A kind of synthetic method of linear high molecular weight polyphenylene sulfide

Abstract

The invention discloses a method for synthesizing linear high molecular weight polyphenylene sulfide and belongs to the technical field of chemical material. The method comprises the following steps: by taking sodium sulphide and dichloro diphenyl as raw materials, synthesizing the linear high molecular weight polyphenylene sulfide (PPP) resin through a solution polycondensation method and a secondary polymerization process in a compound solvent and a cosolvent system. The method is simple in process and convenient to operate; the product has a high molecular weight linear structure; in the whole polymerization process, the molecular weight is controllable. Compared with the prior art, the method has the advantages of good solvent system dissolving property, low salt content and easy separation. The monomer reactivity of the linear polymerization reaction is high and the chain extension is easy to process. The dosage of the alkali metal or the alkaline earth chloride is few and the metal ion can be easily washed. The linear high molecular weight polyphenylene sulfide does not have irritant or carcinogenic property and is environmentally friendly to operate.

Description

technical field

[0001] The invention belongs to the technical field of chemical materials, and in particular relates to a method of synthesizing linear high-molecular-weight polyphenylene by solution polycondensation method and secondary polymerization process using sodium sulfide and p-dichlorobenzene as raw materials, under the system of lye, composite solvent and auxiliary agent Thioether (PPS) resin method. Background technique

[0002] Polyphenylene sulfide (PPS) is a special engineering plastic with excellent comprehensive properties. It has excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, balanced physical and mechanical properties, excellent dimensional stability and excellent electrical properties. It is widely used as a structural polymer material, and can be used as a special engineering plastic after filling and modification. At the same time, it can also be made into various functional films, coatings and comp...

Examples

Embodiment 1

[0026] Add 1.02mol sodium sulfide, 1mol p-dichlorobenzene, 1mol sodium hydroxide, 5mol solvent (N-methylpyrrolidone, N,N- Dimethylacetamide) and 0.005mol lithium chloride, under the protection of nitrogen, turn on the electricity to heat up the temperature, and carry out the prepolymerization reaction at 160°C for 1h, when the temperature rises to 220°C, stop heating, and use the reaction heat to reduce the temperature in the reactor Continue to rise, and at the same time turn on the cooling water to adjust and control the temperature in the reactor. Under the conditions of temperature 240 ° C and pressure 1 MPa, the polycondensation reaction is carried out for 1 hour and then ends. After the reaction kettle was cooled down and the pressure was relieved, the reaction slurry was cooled to 100°C, filtered, and the filter cake was washed once with hydrochloric acid and deionized water once, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol Ch...

Embodiment 2

[0028]Add 1.02mol sodium sulfide, 1mol p-dichlorobenzene, 1.1mol potassium hydroxide, 6mol solvent (N-methylpyrrolidone, hexamethyl Phosphoric triamide) and 0.006mol calcium chloride, under the protection of nitrogen, turn on the electricity to heat up, and carry out the prepolymerization reaction at 170°C for 1.5h. When the temperature rises to 220°C, stop heating, and use the heat of reaction to reduce the temperature in the reactor Continue to rise, and at the same time turn on the cooling water to adjust and control the temperature in the reactor. Under the conditions of temperature 250°C and pressure 1.2MPa, the polycondensation reaction is carried out for 1.5h and then ends. After the reaction kettle was cooled down and the pressure was relieved, the reaction slurry was cooled to 105°C, filtered, the filter cake was washed twice with hydrochloric acid and once with deionized water, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol p ...

