CN108503823B - Polyamide resin and preparation method thereof - Google Patents
Polyamide resin and preparation method thereof Download PDFInfo
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- CN108503823B CN108503823B CN201710102830.9A CN201710102830A CN108503823B CN 108503823 B CN108503823 B CN 108503823B CN 201710102830 A CN201710102830 A CN 201710102830A CN 108503823 B CN108503823 B CN 108503823B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
Abstract
The invention discloses a polyamide 5X melt and polyamide 5X resin prepared from the same. The water content of the polyamide 5X melt was 200-18000 ppm. A polyamide 5X resin obtained by pelletizing a polyamide 5X melt. According to the polyamide 5X resin disclosed by the invention, the problems of filament breakage and influence on the granulating effect and resin quality in the granulating process are greatly improved by adjusting the water content, so that the granulating effect is greatly improved, and the obtained polyamide 5X resin is full in particles and excellent in quality.
Description
Technical Field
The invention relates to a polyamide resin and a preparation method thereof.
Background
The polyamide is a polymer with an amido repeating unit on a high molecular chain, has excellent comprehensive properties such as mechanical property, forming processability, wear resistance, chemical resistance and the like, is mainly applied to fibers and engineering plastics, and can be used for preparing films in a small amount. In the last 30 th century, DuPont first achieved industrial production of polyamides and applied to the fiber field. In the 80 s of the 20 th century, with the rapid development of the automobile industry and the electronic and electrical industry, the polyamide resin becomes the engineering plastic with the largest consumption and the widest application field. Currently widely used polyamide resins are polyamide 6(PA6) and polyamide 66(PA 66).
Polyamide 5X is a novel polyamide which is polymerized from 1, 5-pentanediamine and a dibasic acid. The prior art polyamide 5X resin can be prepared by the following process: concentration → high pressure pre-polycondensation → flash evaporation → normal pressure or vacuum polycondensation → granulation and molding to obtain the resin. On the basis, in order to further increase the polymerization effect and prepare a polyamide 5X product with high viscosity, high strength and high toughness, a catalyst is often added in the polymerization process. The addition of the catalyst further improves the reaction speed, and the mechanical property of the prepared product is also improved to a certain extent. But after the catalyst is added, the phenomena of end breakage and fine wires of the polyamide 5X resin are serious in the granulating process, the granulating effect is poor, the resin particles are different in size, and the overall quality needs to be improved.
Disclosure of Invention
The invention provides a preparation method of polyamide 5X resin and the prepared polyamide 5X resin, aiming at solving the defects that the phenomena of end breakage and filament occur in the pelletizing process of the polyamide 5X resin, and the yield of finished products and the quality of the resin are affected.
The inventors found in the study of the production process of polyamide 5X resin that: although the addition of the catalyst is beneficial to the polymerization process, the catalyst has a certain negative effect on the pelletizing effect, and in order to solve the problem and reduce the phenomenon of pelletizing and filament breakage to obtain polyamide 5X chips with excellent quality, the inventor carries out intensive research, and finally finds that the negative effect of the catalyst on pelletizing can be favorably improved and the pelletizing effect can be improved by adjusting certain specific parameters in the melt preparation process, so that the resin with uniform particles and excellent quality is obtained, and the technical scheme of the invention is obtained.
One object of the present invention is: a polyamide 5X melt having a water content of 200-. The water content is in parts per million by mass of the polyamide 5X melt.
Another object of the invention is: a polyamide 5X resin is obtained by granulating a polyamide 5X melt, wherein the water content of the polyamide 5X melt is 200-18000 ppm. The water content is in parts per million by mass of the polyamide 5X resin.
The following further explains the preferred embodiments of the present invention:
in a preferred embodiment of the present invention, the polyamide 5X comprises a polyamide polymerized from monomers of 1, 5-pentanediamine and dicarboxylic acid. Wherein the dicarboxylic acid can be short-chain dicarboxylic acid (the number of carbon atoms on a carbon chain is less than 10) or long-chain dicarboxylic acid; wherein the short-chain dibasic acid preferably comprises one or more of succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid and sebacic acid, preferably adipic acid and/or sebacic acid; the long carbon chain dibasic acid preferably comprises one or more of undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid and Δ 9-1, 18-octadecenedioic acid.
