CN110408021B - High-strength hydrolysis-resistant high-fluidity polyarylate and preparation method thereof - Google Patents
High-strength hydrolysis-resistant high-fluidity polyarylate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to high-strength hydrolysis-resistant high-fluidity polyarylate and a preparation method thereof, belonging to the field of polymer synthesis. A high-strength hydrolysis-resistant high-fluidity polyarylate, wherein the starting material of the polyarylate consists of the following components: 1 to 290 parts of aromatic diphenol monomer, 455 parts of aromatic diacid chloride 203-. The polyarylate prepared by the invention has excellent heat resistance and hydrolysis resistance, light transmittance, mechanical strength and extremely excellent melt processing fluidity, can be used for preparing high-performance and functional workpieces by precision injection molding, and has wide application prospect.
Description
Technical Field
The invention relates to high-strength hydrolysis-resistant high-fluidity polyarylate and a preparation method thereof, belonging to the field of polymer synthesis.
Background
The polyester has better thermal property, mechanical property and processing property when being used as engineering plastics; the traditional polyester mainly comprises PET (glass transition temperature 69 ℃, melting point 255-; but the stability of the modified polycarbonate resin in high-temperature acid and alkali environments is sharply reduced due to the existence of a large number of ester groups in the molecular chain of the modified polycarbonate resin.
Disclosure of Invention
Aiming at the defects, the invention provides the high-strength hydrolysis-resistant high-fluidity polyarylate and the preparation method thereof, the obtained polyarylate has excellent heat resistance and hydrolysis resistance, light transmission, mechanical strength and extremely excellent melt processing fluidity, can be used for preparing high-performance and functional workpieces by precision injection molding, and has wide application prospect.
The technical scheme of the invention is as follows:
the first technical problem to be solved by the invention is to provide a high-strength hydrolysis-resistant high-fluidity polyarylate, wherein the initial raw material of the polyarylate comprises the following components:
wherein the aromatic diphenol monomer has the formula:
the aromatic dicarboxylic acid chloride has the structural formula:
the structural formula of the diamine monomer is as follows:
Further, the catalyst is any one of 15-crown-5, 18-crown-6, dioctyl sodium succinate, zinc citrate, sodium tartrate, sodium gluconate, sodium nitrilotriacetate, sodium sorbate, sodium ethylene diamine tetracetate, sodium glycocholate, sodium terephthalate, sodium stearate, tetrabutyl ammonium bromide, benzyl triethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium chloride, sodium dodecyl benzene sulfonate, sodium p-methyl benzene sulfonate, sodium alginate or sodium dodecyl sulfonate.
Further, the base is any one of lithium hydroxide, sodium hydroxide, calcium hydroxide, potassium hydroxide, barium hydroxide, aluminum hydroxide, lithium carbonate, sodium carbonate, potassium carbonate, barium carbonate, lithium bicarbonate, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, barium bicarbonate, ammonia water, trimethylamine, triethylamine, tri-tert-butylamine, pyridine, or piperazine.
Further, the organic solvent is any one of 1, 2-dichloroethane, 1,2, 2-tetrachloroethane, dichloromethane, chloroform, carbon tetrachloride, cyclohexane, cyclohexanone, chlorobenzene, m-dichlorobenzene, or 1,2, 4-trichlorobenzene.
The second technical problem to be solved by the present invention is to provide a method for preparing the high-strength hydrolysis-resistant high-fluidity polyarylate, comprising the steps of:
(1) preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product
Sequentially adding 1-290 parts of aromatic diphenol monomer, 0.1-20 parts of catalyst and 20-200 parts of alkali into a reaction kettle filled with 150-1000 parts of water, and stirring and dissolving at-10-20 ℃; dissolving 203-455 parts of aromatic diformyl chloride into a dissolving kettle filled with 300-2000 parts of organic solvent, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of-5-25 ℃, and obtaining a polyarylester prepolymer with a certain molecular weight and containing active acyl chloride end groups (keeping excessive aromatic diformyl chloride) when the aromatic diformyl chloride solution is added into the reaction kettle in an amount of 1/3-2/3; then dissolving 5-100 parts of diamine monomer into 10-200 parts of water, simultaneously dropwise adding a diamine water solution and an incomplete aromatic diformyl chloride solution into the reaction kettle, and continuously stirring and reacting at the temperature of-5-25 ℃ for 1-12 hours to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the mixed solution of the crude polyarylate product, then separating an aqueous solution layer, adding 2000 parts of desalted water of 150 portions into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and circulating the steps for at least 3 times (preferably 3-6 times) to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 0-2000 parts of organic solvent into the preliminarily purified polymer solution for dilution, adding 0.1-50 parts of antioxidant, uniformly stirring, conveying the homogenized solution to an atomization granulation tower through a metering pump for solidification and granulation, and obtaining a solid material, namely the high-strength hydrolysis-resistant high-fluidity polyarylate; wherein the temperature of the atomizing granulation tower is controlled to be 20-160 ℃, and the vacuum degree is controlled to be-0.05 to-0.09 MPa.
