CN112111803B - Preparation method of bio-based chinlon 5X fiber material - Google Patents
Preparation method of bio-based chinlon 5X fiber material Download PDFInfo
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
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- 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
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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Abstract
The invention discloses a preparation method of a bio-based chinlon 5X fiber material. The method comprises the following steps: 1) Mixing 1, 5-pentanediamine mixed fermentation liquor and dibasic acid, then carrying out polymerization reaction to obtain a polyamide salt mixed liquor, and processing to obtain polyamide salt; the 1, 5-pentamethylene diamine mixed fermentation liquor is obtained by preparing 1, 5-pentamethylene diamine by a biological method; 2) Carrying out polymerization reaction on the aqueous solution of the nylon salt and a molecular weight regulator to obtain a nylon 5X polymer; 3) And (3) spraying the melt of the nylon 5X polymer through a spinneret plate to obtain melt trickle, cooling and solidifying the melt trickle to form filaments, and performing fiber post-processing on the solidified filaments to obtain the bio-based nylon 5X fiber material. According to the invention, the 1, 5-pentanediamine mixed fermentation liquor is added with the dibasic acid for reaction, so that the polyamide salt can be directly obtained, the conversion rate can be improved, the energy consumption can be reduced, and the problem of environmental pollution can be avoided; the subsequent reaction is carried out on the crystal of the nylon salt obtained by purifying the nylon salt mixed solution, so that the side reaction is avoided.
Description
Technical Field
The invention relates to a preparation method of a bio-based chinlon 5X fiber material, belonging to the field of fiber materials.
Background
Chinlon is an important engineering material and has the outstanding performances of good wear resistance, corrosion resistance, high fatigue resistance and breaking strength, easy dyeing and the like. Currently, common nylons are PA6, PA66, PA1010, PA1212, etc., wherein the nylon is often used in engineering plastics, fibers and films by itself or in combination with other polymers, with the largest production of PA6 and PA 66. At present, although the process technology of the nylon material widely applied in China is relatively pure and mature and has high yield, the production raw material is basically prepared from petroleum derivatives, and the whole synthesis process is complex and has certain pollution. And foreign companies control the production technology and patents of the raw material hexamethylenediamine for producing chinlon in China, so that the development of the chinlon industry in China is greatly limited.
Disclosure of Invention
The invention aims to provide a preparation method of a bio-based chinlon 5X fiber material, which adopts a biological method to prepare 1, 5-pentanediamine, solves the environmental problem caused by preparing hexanediamine by a petroleum method, and lays a foundation for the independent development of chinlon materials in China.
The invention provides a preparation method of a bio-based chinlon 5X fiber material, which comprises the following steps: 1) Mixing 1, 5-pentamethylene diamine mixed fermentation liquor and dibasic acid, carrying out polymerization reaction to obtain a polyamide salt mixed liquor, and treating to obtain polyamide salt;
the 1, 5-pentanediamine mixed fermentation liquor is obtained by preparing 1, 5-pentanediamine by a biological method;
2) Carrying out polymerization reaction on the aqueous solution of the nylon salt and a molecular weight regulator to obtain a nylon 5X polymer;
3) And (3) spraying the melt of the nylon 5X polymer through a spinneret plate to obtain melt trickle, cooling and solidifying the melt trickle to form filaments, and performing fiber post-processing on the solidified filaments to obtain the bio-based nylon 5X fiber material.
