Polyether-ether-ketone resin as well as preparation method and application thereof

A polyether ether ketone resin, polymerization reaction technology, applied in the field of polyetheretherketone resin, polyether ether ketone resin application, polyether ether ketone resin preparation, can solve the problem of deep color resin, volatile, oxidative deterioration, etc. problem, to achieve the effect of resin color improvement, controllability and stability

Inactive Publication Date: 2012-09-05
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since sulfolane is a polar solvent, its polymerization rate is higher than that of a non-polar solvent such as diphenyl sulfone, and sulfolane is very easy to contain a certain amount of water, which often affects the amount of water generated and water carried during the polymerization process. Effect
In addition, as we all know, for the binary polycondensation reaction, the most important factor affecting the viscosity of the polymerization product is the molar ratio of the monomer, and the allowable fluctuation range of this ratio is in a very narrow range. With the contin

Method used

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  • Polyether-ether-ketone resin as well as preparation method and application thereof

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preparation example Construction

[0045] The invention discloses a preparation method of polyether ether ketone resin, comprising the following steps:

[0046] Step 1, remove the air in the solvent sulfolane and the reaction vessel with a protective gas.

[0047] The protective gas is high-purity nitrogen or high-purity argon, and the air in the liquid phase and the reaction vessel is replaced by first vacuumizing and then filling the high-purity protective gas into the solvent.

[0048] Step 2: Add 4,4'-difluorobenzophenone and carbonate and / or bicarbonate to the reaction vessel under the condition of a protective gas and stirring, and heat the reaction vessel.

[0049] The specific process is to add 4,4'-difluorobenzophenone and carbonate / Bicarbonate, heat the reaction vessel, and discharge the moisture and air in the system. At this time, the water is the water contained in the raw materials. When the temperature of the system rises above 100°C, the water contained in the system evaporates from the syste...

Embodiment 1

[0067] Add 277kg of solvent sulfolane into a 300L reaction vessel, replace the liquid phase and the air in the reaction vessel by vacuuming and passing high-purity argon into the solvent. The flow rate of high-purity argon is 3Nm / min. After about 30min, use The oxygen content in the exhausted air is detected online by a gas-phase oxygen analyzer to be 0.06% (V / V), such as the inPro 6900 gas-phase oxygen detector from METTLER TOLEDO; start stirring, and then react under the protection of 0.5Nm / min argon Add 37.46kg of 4,4'-difluorobenzophenone and 19.82kg of high-purity anhydrous sodium carbonate to the container, heat the reaction container, and set the argon opening to 1.0Nm / min to discharge the moisture in the system. At 100°C, the water in the system evaporates from the system and is taken out of the reactor by the protective gas. After 45 minutes, when the temperature of the system rises to 180°C, the water in the system evaporates from the system and is taken out of the re...

Embodiment 2

[0070] According to the method of Example 1, the solvent sulfolane is 196kg, the protective gas is high-purity nitrogen, and the oxygen content in the discharged air is detected online by a gas phase oxygen detector to be 0.08% (V / V), and 40.06kg4,4' is added to the reaction vessel -Difluorobenzophenone and 22.53kg of high-purity anhydrous sodium carbonate, heating the reaction vessel to discharge the water in the system, the water content in the exhaust gas measured by an online hygrometer is 0.09% (V / V), indicating that the water in the system has evaporated completely , Add 18.72kg hydroquinone and 15kg water-carrying agent toluene. After adding water, the moisture content in the exhaust gas was measured by an online hygrometer to be 0.02% (V / V), and the condensed water was measured as 3.05kg, indicating that the water in the system evaporated completely, and the reaction stopped after 4.5 hours when the temperature was raised to 260-265°C. Release the reaction product, coo...

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Abstract

The invention discloses a preparation method of polyether-ether-ketone resin, and the method comprises the following steps of: adding solvent sulfolane, 4, 4'-DFBP and carbonate/bicarbonate into a reaction container under the condition that protective gas is introduced, heating the reaction container in case of stirring, and discharging moisture and air in a system; after the moisture in the system is completely evaporated, adding hydroquinone and a water-carrying agent in the process of continuously heating, wherein the temperature of the system is 100-200 DEG C; continuously heating, starting water-carrying reaction on the hydroquinone and the carbonate/the bicarbonate to generate the moisture, and continuously taking out the generated moisture by the water-carrying agent, distilling the water-carrying agent after the water carrying is completely carried out, starting polymerization reaction when the temperature reaches 245-265 DEG C, and stopping reaction after 1-5 hours. The invention further discloses polyether-ether-ketone prepared by the method, and an application of the prepared polyether-ether-ketone in a composite material.

Description

[0001] technical field [0002] The invention belongs to the field of chemical polymer materials, and in particular relates to a preparation method of polyetheretherketone resin, polyetheretherketone resin prepared by the method, and the application of the prepared polyetheretherketone resin. [0003] Background technique [0004] Polyaryletherketone polymers are special engineering plastics with various excellent properties such as high temperature resistance, high strength, and radiation resistance. After the polyether ether ketone (PEEK) product was launched by the British ICI company in 1981, it has been developing at a relatively fast speed for nearly 30 years, but all of them use diphenyl sulfone as the solvent. Since the solvent is insoluble in water, it must be used first. Solvents (such as acetone, ethanol, etc.) are extracted multiple times to remove the solvent diphenyl sulfone, and then extracted with water for multiple times to remove by-product salts and obtai...

Claims

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Application Information

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IPC IPC(8): C08G8/02C08L61/16C08K7/14C08K7/06C08K3/04
Inventor 代惊奇饶先花曾祥斌李翰青曹民苏成晓吴浩
Owner KINGFA SCI & TECH CO LTD
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