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Preparation method for melamine derivative

A technology of melamine and its derivatives, applied in the direction of organic chemistry, etc., can solve problems such as untimely detection, use, storage, transportation troubles, and restrictions on commercialization, and achieve simple and clear judgment methods, convenient measurement and operation, and facilitate commercial use Effect

Active Publication Date: 2015-03-04
SICHUAN GOLDEN ELEPHANT SINCERITY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this high degree of substitution derivative has obvious disadvantages: first, the high degree of substitution weakens the reactivity characteristics of melamine amido groups, so its application is limited, especially in the preparation of resins as active co-condensation monomers Second, the product is a semi-solid viscous substance at room temperature, which is very easy to absorb moisture, which brings great trouble to use, storage and transportation, and also limits its commercialization to a certain extent
HPLC can analyze the composition of the product by sampling during the reaction, but it takes a series of operations and a certain period of time to obtain the analysis results, so it cannot be used for the timely detection of the reaction end point in the actual production process; other reasons , the reaction system in the process is a complex mixture including initial raw materials, reaction intermediate products, and catalysts, and the accuracy of HPLC online analysis will be greatly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 5L four-necked flask, electric heating mantle, tail gas absorption device filled with sulfuric acid aqueous solution, condensation reflux device, distillation unit, vacuum pump Add 1260g melamine, 2026g diglycolamine, 126g diglycolamine and 5L four-necked flask Phosphoric acid, hypophosphorous acid complex, start stirring and heat up to 200°C, react under reflux, pass a weak nitrogen flow after 6 hours until the material is clear and transparent, take samples every 2 minutes and mix them with ethanol at a mass ratio of 1:5 until the first No precipitation occurred during sampling for 5 times, and 20 g of solid sodium hydroxide was added, and vacuum was opened to remove and collect unreacted diglycolamine. After the temperature of the material rose to 260°C, the heating was stopped, and the temperature was lowered to 150°C under stirring and nitrogen protection, and the material was released. After cooling, 2552.1g of a translucent white solid was obtained, with a fra...

Embodiment 2

[0033] Add 31.5kg of melamine, 50.65kg of diglycolamine, 3.15kg of diglycolamine, phosphoric acid, and hypophosphorous acid complex into a 200L reactor, start stirring and raise the temperature to 198°C, react under reflux, and pass it in after 6 hours Nitrogen until the material is clear and transparent, take a sample every 2 minutes and mix it with ethanol at a mass ratio of 1:5. No precipitation occurs at the 8th sampling, add 500g of solid sodium hydroxide, turn on vacuum to remove and collect unreacted diglycolamine . When the temperature of the material rose to 250° C., the heating was stopped, and the temperature was lowered to 150° C. under the protection of nitrogen, and the material was released to obtain 64.74 kg of light yellow solid and 14.41 kg of fractions. The average degree of substitution was 1.45 calculated from the material balance. The obtained product has a softening point of 70-75°C and a melting range of 100-110°C.

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Abstract

The present invention discloses a preparation method for a melamine derivative. According to the preparation method, judgments and controls of a reaction material ratio, catalyst optimization, and reaction end point are adopted to prepare a melamine derivative, wherein a main component of the product is a mixture of N-mono-(5-hydroxy-3-oxapentyl)melamine and N,N'-di(5-hydroxy-3-oxapentyl)melamine, and the product is a white or light yellow solid, and is easy to package and use.

Description

technical field [0001] The invention relates to a preparation method of melamine derivatives, in particular to the judgment and control of the reaction end point in the preparation method. Background technique [0002] Melamine aminodiglycol derivatives are widely used in the production and development of fine chemical products. Because it introduces the hydroxyethyloxyethyl group in melamine, which greatly improves the solubility of melamine in the aqueous solution system, so that melamine can be added to the reaction system in a large proportion at any stage of the reaction, especially amino resin The reaction system provides a possibility and provides more choices for process improvement and new product development. [0003] At present, the reaction system using melamine and diglycolamine as the starting material can only obtain N-mono(5-hydroxy-3-oxapentyl) melamine, N,N'-bis(5-hydroxy-3-oxa Pentyl) melamine, N, N', N''-tris(5-hydroxy-3-oxapentyl) melamine mixture, but...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/70
Inventor 李健刘朝慧李刚王顺平邓朝元唐志有余全伟刘浩然
Owner SICHUAN GOLDEN ELEPHANT SINCERITY CHEM CO LTD
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