CN115806670B - Polyphenylene sulfide combined post-treatment purification method - Google Patents
Polyphenylene sulfide combined post-treatment purification method Download PDFInfo
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 78
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 90
- 229920005989 resin Polymers 0.000 claims abstract description 90
- 239000012065 filter cake Substances 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000011324 bead Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 33
- 238000000967 suction filtration Methods 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000005057 refrigeration Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 description 14
- 239000012535 impurity Substances 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 7
- 238000006068 polycondensation reaction Methods 0.000 description 6
- 239000002798 polar solvent Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- 238000001256 steam distillation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920000412 polyarylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention belongs to the field of polyphenylene sulfide resin purification, and particularly provides a polyphenylene sulfide resin post-treatment purification method which comprises the steps of heating and suction filtering a crude product of the polyphenylene sulfide resin, washing and suction filtering with deionized water, drying a filter cake after washing, then putting the filter cake into a ball mill, adding an ethanol solution with the mass concentration of 60% -95%, grinding by zirconia beads with the particle size range of 0.6-1.8mm, separating out the resin, heating and stirring the resin with deionized water for multiple times, washing the resin while the resin is hot, suction filtering the resin, and drying the resin to obtain the high-purity polyphenylene sulfide resin.
Description
Technical Field
The invention belongs to the field of polyphenylene sulfide resin purification, and particularly relates to a polyphenylene sulfide resin post-treatment purification method.
Background
Polyphenylene Sulfide (PPS) is one of the most important and common resin species among polyarylene sulfides. The polyphenylene sulfide has high stability of chemical bond characteristic of molecules due to rigidity and heat resistance of benzene ring structure and stability of chemical bond between benzene ring and sulfur, and has excellent thermal stability, chemical stability, dimensional stability, electrical property and the like.
In the related literature, various reaction routes for synthesizing polyphenylene sulfide are reported, but the industrial production of polyphenylene sulfide resin mainly adopts a sodium sulfide solution polycondensation method. In the process of synthesizing the polyphenylene sulfide resin, sodium chloride is generated simultaneously, other inorganic salt additives are also required to be added, so that when sodium sulfide and paradichlorobenzene are subjected to polycondensation reaction in a solvent system, inorganic salt and products are dissolved in an organic solvent simultaneously, and finally the obtained polyphenylene sulfide resin is wrapped with a large amount of inorganic salt, organic solvent, oligomer and the like, and the impurities can influence the mechanical property, thermal stability, electrical insulation and other properties of the resin, so that the application of the polyphenylene sulfide resin in the fields of national defense, military industry, aerospace, electronic packaging elements and the like is indirectly influenced.
Patent CN112940255A discloses a purification treatment process of polyphenylene sulfide resin, which adopts sodium sulfide and p-dichlorobenzene as raw materials and N-methyl-2-pyrrolidone as solvent to synthesize the polyphenylene sulfide resin, the filter cake obtained by filtering and separating the polyphenylene sulfide resin contains organic impurities, sodium chloride, NMP solvent and water, after washing and drying, adding a mixed solvent, raising the temperature of a solid-liquid system to be lower than the boiling point of the mixed solvent, dissolving the polyphenylene sulfide resin in the mixed solvent, after keeping the temperature for a certain time, adding deionized water, crystallizing and separating out the polyphenylene sulfide, after solid-liquid separation, extracting the high boiling point organic solvent in the mixed solvent by using a low boiling point solvent, and washing the polyphenylene sulfide resin by using deionized water, thus obtaining the high-purity polyphenylene sulfide resin. However, the method is complicated in operation and is not suitable for industrial production.
Patent CN102731785A discloses a method for purifying polyphenylene sulfide, which comprises the following steps: (1) acid-base neutralization: cooling polyphenylene sulfide resin generated by polymerization reaction, adding acid, controlling the PH to be 3-4, and reacting for a period of time under stirring; (2) solid-liquid separation: cooling the reaction product obtained in the step (1) and carrying out solid-liquid separation to obtain polyphenylene sulfide solid; (3) solvent washing: adding an organic solvent into the polyphenylene sulfide solid obtained in the step (2), and washing the polyphenylene sulfide solid in a stirring state; (4) steam distillation and water washing: carrying out steam distillation on the polyphenylene sulfide obtained in the step (3) under the condition of negative pressure, and recovering the organic solvent remained in the polyphenylene sulfide solid particles in the distillation process; when the content of the organic solvent is less than 1%, the polyphenylene sulfide is washed by steam condensate water at 75-85 ℃; (5) drying and packaging: and (3) separating, drying and packaging the polyphenylene sulfide obtained in the step (4). The method is based on steam distillation under the condition of negative pressure, has high requirement and is not suitable for industrial production.