In a preferred embodiment of the present invention, the polyamide 5X resin is obtained by polymerizing 1, 5-pentanediamine and dicarboxylic acid as monomers by adding a catalyst for polyamide polymerization, which is conventional in the art. The catalyst is preferably a phosphorus-containing catalyst, which preferably comprises one or more of phosphoric acid, phosphorous acid, hypophosphorous acid and their corresponding salts or esters, more preferably hypophosphorous acid and its salts or esters, and most preferably sodium hypophosphite. The amount of the catalyst added is preferably 5 to 2000ppm, more preferably 10 to 1000ppm, in parts per million by mass based on the polyamide 5X resin.
In a preferred embodiment of the present invention, the polyamide 5X melt preferably has a water content of 400-9000 ppm.
Years of studies by the inventors on the polymerization of polyamide 5X show that: the polymerization reaction is a dynamic equilibrium process of polymerization and depolymerization, and the addition of the catalyst further promotes the dynamic equilibrium, so that the reaction is intensified, and more end group side reactions are generated to form CO2The formation of small molecular by-products such as ammonia, cyclopentanone, piperidine and the like causes a large amount of bubbles in the polyamide 5X melt, and directly causes the generation of broken filaments. Based on this, the inventor improves the situation by controlling the water content in the melt polymerization process, and finally obtains the technical scheme of the invention.
Another object of the invention is: a polyamide 5X resin is provided, the polyamide 5X resin having a water content of 180-8000 ppm.
In a preferred embodiment of the present invention, the polyamide 5X resin preferably has a water content of 380-6500 ppm.
In a preferred embodiment of the present invention, the polyamide 5X resin has a terminal amino group content of 20 to 70mol/ton, preferably 30 to 60 mol/ton.
In a preferred embodiment of the present invention, the polyamide 5X resin has a carboxyl end group content of 50mol/ton or more, preferably 60 to 120 mol/ton.
Another object of the invention is: a method for preparing a polyamide 5X melt is provided, the method comprising the steps of:
(1) under the condition of nitrogen, 1, 5-pentanediamine, aliphatic dibasic acid, a catalyst and water are uniformly mixed to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the aliphatic dibasic acid is (1-1.05): 1;
(2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure to make the temperature of the reaction system at 232-265 ℃ after the pressure maintaining is finished, reducing the pressure to make the pressure in the reaction system to 0-0.2Mpa, wherein the pressure is gauge pressure, and finally vacuumizing to obtain the polyamide melt.
According to a preferable technical scheme of the invention, the vacuumizing time is 10-45min, and preferably 20-30 min.
According to a preferable technical scheme of the invention, the vacuum degree after vacuumizing is-0.095-0 Mpa (gauge pressure), and preferably-0.06-0.01 Mpa (gauge pressure).
According to a preferable technical scheme of the invention, the temperature after the vacuum pumping is 230-290 ℃.
According to a preferable technical scheme of the invention, the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
The concentration of the salt solution of the polyamide is 30-90%, and the percentage is the mass percentage of the salt solution of the polyamide.
In a preferred embodiment of the present invention, the salt solution of polyamide has a pH value of 6 or more, preferably 7.2 to 8.9, more preferably 7.5 to 8.2 at a concentration of 10%, wherein the percentage is based on the mass of the salt solution of polyamide.
Another object of the invention is: provided is a preparation method of a polyamide 5X resin, the preparation method comprising the steps of: and pelletizing the polyamide 5X melt to obtain the resin.
After the pelletization, drying is preferably carried out under conditions conventional in the art.
According to the polyamide 5X resin disclosed by the invention, the problems of filament breakage and influence on the granulating effect and resin quality in the granulating process are greatly improved by adjusting the water content, so that the granulating effect is greatly improved, and the obtained polyamide 5X resin is full in particles and excellent in quality.
Detailed Description
The present invention will be described in detail below with reference to examples to make the features and advantages of the present invention more apparent. It should be noted that the examples are for understanding the concept of the present invention and the scope of the present invention is not limited to only the examples listed herein.
In the invention, the detection method of each parameter is as follows:
1. the melt water content detection method comprises the following steps: and discharging the melt into a closed container, cooling, accurately weighing about 1g of sample, and measuring by using a Karl Fischer moisture tester at the detection temperature of 200 ℃ for 20 min.
2. Amino-and carboxyl-terminal groups: after the sample is dissolved by using trifluoroethanol, titrating by using hydrochloric acid standard solution and sodium hydroxide standard solution respectively, and calculating.
