CN111363139A - Post-treatment method of polyaryletherketone polymer - Google Patents
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Abstract
The invention provides a post-treatment method of a polyaryletherketone polymer, belonging to the technical field of post-treatment of polymers. The method comprises the following steps: filtering the polyaryletherketone polymer solution by a filter, and then drying by a spray drying tower, wherein the spray drying tower is used for circularly preheating gas in the tower, the temperature of a circulating airflow inlet is set to 180-plus-200 ℃, the temperature of an airflow outlet is set to 120-plus-135 ℃, after the temperature is stabilized, the polyaryletherketone polymer solution is pumped into the spray drying tower by a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is set to 180-plus-200 ℃, the temperature of the airflow outlet is reduced to 105-plus-132 ℃, and after passing through a cyclone separator, the solvent is separated from the polymer and dried to obtain the processed polyaryletherketone polymer. The method ensures that the residual amount of inorganic salt in the polymer is less than 0.1 percent, the residual amount of high-boiling point solvent is less than 1 percent, the low-molecular weight polymer is not lost, and the method also has better improvement effect on the thermal processing of the polymer.
Description
Technical Field
The invention belongs to the technical field of post-treatment of polymers, and particularly relates to a post-treatment method of a polyaryletherketone polymer.
Background
Polyphenylene oxide, polyphenylene sulfide, polyaryletherketone, polyarylethersulfone, polyarylethernitrile homopolymer and copolymer and other special engineering plastics are mainly prepared by an SN2 nucleophilic polycondensation method, in recent years, soluble polymers are more flexible in processing method and better in dimensional stability, and the application fields are wider and wider, but are limited by the price of raw materials and a post-treatment method, so that the cost of the polymers is always high.
Chinese patent CN85108751A discloses a post-treatment method of phenolphthalein type polyaryletherketone: the polymer obtained by the preparation is filtered to remove salt, precipitated in ethanol, boiled and washed by boiling water for three times, filtered and dried to obtain the polymer. The method uses a large amount of deionized water, has large energy consumption and heavy environmental burden, and can expect that the product obtained by the method has porosity, particularly good toughness of the polymer, irregular shape of the crushed precipitate and poor liquidity by the treatment mode of the method of precipitating the precipitate into a poor solvent after dilution by the good solvent. Chinese patents 201711040027.3 and 201711043441.X disclose post-treatment methods of soluble polyaryletherketone and nitrogenous polyaryletherresin polymer, respectively, which can remove a large amount of branched structures, insoluble substances and small molecular oligomers, but need to consume a large amount of solvent, and the post-treatment process also adopts a large amount of water washing method, so that the environmental burden is heavy.
Disclosure of Invention
The invention aims to solve the technical problems that the existing method for post-treating the polyaryletherketone polymer needs to consume a large amount of solvent and has heavy environmental burden, and provides a method for post-treating the polyaryletherketone polymer.
The invention provides a post-treatment method of a polyaryletherketone polymer, which comprises the following steps:
filtering the polyaryletherketone polymer solution by a filter, and then drying by a spray drying tower, wherein the spray drying tower is used for circularly preheating gas in the tower, the temperature of a circulating airflow inlet is set to 180-plus-200 ℃, the temperature of an airflow outlet is set to 120-plus-135 ℃, after the temperature is stabilized, the polyaryletherketone polymer solution is pumped into the spray drying tower by a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is set to 180-plus-200 ℃, the temperature of the airflow outlet is reduced to 105-plus-132 ℃, and after passing through a cyclone separator, the solvent is separated from the polymer and dried to obtain the processed polyaryletherketone polymer.
Preferably, the filtration is specifically as follows: the polyaryletherketone polymer solution is firstly filtered by a plate filter for 2-3 times and then filtered by a fine filter for 1-2 times.
Preferably, the polyaryletherketone polymer solution is a polyaryletherketone polymer solution containing an organic solvent and inorganic insoluble substances, wherein the inorganic insoluble substances and the organic solvent are immiscible;
or a soluble polyaryletherketone solution without inorganic salts.
