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Continuous synthesis method of polyamide and vertical multi-stage reactor

A synthesis method and technology of polyamide, which are applied in the field of continuous synthesis of polyamide and vertical multi-stage reactors, can solve the problems of scarring on the wall of the reactor, surge in heat load, high viscosity of materials, etc., and reduce investment and maintenance expenses. , the effect of reducing energy requirements and low gas phase pressure

Active Publication Date: 2019-05-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned process is the mainstream of the continuous polymerization process of nylon 66 at present, and has the following disadvantages: 1. The process is lengthy, and the construction investment and operation costs are high; 2. The high-pressure precondensation stage uses a tubular reactor, and the entire reaction process maintains a high pressure, which is not conducive to The evaporation of the reaction product water limits the growth of the polyamide molecular weight in terms of chemical balance; 3. It takes a long reaction time for the flash pressure to drop from more than 15 atm to normal pressure, and the viscosity of the material in the process is large, and the condensation water It is not easy to evaporate, which restricts the increase of the molecular weight of polyamide; 4. During the flash evaporation process, the polyamide entrained with the evaporation of condensation water and the fluctuation of the reaction liquid level are likely to cause scarring on the reactor wall, and subsequent cleaning is troublesome
However, in order to ensure that the liquid phase flows from the top of the tower to the bottom of the tower, the gas phase is in contact with the liquid phase retrogradely from the top of the tower, and the pressure of the whole tower gradually increases from top to bottom, resulting in the following defects: 1. The pressure at the inlet of the liquid phase is relatively small , a large amount of water evaporates, and the heat load will increase sharply in order to maintain the temperature required for the reaction; 2. The lower pressure in the upper part of the reactor will cause a large amount of diamine to evaporate, which will affect the condensation reaction; 3. The rapid liquid phase in the upper part of the reactor There is a risk of unreacted polyamide salt precipitation in concentration; 4. The polyamide product flows out of the tower kettle at a relatively high pressure, and it is still necessary to configure a decompression device with a long residence time to enter the subsequent normal pressure or vacuum polycondensation reactor react

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  • Continuous synthesis method of polyamide and vertical multi-stage reactor
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  • Continuous synthesis method of polyamide and vertical multi-stage reactor

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preparation example Construction

[0025] The invention provides a continuous synthesis method of polyamide. The method is as follows: a solution containing polyamide brine is used as a liquid phase stream, and a gas containing inert gas, water vapor, and diamine is used as a gas phase stream to perform a multistage reaction. Polyamide is synthesized, wherein, the flow direction of the liquid phase stream A and the gas phase stream B are the same, and along the flow direction, the gas phase pressure of each stage of reaction decreases step by step. In the early stage of the reaction, the higher gas phase pressure can avoid the escape of a large amount of diamine and water, ensuring the complete reaction of the polyamide salt; in the later stage of the reaction, the gas phase pressure is low, which is beneficial to remove the water in the reaction system and promote the increase of the polyamide molecular weight. increase. This reaction mode of parallel flow and gradually decreasing air pressure makes the degree...

Embodiment 1

[0038] A nylon 66 salt solution with a temperature of 215°C and a concentration of 69% is injected into the tower multi-stage reactor, and the temperature of the first-layer evaporator in the first stage of the reaction is controlled at 216°C and the pressure is 20atm. The gas phase stream and the liquid phase stream pass through 3 sets of evaporators and decompression units, the operating temperature gradually rises to 238°C, and the pressure drops to 12.6 atm. The reaction material is injected into the second stage to continue the reaction. The second stage consists of two sets of evaporators and a decompression unit. The operating temperature is gradually increased from 238°C to 280°C, and the operating pressure is reduced to 1 atm. The rectification device adopts plate rectification tower equipment, the reflux ratio of condensed water at the top of the tower is 0.16, and the recovered hexamethylene diamine material is evenly distributed to the second stage of the reaction. ...

Embodiment 2

[0041] Inject the nylon 66 salt solution with a temperature of 200°C and a concentration of 60% into the tower multi-stage reactor. The temperature of the first-layer evaporator in the first stage of the reaction is controlled at 216°C and the pressure is 18atm. The gas-phase stream and the liquid-phase stream pass through two sets of evaporators and a decompression unit, the operating temperature gradually rises to 232°C, and the pressure drops to 14atm. The reaction material is injected into the second stage to continue the reaction. The second stage consists of two sets of evaporators and a decompression unit. The operating temperature is gradually increased from 238°C to 260°C, and the operating pressure is reduced to 6atm. The rectification device adopts plate rectification tower equipment, the reflux ratio of condensed water at the top of the tower is 0.16, and the recovered hexamethylene diamine material is injected into the two trays of the second stage according to the...

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Abstract

The invention provides a continuous synthesis method of polyamide in a manner of parallel flowing of gas and liquid phases with step-by-step reduction on pressure of the gas phase, so that escape of alarge quantity of diamine and water in the early-stage of the reaction can be avoided, and complete reaction of polyamide salt is guaranteed. In the later period of the reaction, the gas phase pressure is low, so that water in the reaction system can be removed easily and increase of molecular weight of the polyamide is promoted; wherein the polymerization degree of a product can reach 20-60, thus relieving or eliminating the requirement on following pressure-reducing apparatuses. The invention further provides a reactor for carrying out the method, which has the advantages of improving reliability of the reaction process, reducing damage on energy and reducing equipment cost and repair cost.

Description

technical field [0001] The present invention relates to a continuous polymerization method for producing polyamide and an apparatus capable of performing the polymerization method. More precisely, the present invention relates to a continuous polyamide synthesis method and a vertical multi-stage reactor. Background technique [0002] Processes for the continuous production of polyamide materials such as Nylon 66 are known in the prior art, and a traditional production process involves the use of 3-5 different reaction vessels connected in series. The production of polyamide materials by these methods needs to be completed through multiple reaction steps. These steps are usually carried out in tubular reactors or stirred tanks, mainly including processes such as evaporation concentration, high-pressure pre-condensation, flash evaporation, atmospheric final polycondensation and vacuum polycondensation. And these steps are performed separately from each other in space. Page 5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G69/26
Inventor 刘天奇王嘉骏顾雪萍冯连芳
Owner ZHEJIANG UNIV