Further, in the method, the solid material obtained in the step (3) is conveyed to a finished product workshop for standby through a pipeline, and the solvent steam is collected to a solvent recovery tank after being condensed for recycling.
Further, the antioxidant used in the curing and granulating preparation process of the high-strength hydrolysis-resistant high-fluidity polyarylate is any one of phosphorous acid S-9228, antioxidant 1076, antioxidant MB, aluminum dihydrogen phosphate, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, 2, 5-di-tert-butylhydroquinone, 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid or 1,3,5, tris (3, 5-di-tert-butyl-4-hydroxybenzyl) S-triazine-2, 4, 6- (1H, 3H, 5H) trione.
The third technical problem to be solved by the invention is to provide a method for improving the strength and hydrolysis resistance of polyarylate, which comprises the following steps: aromatic diphenol and aromatic diformyl chloride are used as basic monomers, and diamine monomer is introduced, so that the semi-aromatic polyamide molecular chain is introduced into the polyester resin structure; wherein the diamine monomer has a structural formula:
In the invention, the raw materials are in parts by weight except for special specifications.
The invention has the following advantages:
1. the polyester resin adopted in the invention has simple polymerization process flow, mild condition and easy control; in the whole reaction process, except the byproduct salt, no other harmful substances are generated, so that the method is environment-friendly;
2. the copolycondensation is carried out with diamine by adopting a step method, the function is clear, the flow is short, and the defect that the molecular weight of the product is not high due to premature precipitation of a polymer from a solution is avoided;
3. the introduction of the amide structure can not only improve the thermal property of the polyester, but also increase the content of hydrogen bonds in a polymer molecular chain and greatly improve the mechanical property of the resin due to the introduction of the amide structure; meanwhile, due to the introduction of an aliphatic chain structural element in the diamine monomer, the melt flowability of the aromatic polyester can be improved simultaneously, so that the processing performance of the aromatic polyester is greatly improved;
4. the standing chromatography water washing method adopted in the invention can wash and remove the soluble by-product generated in the polymerization process at one time, and by controlling the type and the dosage of the catalyst, a demulsifier is not required to be additionally used, so that the whole process flow is short, the required equipment is few, and the energy consumption in the product washing process is greatly reduced;
5. the atomization and solidification granulation process adopted in the invention can completely separate the solvent from the polymer resin at one time, the obtained resin has high purity, high solvent recovery rate and recovery efficiency, the equipment investment is saved, the fixed asset investment is greatly reduced, the production cost is reduced, and the product market competitiveness is improved;
6. the polymer can be used for special engineering plastics and high-performance polymer composite materials, and can be used for preparing heat-resistant and high-light-transmittance parts and products, is particularly suitable for preparing special thin-wall parts, and has wide application prospect.
Drawings
FIG. 1 is a graph showing the shear complex viscosities at different temperatures of the polyester resins obtained in examples 1 to 4.
Detailed Description
According to the invention, a semi-aromatic polyamide molecular chain is introduced into a polyester resin structure through a two-step method in a polyester molecular chain, so that the hydrolysis resistance of the polyester is improved, and meanwhile, the mechanical strength of the polyester is further improved and the good processing fluidity of the polyester is maintained by increasing the hydrogen bond content in the molecular chain, so that the high-strength hydrolysis-resistant high-fluidity polyarylate with excellent comprehensive performance is finally obtained.
The present invention is described in detail below by way of examples, it should be noted that the examples are only for the purpose of further illustration, and are not to be construed as limiting the scope of the present invention, and that those skilled in the art can make insubstantial modifications and adaptations of the present invention based on the teachings of the present invention described above.
