Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of polyphenylene sulfide and p-dichlorobenzene, which is applied in the field of preparation of polyphenylene sulfide, can solve the problems of low solvent recovery rate, high price, and large consumption, and achieve the effect of improving the hue
Active Publication Date: 2014-04-02
CHONGQING JUSHI NEW MATERIAL TECH CO LTD
View PDF4 Cites 15 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
Hexamethylphosphoric triamide (HMPA) is better as a solvent than N-methylpyrrolidone (NMP), but it is expensive and consumes too much
[0005]Philips method has easy-to-obtain raw materials, high yield, and better product quality than other processes, but this process also has its disadvantages. The price of the solvent N-methylpyrrolidone (NMP) Expensive, high consumption; NMP itself is reactive and will form PPS with pyrrolidone end groups, which will affect the solvent resistance of PPS; high temperature and pressure reaction will promote the decomposition of solvent NMP, and the solvent recovery rate is low
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0027] 1. Mix 120g sodium sulfide (Na 2 S·9H 2 O), 178g of N-methylpyrrolidone (NMP), 1.68g of lithium chloride, and 3.62g of sodium thiosulfate were added to the polymerization kettle, and the inert gas was used to replace the air, followed by heating and dehydration, and the dehydration rate was stopped when the dehydration rate reached 82%.
[0028] 2. Add 116g of p-dichlorobenzene (P-DCB) in NMP solution (containing 75.7g of P-DCB) to the system after dehydration in step (1), and react at 230°C for 5h. After the reaction is finished, a mixed slurry containing PPS resin, solvent, oligomer and inorganic salt is obtained.
[0029] 3. Filter the mixed slurry, add the filter cake into boiled pure water, stir and wash and ultrasonically treat for 15~30min. Repeat this operation 3 times to obtain PPS resin after drying.
[0030] The PPS resin product is white, with a yield of 94.1%, a melting point of 294°C, and an ignition residue of 0.19%.
Embodiment 2
[0032] With embodiment 1, difference is:
[0033] In step (1), sodium thiosulfate is 2.57g, and the dehydration rate is 89%;
[0034] The reaction in step (2) was carried out at 210° C. for 4 h.
[0035] The PPS resin product is white, with a yield of 89.7%, a melting point of 282°C, and an ignition residue of 0.17%.
Embodiment 3
[0037] With embodiment 1, difference is:
[0038] Step (1), the dehydration rate is 80%;
[0039] The PPS resin product is white, with a yield of 91.2%, a melting point of 284°C, and an ignition residue of 0.18%.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Login to view more
Abstract
The invention relates to the field of high molecular material synthesis, in particular to a preparation method of polyphenylene sulfide. The preparation method comprises the following steps of: adding Na2S.9H2O, N-methyl pyrrolidone and a reaction assistant into a polymerization kettle, supplying nitrogen to replace air, then heating to 180 DEG C for dehydration at a dehydration rate of 80-95%, adding an N-methylpyrrolidine solution containing p-dichlorobenzene into a dehydrated system in Step (1) for reaction for 3-8h at 190-230 DEG C, after the reaction finishes, obtaining a size mixture, filtering the size mixture, adding a filter cake into boiled pure water, stirring, washing, and performing 90Hz ultrasonic treatment for 15-30min, repeatedly washing for 2-3 times, and obtaining PPS (polyphenylene sulfide) resin after drying. The method has the advantageous effects that the product hue can be obviously improved since sodium thiosulfate is added, even a water content of the system is higher (the dehydration rate is 80%) and the reaction temperature is higher, and the ultrasonic washing can effectively remove inorganic salt impurities included due to macromolecular chain bending and winding in a reaction process.
Description
technical field [0001] The invention relates to the field of polymer material synthesis, more specifically a preparation method of polyphenylene sulfide. Background technique [0002] Polyphenylene sulfide (PPS) is a new type of engineering plastic with excellent performance that was produced in the 1970s and developed rapidly. It has excellent properties such as molding processability, thermal stability, chemical corrosion resistance, physical and mechanical properties, electrical conductivity, low toxicity, heat resistance, and flame retardancy, so it is widely used in mechanical chemical industry, electrical industry, automobile industry, aviation, food processing, etc. Widely used in various fields. [0003] The Philips method is the earliest method to realize industrialized production in the world, and it is also the most mainstream industrialized production method at present. The process is to dissolve p-dichlorobenzene (P-DCB) and sodium sulfide or sodium bisulfide...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to view more 
Login to view more