Preparation method of glycidol ether base end-capped allyl alcohol random polyether

Abstract

The invention relates to a preparation method of glycidol ether base end-capped allyl alcohol random polyether, which comprises the following steps: (1) adding NaH into a dropwise addition reaction kettle, starting a stirrer and a condenser, vacuumizing to slowly suck epoxy chloropropane into the kettle, and then charging nitrogen gas to 0.4 MPa for later use; (2) adding allyl alcohol random polyether and a phase-transfer catalyst into an end-capping reaction kettle with a reflux condensing device, performing in-kettle nitrogen replacement, then slowly introducing nitrogen gas, slowly adding the NaH and epoxy chloropropane mixture in the step (1), and then performing temperature reaction for a period of time to obtain a crude product; and (3) filtering the crude product to remove salt, neutralizing with neutralizer, then vacuumizing to recover the epoxy chloropropane, adding adsorbent, and refining to obtain the qualified finished end-capped product. The preparation method can satisfy the requirements of high-end products for end-capping rate and color, and is easy to realize industrial application.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of glycidyl ether group-terminated allyl alcohol random polyether. Background technique [0002] Glycidyl ether-terminated allyl alcohol random polyether has two active groups at both ends of the molecular chain: glycidyl ether and allyl, these two groups are two very active functional groups, as Good cross-linking agent, reactive diluent, fabric finishing agent and hardening agent for silver halide photographic materials, 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 two main 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 (ECH...

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

[0007] Chinese patent CN 101928389 A discloses a preparation method of glycidyl ether group-terminated allyl alcohol polyoxyethylene ether, which uses NaH as a ring-opening catalyst , and then add NaOH as a ring-closing catalyst to synthesize the target product. The disadvantage is that NaH is too alkaline, and the color of the product obtained under the condition of no oxygen barrier measures is poor. At the same time, because no P.T.C is added, the conversion rate within 3 hours of reaction time Not high, it needs to add sodium hydroxide to continue the reaction for 1-3 hours to reach a capping rate of 85%-93%

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