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Polyether sulfone synthesis method with high batch stability

A synthesis method, polyethersulfone technology, applied in chemical instruments and methods, chemical/physical/physical-chemical processes, chemical/physical/physical-chemical processes of applied energy, etc. Edge, uneven coating and other problems, to achieve stable product quality control, shorten the reaction time, microwave heating uniform effect

Active Publication Date: 2021-12-17
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional methods of terminating the reaction include: (1) cooling down by adding a cold solvent to terminate the polymerization reaction, but the cooling speed of the traditional heating method is slow, and it takes about 1 hour to lower the reaction from 190°C to room temperature. During the cooling process, there are still Due to the residual heat, the molecular weight continues to increase when the reaction needs to be terminated, and the molecular weight of the product cannot be precisely controlled. There is a large gap between the termination of the polyethersulfone polymerization reaction and the molecular weight of the final product, generally between 1500-3000
(2) It is also possible to terminate the reaction by adding an end-capping agent at the end of the polyethersulfone polymerization reaction. Although this method can quickly terminate the reaction, the addition of the end-capping agent will inevitably introduce a new impurity, and this impurity is difficult to obtain. Complete removal will affect the physical and chemical properties of polyethersulfone products
[0005] (1) When there are many low-molecular-weight parts, flashing is easy to occur during injection molding, the temperature resistance of precision parts is worse, and the end of the parts will be deformed due to local heating; it is easy to break during the spinning process, and the finished product of the hollow fiber membrane rate reduction
[0006] (2) When there are many high-molecular-weight parts, the coating will be uneven when the powder is coated and melted, and there will be unmelted crystal points; poor solubility will occur during the spinning process, and the spinneret will be easily blocked.

Method used

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  • Polyether sulfone synthesis method with high batch stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] With condensing, N 2 50.5545g 4,4'-dihydroxydiphenylsulfone (M: 250.27), 57.4300g 4 ,4'-Dichlorodiphenylsulfone (M: 287.15), 27.9164g K 2 CO 3 (M: 138.2), add 470ml N,N-dimethylacetamide, set the reactor program as:

[0042] Step1: Set the temperature to 80°C; set the reaction time to 25min; set the power to 800W; set the speed to 500rpm. (extraction solvent 200mL)

[0043] Step2: Set the temperature to 130°C; set the reaction time to 2min; set the power to 700W; set the speed to 500rpm.

[0044] Step3: Set the temperature: 160°C; set the reaction time: 85min; set the power: 900W; set the speed: 600rpm.

[0045] Step4: Set the temperature: 70°C; set the reaction time: 3min; set the power: 700W; set the speed: 500rpm.

[0046] Then, the reaction polymerization liquid was filtered three times, and the polymerization liquid was precipitated in 1000 mL of water, crushed, and filtered. Afterwards, the crushed product was boiled in 100°C deionized water (600ml / time) fo...

Embodiment 2

[0048] With condensing, N 2 55.0594g 4,4'-dihydroxydiphenyl sulfone, 57.4300g 4,4'-diphenyl sulfone, 57.4300g 4,4'- Chlorodiphenylsulfone, 30.4040gK 2 CO 3 , add 470ml N,N-dimethylacetamide, set the reactor program as:

[0049] Step1: Set the temperature to 100°C; set the reaction time to 20min; set the power to 700W; set the speed to 400rpm. (extraction solvent 200mL)

[0050] Step2: Set the temperature to 130°C; set the reaction time to 2min; set the power to 700W; set the speed to 400rpm.

[0051] Step3: Set the temperature: 165°C; set the reaction time: 80min; set the power: 800W; set the speed: 450rpm.

[0052] Step4: Set the temperature: 45°C; set the reaction time: 3min; set the power: 750W; set the speed: 450rpm.

[0053] Then, the reaction polymerization liquid was filtered three times, and the polymerization liquid was precipitated in 1000 mL of water, crushed, and filtered. Afterwards, the crushed product was boiled in 100°C deionized water (600ml / time) for 5...

Embodiment 3

[0055] With condensing, N 2 60.0648g 4,4'-dihydroxydiphenyl sulfone, 57.4300g 4,4'-dichloro Diphenylsulfone, 33.1680gK 2 CO 3 , add 470ml N,N-dimethylacetamide, set the reactor program as:

[0056] Step1: Set the temperature to 120°C; set the reaction time to 15min; set the power to 600W; set the speed to 300rpm. (extraction solvent 200mL)

[0057] Step2: Set the temperature: 140°C; set the reaction time: 2min; set the power: 800W; set the speed: 350rpm.

[0058] Step3: Set the temperature: 170°C; set the reaction time: 60min; set the power: 850W; set the speed: 350rpm.

[0059] Step4: Set the temperature: 25°C; set the reaction time: 3min; set the power: 700W; set the speed: 350rpm.

[0060] Then, the reaction polymerization liquid was filtered three times, and the polymerization liquid was precipitated in 1000 mL of water, crushed, and filtered. Afterwards, the crushed product was boiled in 100°C deionized water (600ml / time) for 5 times, and the product was dried in a...

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Abstract

The invention belongs to the technical field of high polymer materials, and particularly relates to a polyethersulfone synthesis method with high batch stability. According to the method, the matching degree of microwaves and polyethersulfone synthesis is screened for the first time, and according to the principle that a large amount of friction heat is generated due to molecular vibration and frequent collision among molecules, the temperature of the material is rapidly increased in a short time, so the salt forming reaction time is greatly shortened. According to the invention, a microwave reactor composite liquid nitrogen rapid cooling technology is adopted, and a cooling program is set, so that the temperature is rapidly reduced to the room temperature when the polymerization later-stage reaction is finished, and the reaction is rapidly terminated, thereby rapidly synthesizing the polyether sulfone with extremely narrow molecular weight distribution, controllable molecular weight and high product batch stability. The microwave reaction is controlled by digital programming, the experiment repetition rate is high, the performance of different batches of products is more stable, and the error between the final molecular weight and the target molecular weight can be controlled within 700 when the reaction is finished.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polyethersulfone synthesis method with high batch stability. Background technique [0002] Polyethersulfone (polyethersulfone), also known as polyphenylene ether sulfone or polyaryl ether sulfone, is a thermoplastic polymer material with excellent comprehensive performance developed by the British ICI company in 1972. It is one of the few special engineering materials currently used One of the plastics, known as the first special engineering plastic that combines high heat distortion temperature, high impact strength and excellent formability. The polyethersulfone molecule has the rigidity of the benzene ring and the flexibility of the ether group. At the same time, the conjugation effect between the sulfone group and the entire structural unit provides the oxidation resistance and thermal stability of the material, so the entire molecule has considerable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23B01J19/12
CPCC08G75/23B01J19/0006B01J19/126B01J2219/0871Y02A20/131
Inventor 史碧波王敏潘家永黄森彪韩斌廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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