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Hyperbranched poly(aryl ether ketone), preparation method and application thereof in viscosity modifier

A technology of polyaryletherketone and polycondensation reaction, applied in hyperbranched polyaryletherketone, application of hyperbranched polyaryletherketone in viscosity modifier, A2+BB2′ type preparation of hyperbranched polyaryletherketone Field, can solve the problems of restricting industrialization, not easy to gel, expensive, etc.

Inactive Publication Date: 2010-12-08
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product obtained by the single monomer method (SMM) has good solubility, and the reaction is not easy to gel, which is suitable for theoretical research, but the monomer synthesis process is cumbersome and the price is generally expensive, which limits the possibility of further industrialization
The dual monomer method (DMM) uses two simple and easy-to-get monomers to react, and can control the structure and end groups of hyperbranched polymers by changing the structure and reaction ratio of the two monomers, but it is easy to gel. The disadvantages greatly limit its development

Method used

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  • Hyperbranched poly(aryl ether ketone), preparation method and application thereof in viscosity modifier
  • Hyperbranched poly(aryl ether ketone), preparation method and application thereof in viscosity modifier
  • Hyperbranched poly(aryl ether ketone), preparation method and application thereof in viscosity modifier

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: Synthesis of fluorine-terminated hyperbranched polyaryletherketone (HPEEK-F)

[0050] BB 2 Preparation of 'type monomer 2, 4', 6-trifluorobenzophenone: using 2,6 difluorobenzoyl chloride and fluorobenzene to prepare by using anhydrous aluminum trichloride as a catalyst through the acylation of 2,6 difluorobenzoyl chloride and fluorobenzene. 88.25g (0.5mol) of 2,6-difluorobenzoyl chloride, 80.1g (0.6mol) of anhydrous aluminum trichloride, and 600ml of fluorobenzene as a solvent in excess, refluxed at 84°C for 8h, discharged in ice hydrochloric acid water, and weighed with petroleum ether. crystallization. For the NMR characterization of the synthesized product, see Image 6 (CDCl 3 , 500Hz, ppm) δ = 7.88-7.92 (c-H, 2H) δ = 7.44-7.48 (a-H.1H) δ = 7.14-7.18 (d-H, 2H) δ = 6.90-7.03 (b-H, 2H) (Bruker500MHz NMR).

[0051] Will A 2 Type monomer hydroquinone 1.10g (0.01mol), BB 2 2.36g (0.01mol) of 'type monomer 2,4',6-trifluorobenzophenone, 0.483g (0.0035mo...

Embodiment 2

[0057] Embodiment 2: Synthesis of fluorine-terminated hyperbranched polyaryletherketone (HPEEK-F)

[0058] Will A 2 Type monomer hydroquinone 1.0725g (0.00975mol), BB 2'Type monomer 2,4', 2.36g (0.01mol) of 6-trifluorobenzophenone, 0.4709g (0.00325mol) of anhydrous potassium carbonate, 0.7235g (0.0065mol) of anhydrous sodium carbonate, and 14g of sulfolane In a three-neck flask equipped with a stirring device, nitrogen gas is passed, stirred, and the temperature is raised. The salt formation temperature is controlled at 140°C for 2 hours, 170°C for 2 hours for prepolymerization, and 210°C for 5 hours. The material is discharged into deionized water, crushed, washed three times with boiling deionized water, and dried. Reflux with ethanol for 5 times, and dry to obtain 2.5 g of hyperbranched polyaryletherketone (HFPEEK-F) whose terminal group is fluorine-terminated, and the yield is about 70%.

[0059] The glass transition temperature Tg of HPEEK-F measured by DSC is 149°C, a...

Embodiment 3

[0060] Embodiment 3: Synthesis of fluorine-terminated hyperbranched polyaryletherketone (HPEEK-F)

[0061] Will A 2 Type monomer hydroquinone 0.99g (0.009mol), BB 2 'Type monomer 2,4', 2.36g (0.01mol) of 6-trifluorobenzophenone, 0.4347g (0.0030mol) of anhydrous potassium carbonate, 0.6678g (0.0060mol) of anhydrous sodium carbonate, and 14g of sulfolane In a three-neck flask equipped with a stirring device, nitrogen gas is passed, stirred, and the temperature is raised. The salt formation temperature is controlled at 140°C for 2 hours, 170°C for 2 hours for prepolymerization, and 210°C for 5 hours. The material is discharged into deionized water, crushed, washed three times with boiling deionized water, and dried. Reflux with ethanol for 5 times, and dry to obtain 2.7 g of hyperbranched polyaryletherketone (HFPEEK-F) whose terminal group is fluorine-terminated, and the yield is about 80%.

[0062] The glass transition temperature Tg of HPEEK-F measured by DSC is 134°C, and t...

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Abstract

The invention relates to a hyperbranched poly (ether ketone), a preparation method thereof and application of the material in viscosity modifiers. The hyperbranched poly(ether ketone) is prepared wit BB2-type monomers 2, 4, 6 trifluoro phenyl ketone and A2-type monomers hydroquinone, resorcin, bisphenol A, and hexafluoro-bisphenol A or biphenyl diphenol as reactants, potassium carbonate or sodiumcarbonate or the mixture of the potassium carbonate and the sodium carbonate as a salification agent, and sulfolane or N, N-dimethyl ketopyrrolidine as a solvent through mixing, salification, polycondensation reaction and after treatment. The solid content is 20 to 30 percent; the dosage of the salification agent is 1 to 1.1 time of the dosage of the A2 monomers. Fluorine terminated hyperbranchedpolyaryletherketone and hydroxy terminated superbranched polyaryletherketone are got respectively by adjusting the ratio of the dosages of the BB2-type and A2-type monomers. The hyperbranched poly (ether ketone) is characterized in that by adding the superbranched polyaryletherketone, the mechanical property and the thermostability of linear polyaryletherketone are not reduced while the melt viscosity of the linear polyaryletherketone is reduced.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, in particular to a kind of hyperbranched polyaryletherketone and hyperbranched polyaryletherketone A 2 +BB 2 ' type preparation method, and the application of the hyperbranched polyaryletherketone in viscosity regulator. Background technique [0002] Hyperbranched polymers are a type of highly branched polymers with a three-dimensional ellipsoidal structure. They have high solubility, low viscosity, and a large number of terminal functional groups. The development and application of , nonlinear optics and other aspects have broad prospects, and have become a hot spot in the field of polymer research in recent years. [0003] As a special engineering plastic, linear polyaryletherketone has excellent heat resistance, chemical corrosion resistance and good mechanical properties, and is widely used in high-tech fields such as aerospace, electronics and nuclear energy. However, as a semi-cry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40C08L71/10
Inventor 姜振华李秀杰张淑玲王贵宾关绍巍
Owner JILIN UNIV
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