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Dodecanedioic acid crystal and preparation method thereof

A dodecanedibasic acid and crystal technology, applied in organic chemistry methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of insufficient nylon polymerization degree, easy agglomeration bulk density, instability, etc.

Pending Publication Date: 2020-10-30
INST OF MICROBIOLOGY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the application of dodecane dibasic acid is becoming more and more widespread, there are still some difficult problems in the actual production and application: (1) long-chain dibasic acid product crystals prepared by biological fermentation and purified by recrystallization Poor particle size, easy agglomeration and unstable bulk density; (2) Although the purity of dodecanedibasic acid is sufficient, the degree of polymerization in nylon production is not enough, etc.

Method used

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  • Dodecanedioic acid crystal and preparation method thereof
  • Dodecanedioic acid crystal and preparation method thereof
  • Dodecanedioic acid crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Heat dodecanedibasic acid and water in a hydrothermal reactor at a mass volume ratio of 1:50 to 95°C, maintain for 2 hours, then slowly cool down at a rate of 1°C / 0.5h, and turn on the water heater when the temperature is lowered to 60°C Reactor, obtain the crystal of described dodecane dibasic acid. The crystal size of the crystal in this embodiment is well controllable, the size range of the crystal size is 100-200 mesh, the crystal is not easy to agglomerate, the bulk density of the crystal is 0.75g / cm3, and the bulk density distribution is stable.

[0025] The structure of gained crystal is analyzed and it is analyzed (its spectrogram is as figure 1 , figure 2 and image 3 shown), the dodecane dibasic acid crystal belongs to the monoclinic system, and the space group is P2 1 / c, the cell parameters are: α=γ=90°, β=97.344(2)°; unit cell volume The number of molecules in the unit cell is Z=2. Its XRD characteristic diffraction peaks appear at 6.82°±0.1, 13....

Embodiment 2

[0027] Compared with Example 1, the distinguishing technical feature is that the specific conditions for crystal preparation are to heat dodecanedioic acid and water in a hydrothermal reactor at a mass volume ratio of 1:60 to 95°C for 2 hours, and then Slowly lower the temperature at a rate of 3° C. / 0.5 h, and turn on the hydrothermal reaction kettle when the temperature is lowered to 80° C. to obtain crystals of the dodecanedioic acid.

[0028] In this embodiment, the crystal particle size ranges from 150 to 220 meshes, the crystals are not easy to agglomerate, the crystal bulk density is 0.7 g / cm3, and the bulk density distribution is stable.

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Abstract

The invention belongs to the technical field of crystal preparation, in particular to a dodecanedioic acid crystal and a preparation method thereof. The method specifically comprises the following steps: putting dodecanedioic acid and water into a hydrothermal reaction kettle, heating to 85-100 DEG C, keeping the temperature for more than 1 hour, slowly cooling at the speed of less than or equal to 3 DEG C / 0.5 hour, and opening the hydrothermal reaction kettle when the temperature is 50-80 DEG C, thereby obtaining the crystal. The dodecanedioic acid crystal prepared by the method is good in crystal particle size controllability and is not easy to agglomerate; the crystal bulk density is high and the bulk density distribution is stable.

Description

technical field [0001] The invention belongs to the technical field of crystal preparation, in particular to a crystal of dodecanedioic acid. Background technique [0002] Since the large-scale fermentation production of dodecane dibasic acid has been realized, the application range of dodecane dibasic acid has been greatly expanded, and it is widely used in nylon production, pharmaceutical intermediates, lubricating oil and other fields. Although the application of dodecane dibasic acid is becoming more and more widespread, there are still some difficult problems in the actual production and application: (1) long-chain dibasic acid product crystals prepared by biological fermentation and purified by recrystallization Problems such as poor particle size, easy agglomeration and unstable bulk density; (2) Although the purity of dodecane dibasic acid is sufficient, the degree of polymerization in nylon production is not enough. These questions are related to the microscopic mo...

Claims

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Application Information

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IPC IPC(8): C07C55/21C07C51/43
CPCC07B2200/13C07C51/43C07C55/21
Inventor 高启合苏毅晏礼明
Owner INST OF MICROBIOLOGY - CHINESE ACAD OF SCI
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