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A technology of glycidyl ester and methacrylic acid, which is applied in the production field of glycidyl methacrylate, can solve the problems of long distillation time, high temperature, low efficiency and the like, and achieves convenient operation, reduced industrial equipment, and reduced production. The effect of the process
Inactive Publication Date: 2016-01-06
DALIAN RES & DESIGN INST OF CHEM IND
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Problems solved by technology
Using the conventional still distillation process, the distillation time is long, the temperature is high, and the efficiency is low. The crude ester will polymerize during the distillation process, which will affect the quality and yield of the product.
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specific Embodiment 2
[0014] Reaction process: Put 240KG epichlorohydrin, 0.4KG phenothiazine, 25.6KG industrial sodium carbonate, 10KG dichloromethane into a 500L reactor, heat up to 75°C, add 40KG methacrylic acid within 1 hour, and reflux to separate water at the same time. After the water separation is completed, continue to raise the temperature to 103°C, distill off the dichloromethane, add catalyst tetramethylammonium chloride 0.02KG, keep the reaction for 2 hours, then cool down to 5°C.
[0015] Post-treatment process: Wash the reaction completed solution with 100KG dilute alkali solution (3%) for 10 minutes, let stand to separate the liquid, and obtain 258KG of the upper organic phase. A thin-film evaporator was used to distill and recover the solvent epichlorohydrin, wherein the vacuum condition was 3500 Pa, the feed temperature was 55°C, and the film jacket temperature was 64°C to obtain 60KG of crude ester liquid. Molecular distillation equipment was used to distill the finished product...
specific Embodiment 3
[0017] Reaction process: Put 240KG epichlorohydrin, 0.4KG phenothiazine, 25.6KG industrial sodium carbonate, 10KG dichloromethane into a 500L reactor, raise the temperature to 70°C, add 40KG methacrylic acid within 1 hour, and reflux to separate water at the same time. After the water separation is completed, continue to raise the temperature to 102°C, distill off the dichloromethane, add catalyst tetramethylammonium chloride 0.02KG, keep the temperature for 3.5 hours, then cool down to 10°C.
[0018] Post-treatment process: wash the reaction completed solution with 100KG dilute alkali solution (1%) for 10 minutes, let stand to separate the liquid, and obtain 260KG of the upper organic phase. A thin-film evaporator was used to distill and recover the solvent epichlorohydrin, wherein the vacuum condition was 1000 Pa, the feed temperature was 50°C, and the film jacket temperature was 60°C to obtain 63KG of crude ester liquid. The finished product was distilled using molecular di...
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Abstract
The invention relates to a production method of glycidyl methacrylate. The method comprises a reaction process and a post-treatment process. The reaction process is characterized in a one-step synthesis method. According to the reaction process, methacrylic acid and sodium carbonate are subjected to a neutralization reaction in excessive epichlorohydrin, such that sodium salt is prepared; without solid-liquid separation, system water content is removed with an azeotropic solvent; under the catalysis effect of a phase transfer catalyst, the glycidyl methacrylate is prepared. The post-treatment process comprises the following steps: a reaction finished liquid is washed; liquid separation is carried out, such that an organic phase is obtained; solvent recovery is carried out with a film evaporation device; and finished product distillation is carried out with a molecular distillation device. With the production method provided by the invention, production process and industrial equipment can be simplified, and operation is convenient. During the post-treatment process, phenomena of poor product polymerization rate and yield caused by high temperature, poor heat transfer effect, low distillation efficiency and the like of a conventional kettle distillation method can be avoided. With the method provided by the invention, product quality and yield can be effectively ensured. The obtained product has a purity higher than 98% and a yield of 85-90%.
Description
technical field [0001] The invention relates to a production method of glycidyl methacrylate, which belongs to the field of organic chemical industry. Background technique [0002] Glycidyl methacrylate (abbreviation: GMA) is an important organic chemical raw material, because its molecular structure contains highly active double bonds and epoxy groups, it can participate in functional group polymerization and ionic reaction polymerization. It can be used for the modification of ethylene polymers and polycondensation polymers. The downstream products of ethylene polymers and polycondensation polymers: powder coatings, emulsion polymerization, resin synthesis, adhesives, plastics, fiber modification, medical technology, etc. The field has a wide range of applications. [0003] The synthesis method of glycidyl methacrylate mainly adopts sodium methacrylate and epichlorohydrin in the industry, and is prepared by esterification in the presence of a phase transfer catalyst, such...
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