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Rod-like triethylene diamine and preparation method thereof

A technology for triethylenediamine and triethylenediamine crude product, which is applied in the field of rod-shaped triethylenediamine and its preparation, can solve the problems of affecting product quality and production efficiency, unfavorable material flow, low crystallinity and the like, and achieves hard agglomeration , Conducive to storage, low moisture content

Pending Publication Date: 2022-04-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain triethylenediamine with larger particle size and less agglomeration, because the product presents needle-like aggregates, it is easy to produce solvent entrapment and high water content, and the crystallinity is low, which is not conducive to product production The flow of materials in the process, which affects product quality and production efficiency

Method used

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  • Rod-like triethylene diamine and preparation method thereof
  • Rod-like triethylene diamine and preparation method thereof
  • Rod-like triethylene diamine and preparation method thereof

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preparation example Construction

[0030] The preparation process of the present invention is carried out in a recrystallizer, and the crystallizer is a kind of in MSMPR crystallizer, DTB crystallizer or Oslo crystallizer, preferably MSMPR crystallizer.

[0031] The purity of the triethylenediamine prepared by the present invention is greater than 99.99%. If one wants to obtain a higher-purity triethylenediamine product, the method described in the present invention can also be used to carry out multiple recrystallizations.

Embodiment 1

[0035] Add 1115g of triethylenediamine crude product and 545g of absolute ethanol to the MSMPR crystallizer, under the action of stirring, dissolve completely at 55°C, then add 10g of gas-phase method hydrophobic silica, and then control its fluid linear velocity to 15cm / s, Gradually lower the temperature to 15°C at a cooling rate of 0.01°C / min to 0.2°C / min, and keep the temperature constant for 30 minutes, in which the temperature is lowered at 0.01°C / min in the cooling range of 38°C to 32°C, and finally the crystalline slurry is suction-filtered, and the obtained solid is wet Dry the material at 40°C and 35KPa for 6 hours, and sieve it with a standard sieve to obtain the triethylenediamine product.

[0036] The X-ray diffraction pattern of gained triethylenediamine product is as figure 1As shown, the X-ray diffraction patterns are at diffraction angles 2θ=16.86, 17.19, 19.30, 19.82, 27.91, 30.64, 33.00, 33.80, 34.88, 35.14, 38.08, 44.64, 45.14, 46.19, 49.08, 52.50, 54.01, 58...

Embodiment 2

[0041] Add 1200g of triethylenediamine and 646g of absolute ethanol into the MSMPR crystallizer, under the action of stirring, dissolve completely at 60°C, then control the fluid linear velocity to 30cm / s, and cool down at 0.01°C / min~0.2°C / min The rate is gradually lowered to 20°C, and the temperature is kept constant for 30 minutes, in which the temperature is lowered at 0.01°C / min within the cooling range of 45°C to 30°C, and finally the crystal slurry is suction-filtered, and the obtained solid wet material is dried at 45°C and 30KPa for 2 hours. Then use a standard sieve to sieve to obtain the triethylenediamine product.

[0042] The X-ray diffraction spectrum of gained triethylenediamine product is at diffraction angle 2θ=16.90,17.02,19.36,19.87,27.81,30.71,33.00,33.72,34.81,35.11,38.12,44.54,45.22,46.16,49.15,52.46,54.10 , 58.50, 60.13, 62.81, 63.75, 71.59, 76.58 degrees have obvious characteristic peaks, and the relative intensity of each diffraction peak is 40.0%, 23.9...

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Abstract

The invention discloses a triethylene diamine crystal and a preparation method thereof, the triethylene diamine is of a rod-like structure, and the X-ray diffraction pattern of the triethylene diamine has main characteristic peaks at the diffraction angles 2theta of 16.86 + / -0.1, 17.19 + / -0.1, 19.30 + / -0.1, 19.82 + / -0.1, 27.91 + / -0.1, 30.64 + / -0.1, 33.00 + / -0.1, 33.80 + / -0.1, 34.88 + / -0.1, 35.14 + / -0.1, 38.08 + / -0.1, 44.64 + / -0.1, 45.14 + / -0.1, 46.19 + / -0.1, 49.08 + / -0.1, 52.50 + / -0.1, 54.01 + / -0.1, 58.48 + / -0.1, 60.16 + The method comprises the following steps: firstly, adding a triethylene diamine crude product into an ethanol solution, completely dissolving at 55-60 DEG C, then adding white carbon black, uniformly dispersing, controlling the cooling rate to be 0.01-0.2 DEG C / min, controlling the cooling rate to be 0.01-0.05 DEG C / min in a cooling interval of 45-30 DEG C, controlling the fluid linear velocity to be 15-65 cm / s, gradually cooling to 15-20 DEG C, keeping for 30-60 minutes, carrying out solid-liquid separation on crystal slurry, and carrying out solid-liquid separation on the crystal slurry to obtain the triethylene diamine white carbon black. And drying and screening the obtained solid wet material to obtain triethylene diamine. The product has the characteristics of large particle size, good fluidity, difficulty in caking, high dissolution rate and low water content, and is beneficial to storage, transportation and use.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and relates to the crystallization of triethylenediamine, in particular to a rod-shaped triethylenediamine and a preparation method thereof. Background technique [0002] Triethylenediamine (another name: triethylenediamine, triethylenediamine, 1,4-diazabicyclo[2.2.2]octane; abbreviation: TEDA), widely used in soft, semi-rigid, Rigid polyurethane foam, elastomer and plastic products. In addition, it can also be used as an epoxy resin curing catalyst, ethylene polymerization catalyst, acrylonitrile polymerization catalyst, ethylene oxide polymerization catalyst, initiator for the production of pesticides such as hexahydropyridine, and an electroplating additive. [0003] At present, triethylenediamine is mainly synthesized from ethanolamine, ethylenediamine, ethyleneimine, piperazine, aminoethylpiperazine, hydroxyethylpiperazine, etc., through condensation reaction under the action of a c...

Claims

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Application Information

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IPC IPC(8): C07D487/08
CPCC07D487/08C07B2200/13
Inventor 吕剑杨建明张前余秦伟梅苏宁王为强惠丰李亚妮袁俊
Owner XIAN MODERN CHEM RES INST
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