Production method of decatalyzed polyphenylene sulfide resin
A technology of polyphenylene sulfide resin and production method, which is applied in the field of polymer material resin synthesis, can solve the problems of high recovery cost, complicated production process, long reaction time, etc., and achieves low cost, short polymerization time and simple operation. Effect
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Embodiment 1
[0055] Add 40kg of solvent NMP and 11kg of sodium sulfide trihydrate (sodium sulfide content 60%) into a 60L pure titanium polymerization reactor A, and heat up to 205°C for azeotropic dehydration under the protection of nitrogen. A total of 7.5kg of liquid is extracted, and the liquid enters a 10L In the pure titanium reactor B, add 12.4kg of p-dichlorobenzene to the 60L polymerization reactor A and raise the temperature from 220°C to 265°C at a heating rate of 10°C / h. It takes about 4.5 hours. Add 250g and 600g of NaOH and 600g of p-dichlorobenzene to the 10L reactor B, raise the temperature to 270°C, wait for the 60L polymerization reactor A to heat up to 265°C at a constant temperature, and the actual waiting time is 2.2 hours. After the 60L polymerization reactor A was heated to 265°C, the material in the 10L reactor B was added, and then the 60L polymerization reactor A was kept at a constant temperature of 265°C for 4 hours. Filter, wash and dry the filter cake. 8.2 kg...
Embodiment 2
[0057] In a 60L pure titanium polymerization reactor A, add solvent NMP 40kg, sodium sulfide trihydrate 11kg (sodium sulfide content 60%) and raise the temperature to 202°C for azeotropic dehydration under the protection of nitrogen. In the pure titanium reactor B, add 12.4kg of p-dichlorobenzene to the 60L polymerization reactor A and raise the temperature from 220°C to 256°C at a heating rate of 8°C / h. It takes about 4.5 hours. Add 200g and 580g of NaOH and p-dichlorobenzene to the 10L reactor B, raise the temperature to 265°C, wait for the 60L polymerization reactor A to heat up to 256°C at constant temperature, and the actual waiting time is 2 hours. After the 60L polymerization reactor A was heated to 256°C, the material in the 10L reactor B was added, and then the 60L polymerization reactor A was kept at a constant temperature of 255°C for 4 hours. Filter, wash and dry the filter cake. 8.0 kg of resin were obtained.
Embodiment 3
[0059] Add 40kg of solvent NMP and 11kg of sodium sulfide trihydrate (sodium sulfide content 60%) into a 60L pure titanium polymerization reactor A, and heat up to 200°C for azeotropic dehydration under the protection of nitrogen. A total of 6.0kg of liquid is extracted, and the liquid enters a 10L In the pure titanium reactor B, add 12.4kg of p-dichlorobenzene to the 60L polymerization reactor A and raise the temperature from 220°C to 268°C at a heating rate of 10°C / h. It takes about 4.8 hours. Add 200g and 580g of NaOH and p-dichlorobenzene to the 10L reactor B, raise the temperature to 265°C, wait for the 60L polymerization reactor A to heat up to 268°C at a constant temperature, and the actual waiting time is 2.8 hours. After the 60L polymerization reactor A was heated to 268°C, the material in the 10L reactor B was added, and then the 60L polymerization reactor A was kept at a constant temperature of 268°C for 4 hours. Filter, wash and dry the filter cake. 8.4 kg of resi...
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