background and overview[1]
ethylene glycol butyl ether acetate (eba) is a high-boiling, multi-functional, low-toxic advanced solvent with excellent performance. it is widely used in synthetic resins, adhesives, inks, printing, textile printing and dyeing and in industries such as leather tanning agents, it can also be used as a coalescing agent for latex paints. it has excellent solubility for a variety of paints and is widely used in colorful paints and emulsion paints.
preparation[1-2]
report 1,
the process flow is shown in figure 1. the raw materials ethylene glycol butyl ether and acetic acid, which are preheated to 110°c, are continuously fed into the first section equipped with 5l solid acid catalyst at a molar ratio of 1:1 at a flow rate of 15l/h. fixed bed reactor 1, esterification reaction temperature is 110°c, and space velocity is 3h-1. the material reacted in the first stage fixed bed reactor 1 enters the distillation tower 3. in the distillation tower 3, the water generated by the esterification reaction forms an azeotrope at 68-70°c in the presence of the water-carrying agent benzene and is continuously being separation. the material from which moisture has been removed is continuously extracted from the stripping section of the distillation tower 3 at a flow rate of 30l/h and transported to the second-stage fixed-bed reactor 2 equipped with 5l solid acid catalyst to continue the esterification reaction. the reaction temperature is 120 ℃, the airspeed is 6h-1. the material flow rate input to the second-stage fixed-bed reactor 2 is twice the feed amount of the first-stage fixed-bed reactor 1. the materials reacted in the second-stage fixed-bed reactor 2 also enter the distillation tower 3 for separation and removal of moisture. after being condensed by the condenser 4, the distillate from the top of the distillation tower 3 enters the stratified tank 5, and is stored in the stratified tank 5. it is divided into an organic phase and an aqueous phase, the aqueous phase is drawn out, and the organic phase is refluxed to the distillation tower 3 with aqueous agent benzene for reuse. the mass ratio of the output from the distillation tower 3 is: ethylene glycol butyl ether acetate 57.4%, acetic acid 14.4%, and ethylene glycol butyl ether 28.2%. the material discharged from the distillation tower 3 still enters the separately equipped light removal tower for distillation. the ethylene glycol butyl ether and acetic acid evaporated from the top of the light removal tower are recovered and recycled. the material from the light removal tower still is sent to the product distillation tower for purification. , it can produce 7.6kg of ethylene glycol butyl ether acetate product per hour. figure 1 is a schematic process flow diagram for preparing ethylene glycol butyl ether acetate through continuous esterification reaction.
report 2,
1 catalyst preparation
weigh 192gmg(no3)2·6h2o crystal and 141gal(no3) 3·9h2o crystals were dissolved in 1l deionized water to prepare al(no3)3 and mg( no3)2 mixed solution. add 300ml of 0.9mol/l na2co3 solution to the above mixed solution, then add 2.25mol/l naoh solution dropwise, and adjust the ph of the solution to 10±0.5 . continue to stir the mixed solution at room temperature for about 5 to 6 hours, then filter with suction, wash until neutral, and dry in an oven at 80°c overnight. take 10g of the dried sample and add it to an isopropyl alcohol solution containing 0.0025g/ml arachidic acid. boil and reflux for about 2 hours, filter with suction, wash until neutral, dry in an oven at 80°c overnight, and finally dry in a muffle furnace. the composite metal oxide catalyst is obtained by calcining at 500°c for 5 hours. the catalyst modified and calcined by arachidic acid is labeled as ldh-1, and the catalyst that is not modified and calcined is labeled ldh-2.
2 product synthesis
the synthesis conditions of ethylene glycol butyl ether acetate are: temperature 120~150℃, eo pressure 0.4mpa, ester-alkane molar ratio 1:1~5:1, mass space velocity 2.5~4.1h– 1, the catalyst loading is 2g. after the reaction, the product is cooled and then gas-liquid separated to obtain the target products ethylene glycol butyl ether acetate and diethylene glycol butyl ether acetate.
apply[3]
cn201710802745.3 discloses a spray ink for automobile signs. the weight percentage of each component of the spray ink is: bisphenol a-epoxy chlorohydrin resin 50%-70%; ethylene glycol butyl ether acetic acid esters 10%-15%; propylene glycol methyl ether acetate 5%-10%; c9 aromatics 5%-10%. the invention can solve the technical problem of poor ductility of automobile logo spray ink in the prior art.
references
[1][china invention, china invention authorization] cn200810021629.9 method for preparing ethylene glycol butyl ether acetate through continuous esterification reaction
[2] zhang jinchang, li tiechun. fixed-bed catalytic synthesis of ethylene glycol butyl ether acetate from butyl acetate [j]. daily chemical industry, 2018, 48(07): 388-391.
[3] [invented in china] cn201710802745.3 a spray ink for automobile signs