58901-12-5Relevant academic research and scientific papers
Preparation method of hydroxyl tertiary amine hydrochloride crystal
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Paragraph 0083; 0084; 0085; 0086, (2021/03/24)
The invention discloses a preparation method of a hydroxyl tertiary amine hydrochloride crystal. The preparation method comprises the following steps of: (1) dissolving hydrochloric acid in lower alcohol to form a hydrochloric acid alcohol solution; (2) adding the hydrochloric acid alcohol solution in the step (1) and hydroxyl tertiary amine into a reactor, and reacting under the N2 protection condition to obtain a hydroxyl tertiary amine hydrochloride primary product; and (3) heating and dissolving the hydroxyl tertiary amine hydrochloride primary product obtained in the step (2) by using anorganic solvent, decolorizing, cooling, crystallizing, separating the crystallized precipitate, and drying to obtain the hydroxyl tertiary amine hydrochloride crystal. The hydroxyl tertiary amine hydrochloride crystal prepared by the method has a high dissolution rate in water and can be accurately metered, and the accuracy of the hydroxyl tertiary amine hydrochloride crystal used for compoundingadditives is improved. As a crystal, compared with liquid, solid quantitative packaging can be adopted, and the packaging cost, the transportation cost and the storage cost are all reduced. The methodhas the advantages of few steps, simple separation of the intermediate product, easy operation of the crystallization purification method, and low production cost.
Preparation method of isopropanolamine
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Paragraph 0015, (2017/01/23)
A preparation method of isopropanolamine comprising the following steps: 1, weighing isopropanolamine with the mole content of 80% or more and hydrochloric acid according to a ratio of 1:1, wherein the isopropanolamine is MIPA, DIPA and TIPA; 2, adding a calculated amount of hydrochloric acid to a flask with three necks, adding a calculated amount of commercial MIPA or TIPA in batches under stirring until the pH value is 2 at below 40DEG C, precipitating crystals, continuously stirring for cooling to 0DEG C, filtering to respectively obtain MIPA.HCl or TIPA.HCl, mixing the above obtained two mother liquors, and carrying out reduced pressure dewatering to obtain DIPA.HCl; or adding the calculated amount of hydrochloric acid to the flask with three necks, adding a calculated amount of commercial DIPA in batches under stirring until the pH value is 2 at below 40DEG C, cooling to 0DEG C, filtering to obtain a filter cake to be processed, and carrying out reduced pressure distillation under 100mmHg on the obtained filtrate until no precipitate precipitates to obtain DIPA.HCl; and 3, respectively carrying out a free reaction on the MIPA.HCl, DIPA.HCl and TIPA.HCl and an equivalent amount of a methanol solution of sodium methoxide, filtering to remove salt, and carrying out reduced pressure distillation on the above obtained methanol recovered solution to respectively obtain high-quality MIPA, DIPA and TIPA with the content of 97-99%. The obtained isopropanolamine can completely substitute imported products, meets domestic needs, and has substantial benefits.