Example 1
(1) Preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product (A-90% -116 diamine-10% -T-40% -I-60%)
Adding 205.2kg of bisphenol A, 15-crown-50.1 kg of bisphenol A and 85kg of sodium hydroxide into a reaction kettle filled with 1000kg of water in sequence, and stirring and dissolving at-10 ℃; dissolving 81.2kg of phthaloyl chloride and 121.8kg of isophthaloyl chloride in a dissolving kettle filled with 1800kg of dichloromethane, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring at the temperature of 5 ℃ for reaction, and obtaining a polyarylate prepolymer containing active acyl chloride end groups (keeping excessive aromatic diformyl chloride) with a certain molecular weight when the amount of the diformyl chloride solution is added to 2/3; then dripping 30kg of dissolved 1, 6-hexamethylene diamine aqueous solution (containing 11.6kg of 1, 6-hexamethylene diamine monomer) and the incomplete aromatic diformyl chloride solution into the reaction kettle simultaneously, and continuously stirring and reacting for 12h at the temperature of 15 ℃ to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the polymer mixed solution, then separating an aqueous solution layer, adding 800 parts of desalted water into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and repeating the steps for 5 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 2000kg of dichloromethane into the preliminarily purified polymer solution for dilution, adding 0.1kg of antioxidant 1076, uniformly stirring, conveying the homogenized solution to an atomization tower and a granulation tower by a metering pump for solidification and granulation, and obtaining a solid material, namely the high-strength hydrolysis-resistant high-fluidity polyarylate; wherein, the temperature of the atomizing granulation tower is controlled to be 60 ℃, and the vacuum degree is controlled to be-0.05 Mpa; the dried and purified resin is prepared into standard mechanical properties and rheological sample bars, and the thermal and mechanical properties (shown in table 1) and the rheological properties (shown in fig. 1) of the resin are respectively detected.
Example 2
(1) Preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product (A-80% -114% diamine-20% -T-20% -I-80%)
182.4kg of bisphenol A, 1kg of sodium glycocholate and 80.5kg of sodium hydroxide are sequentially added into a reaction kettle filled with 400kg of water and stirred and dissolved at 10 ℃; dissolving 40.6kg of phthaloyl chloride and 162.4kg of isophthaloyl chloride in a dissolving kettle filled with 1100kg of m-dichlorobenzene, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of-5 ℃, and obtaining a polyarylester prepolymer containing active acyl chloride end groups (keeping excessive aromatic diformyl chloride) with a certain molecular weight when adding 1/2 parts of diformyl chloride solution; then dripping 50kg of dissolved 1, 4-cyclohexanediamine aqueous solution (containing 11.4kg of 1, 4-cyclohexanediamine monomer) and the incomplete aromatic diformyl chloride solution into the reaction kettle simultaneously, and continuously stirring and reacting for 8 hours at the temperature of 10 ℃ to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the polymer mixed solution, then removing an aqueous solution layer, adding 600 parts of desalted water into the reaction kettle, stirring, washing, standing and layering, removing the aqueous solution layer, and repeating the steps for 6 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 1000kg of m-dichlorobenzene into the preliminarily purified polymer solution for dilution, adding 0.5kg of antioxidant 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid, uniformly stirring, conveying the homogenized solution to an atomization and granulation tower by a metering pump for solidification and granulation, and obtaining a solid material, namely the high-strength hydrolysis-resistant high-fluidity polyarylate; wherein the temperature of the atomizing granulation tower is controlled to be 120 ℃, and the vacuum degree is controlled to be-0.08 Mpa; the dried and purified resin is prepared into standard mechanical properties and rheological sample bars, and the thermal and mechanical properties (shown in table 1) and the rheological properties (shown in fig. 1) of the resin are respectively detected.