Preferably, the organic solvent is one or more selected from diphenyl sulfone, sulfolane, dimethyl sulfoxide, N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide, 1, 3-dimethyl-2-imidazolidinone or N-cyclohexyl pyrrolidone.
Preferably, the inorganic insoluble material is an inorganic salt or an inorganic additive.
Preferably, the inorganic salt is potassium chloride, potassium fluoride, sodium chloride, sodium fluoride, calcium chloride, calcium fluoride, arsenic pentafluoride, potassium carbonate, sodium carbonate, calcium carbonate or cerium carbonate.
Preferably, the inorganic additive is aluminum oxide or ferroferric oxide.
Preferably, the polyaryletherketone polymer is the product of the polycondensation of a bisphenol and a dihalogen monomer, or is a terpolymer or multipolymer comprising structural units represented by formulas 101 and 102:
the mass ratio of the repeating unit represented by the formula 101 to the repeating unit represented by the formula 102 is 0.01-100: 1;
m, R is the residual group of bisphenol compounds after hydroxyl groups are removed;
x, Z is the residue of double-halogen compound containing benzene ring after removing two halogens, and X, Z of them have at least one ketone carbonyl structure;
when M is the same as X in structure, R is the same as Z in structure, namely the polyaryletherketone homopolymer is obtained;
when M and X are the same in structure, and R and Z are different in structure; or M and X are different in structure, and R and Z are the same in structure; namely the polyaryletherketone terpolymer;
when M, X has different structures and R and Z have different structures, it is a tetrapolymer (multipolymer).
Preferably, the polymer includes, but is not limited to, the repeating unit represented by the formula 101,
the repeating unit represented by the formula 102 is
Preferably, the structural formula of the polyaryletherketone polymer is as follows:
the invention has the advantages of
The invention provides a post-treatment method of a polyaryletherketone polymer, which is used for removing inorganic salt, crosslinking byproducts and organic solvents in a polymer solution quickly, efficiently, environmentally and at low cost by combining filtration and spray drying, and separating to obtain polymer powder. The method ensures that the residual amount of inorganic salt in the polymer is less than 0.1 percent, the residual amount of high-boiling point solvent is less than 1 percent, the low-molecular weight polymer is not lost, and the method also has better improvement effect on the thermal processing of the polymer. The method can be used for treating the stock solution containing the inorganic salt obtained by the polymerization reaction and can also be used for recovering and purifying the soluble polymer, and is a post-treatment mode which is more environment-friendly, more energy-saving and more efficient in the purification treatment modes of the materials at present.
Drawings
FIG. 1 is a thermogravimetry curve of phenolphthalein polyaryletherketone coarse powder obtained by the treatment of example 1.
Detailed Description
The invention provides a post-treatment method of a polyaryletherketone polymer, which comprises the following steps:
filtering the polyaryletherketone polymer solution by a filter, wherein preferably, the polyaryletherketone polymer solution is filtered by a plate filter for 2-3 times and a fine filter (10 microns) for 1-2 times;
and then drying the polyaryletherketone by a spray drying tower, wherein the spray drying tower is used for circularly preheating gas in the tower, the temperature of a circulating airflow inlet is set to 180-plus-200 ℃, the temperature of an airflow outlet is set to 120-plus-135 ℃, the polyaryletherketone polymer solution is injected into the spray drying tower by a high-pressure infusion pump after the temperature is stabilized, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is set to 180-plus-200 ℃, the temperature of the airflow outlet is reduced to 105-plus-132 ℃, the solvent is separated from the polymer after passing through a cyclone separator, and the treated polyaryletherketone polymer is obtained after drying.
