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Process of producing dimer acid amide nylon

A dimer acid amide and production process technology, which is applied in the production process field of new dimer acid amide nylon, can solve the problems of consumption of organic solvents, environmental pollution, etc., and achieve the effects of simple process, good low temperature performance and abundant raw material sources

Inactive Publication Date: 2009-10-07
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitation of raw materials and technology in China, there is no research report
[0004] Prior art such as Chinese patent 1302826 discloses a kind of synthetic method of dimer acid amide of low molecular weight, by adding alkane, aromatic hydrocarbon, ester, ketone or their mixture which are miscible with reaction materials in the reaction system at the initial stage of reaction, Reduce the viscosity of the reaction system, promote the surface renewal of the reaction interface, facilitate the removal of small molecules such as water molecules, prevent system agglomeration caused by excessive volume expansion and uneven heating, and greatly shorten the time required for this stage , but this method consumes organic solvents and has environmental pollution problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 181.0g of hexamethylenediamine, 205.6g of adipic acid, 10.2g of stearic acid, and 280.0g of dimer acid with a dimer content of 95.5% were added to a 2L stainless steel reaction kettle, stirring and N 2 Heating to 60°C under protective conditions, forming salt and precondensing for 1 hour under constant stirring at this temperature.

[0015] The temperature was programmed to rise to 380°C within 5 hours, and melt polycondensed for 9 hours, then 38.70g of molten hexamethylenediamine was added to the kettle to adjust the stoichiometric ratio, and then the reaction system was depressurized, and reacted at 380°C and 420Pa for 1.5 hours. , press into 0.8MPa N 2 Gas, open the discharge cock, and after discharging, cooling, and pelletizing, a new type of dimer acid amide nylon product is obtained, with a number-average molecular weight of 45,100g / mol.

Embodiment 2

[0017] Add 2086.7g of hexamethylenediamine adipate, 1048.2g of water, 20.6g of propylamine and 746.5g of an aqueous solution containing 32.5% of hexamethylenediamine into a 10L stainless steel reaction kettle, and stir under N 2 Under the conditions of protection and 7.0MPa atmospheric pressure, the temperature was programmed to rise within 1 hour and the pressure was released slowly. The temperature reached 210°C and the atmospheric pressure at the same time.

[0018] Then drop 1140.2g of dimer acid with a dimer content of 98.9% at this temperature within 3.5 hours, continuously stir and melt and polycondense for 4 hours, separate out 1320.4g of water, and finally depressurize the reaction system and react at 210°C and 560Pa After 2 hours, press into 0.5MPa N 2 Gas, open the discharge cock, after discharging, cooling, and pelletizing, a new type of dimer acid amide nylon product is obtained, with a number-average relative molecular weight of 6,320g / mol.

Embodiment 3

[0020] Add 169.65g of adipic acid and 253.4g of dimer acid with a dimer content of 98.9% into a 1L stainless steel reactor, stir vigorously and N 2 Under protective conditions, it was gradually heated to 120°C. At this temperature, the molten material of 167.55g of hexamethylenediamine and 2.75g of diethanolamine was dropped into the kettle within 10 minutes, and it was continuously stirred to form a salt and pre-condensed for 5.5 hours.

[0021] The temperature was programmed to rise to 300°C within 0.5 hours, and melt polycondensed for 2 hours, then 17.21g of molten hexamethylenediamine was dropped into the kettle within 0.5 hours to adjust the stoichiometric ratio. After reacting at 1000Pa for 17.5 hours, press in 0.4MPa of N 2 Gas, open the discharge cock, after discharging, cooling, and pelletizing, a new type of dimer acid amide nylon product is obtained, with a number-average relative molecular weight of 27,126g / mol.

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Abstract

The invention discloses a novel production process of dimer acid amide nylon. The process is simple, the reaction is stable, and the molecular weight distribution range of the product is narrow. It can be flexibly adjusted in the range of 5,000-45,000 g / mol by changing process parameters and operating conditions as required. Nylon number average relative molecular mass size. This process uses high-purity dimer acid, one or more dibasic amines, dibasic acids, and molecular weight modifiers as comonomers, and puts them into the reaction kettle at a certain molar ratio, and forms a salt at a temperature of 50-400°C. , precondensation, polycondensation, and then remove moisture and free monomers under high vacuum conditions, and further chain growth, gradually complete the bulk polymerization process, and finally discharge and pelletize to obtain a new type of dimer acid amide nylon resin.

Description

technical field [0001] The present invention relates to a kind of production technology of novel nylon, relate to a kind of production technology of novel dimer acid amide nylon more specifically. Background technique [0002] Long-chain nylon has the physical and chemical properties of short-chain nylon and polyolefin, and has the characteristics of long main chain, low amide group density, and many disordered areas, so it is soft, transparent, light, low water absorption, and stable in molding. The general concern of the industry is the variety of engineering plastics with a wide range of uses. The long-chain nylons currently developed and produced in China include nylon 11, 12, 612, 613, 1212, 1013, 1311 and so on. [0003] The dimer acid molecule contains 36 carbon atoms. It is the longest dicarboxylic acid in the main chain. It also contains two large branch chains. It is used to prepare dimer acid amide nylon. In addition to the common characteristics of long-chain ny...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/28
Inventor 姚成王晓辉司南
Owner NANJING TECH UNIV
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