyether polyol.
Description
technical field [0001] The invention relates to the field of polyether polyol synthesis, in particular to a method for preparing a catalyst and a double-hydroxyl-terminated polyether polyol. Background technique [0002] High resilience polyurethane foam has excellent resilience performance, low hysteresis loss performance and high load ratio. Polyether polyol is one of the main raw materials of high resilience polyurethane foam. Usually, high-activity polyether polyols use small molecular polyols as initiators, and are prepared by ring-opening polymerization of propylene oxide (PO) in the presence of a catalyst, and then ring-opening and capping with ethylene oxide (EO). At present, the more mature catalysts are traditional base catalysts (such as KOH) and double metal complex catalysts (DMC). These two methods have their own advantages, but most of the crude polyether polyols obtained by polymerization contain metal ions (such as K + , Zn 2+ , Co 2+ etc.), aldehydes, ...
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