CN111518276A - Washing treatment method of injection molding grade polyphenylene sulfide industrial product - Google Patents
Washing treatment method of injection molding grade polyphenylene sulfide industrial product Download PDFInfo
- Publication number
- CN111518276A CN111518276A CN202010393637.7A CN202010393637A CN111518276A CN 111518276 A CN111518276 A CN 111518276A CN 202010393637 A CN202010393637 A CN 202010393637A CN 111518276 A CN111518276 A CN 111518276A
- Authority
- CN
- China
- Prior art keywords
- polyphenylene sulfide
- filtrate
- crude product
- injection molding
- washing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 76
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 76
- 238000005406 washing Methods 0.000 title claims abstract description 52
- 238000001746 injection moulding Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000009776 industrial production Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- 239000000706 filtrate Substances 0.000 claims description 38
- 239000012043 crude product Substances 0.000 claims description 30
- 239000000047 product Substances 0.000 claims description 28
- 238000003825 pressing Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 12
- 239000011347 resin Substances 0.000 abstract description 12
- 238000002425 crystallisation Methods 0.000 abstract description 11
- 230000008025 crystallization Effects 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 7
- 239000000155 melt Substances 0.000 description 7
- 238000005452 bending Methods 0.000 description 4
- 229910017053 inorganic salt Inorganic materials 0.000 description 4
- 238000004537 pulping Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000006902 nitrogenation reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006135 semi-crystalline thermoplastic polymer Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/0204—Polyarylenethioethers
- C08G75/0277—Post-polymerisation treatment
- C08G75/0281—Recovery or purification
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/0204—Polyarylenethioethers
- C08G75/025—Preparatory processes
- C08G75/0259—Preparatory processes metal hydrogensulfides
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Injection Moulding Of Plastics Or The Like (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a washing treatment method of an injection molding grade polyphenylene sulfide product in an industrial production grade. The washing treatment method has the advantages of simple process, high washing efficiency, conventional treatment equipment, safety and no dangerous medicine, and can be used for industrial production. The treated polyphenylene sulfide resin can reduce ash content, effectively increase the crystallization temperature of polyphenylene sulfide in a molten state, and obviously improve the characteristics of polyphenylene sulfide. Each batch of washing water can be recycled, so that the waste water generated in the process is effectively reduced, and the sewage treatment cost is reduced.
Description
Technical Field
The invention belongs to the field of purification and washing treatment of industrial products, and particularly relates to a washing treatment method of an injection molding grade polyphenylene sulfide product in an industrial production grade.
Background
Polyphenylene Sulfide (PPS) is a semi-crystalline thermoplastic polymer with a crystallinity of about 29% to about 36%, a glass transition temperature of between 80 ℃ and 90 ℃, and a melting point of about 285 ℃. PPS is one of the most potential engineering plastics due to its excellent chemical resistance, low coefficient of friction, dimensional stability, high temperature resistance, and high flame retardancy.
In the process of industrially producing the polyphenylene sulfide resin, along with the generation of sodium chloride, an inorganic salt auxiliary agent is added, so that the environment for producing the polyphenylene sulfide has the existence of the inorganic salt, and the finally obtained polyphenylene sulfide resin is wrapped by a large amount of the inorganic salt and has residual solvent. The presence of these impurities reduces the mechanical properties, thermal stability, electrical insulation, etc. of polyphenylene sulfide resins, and also corrodes electronic components during use. Therefore, special washing treatment process is needed to reduce the content of inorganic salt and other impurities in the polyphenylene sulfide resin, so that the performance of the polyphenylene sulfide resin is better exerted, and the polyphenylene sulfide resin can be applied to various fields. In addition, the melt crystallization temperature is a key index for subsequent injection molding processing, the polyphenylene sulfide for injection molding requires a high melt crystallization temperature so as to be rapidly molded, and a proper washing treatment method is usually selected according to different purposes of the product.
According to the research, the invention discovers that the ash content of the specifically prepared crude polyphenylene sulfide product for injection molding can be reduced, the crystallization temperature of the polyphenylene sulfide in a molten state can be effectively increased, and the processing treatment of subsequent injection molding is facilitated by using acetic acid to treat the crude polyphenylene sulfide product for injection molding under specific conditions.
