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Method for preparing C14 diamine and long carbon chain nylon PA1414

A technology of PA1414 and tetradecane dibasic acid, applied in the field of polymer synthesis, can solve the problems of high energy consumption and harsh reaction conditions, and achieve the effects of simple equipment, short production cycle and low glass transition temperature

Inactive Publication Date: 2015-03-25
HENAN JUNHENG IND GRP BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent 02144535.4 discloses a preparation method of long carbon chain nylon, which uses long carbon chain dibasic acid as the main raw material to synthesize a series of long carbon chain nylon, including the preparation process conditions of nylon 1414. The process method has harsh reaction conditions and high energy consumption, so it must be further improved and perfected to meet the needs of industrial production

Method used

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  • Method for preparing C14 diamine and long carbon chain nylon PA1414
  • Method for preparing C14 diamine and long carbon chain nylon PA1414
  • Method for preparing C14 diamine and long carbon chain nylon PA1414

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Effect test

Embodiment 1

[0028] A method for preparing tetradecanediamine, comprising the steps of:

[0029] (1) Amination reaction: Add 1000kg of tetradecanedibasic acid into the ammoniation reactor, and add silica gel particles soaked in phosphoric acid as a catalyst. The dosage is 0.1% of the weight of tetradecanedioic acid, of which The content of tetradecanedibasic acid is 0.025% of the weight of tetradecanedibasic acid. When the temperature is raised to 160°C, the flow rate of ammonia gas is controlled to be 20-25m 3 / h, the temperature is raised to 310°C within 5h stepwise, and the ammonia gas is continuously introduced, and the flow rate of the ammonia gas is controlled to be 0.5~3m 3 / h, carry out insulation 2h, then this reactant is squeezed in the thick nitrile storage tank with pump, leaves standstill and separates out catalyst recovery, then sucks thick nitrile in the distillation still with vacuum, finally vacuumizes and depressurizes to-0.098MPa, Simultaneously heat up, when still temp...

Embodiment 2

[0040] A method for preparing tetradecanediamine, comprising the steps of:

[0041] (1) Amination reaction: Add 1000kg of tetradecanedibasic acid into the ammoniation reactor, and add silica gel particles soaked in benzenesulfonic acid as a catalyst, the dosage is 0.2% of the weight of tetradecanedioic acid, The content of benzenesulfonic acid is 0.04% of the weight of tetradecanedibasic acid, the temperature is raised to 150°C, ammonia gas is introduced, and the flow rate is controlled at 20-25 m 3 / h, within 5 hours, the temperature is raised to 305°C step by step, and the ammonia gas is continuously introduced, and the flow rate of the ammonia gas is controlled at 0.5-4m 3 / h, keep warm for 2h, then pump the reactant into the thick nitrile storage tank, let it stand to separate the catalyst, then suck it into the still with vacuum, finally vacuumize and depressurize to -0.098MPa, and heat Raise the temperature, when the temperature of the kettle rises to 260°C, the tempera...

Embodiment 3

[0048] A method for preparing tetradecanediamine, comprising the steps of:

[0049] (1) Amination reaction: Add 1000kg tetradecanedibasic acid into the ammoniation reactor, and add silica gel particles soaked in p-toluenesulfonic acid as a catalyst, and the dosage is 0.5% of the weight of tetradecanedibasic acid , wherein the content of p-toluenesulfonic acid is 0.05% of the weight of tetradecanedibasic acid, the temperature is raised to 155°C, ammonia gas is introduced, and the flow rate is controlled at 20-25m 3 / h, at the same time, the temperature is raised to 310 ° C in steps within 5 hours, and the ammonia gas is continuously introduced, and the flow rate of the ammonia gas is controlled to be 0.5 ~ 3m 3 / h, keep warm for 2h, then pump the reactant into the thick nitrile storage tank, let it stand and separate the catalyst for recovery, then use vacuum to suck it in the distillation still, and finally vacuumize and depressurize to -0.096MPa. Heating to raise the tempera...

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Abstract

The invention discloses a method for preparing C14 diamine and long carbon chain nylon PA1414, and belongs to the technical field of macromolecular synthesis. The method comprises the steps of: preparation of C14 dinitrile by ammoniating C14 diacid, hydrogenation preparation of C14 diamine by C14 dinitrile, preparation of nylon 1414 salt by neutralizing C14 diacid and C14 diamine and polymerization of nylon 1414. In a process of preparing C14 dinitrile by ammoniating C14 diacid, C14 diacid is mixed with a catalyst; then, the temperature rises to 150-160 DEG C; ammonia gas is introduced into the mixture for performing dehydration reaction; the temperature rises to 290-310 DEG C within 5-6 hours step by step; ammonia gas is continuously introduced, wherein the flow of the ammonia gas is controlled to be 0.5-5 M<3> / h; the heat insulation reaction is carried out for 1-2 hours, and reduced pressure distillation is then carried out to obtain the C14 dinitrile. The method for preparing C14 diamine and the nylon 1414has the advantages of use of easily available raw materials, short processes, short production period, mild reaction conditions, simple equipment, high yield, low energy consumption and therefore is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of tetradecanediamine, and also relates to a preparation method of long carbon chain nylon 1414. Background technique [0002] Nylon (Nylon) is called Polyamide (PA for short). It is one of the five major engineering plastics. It has excellent mechanical and physical properties, wear resistance, self-lubricating properties, oil resistance, and temperature resistance. A thermoplastic engineering plastic. Nylon containing less than 10 carbon chains is usually called short carbon chain nylon, mainly nylon 6 and nylon 66, accounting for about 80% of the total nylon; nylon containing more than 10 carbon chains is called long carbon chain nylon , mainly nylon 11, nylon 12, nylon 1212. In many applications, the comprehensive performance of long carbon chain nylon is superior to that of short carbon chain nylon, so the development is the faste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/09C07C253/22C07C255/04C08G69/26C08G69/28
Inventor 张振国张振辉杨韶辉高元英吴自胜
Owner HENAN JUNHENG IND GRP BIOTECH CO LTD
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