In the above preparation method, the molar ratio of the 1, 5-pentanediamine mixed fermentation liquor to the dibasic acid may be 1:0.5 to 1.5, specifically 1;
the dibasic acid is selected from at least one of succinic acid, adipic acid, azelaic acid, sebacic acid, terephthalic acid and dodecanedioic acid;
the conditions of the mixing reaction in step 1) are as follows: heating to 40-50 ℃ for reaction, and stirring for 0.5-1 hour;
and/or the presence of a gas in the gas,
in the step 2), the mass percentage concentration of the aqueous solution of the nylon salt is 30-70%, and specifically can be 50%, 30-50%, 50-70% or 40-60%;
the addition amount of the molecular weight regulator is 0.05-0.15 percent of the mass of the chinlon saline water, and specifically can be 0.07 percent, 0.05-0.07 percent, 0.07-0.15 percent or 0.05-0.10 percent;
the molecular weight regulator is at least one of aliphatic or aromatic monobasic acid, dibasic acid, aliphatic or aromatic amine, hydrochloric acid, sodium hydroxide and hydrochloride of amino acid, and specifically can be oxalic acid and 1, 5-pentanediamine.
In the present invention, the molecular weight regulators are all commonly used agents known in the art.
In the present invention, 1, 5-pentanediamine is biologically produced by decarboxylation of L-lysine to obtain the 1, 5-pentanediamine mixed fermentation broth, and the above production process may be performed by fermentation according to the methods known in the art.
In the present invention, the preparation of the 1, 5-pentanediamine solution by a biological method comprises the steps of: l-lysine is subjected to lysine decarboxylation reaction under the action of L-lysine decarboxylase to obtain mixed fermentation liquor containing 1, 5-pentanediamine;
the 1, 5-pentanediamine mixed fermentation liquid is mixed fermentation liquid containing 1, 5-pentanediamine, inorganic salt, sugar, protein, thalli and other metabolic organic matters;
the mass percentage of the 1, 5-pentanediamine contained in the 1, 5-pentanediamine mixed fermentation liquor prepared by a biological method in the field can be generally 50-75%.
In the preparation method, the step 1) further comprises the step of carrying out decolorization treatment on the 1, 5-pentanediamine mixed fermentation liquor;
and/or, the step 1) also comprises the step of cooling, crystallizing and drying the nylon salt mixed solution to obtain the nylon salt, and removing excessive impurities.
In the preparation method, the decoloring treatment process is to add activated carbon which accounts for 1-5% of the mass of the system into the 1, 5-pentanediamine mixed fermentation liquor for treatment, and specifically can be activated carbon which accounts for 3%, 1-3%, 3-5% or 2-4% of the mass of the system;
the decolorizing treatment conditions are as follows: the temperature can be 20-30 ℃, specifically 25 ℃, 25-30 ℃, 20-25 ℃, and the time can be 0.5-1.5 hours, specifically 1 hour, 0.5-1 hour, 1-1.5 hours, and 0.75-1.25 hours.
In the above preparation method, the cooling crystallization is performed as follows: decompressing and concentrating the mixed liquor of the chinlon salt by 4 to 5 times, wherein the concentration temperature can be 55 to 60 ℃, and the concentration pressure can be 110 to 150mmHg, so as to obtain concentrated liquor; then cooling the concentrated solution to 0-5 ℃, centrifuging to obtain crystal precipitation, and filtering to obtain crystals of the chinlon salt; the concentration can be 4 times under reduced pressure, the concentration temperature can be 55 ℃ or 55-58 ℃, the concentration pressure can be 110mmHg, 110 mmHg-120 mmHg or 110 mmHg-140 mmHg, the temperature of the concentrated solution is reduced to 3 ℃, 0-3 ℃ or 3-5 ℃;
the drying adopts reduced pressure drying, and can be vacuum drying.
In the invention, the crystal purity of the polyamide salt obtained after the cooling crystallization treatment can reach more than 99%.
In the preparation method, the step 2) further comprises the step of adding an auxiliary agent into the aqueous solution of the chinlon salt for polymerization reaction;
and/or the presence of a gas in the gas,
the auxiliary agent comprises at least one of a flame retardant, an antistatic agent, an antibacterial finishing agent and an anti-ultraviolet finishing agent;
the addition mass of the auxiliary agent is 0.05-0.15% of the mass of the chinlon salt, and specifically can be 0.07%, 0.05-0.07%, 0.07-0.15% or 0.05-0.10%.
