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Preparation method and modification method of flexible low-melting vinylidene fluoride copolymer

A technology of vinylidene fluoride and low melting point, which is applied in the field of preparation of flexible low melting point vinylidene fluoride copolymer, can solve the problems of complex process, limited application, low grafting rate, etc., achieve simple process, eliminate melt fracture, graft The effect of high branch rate

Active Publication Date: 2019-03-08
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is well known that PVDF is difficult to bond with other materials, which limits its application
The vinylidene fluoride copolymer functionalized by radiation grafting of unsaturated polar monomers described in CN 200780036984.7 can greatly improve the interlayer adhesion of PVDF in multilayer fuel hoses, and at the same time obtain higher co-extrusion line speed, but it needs to be pre-mixed, melted and granulated before irradiation grafting reaction to improve the low grafting rate of conventional free radical initiators, so the process is complicated and the cost is high

Method used

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  • Preparation method and modification method of flexible low-melting vinylidene fluoride copolymer

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Experimental program
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Effect test

Embodiment 1

[0036] The preparation method of flexible low melting point vinylidene fluoride copolymer is as follows:

[0037] Taking a 10L reactor as an example, add 6L of deionized water, 50g of 30wt% sodium lauryl sulfate / polyethylene glycol stearate compound dispersant aqueous solution (the mass ratio of the two is 1:3), evacuate, remove Oxygen to oxygen content ≤ 20ppm, heat the reactor to 35 ° C, add the initial mixed monomer, the initial mixed monomer is a mixture of tetrafluoroethylene and vinylidene fluoride, wherein the amount of tetrafluoroethylene is the total mass of the initial mixed monomer 20% of. When the pressure reaches 4.0±0.1MPa, add 3g of initiator tert-butyl peroxyneodecanoate and 3g of acetone. At the beginning of the reaction, additional mixed monomers are added to the reactor. The additional mixed monomers are a mixture of tetrafluoroethylene and vinylidene fluoride, wherein the amount of tetrafluoroethylene is 5% of the total mass of the additional mixed monomer...

Embodiment 2

[0042] The preparation method of flexible low melting point vinylidene fluoride copolymer is as follows:

[0043]Taking a 10L reactor as an example, add 6L of deionized water, 50g of 30wt% sodium lauryl sulfate / polyethylene glycol stearate compound dispersant aqueous solution (the mass ratio of the two is 1:4), evacuate, remove Oxygen to oxygen content ≤ 20ppm, heat the reactor to 65°C, add the initial mixed monomer, the initial mixed monomer is a mixture of hexafluoropropylene and vinylidene fluoride, and the amount of hexafluoropropylene is the total mass of the initial mixed monomer 10% of. When the pressure reaches 3.5±0.1MPa, add 3g of initiator tert-butyl peroxyneodecanoate and 3.5g of ethyl propionate. At the beginning of the reaction, additional mixed monomers are added to the reactor. The additional mixed monomers are a mixture of hexafluoropropylene and vinylidene fluoride, wherein the amount of hexafluoropropylene is 10% of the total mass of the additional mixed mo...

Embodiment 3

[0048] The preparation method of flexible low melting point vinylidene fluoride copolymer is as follows:

[0049] Taking a 10L reactor as an example, add 6L of deionized water, 50g of 30wt% sodium lauryl sulfate / polyethylene glycol stearate compound dispersant aqueous solution (the mass ratio of the two is 1:3), evacuate, remove Oxygen to oxygen content ≤ 20ppm, heat the reactor to 110°C, add the initial mixed monomer, the initial mixed monomer is a mixture of trifluoroethylene and vinylidene fluoride, wherein the amount of trifluoroethylene is the total mass of the initial mixed monomer 25% of. When the pressure reaches 2.5±0.1MPa, add 3g initiator di-tert-butyl peroxide and 3g acetone. At the beginning of the reaction, additional mixed monomers are added to the reactor. The additional mixed monomers are a mixture of trifluoroethylene and vinylidene fluoride, wherein the amount of trifluoroethylene is 20% of the total mass of the additional mixed monomers. Keep the pressure...

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Abstract

The invention relates to a vinylidene fluoride copolymer, in particular to a preparation method and a modification method of a flexible low-melting point vinylidene fluoride copolymer. The preparation method comprises the following steps: (1) adding deionized water and a dispersing agent into a reaction kettle, vacuumizing and deoxidizing; (2) raising the temperature to the reaction temperature, beginning to introduce an initial mixed monomer, adding an initiator and a molecular weight regulator after completion of the introduction, performing a polymerization reaction, continuously introducing a supplementing mixed monomer during the reaction, supplementing the molecular weight regulator for many times, stopping the reaction after completion of the introduction of the supplementing mixed monomer to obtain vinylidene fluoride copolymer resin; (3) condensing, washing and drying the vinylidene fluoride copolymer resin to obtain the flexible low-melting point vinylidene fluoride copolymer; during modification, maleic anhydride or itaconic acid are grafted, and a grafting initiator is compounded from potassium persulfate and BPO. By the preparation method, melt fracture in the polymer processing process can be effectively eliminated, material accumulation at a mouth die is reduced, and the surface finish of a product is improved; the modification method is high in grafting rate, and the modified product is good in bonding performance.

Description

technical field [0001] The invention relates to a vinylidene fluoride copolymer, in particular to a preparation method and a modification method of a flexible low melting point vinylidene fluoride copolymer. Background technique [0002] Thermoplastic resins, especially polyolefins, during extrusion, especially in the form of films, may experience irregular flow at the exit of the extruder die, resulting in surface defects that impair the mechanical or optical properties of the film performance. Below the critical shear rate, the extrudate is smooth, whereas above this rate obvious surface defects can be observed. These defects, known as "melt fractures", cause extrusion blow molded films to lose their transparency and gloss as well as their mechanical properties. [0003] Mineral or organic fillers are often added to thermoplastic resins. However, added fillers have a tendency to promote apparent surface defects. In this case, the processing aids suggested in the prior ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/22C08F214/26C08F2/38C08F2/26C08F2/30C08F4/30C08F4/34C08F259/08C08F222/06C08F214/28C08F214/18C08F222/02
CPCC08F2/26C08F2/30C08F2/38C08F4/30C08F4/34C08F214/22C08F259/08C08F214/26C08F222/06C08F214/28C08F214/182C08F222/02
Inventor 王汉利杜延华唐妮李秀芬许克韩瑞芹
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL