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Study on Synthesis of N-(4-hydroxyphenyl) Maleimide and Related Physical Properties

Author: YangXinWei
Tutor: LiuGuoJi；ZuoTingLiang
School: Zhengzhou University
Course: Chemical processes
Keywords: N-(4 - hydroxyphenyl ) maleimide Synthesis Density Viscosity Solubility
CLC: TQ245.27
Type: Master's thesis
Year: 2011
Downloads: 56
Quote: 0
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Abstract


Maleimide (BMI) is a heat-resistant polymer monomer may be copolymerized with vinyl monomers to prepare a polymer material having excellent heat resistance. N-(4 - hydroxyphenyl) maleimide (4-HPM) is one of the functional monomer, a bifunctional copolymer prepared having good electrical and mechanical properties and heat resistance, and therefore high homopolymers of chemical modification, in particular, has an important role in the research and development of the insulating material and the heat-resistant polymer material. This article the use of maleic anhydride (MA) and p-aminophenol (4-AP) as a raw material, the dry hydrogen resin as a catalyst, N, N-dimethyl formamide (DMF) as a solvent, toluene as water, through a two-step Preparation of 4-HPM. In order to obtain a higher yield by orthogonal design and single factor experiments to optimize the process. Optimization results are as follows: the amount of catalyst is added to the raw material of the total mass 12% of n-(MA): n (4-AP) = 1.1:1, VToluene: VDMF = 3:1 Tstep 2 = 9 Hours crude product yield was 78% up to 97% purity. The structure of the final products were characterized by means of FT-IR, NMR, etc., recognized as 4-the HPM. The dry hydrogen resin catalyst without activation can be reused three times. Cycle after the deactivation of the activated resin, its catalytic activity the with a fresh dry hydrogen resin considerable. The catalyst with high selectivity, small corrosive to the equipment, to facilitate the separation and recovery, greatly reduces equipment requirements, environment friendly, easy storage and metering, in line with the direction of the development of chemical production. This paper balance method was subjected to atmospheric research of the solid-liquid equilibrium, the solid N-(4 - hydroxyphenyl) maleimide in anhydrous ethanol, isopropanol, ethanol-water (v = 50%) and isopropanol water (V = 50%) in four solvents solubility. Two parametric equations and three-parameter equation regression of experimental data. The results showed that, for the above system, the three-parameter equation fitting better. In addition, the obtained N-(4 - hydroxyphenyl) maleimide in isopropanol solvent solubility of experimental results, for the process Synthesis 4-HPM crude product was separated and purified to provide a data support. Atmospheric pressure under the conditions of the temperature range from 293.15K to 318.15K, the Ostwald-Sprengel-type the pycnometer and Ubbelohbe viscosity meter containing of N-(4 - hydroxyphenyl) maleimide binary, ternary system (4-HPM ethanol ,4-HPM ethanol 50% water ,4-HPM isopropanol ,4-HPM isopropanol 50% water ,4-HPM DMF) the density of the viscosity was measured, and calculate the apparent molar volume and limiting partial molar volume. The VTF equation obtained the experimental density and viscosity data were used to fit. The average standard deviation between the calculated and experimental values ??of less than 2.5%, indicating the VTF equation applicable to the relevant system.

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > The production of aromatic compounds > Aromatic carboxylic acids and their derivatives > Aromatic acid functional derivatives > Nitrogen - containing functional derivatives
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