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Pentamethylenediamine suberate and its crystals

A technology of pentamethylenediamine suberate and suberic acid, which is applied in the field of crystallization of bio-based material monomers, can solve the problems of inconvenient transportation and use, affecting the purity of pentamethylenediamine itself, and achieve convenient storage and transportation, and improve The effect of improving operability and stability

Active Publication Date: 2021-06-25
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pentylenediamine exists in the form of colorless viscous fuming liquid at normal temperature and pressure. It has a foul and pungent odor similar to ammonia. It is highly volatile and easily absorbs carbon dioxide in the air to form pentamethylenediamine carbonate. It greatly affects the purity of pentamethylenediamine. Compared with solid raw materials, it is relatively inconvenient during transportation and use

Method used

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  • Pentamethylenediamine suberate and its crystals
  • Pentamethylenediamine suberate and its crystals
  • Pentamethylenediamine suberate and its crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Add 15.00 g of pentamethylenediamine into 100 mL of 95% aqueous ethanol (volume fraction of ethanol is 95%), and stir well to form an aqueous solution of pentamethylenediamine in ethanol. Add 27.00g of suberic acid solid into 350mL of absolute ethanol aqueous solution to form an ethanol solution of suberic acid, then mix the two in a 500mL crystallizer, control the temperature at 25°C, stir for 48h, a white crystal substance appears, and then tank, and carry out solid-liquid separation by means of suction filtration, wash the solid with 150mL of 95% ethanol, and then blow dry the solid for 3 hours, and maintain the temperature at 60-80°C to obtain the crystalline powder of pentamethylenediamine suberate, the crystal structure of which is as follows: figure 2 , image 3 As shown, detailed crystallographic data such as Figure 8 As shown, the crystal structure is C 13 h 28 N 2 o 4 , monoclinic system, C2 / c space group, α=90.00°, β=117.673(4)°, γ=90.00°, unit cell ...

Embodiment 2

[0076] Add 30.00 g of pentamethylenediamine into 100 g of methanol, and stir well to form a pentamethylenediamine methanol solution. Put 51.15g of suberic acid in 500g of methanol, drop it into the methanol solution of pentamethylenediamine at a flow rate of 2mL / min at 25°C, carry out crystallization under stirring, and monitor the pH changes in the process, at about pH 11.0 , add 0.15g of seed crystals, suspend feeding, after crystal growth for 3 hours, drop suberic acid methanol solution into the crystallization system at a flow rate of 0.5mL / min, continue stirring for 2 hours after the feeding is complete, put it into the tank, and pump Carry out the solid-liquid separation of the crystal paddle by filtration, then wash with 80-100mL ethanol, and then vacuum-dry at 45°C for 8h to obtain pentamethylenediamine suberate crystalline powder, whose powder X-ray diffraction pattern is basically as follows: Figure 4 shown. When it is prepared as an aqueous solution with a mass fr...

Embodiment 3

[0078]Dissolve 50.00g of suberic acid in 500g of isopropanol to form a uniform solution of suberic acid in isopropanol, and then transfer it into a 1000mL crystallizer. 35.00 g of pentamethylenediamine was dissolved in 300 mL of 95% acetone water (acetone accounted for 95% by volume) solution to form pentamethylenediamine acetone aqueous solution. Then with the pump, the aqueous solution of pentamethylenediamine acetone is dripped in the isopropanol solution of suberic acid in the mode of 2mL / min, when the amount of the substance of pentamethylenediamine added is 15% of the amount of substance of suberic acid, add 0.3g seed crystal, add the remaining pentamethylenediamine acetone aqueous solution at 0.2mL / min, the whole process is carried out under stirring, the rotation speed is controlled at 250-400rpm, and the temperature is controlled at 15°C. When the feeding is completed, the crystallization is completed, and the tank for solid-liquid separation, and then wash the filter...

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Abstract

The invention discloses pentamethylenediamine suberate, its crystal structure, and its preparation method. The pentamethylenediamine suberate is a salt in a solid state at normal temperature formed by combining pentamethylenediamine divalent cations and suberic acid dianions in a molar ratio of 1:1. Its crystal structure is C 13 h 28 N 2 o 4 , Monoclinic system, C2 / c space group, α=90.00°, β=117.673(4)°, γ=90.00°, the minimum number of asymmetric units in the cell volume Z=4, does not contain crystal water. The preparation method comprises: crystallizing pentamethylenediamine suberate from a solution containing dissolved pentamethylenediamine and suberic acid, separating the crystals from the solution, and drying the separated crystals.

Description

technical field [0001] The invention belongs to the technical field of monomer crystallization of bio-based materials, and in particular relates to monomer pentamethylenediamine suberate of bio-based nylon 58, its crystal structure, its crystal powder, and its preparation method. Background technique [0002] Nylon 58 is a synthetic material made of bio-based pentamethylenediamine (1-5-Diaminopentane, also known as cadaverine) and petroleum-based suberic acid. In the laboratory stage, it is expected to become a new polyamide material to be introduced to the market. High-quality monomer is the key to the synthesis of high-quality nylon 58. Pentylenediamine is in the form of a colorless viscous fuming liquid at normal temperature and pressure Existence, has a stench and irritating odor similar to ammonia, is highly volatile, and is easy to absorb carbon dioxide in the air to form pentamethylenediamine carbonate, which greatly affects the purity of pentamethylenediamine itself....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/00C07C211/09C07C51/41C07C55/02
CPCC07B2200/13C07C51/412C07C55/02C07C209/00C07C211/09
Inventor 杨朋朋应汉杰李子涵王森黎青青李晓洁庄伟吴菁岚欧阳平凯
Owner NANJING TECH UNIV
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