Example 3
(1) Preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product (F-80% -170 diamine-20% -T-15% -I-85%)
160kg of bisphenol A, 5kg of zinc citrate and 106.5kg of sodium carbonate are sequentially added into a reaction kettle filled with 450kg of water and stirred and dissolved at 15 ℃; dissolving 30.45kg of terephthaloyl chloride and 172.55kg of isophthaloyl chloride into a dissolving kettle filled with 900kg of 1, 2-dichloroethane, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of minus 5 ℃, and obtaining a polyarylester prepolymer containing active acyl chloride end groups (keeping excessive aromatic diformyl chloride) with a certain molecular weight when the amount of the diformyl chloride solution is added into 1/3; then dripping 100kg of dissolved isophorone diamine aqueous solution (containing 34kg of isophorone diamine monomer) and the incomplete aromatic diformyl chloride solution into the reaction kettle simultaneously, and continuously stirring and reacting for 6h at the temperature of 10 ℃ to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the polymer mixed solution, then separating an aqueous solution layer, adding 560 parts of desalted water into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and repeating the steps for 4 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 1000kg of 1, 2-dichloroethane into the preliminarily purified polymer solution for dilution, adding 2kg of antioxidant sodium pyrophosphate, uniformly stirring, conveying the homogenized solution to an atomization tower and a granulation tower by a metering pump for solidification and granulation, and obtaining a solid material, namely the high-strength hydrolysis-resistant high-fluidity polyarylate; wherein, the temperature of the atomizing granulation tower is controlled to be 80 ℃, and the vacuum degree is controlled to be-0.07 Mpa; the dried and purified resin is prepared into standard mechanical properties and rheological sample bars, and the thermal and mechanical properties (shown in table 1) and the rheological properties (shown in fig. 1) of the resin are respectively detected.
Example 4
(1) Preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product (A-70% -biphenol-20% -198 diamine-10% -T-15% -I-85%)
159.6kg of bisphenol A, 6kg of benzyltriethylammonium bromide and 138kg of sodium potassium carbonate are sequentially added into a reaction kettle filled with 750kg of water and stirred and dissolved at 10 ℃; dissolving 30.45kg of terephthaloyl chloride and 172.55kg of isophthaloyl chloride in a dissolving kettle filled with 1400kg of dichloromethane, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring at the temperature of 5 ℃ for reaction, and obtaining a polyarylester prepolymer with a certain molecular weight and containing active acyl chloride end groups (keeping excessive aromatic diformyl chloride) when the diformyl chloride solution is added into the reaction kettle by 2/3; then dripping 90kg of dissolved 4,4 '-diaminodiphenylmethane aqueous solution (containing 19.8kg of 4, 4' -diaminodiphenylmethane monomer) and the incomplete aromatic diformyl chloride solution into the reaction kettle simultaneously, and continuously stirring and reacting for 5 hours at the temperature of 10 ℃ to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the polymer mixed solution, then separating an aqueous solution layer, adding 1500 parts of desalted water into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and repeating the steps for 3 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 1200kg of dichloromethane into the preliminarily purified polymer solution for dilution, adding 10kg of antioxidant MB, uniformly stirring, conveying the homogenized solution to an atomization tower and a granulation tower by a metering pump for solidification and granulation, and obtaining a solid material, namely the high-strength hydrolysis-resistant high-fluidity polyarylate; wherein, the temperature of the atomizing granulation tower is controlled to be 60 ℃, and the vacuum degree is controlled to be-0.05 Mpa; the dried and purified resin is prepared into standard mechanical properties and rheological sample bars, and the thermal and mechanical properties (shown in table 1) and the rheological properties (shown in fig. 1) of the resin are respectively detected.
Comparative example 1
Polyarylate was prepared by the same method as in the steps (1) to (3) of example 1 except that 30kg of an aqueous solution of the diamine monomer 1, 6-hexamethylenediamine (containing 11.6kg of the 1, 6-hexamethylenediamine monomer) was once dissolved in water with diphenol in the step (1), then dropwise addition of diformyl chloride was started, a white powdery polymer was rapidly precipitated from the solvent with addition of diformyl chloride, the system was hardly stirred and uniformly dispersed, and the intrinsic viscosity of the finally obtained resin was 0.29g/dL (the solvent was sulfuric acid). After the obtained resin is melted, the resin cannot be made into a film or a sheet with strength, the pressed film can be broken into small pieces in the demoulding process, a sample is dark yellow brown after being detected by capillary rheology, and the phenomenon of oxidative degradation is serious.
TABLE 1 thermal and mechanical Properties of polyarylates obtained in examples 1 to 4
In Table 1, Tg: glass transition temperature, T5％: weight loss temperature of 5%.
