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Scaly anhydrous piperazine crystal and preparation method thereof

An anhydrous piperazine and scaly technology, applied in the field of scaly anhydrous piperazine crystals and their preparation, can solve the problems of small particle size of anhydrous piperazine crystals, residual purity of easy solvent, poor fluidity and the like, and achieve fluidity. Good, low solvent residue, obvious advantages

Pending Publication Date: 2020-12-22
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies and defects of the prior art, the present invention provides a scaly anhydrous piperazine crystal and a preparation method to solve the problem that the anhydrous piperazine crystal prepared by the existing preparation method has a small particle size, is easy to agglomerate, and flows Poor performance, easy solvent residue and low purity

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  • Scaly anhydrous piperazine crystal and preparation method thereof
  • Scaly anhydrous piperazine crystal and preparation method thereof
  • Scaly anhydrous piperazine crystal and preparation method thereof

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preparation example Construction

[0024] The invention discloses a scale-shaped anhydrous piperazine crystal. It is found through experiments that the anhydrous piperazine crystal has the characteristics of high purity, large particle size, good fluidity, high crystallinity, and looseness without agglomeration. The preparation method of anhydrous piperazine crystal mainly comprises:

[0025] First, the crude piperazine is added into an alcoholic solvent to prepare a suspension, wherein the mass fraction of piperazine in the alcoholic solvent is 51% to 55%;

[0026] The alcoholic solvent is one or a mixed solvent of methanol and dehydrated ethanol, preferably dehydrated ethanol.

[0027] Then, stir at 50-70°C until the crude piperazine is completely dissolved, then control the stirring rate to 30-200rpm, preferably 30-100rpm; then cool down to 15-25°C at a cooling rate of 0.01-0.5°C / min, get crystal slurry;

[0028] Preferably in the present invention, during the cooling process, the cooling rate in the cooli...

Embodiment 1

[0042]In the MSMPR crystallizer, the crude piperazine was added to absolute ethanol to prepare a 54.07% suspension. Under stirring, it was completely dissolved at 60°C, then the stirring rate was controlled at 30rpm, and the temperature was gradually lowered to 25°C. Control the cooling rate to 0.5°C / min in the temperature range of 60-55°C, 0.01°C / min in the temperature range of 46-48°C, and 0.2°C / min or lower in other temperature ranges, and cool down to 25°C After constant temperature for 60 minutes, the crystal slurry was suction filtered, and the obtained solid material was dried at 40°C and 30KPa for 3 hours to obtain the product.

[0043] The product is carried out XRD test, the result is as follows figure 1 As shown, it can be seen that the X-ray diffraction spectrum of the product obtained in this embodiment has characteristic peaks at diffraction angles 2θ=14.47, 16.02, 17.49, 32.19, 42.01, 44.77, 46.24, 66.75, and 67.04 degrees, and each diffraction peak The relativ...

Embodiment 2

[0048] In the MSMPR crystallizer, the piperazine crude product was added to absolute ethanol to prepare a 55% suspension. Under stirring, it was completely dissolved at 65°C, then the stirring rate was controlled at 50rpm, and the temperature was gradually lowered to 20°C. Control the cooling rate to 0.5°C / min in the temperature range of 60-55°C, 0.03°C / min in the temperature range of 48-50°C, and 0.3°C / min or lower in other temperature ranges, and cool down to 25°C After constant temperature for 30 minutes, the crystal slurry was suction-filtered, and the obtained solid material was dried at 40°C and 30KPa for 6 hours to obtain scaly anhydrous piperazine crystals.

[0049] The X-ray diffraction pattern of the obtained crystal product has characteristic peaks at diffraction angles 2θ=14.48, 16.04, 17.48, 32.18, 42.03, 44.76, 46.35, 66.65, and 67.08 degrees, and the relative intensity of each diffraction peak is 5.0%, 100% in turn , 1.2%, 1.7%, 0.1%, 0.2%, 0.1%, 0.1%, 0.2%. Th...

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Abstract

The invention discloses a scaly anhydrous piperazine crystal and a preparation method thereof. The preparation method comprises the steps: firstly, adding an anhydrous piperazine crude product into analcohol solvent to prepare turbid liquid, wherein the mass fraction of the anhydrous piperazine crude product in the alcohol solvent is 51%-55%; conducting stirring at 50-70 DEG C until the anhydrouspiperazine crude product is dissolved, then controlling the stirring rate to be 30-200 rpm, conducting cooling to 15-25 DEG C at the cooling rate of 0.01-0.5 DEG C / min, carrying out solid-liquid separation on crystal slurry, and drying the solid to obtain the anhydrous piperazine crystal. The flaky anhydrous piperazine crystal prepared by the method has the purity of more than 99.99%, the main particle size of 1.7-3.35 mm, the angle of repose of 30-35 degrees and the relative crystallinity of 543%, and is higher in purity, large in particle size, good in flowability, high in crystallinity, loose, free of caking and more beneficial to use, storage and transportation compared with a commercially available blocky anhydrous piperazine crystal product.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a scaly anhydrous piperazine crystal and a preparation method thereof. Background technique [0002] Anhydrous piperazine (another name: bis-dimethylamine, hexahydropyrazine, piperazine, p-diazepine, etc.) is an important pharmaceutical intermediate and fine chemical raw material, widely used in norfloxacin, pyrazinic acid , anthelmintic drug fosperidic acid, piperazine citrate, fluphenazine, chlorpheniramine, rifampin and other drugs synthesis; at the same time in the rubber vulcanizing agent, preservatives, antioxidants, stabilizers, surfactants, slow It is also widely used in the fields of etching agent, foaming agent, coating, pesticide, leather, fiber, wastewater treatment and carbon fixation. [0003] At present, anhydrous piperazine mainly uses ethanolamine, ethylenediamine, diethylenetriamine, hydroxyethylethylenediamine, iminodiacetonitrile, etc...

Claims

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Application Information

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IPC IPC(8): C07D295/023C07D295/027
CPCC07D295/023C07D295/027C07B2200/13
Inventor 吕剑张前杨建明余秦伟王为强梅苏宁李亚妮赵锋伟袁俊惠丰李佳霖
Owner XIAN MODERN CHEM RES INST
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