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The Synthesis And The Quality Standard Research Of Dicyclopentenlyoxyethyl Methacrylate

Posted on:2015-08-03Degree:MasterType:Thesis
Country:ChinaCandidate:C C LiuFull Text:PDF
GTID:2284330452950155Subject:Pharmacy
Abstract/Summary:PDF Full Text Request
Dicyclopentenlyoxyethyl methacrylate have an unsaturated double bond in themolecule and it is widely used in adhesives, acrylic coatings, reactive diluents, andother fields. Monomer with the adhesive has many characteristics such as: a low cureshrinkage, low odor, low volatility, air drying, heat resisitance, moisture resistance,chemical resistance. Given the large quantities of features, Dicyclopentenlyoxyethylmethacrylate has great potential for development in domestic market. Research in itsquality standards would help to promote industrial-scale production, and would get awide range of application and thriving prospect. This study conducted preliminaryexperiments which include their synthesis process, quality standards and stability test.1Reasearch of the preparationAccording to the consult literature material determined factors affecting theesterification reaction conditions: polymerization retarder, catalyst, water carrier,reaction temperature, reaction time, and proportion. By optimizing the reactionconditions would obtain products with high purity and high esterification rate.The first step of optimum conditions: n (DCPD): n (ethylene glycol)=1.2:1;Mixed inhibitor (Hydroquinone0.6%, mass fraction of hydroxy anisole is0.2%);reaction temperature is120℃; reaction time is15h.Step optimum conditions: n (methyl methacrylate): n (ethylene glycol-biscyclopentenyl ether)=1.2:1; mass fraction of catalyst-hydroxy acid (with a total massof the alkyd) is3.0%; n-heptane was mixed with the agent; mass fraction of inhibitor(hydroquinone) is0.8%, mass fraction of hydroxy anisole is0.2%; reactiontemperature is110℃; reaction time is8h.2Reasearch of quality standardThis paper conducted a quality standards study of indicators of laboratory-madedicyclopentenlyoxyethyl methacrylate in accordance with national standards. Traits ofdicyclopentenlyoxyethyl methacrylate are include color, solubility, relative density,viscosity, refractive index, acid value, saponification value and the bromine,etc.Identification tests include functional group identification, UV spectroscopy andinfrared spectroscopy. There are also various tests include moisture content, highpolymer content, retarder content, etc. Compare the method of gas chromatographyand high performance liquid chromatography to determine the content of dicyclopentenlyoxyethyl methacrylate correctly.The most suitable method fordeterminiation was gas chromatography which was validated by methodology, themeasured content can reach98.5%or more.3Reasearch of preliminary stabilityOne group of sample was placed at room temperature for six months and anothergroup of accelerated test samples was placed at temperature of55~65℃,75%relativehumidity conditions for three months.Test proved that the investigated samples ofeach quality testing target conforms to the requirements in the normal roomtemperature stability and in the acceleration stable inspection time,indicating goodstability.Predictly the product is valid for6months.
Keywords/Search Tags:Dicyclopentenlyoxyethyl methacrylate, esterification, retarder, highpolymer, quality standard
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