A kind of industrial synthesis process of polyphenylene sulfide resin without adding any synthetic auxiliary agent

Abstract

The invention discloses an industrial synthesis process of polyphenylene sulfide resin without adding any synthetic auxiliary agent. The formula of raw materials is as follows, the molar ratio of sodium sulfide: sodium hydroxide: p-dichlorobenzene: N-methylpyrrolidone is 0.98- 1.18: 0.10~0.30: 1.00~1.28: 2.30~3.80; first use pipeline filter to filter sodium sulfide and sodium hydroxide solution to deal with the mechanical impurities in it, then add 60%mol sodium hydroxide in the formula to filter sodium sulfide Chemical treatment: In the polycondensation stage, add 0.01-0.03mol sodium sulfide / mol p-dichlorobenzene to adjust the molecular weight and molecular weight distribution coefficient, so that the content of covalent chlorine is adjusted to below 120ppm, and finally the target product of the present invention is obtained. The total content of halogen elements and the polydispersity coefficient in the product obtained in the present invention are low, and the molecular weight distribution is narrow and the oxygen index is high. Coating materials for wires and cables.

Description

technical field

[0001] The invention belongs to the field of polymer material resin synthesis, especially the production of polyphenylene sulfide resin without adding any synthesis auxiliary agent. Background technique

[0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it.

[0003] In U.S. Patent No: 4761468, it is described that chemical substances such as mercapto and mercapto metal salts are used to synthesize polyphenylene sulfide resins. After the synthesis, the polyphenylene sulfide resins are treated to reduce the content of chlorine in the polyphenylene sulfide resins. In the future, the polyphenylene sulfide resin will be applied to the field of electronic components through mod...

Examples

Embodiment 1

[0031] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): NMP molar ratio is 0.98:0.30:1.00:2.30; industrial synthesis process includes:

[0032] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 18%wt Transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle with a molar ratio of 0.98:0.20, and heated to 130 ℃ to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing sodium sulfide into a pipeline ...

Embodiment 2

[0039] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): N-methylpyrrolidone (NMP) molar ratio is 1.18:0.30:1.28:3.80; industrial synthesis process includes:

[0040] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is within 66 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 38%wt Transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 88%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle with a molar ratio of 1.18:0.20, and heated to 130 ℃ to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing so...

Embodiment 3

[0047] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): NMP molar ratio is 1.01:0.14:1.06:2.68; industrial synthesis process includes:

[0048] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33-66 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 18- 38%wt transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38-88%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle at a molar ratio of 1.01:0.10 and heated to 121°C to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing sodium sulfide into a pi...

technical field

[0001] The invention belongs to the field of polymer material resin synthesis, especially the production of polyphenylene sulfide resin without adding any synthesis auxiliary agent. Background technique

[0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it.

[0003] In U.S. Patent No: 4761468, it is described that chemical substances such as mercapto and mercapto metal salts are used to synthesize polyphenylene sulfide resins. After the synthesis, the polyphenylene sulfide resins are treated to reduce the content of chlorine in the polyphenylene sulfide resins. In the future, the polyphenylene sulfide resin will be applied to the field of electronic components through mod...

Examples

Embodiment 1

[0031] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): NMP molar ratio is 0.98:0.30:1.00:2.30; industrial synthesis process includes:

[0032] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 18%wt Transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle with a molar ratio of 0.98:0.20, and heated to 130 ℃ to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing sodium sulfide into a pipeline ...

Embodiment 2

[0039] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): N-methylpyrrolidone (NMP) molar ratio is 1.18:0.30:1.28:3.80; industrial synthesis process includes:

[0040] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is within 66 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 38%wt Transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 88%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle with a molar ratio of 1.18:0.20, and heated to 130 ℃ to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing so...

Embodiment 3

[0047] at 28m 3 316L stainless steel autoclave, sodium sulfide (Na 2 S): sodium hydroxide (NaOH): p-dichlorobenzene (abbreviation: p-DCB): NMP molar ratio is 1.01:0.14:1.06:2.68; industrial synthesis process includes:

[0048] 1) In the dehydration treatment stage of sodium sulfide and sodium hydroxide, under the protection of nitrogen and the stirring speed of the stirring blade is 33-66 rpm, sodium sulfide is dissolved in anaerobic water to form a sodium sulfide concentration of 18- 38%wt transparent solution, sodium hydroxide is dissolved in anaerobic water to form a transparent solution containing sodium hydroxide concentration of 38-88%wt, sodium sulfide and sodium hydroxide are added to a 316L stainless steel reaction kettle at a molar ratio of 1.01:0.10 and heated to 121°C to fully mix and dissolve sodium sulfide and sodium hydroxide to form an aqueous solution of sodium sulfide and sodium hydroxide, and then input the mixed solution containing sodium sulfide into a pi...

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