In the present invention, the flame retardant, the antistatic agent, the antibacterial finishing agent and the ultraviolet-resistant finishing agent are all conventional agents well known in the art, and specifically, the flame retardant is melamine cyanurate.
In the above preparation method, in step 2), the polymerization reaction includes a prepolymerization reaction, a prepolymerization reaction and a postpolymerization reaction;
the prepolymerization conditions are as follows: the temperature can be 240-265 ℃, specifically 260 ℃, 265 ℃, 250-265 ℃, 260-265 ℃ or 240-260 ℃, the pressure can be 1.68-1.85 MPa, specifically 1.75MP, 1.75-1.8 MPa or 1.68-1.75 MPa, and the time can be 1-3 h, specifically 1.5h, 1-1.5 h, 1.5-3 h or 1-2.5 h.
After the prepolymerization reaction, releasing the pressure in the reaction system, raising the temperature to 280-290 ℃, and then carrying out the pre-polymerization reaction; the specific temperature is raised to 280 ℃ and 280-285 DEG C
The conditions of the pre-polymerization are as follows: the temperature can be 280-290 ℃, and the time can be 1-2 h; the specific temperature can be 280 ℃, 280-285 ℃, and the specific time can be 1.5h, 1-1.5 h, 1.5-2 h or 1.3-1.75 h;
the conditions of the postpolymerization are as follows: the temperature can be 280-290 ℃, and the vacuumizing can be carried out for 5-20 min; the specific temperature can be 280 ℃, 280-285 ℃, and the specific time can be 10min, 5-10 min, 10-20 min or 7-15 min.
In the preparation method, in the step 3), the process of spraying the chinlon 5X polymer melt through a spinneret plate to obtain melt trickle is as follows: the method is carried out in a spinning box, and the temperature of the spinning box is as follows: the temperature of a first area of the spinning box body is 260-300 ℃, the temperature of a second area is 260-300 ℃, the temperature of a third area is 250-295 ℃, the temperature of a metering pump is 250-295 ℃, and the temperature of a spinning assembly is 270-290 ℃; the rotating speed of a metering pump is 12-15 rpm/min, and the chinlon 5X polymer melt is distributed in a spinning box body and conveyed to each spinning nozzle by equal retention time and pressure drop; the spinning speed can be 300-4200 m/min, specifically 1000-4200 m/min, 500-2000 m/min, 500-3000 m/min or 500-4000 m/min.
The melt thin stream is cooled and formed by a side blowing device under the following conditions: the side blowing wind speed can be 0.30-0.80 m/min; the wind temperature can be 21-26 ℃; the side blowing air pressure can be 420-480 Pa; the side-blown air speed can be 0.50m/min, 0.30-0.50 m/min, 0.50-0.80 m/min or 0.40-0.70 m/min; the wind temperature can be 25 ℃, 21-25 ℃, 25-26 ℃ or 23-26 ℃; the side blowing air pressure can be 440Pa, 420-440 Pa, 440-480 Pa or 430-470 Pa.