The temperature of the circulating gas flow has great influence on the removal of the solvent, when the temperature is too low (120 ℃), only part of the diluted solvent is carried out, and the high-boiling-point solvent such as sulfolane and the like is still remained in the polymer powder, so that the solvent can be adhered to the bottom of the spray tower and can be blocked for a long time. When the temperature is too high, a large amount of solvent is evaporated, all the diluent and part of the high-boiling point solvent are taken away by hot air flow, although the solvent content of the coarse powder is lower, the polymer powder is in a high elastic state or viscous state at higher temperature and is bonded with each other, but the heat loss in the circulation process is increased, the economy is poor, and the post-treatment cost is not favorably saved. Therefore, a suitable maximum temperature should be 20-30 ℃ below the glass transition temperature of the polymer.
According to the invention, the polyaryletherketone polymer solution is a polyaryletherketone polymer solution containing an organic solvent and inorganic insoluble substances, wherein the inorganic insoluble substances and the organic solvent are immiscible; or a soluble polyaryletherketone solution without inorganic salts. The organic solvent is preferably selected from one or more of diphenyl sulfone, sulfolane, dimethyl sulfoxide, N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide, 1, 3-dimethyl-2-imidazolidinone or N-cyclohexyl pyrrolidone. The inorganic insoluble substance is preferably an inorganic salt or an inorganic additive, and the inorganic salt is preferably potassium chloride, potassium fluoride, sodium chloride, sodium fluoride, calcium chloride, calcium fluoride, arsenic pentafluoride, potassium carbonate, sodium carbonate, calcium carbonate or cerium carbonate. The inorganic additive is preferably aluminum oxide or ferroferric oxide.
According to the invention, the polyaryletherketone polymer is completely dissolved in the presence of the solvent and diluent used in the synthesis.
According to the invention, the polyaryletherketone polymer is a product of polycondensation of a bisphenol and a dihalogen monomer, or is a ternary or multicomponent copolymer comprising structural units represented by formulas 101 and 102:
the mass ratio of the repeating unit represented by the formula 101 to the repeating unit represented by the formula 102 is 0.01-100: 1;
m, R is the residual group of bisphenol compounds after hydroxyl groups are removed;
x, Z is the residue of double-halogen compound containing benzene ring after removing two halogens, and X, Z of them have at least one ketone carbonyl structure;
when M is the same as X in structure, R is the same as Z in structure, namely the polyaryletherketone homopolymer is obtained;
when M and X are the same in structure, and R and Z are different in structure; or M and X are different in structure, and R and Z are the same in structure; namely the polyaryletherketone terpolymer;
when M, X has different structures and R and Z have different structures, it is a tetrapolymer (multipolymer).
Preferably, the polymer includes, but is not limited to, the repeating unit represented by the formula 101,
the repeating unit represented by the formula 102 is
More preferably, the structural formula of the polyaryletherketone polymer is as follows:
the technical scheme of the invention is further described in detail by combining specific examples, wherein the raw materials involved in the examples are all commercially available.
Example 1
Post-treatment of phenolphthalein type polyaryletherketone homopolymer solution
The polymer solution obtained by polymerization contains 4.15kg of potassium carbonate, 23.2kg of potassium fluoride, 99.3kg of phenolphthalein polyaryletherketone homopolymer, 310kg of sulfolane and 1200kg of N, N-dimethylacetamide with the solid content of 6.2%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 3 times and a fine filter (10 μm) 1 time to obtain 1595.2kg of the polymer solution.
The spray drying tower is first preheated by circulating gas in the tower at the inlet temperature of 200 deg.c and the outlet temperature of 120 deg.c, and after the temperature is stabilized, the polymer solution is pumped via high pressure liquid pump into the spray drierIn the drying tower, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is 200 ℃, the temperature of the airflow outlet is reduced to 108 ℃, the solvent is separated from the polymer after passing through a cyclone separator, 118.5kg of phenolphthalein polyaryletherketone homopolymer is obtained, and the solvent content at the material outlet is 11.9 percent. The resulting polymer was further dried to obtain a final polymer solvent residual amount (TGA method) of not more than 0.085% and a bulk density of 0.35kg/cm3. The particle size of the polymer microsphere is 30-85 microns measured by an electron microscope.