Disclosure of Invention
In view of the problems of the prior art, according to one aspect of the present invention, it is an object of the present invention to provide a method for washing and treating an injection-grade polyphenylene sulfide product of industrial production grade, wherein the injection-grade polyphenylene sulfide resin is treated with acetic acid under specific conditions, so that ash content is reduced, the crystallization temperature of the injection-grade polyphenylene sulfide in a molten state is effectively increased, and the subsequent processing of injection molding is facilitated.
The washing treatment method comprises the following steps:
1) conveying the injection molding grade polyphenylene sulfide crude product to a filter press, and adding water to carry out primary slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5, and more preferably 1: 10;
2) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing first filter pressing, and sending filtrate to a subsequent water treatment system;
3) after the filter pressing is finished, adding water into the filter press for secondary slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5, and more preferably 1: 10;
4) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, carrying out secondary filter pressing, and conveying filtrate to a washing water tank for temporary storage so as to facilitate washing and recycling of products of the next batch;
5) after the filter pressing is finished, adding the filtrate obtained in the step 4) into a filter press for third slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5, and more preferably 1: 10;
6) repeating the step 4) for third filter pressing, and conveying the filtrate to a washing water tank for temporary storage so as to facilitate the washing recycling of the next batch of products;
7) after the filter pressing is finished, adding an acetic acid solution and the filtrate obtained in the step 6) into a filter press for carrying out fourth slurrying, and ensuring that the pH value of the mixed slurrying solution is 4.5-5.0, thereby determining the dosage of the acetic acid solution, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5, and more preferably 1: 10;
8) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing fifth filter pressing, and sending filtrate to a subsequent water treatment system;
9) adding desalted water or distilled water into the filter press to carry out fifth slurrying;
10) and starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing fifth filter pressing, sending the injection-grade polyphenylene sulfide to a subsequent drying system from the filter press after the filter pressing is finished, sending filtrate to a washing water tank for temporary storage so as to facilitate next recycling, wherein the weight ratio of the injection-grade polyphenylene sulfide crude product to the desalted water or distilled water is 1: 25-1: 5, and more preferably 1: 10.
Preferably, the concentration of the acetic acid solution in the step 7) is 5 to 30 percent by mass.
Preferably, the injection molding grade polyphenylene sulfide crude product in the step 1) is prepared as follows:
1) adding 20-30 parts by weight of acetic anhydride, 150 parts by weight of sodium hydroxide 140-;
2) and transferring the sodium hydrosulfide solution from the dehydration reaction kettle to a subsequent polymerization reaction kettle, adding 190-weight portions of dihalobenzene, heating the polymerization reaction kettle to 265-weight portions of 280 ℃, keeping the stirring condition for 0.5h for polymerization reaction, then cooling to below 100 ℃ under the condition of keeping the pressure in the reactor unchanged, and finishing the reaction to obtain the injection molding grade polyphenylene sulfide crude product.
The injection molding grade polyphenylene sulfide crude product comprises the following components in percentage by weight: according to the mass percentage, 5 percent of NMP, 39 percent of sodium chloride, 12 percent of sodium acetate, 2 percent of water and the balance of 42 percent of PPS.
The injection molding grade polyphenylene sulfide crude product is a polyphenylene sulfide product for injection molding, and is particularly suitable for being processed into a workpiece or a mold.
Advantageous effects
1. The method has the advantages of simple process, high washing efficiency, conventional treatment equipment, safety and no dangerous medicine, and can be used for industrial production.
2. The treated polyphenylene sulfide resin can reduce ash content, effectively increase the crystallization temperature of polyphenylene sulfide in a molten state, and obviously improve the characteristics of polyphenylene sulfide.
3. Each batch of washing water can be recycled, so that the waste water generated in the process is effectively reduced, and the sewage treatment cost is reduced.