In the preparation method, the fiber post-processing comprises drafting, heat setting, curling and/or winding of the incompletely crystallized formed filament;
the drafting is specifically secondary drafting, but is not limited to the secondary drafting, and can be increased or decreased according to the product performance requirement;
the conditions of the drawing were as follows: the temperature of one roller can be 60-80 ℃; the temperature of the two rollers can be between 150 and 230 ℃; the temperature of the three rollers can be 150-230 ℃; the drafting multiplying power is 2.01 to 3.50 times of the first level and 1.01 to 1.10 times of the second level; specifically, the first-pulling multiplying power is 2.78, 2.01-2.78, 2.78-3.50 or 2.45-3; the second traction multiplying power is 1.09, 1.01 to 1.09, 1.09 to 1.10 or 1.05 to 1.10; the temperature of one roller can be 70 ℃, 80 ℃ or 70-80 ℃; the two-roll temperature is 170 ℃, 180 ℃, 170-180 ℃, 160-200 ℃ or 160-210 ℃; the three-roller temperature is 170 ℃, 180 ℃, 170-180 ℃, 160-200 ℃ or 160-210 ℃;
the heat setting is steam heat setting, hot plate setting or water bath heat setting; the heat setting is carried out at the temperature of 150-230 ℃; the temperature of the hot plate can be 180 ℃, 190 ℃, 180-230 ℃ or 160-210 ℃;
when the nylon long fiber is prepared, the fiber post-processing comprises the steps of winding and oiling solidified strand silk, then winding, cooling, drying and packaging; wherein, the first winding speed can be 500-4000 m/min, specifically 900-900 m/min, 900-4000 m/min, 500-1500 m/min, 500-2000 m/min or 500-3000 m/min, the concentration of the oiling oil agent can be 2-15%, specifically 5%, 2-5%, 5-15% or 2-10%; the oiling oil agent can be F5103 which is commercially available from Japanese bamboo, and the secondary winding speed is 500-1000 m/min, specifically 900m/min;
when the nylon short fiber is prepared, the post-processing of the fiber comprises curling, cooling, drying, cutting and packaging, wherein the curling speed can be 300-350 m/min, specifically 350m/min, and the number of curls can be 10-30, specifically 15.
In the preparation method, the bio-based nylon 5X fiber material comprises at least one of bio-based nylon 54, bio-based nylon 56, bio-based nylon 59, bio-based nylon 510, bio-based nylon 5T and bio-based nylon 512.
The breaking strength of the bio-based chinlon 5X drawn yarn prepared by the invention is not less than 3.5cN/dtex, the elongation at break is not less than 28%, the modulus is not less than 30cN/dtex, the boiling water shrinkage is 7-9%, the moisture regain is not less than 4%, and the limiting oxygen index is 28-35%; the breaking strength of the short fiber is not less than 3.0cN/dtex, and the elongation at break is not less than 50%.
The invention has the following advantages:
according to the invention, 1, 5-pentanediamine is prepared by adopting a biological method, and a petroleum method is not required for preparing hexanediamine, so that the brought environmental problem is avoided, in the invention, dibasic acid is added into the 1, 5-pentanediamine mixed fermentation liquor obtained by preparing 1, 5-pentanediamine by adopting the biological method for reaction, so that the polyamide salt can be directly obtained, and compared with the traditional method of purifying the pentanediamine by distillation, the problems of low conversion rate, large energy consumption and the like caused by high volatility of the pentanediamine can be reduced, and the problem of environmental pollution caused by the volatilization of the pentanediamine can be avoided; on the other hand, the crystal of the chinlon salt obtained by purifying the chinlon salt water solution is subjected to subsequent reaction so as to effectively reduce inorganic salt, sugar, protein, thalli and other metabolic organic matters contained in the pentamethylene diamine solution and prevent the unstable substances from generating side reaction in the high-temperature and high-pressure polymerization process and influencing final products.
Drawings
FIG. 1 is a process flow diagram in an embodiment of the invention.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Examples 1,
1. Preparation of pentamethylene diamine monomer by biological method:
the lysine decarboxylase synthesized by escherichia coli can carry out biocatalysis L-lysine decarboxylation reaction to obtain mixed liquor fermentation liquor containing 1, 5-pentanediamine, inorganic salt, sugar, protein, thalli and other metabolic organic matters, namely 1, 5-pentanediamine mixed liquor fermentation liquor, 5 mass percent of active carbon is added into the 1, 5-pentanediamine-containing fermentation liquor, the mixture is stirred for 1 hour at the temperature of 25 ℃ for decolorization, adipic acid with the same mass is added into filtrate after the decolorization, the reaction is carried out for 40 minutes at the temperature of 40 ℃ to obtain mixed liquor containing polyamide salt, the mixed liquor is concentrated under reduced pressure for 4 times at the temperature of 55 ℃ and 110mmHg to obtain concentrated liquor, the concentrated liquor is cooled to 3 ℃, crystals are separated out, then the crystals are obtained through centrifugation, the crystals are dried in a reduced pressure dryer for several days to obtain polyamide 56 salt, and the purity of the salt is 99.2% through tests.