FIG. 1 is a thermogram (temperature rising rate 10K/min) of phenolphthalein polyaryletherketone coarse powder obtained by treatment of example 1; FIG. 1 illustrates that the solvent content of the meal is 11.85%
Example 2
Post-treatment of phenolphthalein type polyaryletherketone copolymer solution (PHT + DFK +6FBPA)
The polymer solution obtained by polymerization contains 4.15kg of potassium carbonate, 23.2kg of potassium fluoride, 95.2kg of phenolphthalein polyaryletherketone copolymer, 310kg of sulfolane and 700kg of N, N-dimethylacetamide, wherein the solid content of the polymer is 7.9%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 3 times and a fine filter (10 μm) 2 times to obtain 1094.8kg of the polymer solution.
The spray drying tower is first preheated by gas circulation in the tower, the temperature of a circulating gas flow inlet is 180 ℃, the temperature of a gas flow outlet is 120 ℃, after the temperature is stable, polymer solution is pumped into the spray drying tower through a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating gas flow inlet is 180 ℃, the temperature of the gas flow outlet is reduced to 105 ℃, a cyclone separator is used for separating a solvent from the polymer, 118.5kg of phenolphthalein polyaryletherketone homopolymer is obtained, and the content of the solvent in the material outlet is 15.4%. Further drying the obtained polymer to obtain phenolphthalein type polyaryletherketone copolymer with high boiling point solvent content lower than 0.09% and bulk density of 0.32kg/cm3. The polymer is spherical as measured by an electron microscope, and the diameter of the microsphere is 30-85 microns.
Example 3
Post-treatment of phenolphthalein type polyaryletherketone nitrile copolymer solution (PHT + DFDK + DCBN)
The polymer solution obtained by polymerization contained 4.15kg of potassium carbonate, 6.92kg of potassium fluoride, 30.2kg of potassium chloride, 90.6kg of phenolphthalein polyarylethernitrileone copolymer, 190kg of sulfolane and 400kg of N-methylpyrrolidone. The polymer solids content was 13.3%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 2 times and a fine filter (5 μm) 1 time to obtain 673.7kg of the polymer solution.
The spray drying tower is first preheated by gas circulation in the tower, the temperature of a circulating airflow inlet is 180 ℃, the temperature of an airflow outlet is 130 ℃, after the temperature is stable, polymer solution is pumped into the spray drying tower through a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is 180 ℃, the temperature of the airflow outlet is reduced to 115 ℃, a cyclone separator is used for separating a solvent from the polymer, 103.5kg of phenolphthalein polyaryl ether nitrile ketone copolymer is obtained, and the content of the solvent in the material outlet is 21.4%. The resulting polymer was further dried to obtain a final polymer solvent residual amount (TGA method) of not more than 0.095% and a bulk density of 0.20kg/cm3. The particle size of the polymer microsphere is 30-85 microns measured by an electron microscope.
Example 4
Post-treatment of carbazolyl phenolphthalein type polyaryletherketone homopolymer solution
The polymer solution obtained by polymerization contains 3.2kg of sodium carbonate, 5.0kg of sodium fluoride, 30.2kg of sodium chloride, 110.6kg of phenolphthalein polyaryletherketone copolymer, 240kg of sulfolane and 600kg of N, N-dimethylacetamide. The polymer solids content was 11.6%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 4 times and a fine filter (15 μm) 4 times to obtain 942.7kg of the polymer solution.
The spray drying tower is first preheated by gas circulation in the tower, the temperature of a circulating gas flow inlet is 195 ℃, the temperature of a gas flow outlet is 135 ℃, after the temperature is stable, polymer solution is pumped into the spray drying tower through a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating gas flow inlet is 200 ℃, the temperature of the gas flow outlet is reduced to 132 ℃, a cyclone separator is used for separating the solvent from the polymer, 120.5kg of phenolphthalein polyaryletherketone homopolymer is obtained, and the content of the solvent in the material outlet is 11.2%. The resulting polymer was further dried to obtain a final polymer solvent residual amount (TGA method) of not more than 0.08% and a bulk density of 0.22kg/cm3. The granularity of the polymer microsphere is measured by an electron microscope to be 40-95 microns.