Disclosure of Invention
In order to remove impurities wrapped in the polyphenylene sulfide resin as much as possible and obtain the high-purity polyphenylene sulfide resin, the invention provides a polyphenylene sulfide resin post-treatment purification method which has the characteristics of simplicity and high efficiency.
In order to achieve the purpose of the invention, the technical scheme adopted is as follows:
A polyphenylene sulfide resin post-treatment purification method comprises the following steps:
Heating and suction filtering a polyphenylene sulfide resin crude product, washing and suction filtering deionized water (a filter cake contains impurities such as solvent and sodium chloride, and the filter cake is washed and suction filtered by deionized water, so that part of the impurities in the resin can be removed, but a small amount of impurities such as sodium chloride are also wrapped in the resin, and the impurities can influence the performance of the polyphenylene sulfide in the use process), drying the washed filter cake, then putting the dried filter cake into a ball mill, adding an ethanol solution, grinding zirconia beads with different particle diameters, separating out the resin, heating and stirring the resin with deionized water for multiple times, washing the resin while the resin is hot, suction filtering the resin, and then drying the resin to obtain the high-purity polyphenylene sulfide resin.
The ethanol solution is added and milled together, and during milling some impurities (partial salts and solvents) are more soluble in the ethanol solution with rapid rotation, in which case the largest amount of impurities can be subsequently removed with the least amount of deionized water.
Further, the method for obtaining the polyphenylene sulfide resin crude product comprises the following steps: the industrial anhydrous sodium sulfide and industrial paradichlorobenzene are used as raw materials, lithium chloride is used as a catalyst, N-methylpyrrolidone (NMP) is used as a solvent to synthesize the polyphenylene sulfide resin, and the molecular weight of the polyphenylene sulfide resin is 4.2-4.8 ten thousand.
Further, the crude product of the polyphenylene sulfide resin is heated and filtered for more than 10 minutes at the temperature of more than 80 ℃, and is filtered while the crude product is still hot, and the solid obtained by the filtering can be separated by 90 percent, namely more than 90 percent of polar solvent is separated.
Further, the resin is heated, stirred and washed for a plurality of times for 2 to 3 times after grinding, the heating temperature is more than 80 ℃ and maintained for more than 10 minutes, and then the resin is filtered while the resin is still hot.
Furthermore, the particle size of the zirconia balls is in the range of 0.6-12mm, the dissolution effect of ethanol solution on impurities can be better promoted in the grinding process, the preferred particle size range is in the range of 0.6-1.8mm, the sample loading amount of the filter cake is 50-80% of the volume of the ball milling tank, and the preferred sample loading amount is 66% of the volume of the ball milling tank.
Furthermore, the grinding machine is a refrigeration planetary ball mill, and the working mode is that four tanks are operated simultaneously; the revolution range of the refrigeration planetary ball mill is 180-290r/min, preferably 290r/min, the rotation range is 360-580r/min, and preferably 580r/min.
Further, the concentration of the ethanol solution is 60% -95%, and the preferable concentration range is 70% -95%.
Further, the drying method is that the drying is carried out for 8 to 10 hours at the temperature of 80 to 100 ℃.
On the basis of hot suction filtration and heating washing suction filtration of the crude product, the invention combines grinding with ethanol solution dissolution and washing to realize effective removal of chloride ions and organic solvents, and has the characteristics of simplicity and high efficiency compared with the prior art.
Drawings
FIG. 1 is a process flow diagram of the preparation and post-treatment of polyphenylene sulfide in an embodiment of the invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The method for obtaining the polyphenylene sulfide resin in the following examples and comparative examples includes: the industrial anhydrous sodium sulfide and industrial paradichlorobenzene are used as raw materials, lithium chloride is used as a catalyst, N-methylpyrrolidone (NMP) is used as a solvent to synthesize the polyphenylene sulfide resin, and the molecular weight of the polyphenylene sulfide resin is 4.2-4.8 ten thousand.