2. Preparation of bio-based PA56 long fiber
Preparing a nylon saline solution with the mass percentage concentration of 50% under the protection of nitrogen atmosphere. 5kg of prepared nylon saline solution and 1.75g of molecular weight regulator oxalic acid are added into a reactor together with the pH value being adjusted to 7.85, and the material outlet temperature of a concentration tank is as follows: 119 ℃; reactor feed temperature control inlet temperature: 260 ℃, outlet 1 temperature: 265 ℃, outlet 2 temperature: the temperature of 265 ℃, the pressure of the reactor is 17.5MPa, and the time is 1.5h; temperature of the pre-polymerization heat medium: the temperature is 280 ℃, and the time is 1.5h; temperature of post-polymerization heat medium: 280 ℃, time 10min, post-vacuum: 65kPa; controlling the viscosity of the spinning melt to be 2.5, and the pressure of a booster pump: 12MPa; spinning box temperature: 285 ℃ in the first area, 285 ℃ in the second area, 285 ℃ in the third area, 13rpm/min of the rotating speed of a metering pump, 1000m/min of spinning speed and 0.50m/min of side blowing speed; the wind temperature is 25 ℃, the side-blown wind pressure is 440Pa, the concentration of the winding oil agent is 5 percent (the winding oil agent is F5103, commercially available from Japanese bamboo, and wound at the speed of 900 m/min), the post-spinning draft ratio and the heating temperature are as follows: the first drawing ratio is 2.78; the second traction multiplying power is 1.09; the temperature of the drawing box is 80 ℃; the second pulling temperature is 180 ℃; the temperature of a hot plate is 190 ℃; the temperature of the three-drawing is 180 ℃, finally the bio-based PA56 long fiber can be obtained after winding and spooling at the speed of 900m/min, the sample is marked as No. 1, and the mechanical property test of the drawn fiber is shown in Table 1.
Example 2 preparation of PA56 with flame-retardant Effect
In the invention, no auxiliary agent is added when pure PA56 is prepared in the embodiment 1, and different auxiliary agents are required to be added when PA56 with antistatic/flame retardant effects is produced.
The chinlon 56 salt prepared in the embodiment 1 of the invention is adopted to prepare 50% chinlon salt water solution under the protection of nitrogen atmosphere, and the pH value is adjusted to 7.85. 5kg of prepared nylon salt aqueous solution, 1.75g of molecular weight regulator and 1.75g of flame retardant MAC (melamine cyanurate) are added into a reactor, and the outlet temperature of the material of a concentration tank is as follows: 119 ℃; reactor feed temperature control inlet temperature: 265 ℃, outlet 1 temperature: 265 ℃, outlet 2 temperature: the temperature of 265 ℃ and the pressure of the reactor are 17.5MPa; temperature of the pre-polymerization heat medium: the temperature is 280 ℃, and the time is 1.5h; temperature of post-polymerization heat medium: 280 ℃ for 10min, post-polymerization vacuum: 65kPa; controlling the viscosity of the spinning melt to be 2.5, and the pressure of a booster pump: 12MPa.
The subsequent spinning step is the same as step 2 in the embodiment 1 of the invention, so that the flame retardant PA5 is obtained and marked as sample No. 2, and the mechanical property test of the drawn fiber is shown in Table 1.
