Preparation method of polyphenylene sulfide resin for melt blowing

A polyphenylene sulfide resin, melt-blown technology, applied in the direction of single-component synthetic polymer rayon, textile and papermaking, fiber chemical characteristics, etc., can solve the difficulty of resin melt-blown, resin molecular chain breakage, fiber mechanical properties low level issues

Pending Publication Date: 2018-02-23
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many difficulties in the processing of conventional polyphenylene sulfide resins in the melt-blown process: the processing temperature of the melt-blown process is 5-60°C higher than that of the PPS melt-spun process. Repolymerization, crosslinking and decomposition of carbon and formation of carbon
In the process of extrusion of molten conventional fiber with PPS resin from the spinneret hole, due to factors such as high viscous flow activation energy of PPS resin itself, sensitivity to temperature changes, and small resin processing window, the melt blown processing performance of PPS resin is poor. That is, high temperature forming is difficult and low temperature is easy to block the spinneret hole, etc.
In particular, the molecular weight distribution range of PPS resin for conventional fibers is wide, and the existence of low molecular weight PPS leads to easy shots in fabrics (shots in fabric), while the existence of ultra-high molecular weight PPS makes it difficult to melt the resin, and PPS resin for conventional fibers Fibers prepared by melt blown have strong rigidity, low curl rate, large fiber density, and poor fiber fingertip cohesion, which is not conducive to the improvement of the overall mechanical properties of the fabric and the increase of filtration accuracy.
[0003] At present, high-viscosity resins such as filaments, short filaments, and films are usually used as PPS melt-blown materials at home and abroad. In order to improve the melt fluidity, it is necessary to increase the melting temperature of the resin and the temperature of the spinneret, but the high temperature causes resin molecules Chain scission, decomposition, desulfurization, carbonation and oxidation
However, although the low-viscosity resin has good fluidity, the mechanical properties of the fiber are not high after the resin is formed.

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0013] The invention provides a kind of preparation method of polyphenylene sulfide resin for melt blowing, it is characterized in that the method comprises the following steps:

[0014] (1) Take p-dihalobenzene and S -2 compound as raw material, amide organic compound as solvent, and basic salt as catalyst, react at 180-250°C for 1-24 hours, and the reaction pressure is 0.1-5.0MPa to obtain a linear PPS prepolymer containing terminal mercapto groups (referred to as linear PPS prepolymer); The p-dihalobenzene and S-containing -2 The molar ratio of the compound is 1:1.03~1;

[0015] The containing S -2 The compound is anhydrous lithium sulfide, anhydrous sodium sulfide, anhydrous potassium sulfide, anhydrous rubidium sulfide, anhydrous cesium sulfide, anhydrous lithium hydrogen sulfide, anhydrous sodium hydrogen sulfide, anhydrous potassium hydrogen sulfide, anhydrous rubidium hydrogen sulfide , anhydrous cesium hydrosulfide or H 2 at least one of S;

[0016] The amide org...

Embodiment 1

[0027] Take 150L of N-methylpyrrolidone, 18.40 kg of p-dichlorobenzene, 10.37 kg of anhydrous sodium sulfide (dehydrated to a content of 95.0%) and 9 kg of catalyst 12 hydrated trisodium phosphate, react in a 300L polymerization kettle, and react at 210°C respectively 2 hours, react at 260° C. for 4 hours, separate after cooling, wash and dry to obtain a PPS resin for melt blowing with a viscosity of 560 g / min. The resin terminal chlorine content is 96%, and the terminal mercapto group is 4%. The obtained resin is melt-blown into fibers on a single screw to prepare superfine fibers with a fiber diameter of 0.4-3 microns, the fiber strength reaches 2.0, and the elongation at break is 9.2%. The PM2.5 filtration accuracy of meltblown nonwovens reaches over 94%.

Embodiment 2

[0029] Take 150L of N-methylpyrrole, 18.40 kg of p-dichlorobenzene, 10.37 kg of anhydrous sodium sulfide (dehydrated to a content of 95.0%) and 9 kg of catalyst 12 hydrated trisodium phosphate, react in a 300L polymerization kettle, and react at 210°C respectively For 4 hours, use a plunger pump to inject 249 grams of 1,3-dichloronaphthalene (1,3-dichloronaphthalene is dissolved in 2 kg of N-methylpyrrolidone), then raise the temperature to 260 ° C for 4 hours, and separate after cooling , washing and drying to obtain a viscosity of 410g / min melt-blown PPS resin. The resin terminal chlorine content is 97%, and the terminal mercapto group is 3%. The obtained resin is melt-blown into fibers on a single screw to prepare superfine fibers with a fiber diameter of 0.8-3.5 microns, the fiber strength reaches 2.6, and the elongation at break is 12.6%. The PM2.5 filtration accuracy of meltblown nonwovens reaches over 93%.

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Abstract

The invention discloses a preparation method of polyphenylene sulfide resin for melt blowing. The preparation method is characterized by comprising the following steps: reacting p-dihalogenated benzene, an S<-2>-containing compound, an amide organic compound with alkali salt at a temperature 180-250 DEG C and a pressure of 0.1MPa-5.0MPa for 1-24 hours, so as to obtain a linear PPS prepolymer; andreacting the linear PPS prepolymer with dihalogenated hydrocarbon at a temperature of 230-280 DEG C and a reaction pressure of 0.1MPa-5.0MPa for 1-24 hours, so as to obtain PPS resin for melt blowing,wherein dihalogenated hydrocarbon is m-dihalogenated aromatic hydrocarbon or p-dihalogenated hydrocarbon. When being added, m-dihalogenated aromatic hydrocarbon is taken as a structural regulator, and the high-entanglement helical-structure or spring-structure PPS resin for melt blowing is obtained; and when being added, p-dihalogenated hydrocarbon is taken as a chain extender, and high-linearityand relatively-low-viscosity PPS resin for melt blowing is obtained. The preparation method is relatively low in processing temperature, so that the decomposition and carbonization of PPS can be inhibited, and the oxidation and crosslinking of PPS can be prevented.

Description

technical field [0001] The invention relates to the field of environmental filtration, in particular to a preparation method of polyphenylene sulfide resin for melt blowing. Background technique [0002] Polyphenylene sulfide (PPS) is a crystalline thermoplastic special engineering plastic with superior comprehensive properties. Polyphenylene sulfide melt-blown nonwovens have excellent high temperature resistance, chemical corrosion resistance and filtration accuracy, and can be widely used in industrial coal-fired boilers, waste incineration, cement plants and power plants as filters for flue dust collectors. material. However, there are many difficulties in the processing of conventional polyphenylene sulfide resins in the melt-blown process: the processing temperature of the melt-blown process is 5-60°C higher than that of the PPS melt-spun process. repolymerization, crosslinking and decomposition of carbon, and carbon formation. In the process of extruding the melted ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254D01F6/76
CPCC08G75/0254D01F6/765
Inventor 李振环张永志程博闻
Owner TIANJIN POLYTECHNIC UNIV
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