3. The method for detecting the water content of the resin comprises the following steps: taking 1g of resin sample, and measuring by using a Karl Fischer moisture tester, wherein the detection temperature is 200 ℃, and the detection time is 20 min.
Example 1
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, a catalyst (10ppm of sodium phosphate, wherein the mass percent of the sodium phosphate accounts for the mass percent of the polyamide 56 resin) and water are uniformly mixed to prepare 80 percent of salt solution of polyamide, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 8.2 when the concentration of the salt solution of the polyamide is 10 percent, wherein the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.7Mpa, exhausting, maintaining the pressure, keeping the temperature of the reaction system at 245 ℃ after the pressure maintaining is finished, then reducing the pressure in the reaction system to 0Mpa (gauge pressure), keeping the temperature of the reaction system at 268 ℃ after the pressure reducing is finished, and keeping the temperature and the pressure for 40min to obtain a polyamide melt;
the water content of the polyamide 56 melt was 9000ppm (in parts per million of the polyamide melt);
(3) cutting into granules, and drying to obtain resin;
the polyamide 56 resin obtained had a water content of 2650ppm (in parts per million of the polyamide resin).
Example 2
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, a catalyst (1000ppm of sodium phosphite, wherein the mass percent of sodium phosphite accounts for 56 mass percent of polyamide resin) and water are uniformly mixed to prepare a 60% polyamide salt solution, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 7.3 when the concentration of the salt solution of the polyamide is 10 percent, wherein the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.2Mpa, exhausting, maintaining the pressure, reducing the pressure to 0.05Mpa (gauge pressure) when the pressure maintaining is finished, maintaining the temperature of the reaction system at 265 ℃, vacuumizing to-0.06 Mpa, vacuumizing for 12min, and maintaining the temperature at 278 ℃ after vacuumizing to obtain a polyamide melt;
the water content of the polyamide 56 melt was 3500ppm (parts per million of the polyamide melt);
(3) cutting into granules, and drying to obtain resin;
the polyamide 56 resin obtained had a water content of 2500ppm (in parts per million of the polyamide resin).
Example 3
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, a catalyst (100ppm of sodium hypophosphite, wherein the mass percent of the sodium hypophosphite accounts for 5X resin of polyamide) and water are uniformly mixed to prepare a 75% polyamide salt solution, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 7.8 when the concentration of the salt solution of the polyamide is 10 percent, wherein the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.6Mpa, exhausting, maintaining the pressure, reducing the pressure to 0.01Mpa (gauge pressure) when the pressure maintaining is finished, reducing the temperature of the reaction system to 262 ℃, vacuumizing to-0.04 Mpa, vacuumizing for 25min, and maintaining the temperature after vacuumizing to 278 ℃ to obtain a polyamide melt;
the water content of the polyamide 56 melt was 5200ppm (parts per million based on the polyamide melt);
(3) cutting into granules, and drying to obtain resin;
the polyamide 56 resin obtained contained 1800ppm (in parts per million) of water based on the polyamide resin.
Example 4
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid and water are uniformly mixed to prepare a 60% polyamide salt solution, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 8.1 when the concentration of the salt solution of the polyamide is 10 percent, wherein the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.1MPa, exhausting, maintaining the pressure, reducing the pressure to 0.1MPa (gauge pressure) when the pressure maintaining is finished, wherein the temperature of the reaction system is 245 ℃, reducing the pressure to 262 ℃, vacuumizing to-0.095 MPa, vacuumizing for 32min, and vacuumizing to 278 ℃ to obtain a polyamide melt;
the water content of the polyamide 56 melt was 400ppm (in parts per million of the polyamide melt);
(3) cutting into granules, and drying to obtain resin;
the polyamide 56 resin obtained had a water content of 1200ppm (in parts per million of the polyamide resin).
Comparative example 1
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, a catalyst (2200ppm of sodium phosphite accounts for the mass percent of polyamide 5X resin) and water are uniformly mixed to prepare a 60% polyamide salt solution, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 8.38 when the concentration of the salt solution of the polyamide is 10 percent, and the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.8Mpa, exhausting, maintaining the pressure, reducing the pressure to 0.01Mpa (gauge pressure) when the pressure maintaining is finished and keeping the temperature of the reaction system at 275 ℃ after the pressure reducing is finished, and keeping the temperature and the pressure for 10min to obtain a polyamide melt;
the water content of the polyamide 56 melt is 20000ppm (parts per million of the polyamide melt);
(3) and (4) granulating and drying to obtain the resin.