Embodiment 3

[0030] Add 1.03mol sodium sulfide, 1mol p-dichlorobenzene, 1.2mol calcium hydroxide, 7mol solvents (N-methylpyrrolidone, pyridine) and 0.006mol Potassium Chloride, under the protection of nitrogen, turn on the electricity to heat up the temperature, and carry out the prepolymerization reaction at 180°C for 2 hours. When the temperature rises to 220°C, stop heating, use the heat of reaction to continue to rise the temperature in the reactor, and turn on the cooling water at the same time In order to adjust and control the temperature in the reactor, under the conditions of temperature 260° C. and pressure 1.3 MPa, the polycondensation reaction was carried out for 2 hours and then ended. After the reaction kettle was cooled and the pressure was relieved, the reaction slurry was cooled to 110°C, filtered, the filter cake was washed twice with hydrochloric acid and twice with deionized water, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol C...

technical field

[0001] The invention belongs to the technical field of chemical materials, and in particular relates to a method of synthesizing linear high-molecular-weight polyphenylene by solution polycondensation method and secondary polymerization process using sodium sulfide and p-dichlorobenzene as raw materials, under the system of lye, composite solvent and auxiliary agent Thioether (PPS) resin method. Background technique

[0002] Polyphenylene sulfide (PPS) is a special engineering plastic with excellent comprehensive properties. It has excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, balanced physical and mechanical properties, excellent dimensional stability and excellent electrical properties. It is widely used as a structural polymer material, and can be used as a special engineering plastic after filling and modification. At the same time, it can also be made into various functional films, coatings and comp...

Examples

Embodiment 1

[0026] Add 1.02mol sodium sulfide, 1mol p-dichlorobenzene, 1mol sodium hydroxide, 5mol solvent (N-methylpyrrolidone, N,N- Dimethylacetamide) and 0.005mol lithium chloride, under the protection of nitrogen, turn on the electricity to heat up the temperature, and carry out the prepolymerization reaction at 160°C for 1h, when the temperature rises to 220°C, stop heating, and use the reaction heat to reduce the temperature in the reactor Continue to rise, and at the same time turn on the cooling water to adjust and control the temperature in the reactor. Under the conditions of temperature 240 ° C and pressure 1 MPa, the polycondensation reaction is carried out for 1 hour and then ends. After the reaction kettle was cooled down and the pressure was relieved, the reaction slurry was cooled to 100°C, filtered, and the filter cake was washed once with hydrochloric acid and deionized water once, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol Ch...

Embodiment 2

[0028]Add 1.02mol sodium sulfide, 1mol p-dichlorobenzene, 1.1mol potassium hydroxide, 6mol solvent (N-methylpyrrolidone, hexamethyl Phosphoric triamide) and 0.006mol calcium chloride, under the protection of nitrogen, turn on the electricity to heat up, and carry out the prepolymerization reaction at 170°C for 1.5h. When the temperature rises to 220°C, stop heating, and use the heat of reaction to reduce the temperature in the reactor Continue to rise, and at the same time turn on the cooling water to adjust and control the temperature in the reactor. Under the conditions of temperature 250°C and pressure 1.2MPa, the polycondensation reaction is carried out for 1.5h and then ends. After the reaction kettle was cooled down and the pressure was relieved, the reaction slurry was cooled to 105°C, filtered, the filter cake was washed twice with hydrochloric acid and once with deionized water, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol p ...

Embodiment 3

[0030] Add 1.03mol sodium sulfide, 1mol p-dichlorobenzene, 1.2mol calcium hydroxide, 7mol solvents (N-methylpyrrolidone, pyridine) and 0.006mol Potassium Chloride, under the protection of nitrogen, turn on the electricity to heat up the temperature, and carry out the prepolymerization reaction at 180°C for 2 hours. When the temperature rises to 220°C, stop heating, use the heat of reaction to continue to rise the temperature in the reactor, and turn on the cooling water at the same time In order to adjust and control the temperature in the reactor, under the conditions of temperature 260° C. and pressure 1.3 MPa, the polycondensation reaction was carried out for 2 hours and then ended. After the reaction kettle was cooled and the pressure was relieved, the reaction slurry was cooled to 110°C, filtered, the filter cake was washed twice with hydrochloric acid and twice with deionized water, and the obtained polyphenylene sulfide polymer was mixed with 1mol sodium sulfide, 1mol C...

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