4. The treated polyphenylene sulfide resin has improved application performance, can be better processed into a workpiece or a die, and is applied to high-end fields.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a DSC analysis chart of a product before washing treatment in example 1;
FIG. 2 is a DSC analysis chart of the product after the washing treatment of example 1.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The washing treatment method needs to be carried out at a specific temperature, namely 85-95 ℃, and the residual solvent NMP in the injection molding grade polyphenylene sulfide product can be better washed within the temperature range, so that the NMP residue is reduced as much as possible. When the content is outside the above range, the effect of removing NMP as a solvent is not satisfactory.
The amount of water added per time in the washing treatment method according to the present invention is not particularly limited, but in view of efficiency and economy, the weight ratio of injection-grade polyphenylene sulfide crude product to the added water or filtrate is 1:25 to 1:5, more preferably 1: 10. If the ratio is more than 1:25, the added water or filtrate is too much, so that the impurity removal rate can be improved each time, but more waste water is generated, and the method is not economical and environment-friendly; if the ratio is less than 1:5, namely the added water or the filtrate is insufficient, the impurity removal rate per time is reduced, and the washing and pressure filtration times are increased to improve the total impurity removal rate, which is not economical.
According to the washing treatment method, the acetic acid solution is used as the washing additive for the injection molding grade crude polyphenylene sulfide product with specific components, impurities and contents, so that the content of the impurities in the injection molding grade crude polyphenylene sulfide product is greatly reduced. The acetic acid solution is added in the fourth pulping in the washing treatment method of the invention, and the pH value of the mixed pulping liquid is ensured to be 4.5-5.0, so that the dosage of the acetic acid solution is determined. If the pH value of the mixed slurry liquid in the fourth slurry process is lower than 4.5, the filtrate is too strong in acidity, and the burden of a subsequent water treatment system is caused; if the pH value is higher than 5.0, the optimum effect on the product is not significant, and it is further preferable that the pH value of the mixed slurry is 4.8.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
And (3) performance testing:
1. the melt index change of polyphenylene sulfide before and after the washing treatment (temperature: 316 ℃ C., load: 5kg) was measured by a melt index meter.
2. The changes in the melting crystallization points before and after the washing treatment of the polyphenylene sulfide resin were measured by Differential Scanning Calorimetry (DSC).
3. The ash change of the polyphenylene sulfide resin before and after washing treatment can be tested by adopting a muffle furnace combustion method.
Example 1
The injection molding grade polyphenylene sulfide crude product is prepared as follows:
20kg of acetic anhydride, 140kg of sodium hydroxide and 440kg of organic solvent are added into a dehydration reaction kettle, the temperature is gradually raised to 100-150 ℃ under the protection of nitrogen, and dehydration and acid-base neutralization reaction are carried out to generate sodium acetate. And adding 170kg of sodium hydrosulfide into the reaction kettle, and raising the temperature to 200-210 ℃ for dehydration reaction for 2 hours to obtain a dehydrated solution. Transferring the solution from the dehydration reaction kettle to a subsequent polymerization reaction kettle, adding 195kg of p-dichlorobenzene, heating the medium in the reaction kettle to 265-280 ℃, then keeping the temperature at 265-280 ℃ for 1h, cooling to below 100 ℃, and filtering to obtain the injection molding grade polyphenylene sulfide crude product.
The melting state crystallization point of the injection molding grade polyphenylene sulfide crude product is 221.0 ℃ (DCS analysis is shown in a detailed diagram 1), the melt index is 415g/10min, and the types and the contents of the components are as follows: according to the mass percentage, 5 percent of NMP, 39 percent of sodium chloride, 12 percent of sodium acetate, 2 percent of water and the balance of 42 percent of PPS.
130kg of acetic acid solution was prepared in advance in the additive tank.
