Polysulfone resin preparing method with microwaves as heat source
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A polysulfone resin and heat source technology, applied in the field of polymer materials, can solve the problems of easy "paste", low heat transfer efficiency of high-viscosity medium, uneven heat transfer, etc., to achieve stable reaction, shorten reaction time, and improve production efficiency. Effect
Inactive Publication Date: 2015-10-21
SHANDONG JINLAN SPECIAL POLYMER CO LTD
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Problems solved by technology
No matter which way, you will encounter the problems of low heat transfer efficiency, uneven heat transfer, and easy "pasting" of high-viscosity media
Method used
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Examples
Experimental program
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Effect test
Embodiment 1
[0019] 4,4'-dichlorodiphenylsulfone (DCDPS, 28.7160g, 100mmol), 4,4'-biphenyldiphenol (BP, 18.6210g, 100mmol), anhydrous potassium carbonate (K 2 CO 3 , 27.6420g, 200mmol), 237mL N,N-dimethylacetamide (DMAc) were mixed, the power of the microwave reactor was turned on to 3 kW, the reaction temperature was raised to 180°C, and the reaction was carried out for 3 hours. Turn off the microwave reactor and stirrer, and cool to room temperature naturally. The reaction solution was slowly poured into 2L of deionized water to obtain a white fibrous polymer, soaked in 4L of deionized water for 8 hours at 80°C, repeated three times, filtered, dried, and then vacuum-dried at 100°C for 24 hours to obtain a white Fibrous polymer, 39.7g, yield: 99%, intrinsic viscosity: 0.73dL / g.
Embodiment 2-8
[0021] With reference to the method of Example 1, polysulfone can be synthesized by using different microwave reactor powers, reaction times, solvents and potassium carbonate, and the specific results are shown in the following table:
[0022]
[0023] Result description:
[0024] (1) Adopting the experimental method of the present invention, there is no phenomenon of "sticky pot", and the reaction is stable.
[0025] (2) By adopting the experimental method of the present invention, the intrinsic viscosity of the polymer can reach the level achieved by the 12-hour reaction time in the comparative example in a very short period of time, which greatly shortens the reaction time.
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PUM
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Abstract
The invention discloses an efficient polysulfone resin preparing method with microwaves as a heat source. The preparing method includes the steps that 4,4'-dichloro(di)phenyl sulfone and bisphenol A serve as initial raw materials, carbonate with the mole number two times that of the bisphenol A is added to serve as alkali, and the mixture is heated and reacted for 2 hours to 5 hours through a microwave reactor in high-boiling-point aprotic polar solvents; then the reaction liquid is slowly poured into deionized water, white fiber-shaped polymers are obtained, then the polymers are soaked for 5 hours to 10 hours under the 60-DEG-C-to-80-DEG-C condition, the process is repeated three times to five times, filtering and drying are carried out, and polysulfone resin is obtained through vacuum drying. By means of the preparing method, the reaction time is shortened to a great degree, energy consumption is reduced, the cost for the production technology is reduced accordingly, and the working efficiency is improved.
Description
technical field [0001] The invention belongs to the technical field of polymer materials and relates to a preparation method of polysulfone resin, in particular to an efficient preparation method of polysulfone resin using microwave as a heat source. At the same time, this application was supported by the major special project of Tianjin Science and Technology Commission (contract number: 12ZCDZSF07000) and the national "863" project (project number: 2012AA03A601). Background technique [0002] As a special engineering plastic, polysulfone is widely used in many fields such as aerospace, automobile, electronic appliances, precision machinery, food, industrial equipment and medical equipment. Its production process is mainly divided into two types: two-step method and one-step method. The two-step method uses sodium hydroxide as a strong base, first converts bisphenol A into sodium salt, and then polymerizes with 4,4'-dichlorodiphenyl sulfone in dimethyl sulfoxide to obtain ...
Claims
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Application Information
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