Comparative example 2
(1) Under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, a catalyst (100ppm of sodium phosphite accounts for the mass parts per million of polyamide 5X resin) and water are uniformly mixed to prepare a 60% polyamide salt solution, wherein the weight of the salt is 20 kg; the molar ratio of 1, 5-pentanediamine to adipic acid is (1-1.05): 1, the pH value of the salt solution of the polyamide is 8.38 when the concentration of the salt solution of the polyamide is 10 percent, and the percentage is the mass percentage of the salt solution of the polyamide;
(2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 1.8Mpa, exhausting, maintaining the pressure, reducing the pressure to 0.01Mpa (gauge pressure) when the pressure maintaining is finished and keeping the temperature of the reaction system at 275 ℃ after the pressure reducing is finished, and keeping the temperature and the pressure for 10min to obtain a polyamide melt;
the water content of the polyamide 56 melt was 19500ppm (parts per million based on the polyamide melt);
(3) and (4) granulating and drying to obtain the resin.
The numbers of breakages and filaments obtained for the polyamide 5X resin chips obtained in examples 1 to 4 and comparative examples 1 to 2 are shown in the following table:
| granulation effect | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Broken end | 7 | 8 | 2 | 3 | 29 | 25 |
| Filament | 5 | 3 | 3 | 3 | 35 | 30 |
| Total of | 12 | 11 | 5 | 6 | 64 | 55 |
The above embodiments are merely illustrative of the technical solutions and do not constitute limitations of the present invention.
Unless otherwise defined, all terms used herein have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of the present invention, and those skilled in the art may make various other substitutions, alterations, and modifications within the scope of the present invention, and thus, the present invention is not limited to the above-described embodiments but only by the claims.
Claims (21)
1. A polyamide 5X melt, the polyamide 5X melt having a water content of 200-:
(1) under the condition of nitrogen, 1, 5-pentanediamine, aliphatic dibasic acid, a catalyst and water are uniformly mixed to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the aliphatic dibasic acid is (1-1.05): 1; the concentration of the polyamide salt solution is 30-90%, and the percentage is the mass percentage of the polyamide salt solution; and the pH value of the salt solution of the polyamide is more than 6 when the concentration of the salt solution of the polyamide is 10%, wherein the percentage is the mass percentage of the salt solution of the polyamide; the catalyst is a phosphorus-containing catalyst, the addition amount of the catalyst is 5-2000ppm, the parts per million accounts for the parts per million by mass of the polyamide 5X resin, and the polyamide 5X resin is obtained by granulating a polyamide 5X melt;
(2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure to ensure that the temperature of the reaction system is 232-265 ℃ when the pressure maintaining is finished, then reducing the pressure to ensure that the pressure in the reaction system is reduced to 0-0.2Mpa, wherein the pressure is gauge pressure, and finally vacuumizing to obtain a polyamide 5X melt;
wherein the vacuumizing time is 10-45 min; the vacuum degree after vacuumizing is-0.095-0 Mpa, and the pressure is gauge pressure; the temperature after the vacuum pumping is 230-290 ℃; the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
2. The polyamide 5X melt of claim 1 wherein the polyamide 5X melt has a water content of 400-9000 ppm.
3. A polyamide 5X resin obtained by pelletizing a polyamide 5X melt, wherein the polyamide 5X melt has a water content of 200-18000ppm, and the polyamide 5X melt is prepared by a preparation method comprising the following steps:
(1) under the condition of nitrogen, 1, 5-pentanediamine, aliphatic dibasic acid, a catalyst and water are uniformly mixed to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the aliphatic dibasic acid is (1-1.05): 1; the concentration of the polyamide salt solution is 30-90%, and the percentage is the mass percentage of the polyamide salt solution; and the pH value of the salt solution of the polyamide is more than 6 when the concentration of the salt solution of the polyamide is 10%, wherein the percentage is the mass percentage of the salt solution of the polyamide; the catalyst is a phosphorus-containing catalyst, the addition amount of the catalyst is 5-2000ppm, and the parts per million is the parts per million by mass of the polyamide 5X resin;
(2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure to ensure that the temperature of the reaction system is 232-265 ℃ when the pressure maintaining is finished, then reducing the pressure to ensure that the pressure in the reaction system is reduced to 0-0.2Mpa, wherein the pressure is gauge pressure, and finally vacuumizing to obtain a polyamide 5X melt;
wherein the vacuumizing time is 10-45 min; the vacuum degree after vacuumizing is-0.095-0 Mpa, and the pressure is gauge pressure; the temperature after the vacuum pumping is 230-290 ℃; the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