1) Sending 120kg of injection molding grade polyphenylene sulfide crude product to a filter press, and adding 1200kg of clean water filtrate for primary slurrying;
2) starting a stirring device of the filter press, stirring and mixing for 15min at 90 ℃, carrying out first filter pressing, and sending filtrate to a subsequent water treatment system;
3) after the filter pressing is finished, 1200kg of water is added into the filter press for secondary slurrying;
4) starting a stirring device of the filter press, stirring and mixing for 15min at 90 ℃, carrying out secondary filter pressing, and temporarily storing filtrate in a washing water tank so as to facilitate the washing recycling of the next batch of products;
5) after the filter pressing is finished, 1200kg of filtrate obtained in the step 4) is added into a filter press for third slurrying;
6) repeating the step 4) for third filter pressing, and conveying the filtrate to a washing water tank for temporary storage so as to facilitate the washing recycling of the next batch of products;
7) after the filter pressing is finished, 130kg of acetic acid solution and 1200kg of filtrate obtained in the step 6) are added into a filter press for carrying out fourth pulping, and the PH value of the mixed pulping liquid is ensured to be 4.8;
8) starting a stirring device of the filter press, stirring and mixing for 15min at 90 ℃, performing fifth filter pressing, and sending filtrate to a subsequent water treatment system;
9) adding desalted water or distilled water into the filter press to carry out fifth slurrying;
10) and starting a stirring device of the filter press, stirring and mixing for 15min at 90 ℃, performing fifth filter pressing, conveying injection molding-grade polyphenylene sulfide to a subsequent drying system from the filter press after the filter pressing is finished, and conveying filtrate to a washing water tank for temporary storage so as to be recycled for the next time.
The detection result shows that after the washing treatment of the embodiment, the molten state crystallization point of the product is 219.6 ℃ (DCS analysis is shown in detail figure 2), the melt index is 289g/10min, wherein the types and the contents of the components are as follows, according to the mass percentage, 0.07 percent of NMP, 0.04 percent of sodium chloride, 0.04 percent of sodium acetate, 48.07 percent of water and the balance of 51.78 percent of PPS, the product is used for subsequent injection molding parts or mold application, the performance is obviously improved, the bending strength is measured according to GB/T9341-4) Measured according to GB/T9341-2000, the requirement is more than or equal to 1.2MPa, and the measured value is 2.3 MPa; the notched impact strength of the cantilever beam is measured according to GB/T1843-1996, and the requirement is that the notched impact strength is more than or equal to 10.0KJ/m2The measurement value was 15.4.
Example 2
An injection-grade polyphenylene sulfide crude product was washed in the same manner as in example 1, except that the concentration of the acetic acid solution was set to 10% by mass.
And (3) detection results: after washing treatment, the molten state crystallization point of the product is 218.1 ℃, the melt index is 288 g/10min, and the types and the contents of the components are as follows: 0.05% of NMP, 0.03% of sodium chloride, 0.04% of sodium acetate, 49.55% of water, and the balance of 50.33% of PPS. The performance of the material is obviously improved when the material is used for subsequent injection molding parts or molds. The bending strength is measured according to GB/T9341-a, measured at 264.5MPa, flexural modulus of elasticity (× 10)4) Measured according to GB/T9341-2000, the requirement is more than or equal to 1.2MPa, and the measured value is 2.2 MPa; the notched impact strength of the cantilever beam is measured according to GB/T1843-1996, and the requirement is that the notched impact strength is more than or equal to 10.0KJ/m2Measured at 14.8KJ/m2。
Comparative example 1
Injection molding grade polyphenylene sulfide crude product was washed in the same manner as in example 1, except that no acetic acid solution was used.