Example 1
(1) After the polyphenylene sulfide polycondensation reaction is completed, heating the polyphenylene sulfide resin mixture to more than 80 ℃ and maintaining for about 10 minutes, and then carrying out suction filtration while the mixture is hot to obtain solid, wherein the separation rate of the solid obtained by suction filtration reaches 90 percent, namely more than 90 percent of polar solvent is separated, the solid of a filter cake is for later use, and filtrate is recovered;
(2) Stirring and washing the solid components of the filter cake in the step (1) by using deionized water, wherein the water consumption is 2L, the temperature is required to be higher than 80 ℃, the filter cake is maintained for about 10 minutes, and then the filter cake is filtered while the filter cake is hot, and the filter cake is dried for standby;
(3) Taking out 10 g of the solid component of the dried filter cake in the step (2), putting the solid component into a 500mL ball milling tank, adding 100mL of ethanol solution with the concentration of 95%, putting zirconia balls with the particle size of 0.6-0.8mm, and setting the total sample loading amount to 66% of the volume of the ball milling tank, wherein the rotating speed of the ball milling machine is revolution: 290r/min, autorotation: 580r/min, grinding for 10 minutes, separating, and standing the separated resin for later use;
(4) Heating and stirring the resin separated in the step (3) by using deionized water, wherein the water consumption is 2L, the resin is heated to more than 80 ℃ and maintained for about 10 minutes, and then carrying out suction filtration while the resin is hot, repeating for 2-3 times, and detecting the Cl - content to be 0.01% for standby of filter cake solids;
(5) Putting the filter cake solid in the step (4) into a baking oven, and baking for 8-10 hours at the temperature of 80-100 ℃;
(6) Weighing a certain amount of polyphenylene sulfide resin dried in step (5), putting into a muffle furnace for roasting, and setting the temperature of the muffle furnace: the room temperature was raised to 800℃for 1 hour, maintained at 800℃for 8 hours, lowered to room temperature for 3 hours, and then taken out, and the weight of ash was weighed to be 0.08%.
Example 2
(1) After the polyphenylene sulfide polycondensation reaction is completed, heating the polyphenylene sulfide resin mixture to more than 80 ℃ and maintaining for about 10 minutes, and then carrying out suction filtration while the mixture is hot to obtain solid, wherein the separation rate of the solid obtained by suction filtration reaches 90 percent, namely more than 90 percent of polar solvent is separated, the solid of a filter cake is for later use, and filtrate is recovered;
(2) Stirring and washing the solid components of the filter cake in the step (1) by using deionized water, wherein the water consumption is 2L, the temperature is required to be higher than 80 ℃, the filter cake is maintained for about 10 minutes, and then the filter cake is filtered while the filter cake is hot, and the filter cake is dried for standby;
(3) Taking out 10 g of the solid component of the dried filter cake in the step (2), putting the solid component into a 500mL ball milling tank, adding 100mL of ethanol solution with the concentration of 95%, putting zirconia balls with the particle size of 0.8-1.0mm, and setting the total sample loading amount to 66% of the volume of the ball milling tank, wherein the rotating speed of the ball milling machine is revolution: 290r/min, autorotation: 580r/min, grinding for 10 minutes, separating, and standing the separated resin for later use;
(4) Heating and stirring the resin separated in the step (3) by using deionized water, wherein the water consumption is 2L, the resin is heated to more than 80 ℃ and maintained for about 10 minutes, and then carrying out suction filtration while the resin is hot, repeating for 2-3 times, and detecting the Cl - content of the filter cake for later use;
(5) Putting the filter cake solid in the step (4) into a baking oven, and baking for 8-10 hours at the temperature of 80-100 ℃;
(6) Weighing a certain amount of polyphenylene sulfide resin dried in step (5), putting into a muffle furnace for roasting, and setting the temperature of the muffle furnace: the room temperature was raised to 800 ℃, for 1 hour, kept at 800 ℃ for 8 hours, cooled to room temperature, for 3 hours, and then taken out, and the weight of ash was weighed to be 0.12%.
