Preparation method for compositing dipentaerythritol with tripentearythritol with high yield coefficient

Abstract

The invention discloses a preparation method for compositing dipentaerythritol with tripentearythritol with a high yield coefficient. A catalytic agent is activated macromolecule loading solid alkali which is composed of a carrier and active components, wherein the carrier is a macromolecule base body in a styrene copolymerization cross-linked structure, and the active components come from quaternary amine or hydroxy radical combined with the quaternary amine. Highly purified tripentearythritol, crude dipentaerythritol and pentaerythritol are obtained, and purified dipentaerythritol is obtained by refining the crude dipentaerythritol. A yield coefficient of the tripentearythritol is more than 20%, and the content is more than 90%. The dipentaerythritol with a yield coefficient more than 40% is obtained at the same time, and the content is more than 90%. A yield coefficient of pentaerythritol is less than 20%. Few by-product is contained in reaction liquid, and purity is high. The catalytic agent obtained through the preparation method is high in mechanical strength and recyclable, so that the preparation method is environment-friendly and can be carried out on a traditional pentaerythritol production device. The preparation method has a good industrialization prospect.

Description

technical field [0001] The invention relates to a preparation method of dipentaerythritol and tripentaerythritol, in particular to a method for preparing dipentaerythritol and tripentaerythritol with a high yield under the condition of using a treated polymer loaded solid base as a catalyst. Background technique [0002] Dipentaerythritol is mainly used as a stabilizer for synthetic lubricants and non-toxic PVC processes, and is also a raw material for the synthesis of polyethers, polyesters, polyurethanes, acrylates, high-density cross-linked products, coatings, inks and adhesives; it can also be used in Fire protection system (expanded part or brominated part), resin and radiation-treated acrylate, can also be used to synthesize alkyd resin; tripentaerythritol is mainly used in foaming environment-friendly flame-retardant coatings and synthetic textile activation cosolvents. One of the most compelling new application materials in years. [0003] However, at present, the a...

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Problems solved by technology

[0004] The current mainstream synthesis technology is a one-step reaction at medium temperature in a conventional condensation reactor to generate monopentaerythritol, dipentaerythritol and tripentaerythritol. For example, the patent application whose application number is 200710053987.3 and whose publication number is CN101012156A discloses a method that utilizes calcium hydroxide as a catalyst and formaldehyde, ethyl alcohol Aldehyde is a production process for synthesizing dipentaerythritol and / or tripentaerythritol. Due to the presence of by-product impurities such as condensed aldehydes and corresponding acid salts, calcium formate needs to be separated under high temperature conditions, which consumes too much energy and leads to separation It is very difficult to obtain high-purity dipentaerythritol and tripentaerythritol, and the pure color of the product is poor. It needs to be hydrolyzed and decolorized by activated carbon again. The operation is complicated and does not conform to the industrial concept of green and environmentally friendly production; A synthetic method for generating dipentaerythritol and tripentaerythritol, such as the patent application whose application number is 200710037512.5 and whose publication number is CN101016232A, discloses a rare earth or alkaline earth oxide that uses formaldehyde, acetaldehyde, and pentaerythritol as raw materials and is loaded on a porous material SBA-15. Under the action of a catalyst, the method for preparing dipentaerythritol, the method needs to separate the catalyst in the reaction stage, the reaction process is divided into two parts, and the preparation of the catalyst is complicated, which makes the production process complicated and the cost is high. In addition, although the method improves the The yield of dipentaerythritol and tripentaerythritol, but there is also the problem of separation difficulty when higher yield tripentaerythritol is obtained, resulting in poor product color and purity, and by-product impurities such as condensed aldehydes and corresponding acid salts cannot be effectively removed; In addition, the patent application whose application number is 200810024057.X and whose publication number is CN101265166A, in order to avoid other by-product impurities such as formaldehyde and acetaldehyde to condense aldehydes, proposes a pre-condensation reactor and a main condensation reaction using inert gas pressurization Still react to obtain the production method of monopentaerythritol, dipentaerythritol and tripentaerythritol, the method equipment is complex, and need inert gas pressurization cost is higher, process is more complicated; In order to avoid the above problems, the application number is 200910172347.3 and the publication number is the patent of CN101696158A The application proposes a method for preparing high-quality monopentaerythritol and dipentaerythritol by reducing the generation of tripentaerythritol as much as possible by precisely controlling the ratio and concentration of raw materials, reaction temperature and feeding procedures. The process is simple, but the raw materials cannot be fully utilized to obtain high yields. high-efficiency tripentaerythritol, and the product still needs activated carbon for decolorization, which does not fundamentally solve the problem of by-product impurities, and cannot meet the growing demand for high-quality and quantitative dipentaerythritol and tripentaerythritol

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