To further illustrate the effect of recycle gas stream inlet temperature on polymer meal solvent residue in this protocol, comparative analyses were conducted on the conditions in example 1, respectively.
Comparative example 1:
post-treatment of phenolphthalein type polyaryletherketone homopolymer solution
The polymer solution obtained by polymerization contains 4.15kg of potassium carbonate, 23.2kg of potassium fluoride, 99.3kg of phenolphthalein polyaryletherketone homopolymer, 310kg of sulfolane and 1200kg of N, N-dimethylacetamide with the solid content of 6.2%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 3 times and a fine filter (10 μm) 1 time to obtain 1595.2kg of the polymer solution.
The method comprises the steps of firstly, circularly preheating gas in a spray drying tower, wherein the inlet temperature of a circulating gas flow is 170 ℃, the outlet temperature of the gas flow is 102 ℃, after the temperature is stable, pumping a polymer solution into the spray drying tower through a high-pressure infusion pump, the pressure is 0.102MPa, the inlet temperature of the circulating gas flow is 170 ℃, the outlet temperature of the gas flow is reduced to 98 ℃, separating a solvent from the polymer after passing through a cyclone separator, treating the obtained phenolphthalein polyaryletherketone homopolymer coarse powder immediately, easily adhering, and enabling the solvent content of a sample at a material outlet to be 27.2%.
Comparative example 2:
post-treatment of phenolphthalein type polyaryletherketone homopolymer solution
The polymer solution obtained by polymerization contains 4.15kg of potassium carbonate, 23.2kg of potassium fluoride, 99.3kg of phenolphthalein polyaryletherketone homopolymer, 310kg of sulfolane and 1200kg of N, N-dimethylacetamide with the solid content of 6.2%. Note: the polymer solids content is the polymer mass/(polymer mass + solvent mass + diluent mass).
The polymer solution was passed through a plate filter 3 times and a fine filter (10 μm) 1 time to obtain 1595.2kg of the polymer solution.
The method comprises the steps of firstly, circularly preheating gas in a spray drying tower, enabling the temperature of a circulating gas flow inlet to be 240 ℃ and the temperature of a gas flow outlet to be 180 ℃, after the temperature is stable, pumping a polymer solution into the spray drying tower through a high-pressure infusion pump, enabling the pressure to be 0.102MPa, the temperature of the circulating gas flow inlet to be 240 ℃ and the temperature of the gas flow outlet to be reduced to 175 ℃, separating a solvent from the polymer after passing through a cyclone separator, and obtaining phenolphthalein polyaryletherketone homopolymer coarse powder, wherein the content of the solvent in the material outlet is 7.1%, the sample has an adhesion phenomenon, and.
As can be seen from a comparison of example 1 with comparative examples 1-2, the establishment of the recycle gas stream temperature system is critical to this scheme. The volatilization of the solvent in the polymer solution is obviously different from that of a pure solvent, the concentration is gradually increased along with the volatilization of the solvent, the volatilization of the solvent can be hindered after the polymer becomes a main component of a mixed system, and the solvent is not easy to volatilize even if the boiling point of the solvent is reached. Thus, the inlet temperature of the recycle gas stream is much higher than the boiling point of the diluent. Thus, as the solvent is volatilized, the temperature gradually decreases, a stable solution gradient is formed in the longitudinal space, and the solvent content is lower as the outlet is closer. When the temperature of the circulating airflow inlet is determined, along with the change of the liquid spraying amount and the content of the solvent of the material liquid, the temperature of the circulating airflow outlet and the stabilized temperature of the inlet and the outlet are gradually balanced. The solvent contents of the respective polymer meals were 27.2%, 11.9% and 7.1% when the inlet temperatures of the circulating gas streams were set at 170 deg.C, 200 deg.C and 240 deg.C, respectively. Whether the solvent is fused and adhered or the solvent is adhered, the separation of the solvent and the polymer is influenced, the value has great influence on the later drying mode and the drying difficulty and easiness, and the spray drying step needs to be completed by selecting proper temperature conditions.
