Pentanediamine sebacate and crystal thereof

A technology of pentamethylenediamine sebacate and pentamethylenediamine, which is applied to the preparation of carboxylate, separation/purification of carboxylic acid compounds, preparation of amino compounds, etc.

Inactive Publication Date: 2018-09-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report about the polymerized monomer raw material of nylon 510 - pentamethylenediamine sebacic acid cry...

Method used

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  • Pentanediamine sebacate and crystal thereof
  • Pentanediamine sebacate and crystal thereof
  • Pentanediamine sebacate and crystal thereof

Examples

Experimental program
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Embodiment 1

[0068] Add 15.00 g of pentamethylenediamine into 130 g of methanol solution and stir well to form a pentamethylenediamine methanol solution. Dissolve 29.69g of sebacic acid in 350g of methanol, drop it into the methanol solution of pentamethylenediamine at a flow rate of 2mL / min at 25°C, crystallize while stirring, and monitor the pH changes in the process, and the pH is around 10.5 , add 0.15g seed crystals, suspend feeding, after crystal growth for 3 hours, drop sebacic acid methanol solution into the crystallization system at a flow rate of 0.7mL / min, continue stirring for 2 hours after the feeding is complete, put it into the tank, and pump The solid-liquid separation of the crystal paddle was carried out by filtration, and then washed with 80-100 mL of methanol, and then vacuum-dried at 45°C for 8 hours to obtain pentamethylenediamine sebacate crystalline powder. The powder X-ray diffraction pattern is as follows: Figure 4 As shown, the diffraction angle 2θ±0.1 is express...

Embodiment 2

[0070] Add 15.00 g of pentamethylenediamine into 100 mL of 90% ethanol aqueous solution (the volume fraction of ethanol is 90%), and fully stir to form an ethanol aqueous solution of pentamethylenediamine. 35g sebacic acid solids are added in 350mL 90% ethanol water solution (ethanol volume fraction is 90%), form the ethanol water solution of sebacic acid, then the two are mixed in the 500mL crystallizer, control temperature at 25 ℃, stir After 48 hours, a white crystal substance appeared, put it into the tank, and separated the solid and liquid by suction filtration, washed the solid with 150mL of 95% ethanol, then dried the solid in microwave for 8 hours, and maintained the temperature at 45-60°C to obtain pentamethylenediamine sebacate Crystalline powder, the powder X-ray pattern of the product is as attached Figure 4 As shown, the diffraction angle 2θ±0.1 is expressed as: 19.96, 24.06, 9.62, 27.28, 25.42, 21.08, 24.48, 11.06, 26.14, 23.68, 30.52, etc., as attached Figure...

Embodiment 3

[0072] Dissolve 45.00g of sebacic acid in 500g of absolute ethanol to form a uniform sebacic acid ethanol solution, and then transfer it into a 1000mL crystallizer. 30.00 g of pentamethylenediamine was dissolved in 300 mL of 95% acetone-water (acetone accounted for 95% by volume) solution to form an aqueous solution of pentamethylenediamine-acetone. Then the aqueous solution of pentamethylenediamine acetone is dripped in the ethanol solution of sebacic acid with the mode of 3mL / min with the pump, when the amount of the substance of the pentamethylenediamine added is 20% of the amount of the substance of sebacic acid, add 0.3g For seed crystals, add the remaining pentamethylenediamine acetone aqueous solution at 0.3mL / min. The whole process is carried out under stirring, and the temperature is controlled at 50°C. After the end, go to the tank for solid-liquid separation, and then wash the filter cake with 100mL of absolute ethanol, and dry it under microwave vacuum at 35-45°C f...

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Abstract

The invention discloses pentanediamine sebacate, and a crystal and a preparation method thereof. The pentanediamine sebacate is a salt which is in a solid state at normal temperature and is formed bycombining pentanediamine divalent cations with sebacic acid divalent anions in a molar ratio of 1: 1. The crystal of the pentanediamine sebacate has a structure of C11H24N2O4, belongs to a monocliniccrystal system, has a space group of C2, and comprises the following cell parameters: a is 20.0833(18) angstroms; b is 8.5161(9) angstroms; c is 5.3379(7) angstroms; beta is 92.394(2) degrees; a unitcell volume V is 912.15(17) angstroms<3>; and the number of smallest asymmetric units in a unit cell Z is 2. The preparation method comprises the following steps: crystallization of pentanediamine sebacate from a solution containing dissolved pentanediamine and sebacic acid, separation of the crystal from the solution, and drying of the separated crystal.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to monomer pentamethylenediamine sebacate of bio-based nylon 510, its crystal structure, its crystal powder, and its preparation method. Background technique [0002] Polyamide ranks first among the five major engineering plastics due to its good mechanical properties, heat resistance, wear resistance, chemical corrosion resistance, and self-lubrication. It is widely used in aviation, packaging materials, textiles, household appliances, Auto parts manufacturing and medical and other fields. At present, the main varieties are polyamide 6 and polyamide 66. Among them, the monomer of polyamide 6 is crystalline powder caprolactam, and the monomer of polyamide 66 is hexamethylenediamine adipate crystal. Both polyamide 6 and polyamide 66 are produced chemically from petroleum. In recent years, the domestic biological preparation technology of pentamethylenediamine h...

Claims

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Application Information

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IPC IPC(8): C07C209/86C07C211/09C07C209/00C07C51/41C07C51/43C07C55/20
CPCC07C55/20C07C211/09C07B2200/13
Inventor 杨朋朋应汉杰李子涵王森李晓洁黎青青吴菁岚陈勇欧阳平凯
Owner NANJING UNIV OF TECH
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