Process for producing polyphenyl thioether

Abstract

The invention relates to a process for producing polyphenyl thioether, comprising the following steps of:, mixing hydrogenous sodium sulfide, lithium chloride and N-methyl pyrrolidone in the weight ratio of (20-25): (2-6): (70-80), co-boiling the mixture and inert gases at 150-210 DEG C for distilling and dehydrating; separating solvent by refining; respectively adding santochlor, solvent and lithium chloride in anhydrous sodium sulfide, separating after complete reaction to obtain polyphenylene sulfide; compositely washing the polyphenylene sulfide to obtain pure polyphenylene sulfide; and reclaiming the lithium chloride by filtering, reclaiming the solvent and flashly evaporating dimethylbenzene solution in a two-period mode and cooling and crystallizing. The invention has the advantages of low cost, simple process, excellent performance of synthetic resin and high solvent recovering rate.

Description

technical field

[0001] The invention relates to a production process of a polymer material, in particular to a process for producing polyphenylene sulfide. Background technique

[0002] Polyphenylene sulfide is referred to as PPS, which has excellent thermal stability, short-term heat resistance and long-term continuous use thermal stability, as well as good corrosion resistance, adhesion and fluidity, while PPS has very low dielectric constant, inductance and dielectric loss factor, and has excellent insulation and dielectric properties in high temperature, high humidity and other environments. Therefore, as a special engineering plastic with excellent performance, it has been widely used in the fields of automobiles, electrical electronics and machinery.

[0003] At present, there are many synthetic routes of polyphenylene sulfide, but there are only two routes that have been industrialized or have industrial value: one is the industrialized Phillips route (i.e. sodium su...

Examples

Embodiment 1

[0038] Embodiment 1 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0039] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP in a weight percentage of 20:2:70, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 150°C. 1. Stirring at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0040] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0041] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 450ml of NMP and 30g of lithium chloride according to 1mol of the mixture, and react for 3 to 4 hours at a temperature of 210°C. After 1 hour, react at 250° C. ...

Embodiment 2

[0052] Embodiment 2 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0053] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP in a weight percentage of 22:3:74, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 170°C. Next, stir at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0054] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0055] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 550ml of NMP and 40g of lithium chloride respectively according to 1mol of the mixture, and react at a temperature of 220°C for 3 to 4 After 1 hour, react at 260...

Embodiment 3

[0062] Embodiment 3 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0063] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP according to the weight percentage of 24:5:77, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 190°C. Next, stir at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0064] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0065] (3) In anhydrous sodium sulfide, first add p-dichlorobenzene in a molar ratio of 1:1, then add 600ml of N-methylpyrrolidone and 50g of lithium chloride respectively according to 1mol of the mixture, and react at 230°C for 3 to 4 After 1 hour, react at 270° C....

technical field

[0001] The invention relates to a production process of a polymer material, in particular to a process for producing polyphenylene sulfide. Background technique

[0002] Polyphenylene sulfide is referred to as PPS, which has excellent thermal stability, short-term heat resistance and long-term continuous use thermal stability, as well as good corrosion resistance, adhesion and fluidity, while PPS has very low dielectric constant, inductance and dielectric loss factor, and has excellent insulation and dielectric properties in high temperature, high humidity and other environments. Therefore, as a special engineering plastic with excellent performance, it has been widely used in the fields of automobiles, electrical electronics and machinery.

[0003] At present, there are many synthetic routes of polyphenylene sulfide, but there are only two routes that have been industrialized or have industrial value: one is the industrialized Phillips route (i.e. sodium su...

Examples

Embodiment 1

[0038] Embodiment 1 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0039] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP in a weight percentage of 20:2:70, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 150°C. 1. Stirring at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0040] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0041] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 450ml of NMP and 30g of lithium chloride according to 1mol of the mixture, and react for 3 to 4 hours at a temperature of 210°C. After 1 hour, react at 250° C. ...

Embodiment 2

[0052] Embodiment 2 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0053] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP in a weight percentage of 22:3:74, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 170°C. Next, stir at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0054] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0055] (3) In the reactor, first add p-dichlorobenzene in anhydrous sodium sulfide at a molar ratio of 1:1, then add 550ml of NMP and 40g of lithium chloride respectively according to 1mol of the mixture, and react at a temperature of 220°C for 3 to 4 After 1 hour, react at 260...

Embodiment 3

[0062] Embodiment 3 A kind of technique of producing polyphenylene sulfide, comprises the following steps:

[0063] (1) After mixing sodium polyhydrate, lithium chloride and solvent NMP according to the weight percentage of 24:5:77, they are added to a 30L reaction kettle with magnetic stirring, and after feeding inert gas nitrogen, the mixture is heated at a temperature of 190°C. Next, stir at a rate of 10-30 rpm for 20-30 minutes to make it dehydrated by azeotropic distillation to obtain mixed steam and anhydrous sodium sulfide.

[0064] (2) The mixed steam in step (1) is rectified by a rectifier to separate the solvent NMP, and the rest of the steam is cooled by a rectifier to be a dehydration cooling liquid.

[0065] (3) In anhydrous sodium sulfide, first add p-dichlorobenzene in a molar ratio of 1:1, then add 600ml of N-methylpyrrolidone and 50g of lithium chloride respectively according to 1mol of the mixture, and react at 230°C for 3 to 4 After 1 hour, react at 270° C....