Claims (8)
1. A high-strength hydrolysis-resistant high-fluidity polyarylate, wherein the starting materials of the polyarylate consist of the following components:
wherein the aromatic diphenol monomer has the formula:
the aromatic dicarboxylic acid chloride has the structural formula:
the structural formula of the diamine monomer is as follows:
and, the polyarylate is prepared by the following preparation method:
(1) preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product
Sequentially adding 1-290 parts of aromatic diphenol monomer, 0.1-20 parts of catalyst and 20-200 parts of alkali into a reaction kettle filled with 150-1000 parts of water, and stirring and dissolving at-10-20 ℃; dissolving 203-455 parts of aromatic diformyl chloride into a dissolving kettle filled with 300-2000 parts of organic solvent, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of-5-25 ℃, and obtaining a polyarylester prepolymer containing active acyl chloride end groups and having a certain molecular weight when the aromatic diformyl chloride solution is added in an amount of 1/3-2/3; then dissolving 5-100 parts of diamine monomer into 10-200 parts of water, simultaneously dropwise adding a diamine water solution and an incomplete aromatic diformyl chloride solution into the reaction kettle, and continuously stirring and reacting at the temperature of-5-25 ℃ for 1-12 hours to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the mixed solution of the crude polyarylate product, then separating an aqueous solution layer, adding 2000 parts of desalted water of 150 portions into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and circulating the steps for at least 3 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 0-2000 parts of organic solvent into the polymer solution after primary purification for dilution, adding 0.1-50 parts of antioxidant, and uniformly stirring; the homogenized solution is sent to an atomization granulation tower through a metering pump for solidification and granulation, and the obtained solid material is high-strength hydrolysis-resistant high-fluidity polyarylate; wherein the temperature of the atomizing granulation tower is controlled to be 20-160 ℃, and the vacuum degree is controlled to be-0.05 to-0.09 MPa.
2. The high strength, hydrolysis resistant, high flow polyarylate of claim 1 wherein the catalyst is any of 15-crown-5, 18-crown-6, dioctyl sodium succinate, zinc citrate, sodium tartrate, sodium gluconate, sodium nitrilotriacetate, sodium sorbate, sodium ethylenediaminetetraacetic acid, sodium ethylenediamineteromethylidene phosphate, sodium glycocholate, sodium terephthalate, sodium stearate, tetrabutylammonium bromide, benzyltriethylammonium chloride, hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, sodium dodecylbenzenesulfonate, sodium p-toluenesulfonate, sodium alginate or sodium dodecylsulfonate.
3. The high-strength hydrolysis-resistant high-flow polyarylate according to claim 1 or 2, wherein the base is any one of lithium hydroxide, sodium hydroxide, calcium hydroxide, potassium hydroxide, barium hydroxide, aluminum hydroxide, lithium carbonate, sodium carbonate, potassium carbonate, barium carbonate, lithium bicarbonate, sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, barium bicarbonate, ammonia, trimethylamine, triethylamine, tri-t-butylamine, pyridine, or piperazine.
4. The high strength, hydrolysis resistant and high flow polyarylate as claimed in claim 1 or 2, wherein the organic solvent is any one of 1, 2-dichloroethane, 1,2, 2-tetrachloroethane, dichloromethane, chloroform, carbon tetrachloride, cyclohexane, cyclohexanone, chlorobenzene, m-dichlorobenzene or 1,2, 4-trichlorobenzene.
5. The preparation method of the high-strength hydrolysis-resistant high-fluidity polyarylate as described in any one of claims 1 to 4, wherein the preparation method comprises the steps of:
(1) preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product
Sequentially adding 1-290 parts of aromatic diphenol monomer, 0.1-20 parts of catalyst and 20-200 parts of alkali into a reaction kettle filled with 150-1000 parts of water, and stirring and dissolving at-10-20 ℃; dissolving 203-455 parts of aromatic diformyl chloride into a dissolving kettle filled with 300-2000 parts of organic solvent, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of-5-25 ℃, and obtaining a polyarylester prepolymer containing active acyl chloride end groups and having a certain molecular weight when the aromatic diformyl chloride solution is added in an amount of 1/3-2/3; then dissolving 5-100 parts of diamine monomer into 10-200 parts of water, simultaneously dropwise adding a diamine water solution and an incomplete aromatic diformyl chloride solution into the reaction kettle, and continuously stirring and reacting at the temperature of-5-25 ℃ for 1-12 hours to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the mixed solution of the crude polyarylate product, then separating an aqueous solution layer, adding 2000 parts of desalted water of 150 portions into the reaction kettle, stirring, washing, standing and layering, separating the aqueous solution layer, and circulating the steps for at least 3 times to obtain a preliminarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 0-2000 parts of organic solvent into the polymer solution after primary purification for dilution, adding 0.1-50 parts of antioxidant, and uniformly stirring; the homogenized solution is sent to an atomization granulation tower through a metering pump for solidification and granulation, and the obtained solid material is high-strength hydrolysis-resistant high-fluidity polyarylate; wherein the temperature of the atomizing granulation tower is controlled to be 20-160 ℃, and the vacuum degree is controlled to be-0.05 to-0.09 MPa.