The detection result is that after washing treatment, the molten state crystallization point of the product is 217.9 ℃, the melt index is 281 g/10min, the types and the contents of the components are 0.05 percent of NMP, 0.06 percent of sodium chloride, 0.02 percent of sodium acetate, 48.77 percent of water and the rest 51.10 percent of PPS, the product is used for subsequent injection molding parts or molds, the performance is not obviously improved, the bending strength is measured according to GB/T9341-one 2000, the requirement is more than or equal to 230MPa, the measured value is 234.8MPa, and the bending elastic modulus (× 10) is used for subsequent injection molding parts or molds4) Measured according to GB/T9341-2000, the pressure is required to be more than or equal to 1.2MPa, and the measured value is 1.2 MPa; the notched impact strength of the cantilever beam is measured according to GB/T1843-1996, and the requirement is that the notched impact strength is more than or equal to 10.0KJ/m2Measured value of 9.9KJ/m2。
Claims (9)
1. A washing treatment method of an industrial production grade injection molding grade polyphenylene sulfide product comprises the following steps:
1) conveying the injection molding grade polyphenylene sulfide crude product to a filter press, and adding water to carry out primary slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5;
2) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing first filter pressing, and sending filtrate to a subsequent water treatment system;
3) after the filter pressing is finished, adding water into the filter press for secondary slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5;
4) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, carrying out secondary filter pressing, and conveying filtrate to a washing water tank for temporary storage so as to facilitate washing and recycling of products of the next batch;
5) after filter pressing is finished, adding the filtrate obtained in the step 4) into a filter press for third slurrying, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5;
6) repeating the step 4) for third filter pressing, and conveying the filtrate to a washing water tank for temporary storage so as to facilitate the washing recycling of the next batch of products;
7) after the filter pressing is finished, adding an acetic acid solution and the filtrate obtained in the step 6) into a filter press for carrying out fourth slurrying, and ensuring that the pH value of the mixed slurrying liquid is 4.5-5.0, so as to determine the dosage of the acetic acid solution, wherein the weight ratio of the injection molding grade polyphenylene sulfide crude product to the filtrate is 1: 25-1: 5;
8) starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing fifth filter pressing, and sending filtrate to a subsequent water treatment system;
9) adding desalted water or distilled water into the filter press to carry out fifth slurrying;
10) and starting a stirring device of the filter press, stirring and mixing for 15min at 85-95 ℃, performing fifth filter pressing, conveying the injection-grade polyphenylene sulfide to a subsequent drying system from the filter press after the filter pressing is finished, and conveying filtrate to a washing water tank for temporary storage so as to facilitate next recycling, wherein the weight ratio of the injection-grade polyphenylene sulfide crude product to the desalted water or distilled water is 1: 25-1: 5.
2. The washing treatment method according to claim 1, characterized in that the weight ratio of injection-grade polyphenylene sulfide crude product to the filtrate in step 1) is 1: 10.
3. The washing treatment method according to claim 1, characterized in that the weight ratio of injection-grade polyphenylene sulfide crude product to the filtrate in step 3) is 1: 10.
4. The washing treatment method according to claim 1, characterized in that the weight ratio of injection-grade polyphenylene sulfide crude product to the filtrate in step 5) is 1: 10.
5. The washing treatment method as claimed in claim 1, wherein the weight ratio of the injection-grade polyphenylene sulfide crude product to the filtrate in step 7) is 1: 10.
6. The washing treatment method according to claim 1, characterized in that the weight ratio of the injection-grade polyphenylene sulfide crude product to the demineralized or distilled water in step 10) is 1: 10.
7. The washing treatment method according to claim 1, wherein the concentration of the acetic acid solution in step 7) is 5% to 30% by mass.
8. The washing treatment method according to claim 1, characterized in that the injection-grade polyphenylene sulfide raw product in step 1) is prepared as follows:
1) adding 20-30 parts by weight of acetic anhydride, 150 parts by weight of sodium hydroxide 140-;
2) and transferring the sodium hydrosulfide solution from the dehydration reaction kettle to a subsequent polymerization reaction kettle, adding 190-280 parts by weight of p-dichlorobenzene, heating the polymerization reaction kettle to 265-280 ℃, keeping the stirring condition for 0.5h for polymerization reaction, then cooling to below 100 ℃ under the condition of keeping the pressure in the reactor unchanged, and finishing the reaction to obtain the injection molding grade polyphenylene sulfide crude product.