Claims (10)
1. A method for post-treating a polyaryletherketone polymer, comprising:
filtering the polyaryletherketone polymer solution by a filter, and then drying by a spray drying tower, wherein the spray drying tower is used for circularly preheating gas in the tower, the temperature of a circulating airflow inlet is set to 180-plus-200 ℃, the temperature of an airflow outlet is set to 120-plus-135 ℃, after the temperature is stabilized, the polyaryletherketone polymer solution is pumped into the spray drying tower by a high-pressure infusion pump, the pressure is 0.102MPa, the temperature of the circulating airflow inlet is set to 180-plus-200 ℃, the temperature of the airflow outlet is reduced to 105-plus-132 ℃, and after passing through a cyclone separator, the solvent is separated from the polymer and dried to obtain the processed polyaryletherketone polymer.
2. The method of claim 1, wherein the filtration is specifically as follows: the polyaryletherketone polymer solution is firstly filtered by a plate filter for 2-3 times and then filtered by a fine filter for 1-2 times.
3. The method of claim 1, wherein the polyaryletherketone polymer solution is a polyaryletherketone polymer solution containing an organic solvent and an inorganic insoluble substance, and the inorganic insoluble substance and the organic solvent are immiscible;
or a soluble polyaryletherketone solution without inorganic salts.
4. The method as claimed in claim 3, wherein the organic solvent is selected from one or more of diphenyl sulfone, sulfolane, dimethyl sulfoxide, N-methylpyrrolidone, N-dimethylformamide, N-dimethylacetamide, 1, 3-dimethyl-2-imidazolidinone or N-cyclohexylpyrrolidone.
5. The method of claim 3, wherein the inorganic insoluble material is inorganic salt or inorganic additive.
6. The method of claim 5, wherein the inorganic salt is selected from potassium chloride, potassium fluoride, sodium chloride, sodium fluoride, calcium chloride, calcium fluoride, arsenic pentafluoride, potassium carbonate, sodium carbonate, calcium carbonate, and cerium carbonate.
7. The post-treatment method of polyaryletherketone polymer as claimed in claim 5, wherein said inorganic additive is alumina or ferroferric oxide.
8. The method of claim 1, wherein the polyaryletherketone polymer is a product of polycondensation of a bisphenol and a dihalogen monomer, or a terpolymer or multipolymer comprising structural units represented by formulas 101 and 102:
the mass ratio of the repeating unit represented by the formula 101 to the repeating unit represented by the formula 102 is 0.01-100: 1;
m, R is the residual group of bisphenol compounds after hydroxyl groups are removed;
x, Z is the residue of double-halogen compound containing benzene ring after removing two halogens, and X, Z of them have at least one ketone carbonyl structure;
when M is the same as X in structure, R is the same as Z in structure, namely the polyaryletherketone homopolymer is obtained;
when M and X are the same in structure, and R and Z are different in structure; or M and X are different in structure, and R and Z are the same in structure; namely the polyaryletherketone terpolymer;
when M, X has different structures and R and Z have different structures, it is a tetrapolymer (multipolymer).
9. The method of claim 8, wherein the polymer includes but is not limited to the repeating unit represented by formula 101,
the repeating unit represented by the formula 102 is
10. The method of claim 8, wherein the structural formula of the polyaryletherketone polymer is as follows:
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| CN113461932A (en) * | 2021-07-29 | 2021-10-01 | 浙江大学 | Preparation method of polyaryletherketone |
| CN113861409A (en) * | 2021-10-19 | 2021-12-31 | 中国科学院大连化学物理研究所 | Post-treatment method for industrial production of amorphous polyaryletherketone |
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