4. The polyamide 5X resin of claim 3 wherein the polyamide 5X melt has a water content of 400-9000 ppm.
5. The polyamide 5X resin of claim 3, wherein the aliphatic dibasic acid comprises one or more of succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid, and Δ 9-1,18 octadecenedioic acid.
6. The polyamide 5X resin of claim 3, wherein the phosphorus-containing catalyst comprises one or more of phosphoric acid, phosphorous acid, hypophosphorous acid, and their corresponding salts or esters.
7. The polyamide 5X resin of claim 3, wherein the phosphorus-containing catalyst comprises hypophosphorous acid and salts or esters thereof.
8. The polyamide 5X resin of claim 3, wherein the phosphorus-containing catalyst is sodium hypophosphite.
9. The polyamide 5X resin of claim 3, wherein the catalyst is added in an amount of 10 to 1000ppm, the parts per million being parts by mass of the polyamide 5X resin.
10. The polyamide 5X resin of claim 3, wherein: the polyamide 5X resin has a water content of 180-8000 ppm.
11. The polyamide 5X resin of claim 3, wherein: the polyamide 5X resin has a water content of 380-6500 ppm.
12. The polyamide 5X resin according to claim 3 or 4, characterized in that: the content of the terminal amino groups of the polyamide 5X resin is 20-70 mol/ton;
and/or the polyamide 5X resin has a carboxyl end group content of 50mol/ton or more.
13. The polyamide 5X resin of claim 12, wherein the polyamide 5X resin has an amino end group content of 30-60 mol/ton.
14. The polyamide 5X resin of claim 12, wherein the polyamide 5X resin has a carboxyl end group content of 60 to 120 mol/ton.
15. A process for the preparation of a polyamide 5X melt according to claim 1, comprising the steps of:
(1) under the condition of nitrogen, 1, 5-pentanediamine, aliphatic dibasic acid, a catalyst and water are uniformly mixed to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the aliphatic dibasic acid is (1-1.05): 1; the concentration of the polyamide salt solution is 30-90%, and the percentage is the mass percentage of the polyamide salt solution; and the pH value of the salt solution of the polyamide is more than 6 when the concentration of the salt solution of the polyamide is 10%, wherein the percentage is the mass percentage of the salt solution of the polyamide; the catalyst is a phosphorus-containing catalyst, the addition amount of the catalyst is 5-2000ppm, the parts per million accounts for the parts per million by mass of the polyamide 5X resin, and the polyamide 5X resin is obtained by granulating a polyamide 5X melt;
(2) heating the salt solution of polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure to ensure that the temperature of the reaction system is 232-265 ℃ when the pressure maintaining is finished, then reducing the pressure to ensure that the pressure in the reaction system is reduced to 0-0.2Mpa, wherein the pressure is gauge pressure, and finally vacuumizing to obtain a polyamide 5X melt;
wherein the vacuumizing time is 10-45 min; the vacuum degree after vacuumizing is-0.095-0 Mpa, and the pressure is gauge pressure; the temperature after the vacuum pumping is 230-290 ℃; the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
16. The method of claim 15, wherein the evacuation time is 20-30 min.
17. The method according to claim 15, wherein the degree of vacuum after the evacuation is from-0.06 to-0.01 Mpa.
18. The production process according to claim 15, wherein the salt solution of the polyamide has a pH value of 7.2 to 8.9 at a concentration of 10%.
19. The production process according to claim 15, wherein the salt solution of the polyamide has a pH value of 7.5 to 8.2 at a concentration of 10%.
20. A method for preparing a polyamide 5X resin, the method comprising the steps of:
preparing a polyamide 5X melt by the process of any one of claims 15-19;
and pelletizing the polyamide 5X melt to obtain the resin.
21. The method of claim 20, wherein the resin is dried after being pelletized.
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