Triethylenediamine crystal and preparation method thereof

A technology of triethylenediamine and crude triethylenediamine, which is applied in the direction of organic chemistry, can solve the problems of difficult transportation and use of liquid products, difficult particle size and fluidity control, high temperature requirements, etc., to achieve reduction The effect of artificial control factors, favorable storage and subsequent processing requirements, and uniform particle size distribution

Active Publication Date: 2018-10-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the existing method can obtain TEDA products with a slightly higher purity, the distillation process requires too high a temperature, consumes a lot of energy, and the liquid product brings difficulties to the later transportation and use process
Moreover, whether it is a distillation process or a liquid product, it is difficult to control factors such as particle size and fluidity
[0006] The TEDA products in the prior art are small particles, which have poor fluidity and need to consume more power during product transportation and filling
In the prior art, there is still a lack of a TEDA product with a suitable particle size and its preparation method, which can solve the above technical problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0031] The instrument that is used to detect product property and structure among the present invention is as follows:

[0032] (1), the purity is detected by the 7890A gas chromatograph produced by Agilent brand, detection conditions: DB-5 chromatographic column, inlet temperature 280°C, FID detector temperature 300°C, column flow rate 1.5ml / min, hydrogen flow rate 30ml / min, the air flow rate is 300ml / min, the temperature program is 50°C for 2min, 5°C / min to 80°C, 15°C / min to 280°C, and 15min. The built-in software was used for data processing, and the area normalization was used to determine the component content.

[0033] (2) The particle size distribution is detected by Malvern G3, the detection conditions: injection pressure 2.8bar, injection time 20ms, stabilization time 60s.

[0034] (3) The water content is detected by a Metrohm 915KF water analyzer, and the detection conditions are: pre-add 50ml of methanol in the titration cup, drop to an anhydrous state with Karl F...

Embodiment 1

[0038] (1) 35g TEDA crude product (containing TEDA 82wt%, PIP 17.3wt%, methyl TEDA 0.4wt%, methylpiperazine 0.1wt%, nitrogen-containing heterocyclic compound 0.2wt%) was added in 40g toluene, stirred, and heated to 68°C;

[0039] (2) After the solution is completely dissolved, grow crystals at 64°C for 2 hours at 2°C / hour in the range of 68°C to 64°C, and then continue to cool at a cooling rate of 4°C / hour in the range of 64°C to 52°C; Finally, the temperature was lowered at 8.3°C / hour in the range of 50°C to 20°C, filtered, and vacuum-dried at 40°C and vacuum degree of 0.06MPa for 2 hours to obtain the TEDA product.

[0040] The purity of the obtained TEDA product is 99.8wt%, PIP 0.2wt%, the particle size distribution of the product is mainly concentrated (≥85wt%) at 800-1000 μm, the angle of repose is 39°, the water content is 1.4wt%, and the yield is 78%.

Embodiment 2

[0042] (1) 100g TEDA crude product (containing TEDA 63wt%, PIP 35wt%, methyl TEDA 0.7wt%, methylpiperazine 0.3wt%, nitrogen-containing heterocyclic compound 1wt%) was added in 120g methyl tert-butyl ether, Stir and heat to 70°C;

[0043] (2) After the solution is completely dissolved, cool down at a rate of 2°C / hour between 70°C and 67°C, grow crystals at 67°C for 1.5 hours, and then continue to cool down at a rate of 4°C / hour between 67°C and 55°C ; Finally, the temperature was lowered at 9°C / hour in the range of 55°C to 28°C, filtered, and vacuum-dried at 45°C and vacuum degree of 0.06MPa for 1.5h to obtain the TEDA product.

[0044] Gained TEDA product purity is 99.3wt%, PIP content 0.69wt%, methyl TEDA0.01wt%; Product particle size distribution mainly concentrates (≥85wt%) in 800-1000 μ m, angle of repose is 38 °, water content is 1.2wt%, The yield was 85%.

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PUM

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Abstract

The invention discloses a triethylenediamine (TEDA) crystal and a preparation method thereof. The method comprises the following steps: (1) adding a TEDA crude product into a solvent to obtain a TEDAsuspension solution; (2) heating the suspension solution obtained by step (1) to dissolving temperature of 60 to 70 DEG C to completely dissolve a solid; then slowly cooling; after separating out a seed crystal, culturing the crystal for 0.5 to 2 hours at a place with the temperature which is 2 to 4 DEG C lower than the dissolving temperature; (3) after finishing constant-temperature crystal culture, continually cooling to 20 to 30 DEG C, preferably 23 to 28 DEG C; filtering and drying to obtain the TEDA crystal. The granularity of 85 weight percent or more of the TEDA crystal is 800 to 1,000mu m, the purity is 99.3 to 99.8 weight percent, the water content is lower than 2 weight percent and the repose angle is 36 degrees to 40 degrees. The TEDA crystal has the advantages of large particles, good mobility, poor moisture absorption, easiness for separation and drying, and meets the requirements of transportation and storage.

Description

technical field [0001] The invention belongs to the technical field of industrial crystallization, and in particular relates to a triethylenediamine crystal with high purity, large particles, good fluidity and high yield and a preparation method thereof. Background technique [0002] Triethylenediamine (CAS: 280-57-9), chemical name is 1,4-diazabicyclo[2,2,2]octane, English name is triethylenediamine, abbreviated as TEDA, DABCO, molecular formula: C 6 h 12 N 2 , The relative molecular weight is 112.7. [0003] TEDA is a tertiary amine compound with a diheterocyclic structure. It is mainly used as a gel catalyst for polyurethane foams. It is widely used in soft, semi-rigid, and rigid polyurethane foams and elastomers. In addition, it can also be used as a ring Oxygen resin curing catalysts, ethylene polymerization catalysts, acrylonitrile polymerization catalysts and ethylene oxide hydrocarbon polymerization catalysts, initiators for the production of pesticides such as he...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/08
CPCC07D487/08
Inventor 龚俊波张聪颖许史杰刘振国全煜峰王小龙陈浩华卫琦
Owner WANHUA CHEM GRP CO LTD
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