Pentanediamine dodecanedioate and crystal thereof

The technology of pentamethylenediamine dodecanedioic acid salt and dodecanedioic acid is applied in the field of crystallization of bio-based material monomers, and can solve the problems of affecting the purity of pentamethylenediamine itself, inconvenient transportation and use process, etc.

Active Publication Date: 2019-01-25
NANJING UNIV OF TECH
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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 irritating odor similar to ammonia gas. 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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  • Pentanediamine dodecanedioate and crystal thereof
  • Pentanediamine dodecanedioate and crystal thereof
  • Pentanediamine dodecanedioate and crystal thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Add 15.00 g of pentamethylenediamine into 150 g of methanol and stir well to form a pentamethylenediamine methanol solution. Put 25.00 g of dodecanedioic acid in 200 g of methanol, stir evenly, mix the two in a 500 mL crystallizer at room temperature, control the stirring rate at 250-400 rpm, stir for 60 h, put it into the tank, and filter it with suction to carry out crystal paddle solid-liquid separation, and then washed with 60-80mL of anhydrous methanol, and then air-dried at 100°C for 10 hours to obtain pentamethylenediamine dodecanedioate crystalline powder with a water content of less than 0.5%, which was prepared as a mass fraction When it is 5% aqueous solution, the pH value of the system is 7.2.

Embodiment 2

[0085] Add 10.00 g of pentamethylenediamine into 20 mL of water, and stir well to form an aqueous solution of pentamethylenediamine. Add 16.67g of dodecanedioic acid solid into 100mL of water, stir and mix well, then mix the two in a 1000mL crystallizer, use a three-blade propulsion stirrer, control the stirring speed at 280-500rpm, and control the temperature at Stir at 50°C for 1 hour, then slowly drop absolute ethanol into the system, control the flow rate at 0.5mL / min until 5 times the volume of ethanol is added, stop adding, continue stirring, and start to cool down at a rate of 2°C / h , when the temperature drops to 10°C, continue to stir for 5 hours. After the crystallization is completed, put it into the tank and perform solid-liquid separation by suction filtration. Wash the solid with 200mL of 95% ethanol, then put it in an environment of 45°C, and dry it by air for 8 hours. , to obtain the crystalline powder of pentamethylenediamine dodecanedioate, which contains 2 c...

Embodiment 3

[0087] Dissolve 30.00g of dodecanedioic acid in 500g of DSMO-isopropanol (the mass ratio of DSMO to isopropanol is 2:1) to form a uniform dodecanedioic acid DSMO-isopropanol solution, and then transfer it to 1000mL crystallizer. 18.00 g of pentamethylenediamine was dissolved in 200 mL of 95% acetone-water (acetone accounted for 95% by volume) solution to form an aqueous solution of pentamethylenediamine-acetone. Then use a pump to drip pentanediamine acetone aqueous solution into the dodecanedioic acid DSMO-isopropanol solution at a rate of 2 mL / min, when the amount of the added pentamethylenediamine is the amount of dodecanedioic acid 17%, stop feeding, stir for 2h, and then add the remaining pentamethylenediamine acetone aqueous solution at a flow rate of 0.2mL / min. The whole process is carried out under stirring, and the temperature is controlled at 30°C. Cool down to 10°C at a rate of 2°C / h. After the crystallization is complete, put it into the tank for solid-liquid sepa...

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Abstract

The invention discloses pentanediamine dodecanedioate, a crystal thereof, crystalline powder thereof and a preparation method thereof. The pentanediamine dodecanedioate is a salt which is formed in the manner of combining the divalent cation of pentanediamine with the divalent anion of dodecanedioic acid in a mole ratio of 1 to 1 and presents a solid state at normal temperature. The crystal structure of the pentanediamine dodecanedioate is C17H36N2O4.nH2O, belongs to a triclinic system and has a space group P-1; a is equal to 8.4747(7) angstroms; b is equal to 8.5175(7) angstroms; c is equal to 15.3901(14) angstroms; alpha is equal to 82.473(2) degrees; beta is equal to 78.06(10) degrees; gamma is equal to 86.313(2) degrees; the volume V of a crystal cell is equal to 1076.71(16) angstroms;and a minimal asymmetric unit number Z in the crystal cell is equal to 2. According to the pentanediamine dodecanedioate, the existing form of the pentanediamine is changed; the stability of a product is improved; and an original foul odor is greatly decreased.

Description

technical field [0001] The invention belongs to the technical field of crystallization of bio-based material monomers, in particular, it relates to monomer pentamethylenediamine dodecanedioate of bio-based nylon 512, its crystal structure, its crystal powder, and its preparation method . Background technique [0002] Currently, the monomers used to produce nylon are mainly obtained through chemical processing and are derivatives of fossil resources. With the depletion of fossil resources and the strengthening of people's awareness of environmental protection, bio-based environmentally friendly materials have begun to receive more attention. The development of biomass-based fibers (especially biomass synthetic fibers) is in line with the trend of social development in terms of both resources and the environment: on the one hand, it can replace fossil raw materials and reduce excessive dependence on petroleum resources; on the other hand Realize the substitution of chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/09C07C51/41C07C55/21
CPCC07B2200/13C07C51/412C07C55/21C07C209/00C07C211/09
Inventor 杨朋朋应汉杰李子涵吴菁岚庄伟王森李晓洁黎青青欧阳平凯
Owner NANJING UNIV OF TECH
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