Example 3
(1) After the polyphenylene sulfide polycondensation reaction is completed, heating the polyphenylene sulfide resin mixture to more than 80 ℃ and maintaining for about 10 minutes, and then carrying out suction filtration while the mixture is hot to obtain solid, wherein the separation rate of the solid obtained by suction filtration reaches 90 percent, namely more than 90 percent of polar solvent is separated, the solid of a filter cake is for later use, and filtrate is recovered;
(2) Stirring and washing the solid components of the filter cake in the step (1) by using deionized water, wherein the water consumption is 2L, the temperature is required to be higher than 80 ℃, the filter cake is maintained for about 10 minutes, and then the filter cake is filtered while the filter cake is hot, and the filter cake is dried for standby;
(3) Taking out 10 g of the solid component of the dried filter cake in the step (2), putting the solid component into a 500mL ball milling tank, adding 100mL of ethanol solution with the concentration of 95%, putting zirconia balls with the particle size of 1.0-1.2mm, and setting the total sample loading amount to 66% of the volume of the ball milling tank, wherein the rotating speed of the ball milling machine is revolution: 290r/min, autorotation: 580r/min, grinding for 10 minutes, separating, and standing the separated resin for later use;
(4) Heating and stirring the resin separated in the step (3) by using deionized water, wherein the water consumption is 2L, the resin is heated to more than 80 ℃ and maintained for about 10 minutes, and then carrying out suction filtration while the resin is hot, repeating for 2-3 times, and detecting the Cl - content to be 0.09% for later use;
(5) Putting the filter cake solid in the step (4) into a baking oven, and baking for 8-10 hours at the temperature of 80-100 ℃;
(6) Weighing a certain amount of polyphenylene sulfide resin dried in step (5), putting into a muffle furnace for roasting, and setting the temperature of the muffle furnace: the room temperature was raised to 800 ℃, for 1 hour, kept at 800 ℃ for 8 hours, cooled to room temperature, for 3 hours, and then taken out, and the weight of ash was weighed to be 0.16%.
Example 4
The same procedure as in example 1 is followed, except that:
The grain diameter of the zirconia balls is changed to 1.2-1.4mm;
Operating according to the conditions, the Cl - detection content is 0.13%; the ash weighed 0.20% by weight.
Example 5
The same procedure as in example 1 is followed, except that:
The grain diameter of the zirconia balls is changed to 1.4-1.6mm;
Operating according to the conditions, the Cl - detection content is 0.17%; the ash weighed 0.24% by weight.
Example 6
The same procedure as in example 1 is followed, except that:
the grain diameter of the zirconia balls is changed to 1.6-1.8mm;
Operating according to the conditions, the Cl - detection content is 0.21%; the ash weighed 0.28% by weight.
Example 7
The same procedure as in example 1 is followed, except that:
The ethanol concentration is changed to 90%;
operating according to the condition, the Cl - detection content is 0.03%; the ash weighed 0.10% by weight.
Example 8
The same procedure as in example 1 is followed, except that:
The ethanol concentration is changed to 85%;
operating according to the conditions, the Cl - detection content is 0.05%; the ash weighed 0.12% by weight.
Example 9
The same procedure as in example 1 is followed, except that:
the concentration of ethanol is changed to 80%;
Operating according to the conditions, the Cl - detection content is 0.07%; the ash weighed 0.14% by weight.
Example 10
The same procedure as in example 1 is followed, except that:
Ethanol concentration was changed to 75%;
operating according to the conditions, the Cl - detection content is 0.09%; the ash weighed 0.16% by weight.
Example 11
The same procedure as in example 1 is followed, except that:
The ethanol concentration is changed to 70%;
Operating according to the conditions, the Cl - detection content is 0.11%; the ash weighed 0.18% by weight.
Comparative example 1
The same procedure as in example 1 is followed, except that:
the concentration of the ethanol solution is changed to 50%;
The grain diameter of the zirconia balls is changed to 0.6-0.8mm;
Operating according to the conditions, the Cl - detection content is 2.3%; the ash weighed 3.5% by weight.
Comparative example 2
The same procedure as in example 1 is followed, except that:
The concentration of the ethanol solution is changed to 60%;
The grain diameter of the zirconia balls is changed to 0.8-1.0mm;
Operating according to the conditions, the Cl - detection content is 2.5%; the ash weighed 3.8% by weight.
Comparative example 3
The same procedure as in example 1 is followed, except that:
the concentration of the ethanol solution is changed to 95%;
The grain diameter of the zirconia balls is changed to 2mm;
operating according to the conditions, the Cl - detection content is 2.8%; the ash weighed 4.0% by weight.
Comparative example 4
The same procedure as in example 1 is followed, except that:
The concentration of the ethanol solution is changed to 90%;
the grain diameter of the zirconia balls is changed to 3mm;
Operating according to the conditions, the Cl - detection content is 3.0%; the ash weighed 4.2% by weight.
Comparative example 5
The same procedure as in example 5 is followed, except that:
the rotation speed of the ball mill is set as revolution: 100r/min, rotation: 200r/min
Operating according to the conditions, the Cl - detection content is 2.4%; the ash weighed 3.6% by weight.
