Overview of the preparation of n-butyl glycidyl ether
N-butyl glycidyl ether is a colorless liquid with a slightly pungent odor. It is used as a viscosity reducer and chemical intermediate for epoxy resins, and as a solvent stabilizer for chlorination. This product is a central nervous system depressant. It has mild irritation to the respiratory tract. Repeated exposure has a moderate accumulation effect. Animal experiments have proven that it significantly inhibits growth. GBZ2.1-2007 “Occupational Exposure Limits for Hazardous Factors in the Workplace – Chemical Hazardous Factors” stipulates that n-butyl glycidyl ether PC-STEL is 60mg/m3 and PC-TWA is 120mg/m3.
Preparation of n-butyl glycidyl ether
Method 1: n-butyl glycidyl ether was synthesized using n-butanol and epichlorohydrin as raw materials, boron trifluoride ether complex as catalyst, and sodium hydroxide as the ring-closing agent for the ring-forming reaction. The better synthesis reaction conditions are: boron trifluoride ether complex mass fraction is 0.40%, n (epoxy chloropropane): n (n-butanol) = 1.8: 1, n (sodium hydroxide): n ( n-butanol)=1.4:1, and the ring-forming reaction temperature is 30°C.
Method 2: Put 74 kilograms of n-butanol and 8 kilograms of toluene into the reactor, add 3 kilograms of polymer carrier solidly loaded with composite catalyst while stirring calcium and magnesium carbonate, and maintain stirring for 15 minutes. Add 100 kg of ECH dropwise at 50-70°C, control the temperature at 50-70°C, drop for 2 hours, then maintain the temperature at 40-45°C for 3 hours, filter out the catalyst, and then add benzyltriethylammonium chloride and sulfuric acid Hydrotetrabutylammonium and polyquaternium-6 three-way composite catalysts are used as catalysts (in the three-way composite catalyst, the dosage of benzyltriethylammonium chloride is 0.5 to 1% of the reactant mass, and the dosage of tetrabutylammonium hydrogen sulfate is The dosage is 1 to 3% of the mass of the reactants, the dosage of polyquaternium-6 is 0.5 to 0.9% of the reactants), add 90 kg of liquid caustic soda (48%) dropwise at 50-55°C for 2 hours, at 50-55°C Maintain the temperature for 3 hours. After the reaction is completed, filter to remove the by-product NaCl, separate the lower brine, and dehydrate to obtain 130 kilograms of n-butyl glycidyl ether, with an epoxy value of 0.595 eq tricyclohexylphosphine fluoroborate/100g.
Research on the preparation and application of n-butyl glycidyl ether
Cao Cong and others studied the effect of n-butyl glycidyl ether (501) on the properties of epoxy resin through viscosity, mechanical property testing, differential scanning calorimetry analysis and thermogravimetric analysis, and studied the effect of 501/epoxy resin Curing reaction kinetics of the system. The results show that as the amount of 501 increases, the viscosity of the system decreases significantly, the tensile strength and heat resistance decrease, while the flexural strength first increases and then decreases, but still improves. The constant temperature curing temperature of the system gradually decreases with the increase in the amount of 501, and the activation energy also shows a decreasing trend, while the reaction order fluctuates around 0.93. The addition of 501 has no obvious effect on the curing reaction mechanism of the epoxy resin system.