6. The method for preparing polyarylate with high strength, hydrolysis resistance and high fluidity as claimed in claim 5, wherein the solid material obtained in the step (3) is transported to a finished product workshop for standby by a pipeline, and the solvent vapor is collected to a solvent recovery tank after being condensed for recycling.
7. The method for preparing a high-strength, hydrolysis-resistant and high-fluidity polyarylate as described in claim 5, wherein in the step (3), the antioxidant is any one of phosphite S-9228, antioxidant 1076, antioxidant MB, aluminum dihydrogen phosphate, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, 2, 5-di-tert-butylhydroquinone, 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid or 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) S-triazine-2, 4, 6- (1H, 3H, 5H) trione.
8. A method of increasing polyarylate strength and hydrolysis resistance, said method comprising: aromatic diphenol and aromatic diformyl chloride are used as basic monomers, and diamine monomer is introduced, so that the semi-aromatic polyamide molecular chain is introduced into the polyester resin structure; wherein the aromatic diphenol monomer has the formula:
the aromatic dicarboxylic acid chloride has the structural formula:
the structural formula of the diamine monomer is as follows:
(1) preparation of high-strength hydrolysis-resistant high-fluidity polyarylate crude product
Sequentially adding 1-290 parts of aromatic diphenol monomer, 0.1-20 parts of catalyst and 20-200 parts of alkali into a reaction kettle filled with 150-1000 parts of water, and stirring and dissolving at-10-20 ℃; dissolving 203-455 parts of aromatic diformyl chloride into a dissolving kettle filled with 300-2000 parts of organic solvent, dropwise adding an acyl chloride solution in the dissolving kettle into the reaction kettle, stirring and reacting at the temperature of-5-25 ℃, and obtaining a polyarylester prepolymer containing active acyl chloride end groups and having a certain molecular weight when the aromatic diformyl chloride solution is added in an amount of 1/3-2/3; then dissolving 5-100 parts of diamine monomer into 10-200 parts of water, simultaneously dropwise adding a diamine water solution and an incomplete aromatic diformyl chloride solution into the reaction kettle, and continuously stirring and reacting at the temperature of-5-25 ℃ for 1-12 hours to obtain a high-strength hydrolysis-resistant high-fluidity polyarylate crude product;
(2) purification of high-strength hydrolysis-resistant high-fluidity crude polyarylate
Standing and layering the mixed solution of the crude polyarylate product, removing an aqueous solution layer, adding 150-2000 parts of desalted water into the reaction kettle, stirring, washing, standing and layering, removing the aqueous solution layer, and circulating for at least 3 times to obtain a primarily purified polymer solution;
(3) solidifying and granulating process of high-strength hydrolysis-resistant high-flowability polyarylate
Adding 0-2000 parts of organic solvent into the polymer solution after primary purification for dilution, adding 0.1-50 parts of antioxidant, and uniformly stirring; the homogenized solution is sent to an atomization granulation tower through a metering pump for solidification and granulation, and the obtained solid material is high-strength hydrolysis-resistant high-fluidity polyarylate; wherein the temperature of the atomizing granulation tower is controlled to be 20-160 ℃, and the vacuum degree is-0.05 to-0.09 MPa.
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| CN102875802A (en) * | 2012-10-11 | 2013-01-16 | 南昌博生复合材料有限公司 | High-impact and heat-resistant copolymer and preparation method thereof |
| CN109503831A (en) * | 2018-11-29 | 2019-03-22 | 中仑塑业（福建）有限公司 | A kind of polyarylate copolymerization transparent nylon and preparation method thereof |
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| JP3519508B2 (en) * | 1995-07-13 | 2004-04-19 | ユニチカ株式会社 | Polyesteramide and electrophotographic photoreceptor using the same |
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| CN102875802A (en) * | 2012-10-11 | 2013-01-16 | 南昌博生复合材料有限公司 | High-impact and heat-resistant copolymer and preparation method thereof |
| CN109503831A (en) * | 2018-11-29 | 2019-03-22 | 中仑塑业（福建）有限公司 | A kind of polyarylate copolymerization transparent nylon and preparation method thereof |
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