Polyester compound for preparing olefine polymerizing catalyst
A technology of ester compounds and compounds, applied in the field of new compounds, can solve the problems of narrow molecular weight distribution of polypropylene
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Embodiment 1
[0252] 4. The isotacticity of the polymer is determined by the heptane extraction method (heptane boiling extraction for 6 hours). Embodiment 1 9, the synthesis of 9-two (benzyl carboxymethyl) fluorene
[0253] (1) Synthesis of 9,9-dimethylolfluorene (see CN1141285A for its preparation method) 9g (0.3mol) paraformaldehyde (vacuum dehydration 8h) by adding 60ml dimethyl sulfoxide (DMSO, using CaH 2 Remove water) and the sodium ethylate solution after the reaction of 0.4gNa and 8ml absolute ethanol, and ice will be cooled. Under stirring, 100 ml of DMSO solution containing 16.6 g of fluorene (0.1 mol, dehydrated in vacuum for 8 h) was added within 30 seconds, and reacted for 10 min.
[0254] Add hydrochloric acid to terminate the reaction, and make the solution neutral, pour it into 300ml saturated brine, extract with ethyl acetate, separate the organic phase, wash twice with saturated brine, and dry over anhydrous sodium sulfate. The solvent was removed, and toluene was recry...
Embodiment 2
[0264] 7.25~7.75 (m, 18H, aromatic ring hydrogen) Example 2. Synthesis of 2-isopropyl-2-isopentyl-1,3-dibenzylcarboxypropane
[0265] (1) Synthesis of 2-isopropyl-5-methyl-2-hexenal (see CN1036846C for its preparation method)
[0266] 207g of isovaleraldehyde and 26ml of OH - Form Amberlite IRA910 resin (manufactured by Rohm & Hass) was heated to reflux. Remove the generated water with a water separator, stop the reaction after collecting about 26ml of water, and filter out the resin. Distill under reduced pressure and collect fractions at 85-90°C / 20mmHg.
[0267] (2) Synthesis of 2-isopropyl-5-methylhexanal
[0268] Add 70ml of ethanol, 1ml of saturated NaHCO to 10g of 2-isopropyl-5-methyl-2-hexenal 3 solution and 0.25 g of 10% Pd on carbon support. Access to N 2 , then pass into H 2 , means filled with graduated H 2 connected to the burette. The reaction was stirred at normal temperature and pressure until H 2 The absorption reaches the calculated value. Filter an...
Embodiment 3
[0282] 7.38~8.02 (m, 10H, aromatic ring hydrogen) embodiment 3.2-isopropyl-2-isopentyl-1,3-dipropylene carboxypropane synthesis
[0283] Add 7.5ml of acrylic acid (0.11mol) and 30ml of toluene to 9.4g of 2-isopropyl-2-isoamyl-1,3-propanediol (0.05mol) prepared by the method of Example 2. After stirring evenly, add 0.2ml concentrated sulfuric acid. Heat to reflux for 7h, and use a water separator to remove the water generated by the reaction during the reaction.
[0284] Cool to 70°C, neutralize to alkaline with saturated sodium carbonate solution, extract with ethyl acetate, wash the organic phase with saturated brine until neutral, and dry over anhydrous sodium sulfate. The solvent was removed, and 2-isopropyl-2-isopentyl-1,3-dipropylenecarboxypropane was obtained as a light yellow liquid by GF254 silica gel column chromatography with a yield of 65%.
[0285] 2-isopropyl-2-isopentyl-1,3-dipropylenecarboxypropane 1 H-NMR (CDCL 3 )δ(ppm):
[0286] 0.87 (d, 6H, methyl hydro...
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