Comparative example 6
The same procedure as in example 6 is followed, except that:
the rotation speed of the ball mill is set as revolution: 50r/min, rotation: 100r/min
Operating according to the conditions, the Cl - detection content is 2.9%; the ash weighed 4.1% by weight.
Comparative example 7
The treatment process and test data of the polyphenylene sulfide resin are shown in table 1:
(1) After the polyphenylene sulfide polycondensation reaction is completed, heating the polyphenylene sulfide resin mixture to more than 80 ℃ and maintaining for about 10 minutes, and then carrying out suction filtration while the mixture is hot to obtain solid, wherein the separation rate of the solid obtained by suction filtration reaches 90 percent, namely more than 90 percent of polar solvent is separated, the solid of a filter cake is for later use, and filtrate is recovered;
(2) Stirring and washing the solid components of the filter cake in the step (1) by using deionized water, wherein the water consumption is 2L, the temperature is required to be higher than 80 ℃, the filter cake is maintained for about 10 minutes, and then the filter cake is filtered while the filter cake is hot, the filter cake is repeated for 2-3 times, and the content of Cl - is detected to be 3.8%;
(3) Putting the filter cake solid in the step (2) into a baking oven, and drying for 8-10 hours at the temperature of 80-100 ℃;
(4) Weighing a certain amount of polyphenylene sulfide resin dried in the step (3), putting the polyphenylene sulfide resin into a muffle furnace for roasting, and setting the temperature of the muffle furnace: the room temperature was raised to 800 ℃, for 1 hour, kept at 800 ℃ for 8 hours, cooled to room temperature, for 3 hours, and then taken out, and the weight of ash was weighed to be 5%.
TABLE 1
| Sample of | Ash (%) | Cl - content (%) |
| Homemade polyphenylene sulfide resin | 5 | 3.8 |
The low-salt and low-impurity polyphenylene sulfide resin can be obtained by the post-treatment method, and test data are summarized in the following tables 2 and 3:
TABLE 2
TABLE 3 Table 3
The purification method can improve the purity of the polyphenylene sulfide, thereby improving the subsequent processing performance of the polyphenylene sulfide.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme and the concept of the present invention, and should be covered by the scope of the present invention.
Claims (6)
1. A polyphenylene sulfide resin post-treatment purification method is characterized in that: heating and suction-filtering a polyphenylene sulfide resin crude product, washing and suction-filtering with deionized water, drying a filter cake after washing, putting into a ball mill, adding an ethanol solution with the mass concentration of 70% -95%, grinding by zirconia beads with the particle size range of 0.6-1.8 mm, separating out resin, heating and stirring with deionized water for multiple times, washing and suction-filtering while hot, and drying to obtain high-purity polyphenylene sulfide resin;
the resin is heated, stirred and washed for a plurality of times for 2 to 3 times after grinding, the heating temperature is more than 80 ℃ and maintained for more than 10 minutes, and then the resin is filtered while the resin is hot;
the grinding machine is a refrigeration planetary ball mill, and the working mode is that four tanks are operated simultaneously; the revolution range is 180-290r/min, and the rotation range is 360-580 r/min.
2. The polyphenylene sulfide resin post-treatment purification method according to claim 1, wherein: the method for obtaining the polyphenylene sulfide resin crude product comprises the following steps: the industrial anhydrous sodium sulfide and industrial paradichlorobenzene are used as raw materials, lithium chloride is used as a catalyst, N-methylpyrrolidone is used as a solvent to synthesize the polyphenylene sulfide resin, and the molecular weight of the polyphenylene sulfide resin is 4.2-4.8 ten thousand.
3. The polyphenylene sulfide resin post-treatment purification method according to claim 1, wherein: the temperature of the heating and suction filtration of the polyphenylene sulfide resin crude product is more than 80 ℃ and maintained for more than 10 minutes, and then the suction filtration is carried out while the polyphenylene sulfide resin crude product is hot, and the separation rate of the solid obtained by the suction filtration reaches 90 percent.
4. The polyphenylene sulfide resin post-treatment purification method according to claim 1, wherein: the sample loading amount of the filter cake is 50% -80% of the volume of the ball milling tank.
5. The polyphenylene sulfide resin post-treatment purification method according to claim 1, wherein: the loading of the filter cake was 66% of the ball milling pot volume.
6. The polyphenylene sulfide resin post-treatment purification method according to claim 1, wherein: the drying method is that the drying is carried out for 8-10 hours at the temperature of 80-100 ℃.
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