9. The washing treatment method as claimed in claim 1, wherein the injection-grade polyphenylene sulfide crude product comprises the following components in percentage by weight: according to the mass percentage, 5 percent of NMP, 39 percent of sodium chloride, 12 percent of sodium acetate, 2 percent of water and the balance of 42 percent of PPS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393637.7A CN111518276A (en) | 2020-05-11 | 2020-05-11 | Washing treatment method of injection molding grade polyphenylene sulfide industrial product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393637.7A CN111518276A (en) | 2020-05-11 | 2020-05-11 | Washing treatment method of injection molding grade polyphenylene sulfide industrial product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111518276A true CN111518276A (en) | 2020-08-11 |
Family
ID=71912532
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010393637.7A Pending CN111518276A (en) | 2020-05-11 | 2020-05-11 | Washing treatment method of injection molding grade polyphenylene sulfide industrial product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111518276A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612102A (en) * | 2022-10-18 | 2023-01-17 | 重庆聚狮新材料科技有限公司 | Polyphenylene sulfide purification production process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08170016A (en) * | 1994-12-19 | 1996-07-02 | Tonen Chem Corp | Polyarylene sulfide resin composition |
| JP2012092292A (en) * | 2010-09-30 | 2012-05-17 | Toray Ind Inc | Method for producing polyarylene sulfide resin, polyarylene sulfide resin, molding produced therefrom, and method for producing the same |
| CN102482420A (en) * | 2009-08-27 | 2012-05-30 | 东丽株式会社 | Polyarylene sulfide and method for producing same |
-
2020
- 2020-05-11 CN CN202010393637.7A patent/CN111518276A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08170016A (en) * | 1994-12-19 | 1996-07-02 | Tonen Chem Corp | Polyarylene sulfide resin composition |
| CN102482420A (en) * | 2009-08-27 | 2012-05-30 | 东丽株式会社 | Polyarylene sulfide and method for producing same |
| JP2012092292A (en) * | 2010-09-30 | 2012-05-17 | Toray Ind Inc | Method for producing polyarylene sulfide resin, polyarylene sulfide resin, molding produced therefrom, and method for producing the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612102A (en) * | 2022-10-18 | 2023-01-17 | 重庆聚狮新材料科技有限公司 | Polyphenylene sulfide purification production process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20180090886A (en) | A method for producing granular polyarylene sulfide, a method for increasing the average particle size of the granular polyarylene sulfide, a method for improving the grain strength of the granular polyarylene sulfide, | |
| JPH0214221A (en) | Treatment of arylene sulfide resin | |
| CN111454518B (en) | Method for preparing low-odor polypropylene by using intermittent liquid-phase bulk process | |
| CN114395216A (en) | Bio-based hyperbranched polymer epoxy resin and preparation method thereof | |
| CN111518276A (en) | Washing treatment method of injection molding grade polyphenylene sulfide industrial product | |
| US11440996B2 (en) | Preparation method of polyphenylene sulfide resin, and polyphenylene sulfide resin prepared thereby | |
| CN106832284A (en) | The production method of polyphenylene sulfide and its recovery method of distillation residual liquid | |
| CN107936250B (en) | Method for recycling polyphenylene sulfide oligomer | |
| CN104292391A (en) | Melting production method for unsaturated anhydride grafted chlorinated polyethylene | |
| CN101638396A (en) | Production process for rubber accelerator 2-thiol group benzothiazole | |
| US5364581A (en) | Process of making polyacrylonitrile fibers | |
| CN111548493A (en) | Washing treatment method of fiber-grade polyphenylene sulfide industrial product | |
| CN115368668B (en) | Modified EVOH resin and preparation method thereof | |
| JP5001017B2 (en) | Method for recovering and reusing thermosetting resin and method for producing modified styrene-fumaric acid copolymer | |
| CN109988263B (en) | Anhydride polymer chain extender and preparation method thereof | |
| CN114149586B (en) | Chain-extended polysulfate and preparation method thereof | |
| CN1095481C (en) | Process for preparing high-density high-molecular linear polyphenyl thioether | |
| JPH02225564A (en) | Polyarylene sulfide resin composition of stabilized hue | |
| US5708111A (en) | Process for the preparation of an acrylonitrile copolymer and product prepared therefrom | |
| CN108676334B (en) | Silica gel modified polylactic acid material and preparation method thereof | |
| JP5270871B2 (en) | Low shrinkage material for plastic, plastic molded product using the same, method for producing low shrinkage material for plastic, and method for recovering and reusing plastic | |
| CN111040282A (en) | High-strength high-heat-resistance polyethylene glass fiber reinforced belt and preparation method thereof | |
| JP2000080199A (en) | Method for separating polyamide and glass fiber from glass fiber-containing polyamide molded article | |
| CN117384380A (en) | Method for synthesizing polyphenylene sulfide by pressurizing inert gas without aid | |
| KR101102241B1 (en) | Method of manufacturing polyvinyl alcohol of highly degree of polymerization and highly degree of sponification with new solvent recovery strategy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200811 |