A kind of new crystal form of anilinoacetonitrile and preparation method thereof

A technology of anilinoacetonitrile and crystal form, which is applied in the field of new crystal form of anilinoacetonitrile and its preparation, can solve the problems of fragile, easy to harden, products with poor flow properties, etc., and achieve small particle size difference, high yield, Good product quality

Active Publication Date: 2017-03-01
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current anilinoacetonitrile granule products are fragile, easy to harden during transportation, have poor fluidity, and have certain limitations in transportation and use of the product; the granules have high water content and must be stored under dry and ventilated conditions. The melting point is Around 40°C, the maximum temperature during storage and transportation should be less than 35°C, keep away from fire sources, avoid direct sunlight, and have strict storage conditions

Method used

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  • A kind of new crystal form of anilinoacetonitrile and preparation method thereof
  • A kind of new crystal form of anilinoacetonitrile and preparation method thereof
  • A kind of new crystal form of anilinoacetonitrile and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] In a four-neck flask equipped with a reflux condenser, a thermometer, an agitator, and a constant pressure dropping funnel, add aniline (94.0g, content 99%, 1mol), sodium carbonate (1.1g, content 99%, 0.01mol) , stir and heat to 105°C, add dropwise 50% aqueous solution of hydroxyacetonitrile (119.7g, 1.05mol) between 105°C and 110°C at temperature control, keep warm for 2 hours after the dropwise addition, take samples, analyze the aniline content of 0.7% by GC, stop the reaction , stop stirring, let the reaction solution stand still for 0.5h, separate the organic phase, cool down to 43°C, the organic phase enters the spray cooling device, and cool the spray droplets with cold air at about 8°C countercurrently, and cool for 6-9s to 24 -26°C, collect the cooled solid to obtain 129.6 g of yellow-brown anilinoacetonitrile crystals, with a content of 99.3% and a yield of 97.5%, all in terms of mass percentage.

Embodiment 2

[0039] With the anilinoacetonitrile crystal that embodiment 1 makes, do XRD test:

[0040] The radiation source is a Cu target, the wavelength is 1.54060nm, the scanning angle is 10°-80°, the voltage is 35kV, the current is 25mA, and the scanning speed is 2.4° / min. Its X-ray powder diffraction pattern is as figure 1 shown.

[0041]The crystalline anilinoacetonitrile crystal form has diffraction angles 2θ at 15.440±0.2°, 22.800±0.2°, 24.639±0.2°, 18.368±0.2°, 27.087±0.2°, 31.124±0.2°, 16.684±0.2°, 22.367 There are diffraction peaks at ±0.2°, 28.839±0.2°, and 23.646±0.2°.

[0042] Crystalline anilinoacetonitrile of the present invention, its powder X-ray diagram expresses with interplanar distance D, Bragg angle (2θ), percentage I (%) of relative intensity and intensity (I value) crystal form, as follows:

[0043]

[0044] The differential scanning calorimetry (DSC) diagram of crystalline anilinoacetonitrile figure 2 As shown, its endothermic transition temperature is 47...

Embodiment 3

[0047] A kind of preparation method of anilinoacetonitrile crystal form, adopts following steps:

[0048] Preliminarily cool the organic phase of the anilinoacetonitrile reaction solution obtained in the synthesis process to 50°C; use a spray cooling device to carry out spray cooling and granulation of the organic phase after the preliminary cooling, and pass in 10°C cold air to countercurrently cool the spray droplets , cooled for 16s and cooled to 25°C, collected the cooled solid to obtain yellow-brown crystals, which were identified by the method of Example 2, which was the new crystal form of anilinoacetonitrile of the present invention.

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Abstract

A novel crystal form of n-phenylglycinenitrile has diffraction peaks at the degrees of 2theta, 15.440+ / -0.2, 22.800+ / -0.2, 24.639+ / -0.2, 18.368+ / -0.2, 27.087+ / -0.2 and 31.124+ / -0.2. The novel crystal form of n-phenylglycinenitrile is used for producing n-Phenylglycine potassium salt, and the obtained product is good in quality and high in yield. The melting point peak temperature of the crystal form of the n-phenylglycinenitrile is high at 47-48 degrees Centigrade, product stability is good and successive storage, and production and utilization are facilitated. The n-phenylglycinenitrile in the crystal form is round-like, uniform in shape and small in grain diameter difference. Meanwhile, the crystal form of the n-phenylglycinenitrile is excellent in processing mobility performance and solves the technical problems of easy clotting, dust splashing during transport and inconvenience in use and the like of existing n-phenylglycinenitrile products. In addition, the preparation of the novel crystal form overcomes the problem of high water consumption by crystallization of the prior art and is clean and environment friendly.

Description

technical field [0001] The invention relates to a new crystal form of anilinoacetonitrile and a preparation method thereof. Background technique [0002] The molecular formula of N-Phenylglycinonitrile is C 8 h 8 N 2 , khaki or tan powder, hardly soluble in water, easily soluble in acetone; mainly used in the production of potassium anilinoacetate to synthesize the dye indigo, for denim dyeing, and can also be used in other organic synthesis. [0003] Patent CN 102627581A reports a preparation process of N-anilinoacetonitrile, discloses a synthesis method, cooling to 30-50°C for crystallization, this process greatly reduces the amount of catalyst used, fully recovers the organic matter in the mother liquor, and completely solves the problem of The treatment of production wastewater improves the yield and saves the cost. Patent CN 101613306A discloses a production method of environment-friendly anilinoacetonitrile, which discloses synthesis, cooling to 45°C for crystalliz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/25C07C253/34
Inventor 丁永良徐代行郑道敏幸勇张正伟陈薛强韩永松姚如杰柳亚玲金海琴
Owner CHONGQING UNISPLENDOUR CHEM
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