Preparation method of double-epoxy blocked polypropylene glycol

A polypropylene glycol and double epoxy group technology, applied in the chemical industry, can solve the problems of poor product color, too strong NaH basicity, troublesome solvent, etc., and achieve the effect of high end capping rate and light color.

Active Publication Date: 2015-03-04
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the color of the product prepared under the condition of oxygen barrier is better, but the addition of solvent will bring a lot of troubles to the actual production, and the reaction time as long as 20h is not conducive to improving production efficiency
[0006] Chinese patent CN101928389A discloses a preparation method of epoxy-terminated allyl alcohol polyoxyethylene ether. This method uses NaH as the ring-opening catalyst, and then adds NaOH as the ring-closing catalyst to synthesize the target product. The disadvantage is that NaH is alkaline Too strong, the color of the product obtained under the condition of no oxygen barrier measures is poor. At the same time, because no phase transfer catalyst is added, the conversion rate is not high within the reaction time of 3 hours. It is necessary to add sodium hydroxide to continue the reaction for 1-3 hours to reach 85 %—93% sealing rate
[0007] In view of the fact that the existing technology is difficult to meet the requirements of high-end products without adding solvents, that is, the end-capping rate reaches more than 95%, and the color of the product is colorless or close to colorless (color ≤ 40, Pt-Co method), therefore, The present invention is proposed to solve the above-mentioned problems

Method used

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  • Preparation method of double-epoxy blocked polypropylene glycol
  • Preparation method of double-epoxy blocked polypropylene glycol
  • Preparation method of double-epoxy blocked polypropylene glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Put 112.9g (4.706moL) of NaH and 478.9g (5.176moL) of epichlorohydrin into the dripping reactor with nitrogen, stir for 30min and then fill with nitrogen to 0.4MPa; to the end-capped reactor with reflux condensation and stirring device Add 1000g (2.353moL) PPG-425, 0.782g (0.002353moL) tetra-n-butylammonium bromide, after vacuuming the nitrogen, open the nitrogen valve and the outlet valve of the reflux condensing device, and continue to pass nitrogen (nitrogen The end-capped kettle flows to the reflux condenser, and finally enters the tail gas device through the outlet valve); open the connection valve, and the dripping kettle presses the materials into the end-capped kettle for about 1h; after the dripping is completed, the temperature is raised to 40°C, at this temperature Reaction for 5h. After the reaction is completed, the temperature is lowered to 30°C, and a crude product is obtained; after the crude product is filtered and desalted, 50% phosphoric acid is added ...

Embodiment 2

[0055] Put 58.5g (2.439moL) of NaH and 234.7g (2.537moL) of epichlorohydrin into the nitrogen-filled dripping reactor, stir for 30min and then fill with nitrogen to 0.4MPa; to the end-capped reactor with reflux condensation and stirring device Add 1000g (0.976moL) PPG-1025, 0.808g (0.00488moL) tetraethylammonium chloride, after vacuuming the nitrogen, open the nitrogen valve and the outlet valve of the reflux condenser, and continue to pass nitrogen to the end-capped kettle (nitrogen is sealed The end kettle flows to the reflux condensing device, and finally enters the tail gas device through the outlet valve); open the connection valve, and the dripping kettle presses the material into the end kettle for about 1h; after the dripping is completed, the temperature is raised to 60°C and reacts at this temperature 8h. After the reaction is completed, the temperature is lowered to 30°C, and a crude product is obtained; after the crude product is filtered and desalted, 50% glacial a...

Embodiment 3

[0057] Put 35.6g (1.481moL) of NaH and 137.1g (1.481moL) of epichlorohydrin into the nitrogen-filled dropping reactor, stir for 30min and then fill with nitrogen to 0.4MPa; to the end-capped reactor with reflux condensation and stirring device Add 1000g (0.494moL) PPG-2025, 1.372g (0.00494moL) tetrabutylammonium chloride, after vacuuming nitrogen, open the nitrogen valve and the outlet valve of the reflux condenser, and continue to pass nitrogen to the capped kettle (nitrogen is sealed The end kettle flows to the reflux condensing device, and finally enters the tail gas device through the outlet valve); open the connection valve, and the dripping kettle presses the materials into the end kettle for about 1h; after the dripping is completed, the temperature is raised to 80°C and reacts at this temperature 10h. After the reaction is completed, the temperature is lowered to 30° C. to obtain a crude product; after the crude product is filtered to remove salt, 1% hydrochloric acid i...

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Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of double-epoxy blocked polypropylene glycol. The preparation method comprises the following steps: (1) dropwise adding a certain amount of NaH into a dripping reaction kettle, stirring, starting a condenser, vacuumizing to slowly suck epoxy chloropropane into the kettle, and then introducing nitrogen until the pressure is 0.4MPa for later use; (2) adding a certain amount of polypropylene glycol and a phase transfer catalyst into a blocking reaction kettle provided with a reflux condensing device, replacing the nitrogen in the kettle, slowly introducing nitrogen, slowly adding a mixture of NaH and epoxy chloropropane obtained in the step (1), and then heating for a certain time to obtain a crude product; and (3) filtering and desalting the crude product obtained in the step (2), adding a neutralizing agent for neutralization, subsequently vacuumizing for recycling epoxy chloropropane, then adding an adsorbent and refining to obtain a qualified finished product. The double-epoxy blocked polypropylene glycol prepared by the method disclosed by the invention has the advantages of light color (smaller than or equal to 40, platinum-cobalt colorimetric method) and high blocking rate (larger than or equal to 95%).

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of diepoxide-terminated polypropylene glycol. Background technique [0002] Diepoxide-terminated polypropylene glycol has epoxy groups at both ends of the molecular chain - a very active functional group, which is a good cross-linking agent, reactive diluent, fabric finishing agent and silver halide photographic material Hardening agent, etc. At present, high-end products not only put forward high requirements on the sealing rate (up to 95%), but also the color of the product must be colorless or close to colorless (color ≤ 40, Pt-Co method). [0003] There are mainly two kinds of synthetic methods reported in the literature, two-step method and one-step method: the two-step method refers to the ring-opening addition reaction of polyether and epichlorohydrin (epichlorohydrin) through the action of an acidic catalyst, and then With the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48
Inventor 金一丰张美军颜吉校陈英杰王磊
Owner ZHEJIANG HUANGMA TECH
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