Example 3 preparation of Nylon staple fibers
The preceding polymerization, step 2 in example 1 of the invention, with variations in draw back, was as follows:
the drawing times and heating temperatures were: the first drawing ratio is 2.78; the second-pulling multiplying power is 1.05; the first roller temperature of the drawing box is 70 ℃; the temperature of the two rollers is 170 ℃; the temperature of a hot plate is 180 ℃; the three-roll temperature is 170 ℃, the curling rate can be 300m/min, the number of curls is 15, and the nylon staple fiber is obtained by cutting, wherein the mechanical properties of the staple fiber are shown in Table 2.
The test method comprises the following steps:
1. the linear density was tested according to GB/T14335-2008;
2. strength and elongation: the breaking strength and the breaking elongation are tested according to GB/T14337-2008;
3. the limiting oxygen index is tested according to GB/T5454-1997;
4. differential Scanning Calorimeter (DSC) measurement of melting enthalpy (Δ H) of fibers f ) Melting Point (T) m ) Degree of crystallinity (X) c )；
5. Curling property: the number of crimps and the degree of crimps were tested according to GB/T14338-2008;
6. the moisture regain is tested according to GB/T6503-2008.
The technical parameters of the bio-based chinlon 5X fiber prepared by the invention are as follows:
TABLE 1 mechanical Properties of drawn fibers
TABLE 2 short fiber test data
| Item | Test data | Item | Test data |
| Linear density/dtex | 1.80 | Moisture regain/% | 2.06 |
| Deviation of linear density/%) | 7.80 | Oil content/%) | 0.56 |
| Breaking strength/cN/dtex | 3.27 | Number of crimps/25 mm | 15.4 |
| Elongation at break/% | 65.5 | Volume specific resistance/omega cm | 1.85*10 8 |
Comparative example (c),
The same preparation method as that in the embodiment 1 of the invention, 1, 5-pentanediamine fermentation liquor with equal mass is adopted to react with adipic acid, the difference is that the fermentation liquor containing 1, 5-pentanediamine is purified and then reacts with adipic acid, the 1, 5-pentanediamine fermentation liquor is decolored and then is purified by adopting a multiple distillation method, the primary distillation temperature is 110 ℃, the secondary distillation temperature is 140 ℃, the tertiary distillation temperature is 165 ℃, inorganic salt, sugar, protein, thallus and other metabolic organic matters in the mixed liquor are removed by multiple distillation, the 1, 5-pentanediamine obtained after rectification reacts with adipic acid, and pure polyamide salt is obtained after cooling and filtering.
Experiments show that 1, 5-pentamethylene diamine fermentation liquor is purified in the experimental process to obtain 1, 5-pentamethylene diamine, and after repeated high-temperature distillation, part of 1, 5-pentamethylene diamine volatilizes, and the experimental environment has strong pungent taste of 1, 5-pentamethylene diamine, so that the energy consumption in the distillation process is high, the most direct result is that the subsequent amount of 1, 5-pentamethylene diamine entering the distillation process is less, the conversion rate of the 1, 5-pentamethylene diamine fermentation liquor is low, the yield of pure polyamide salt is influenced, and the yield of finally generated bio-based PA56 long fibers is improved.
Claims (7)
1. A preparation method of a bio-based chinlon 5X fiber material comprises the following steps: 1) Mixing the 1, 5-pentanediamine mixed fermentation liquor with dibasic acid, carrying out polymerization reaction to obtain a polyamide salt mixed liquor, and processing to obtain polyamide salt;
the step 1) also comprises a step of carrying out decoloration treatment on the 1, 5-pentanediamine mixed fermentation liquor;
the decolorization treatment process is to add active carbon accounting for 1-5 percent of the mass of the system into the 1, 5-pentanediamine mixed fermentation liquor for treatment;
the decolorizing treatment conditions are as follows: the temperature is 25-30 ℃, and the time is 0.5-1.5 hours;
the step 1) also comprises the steps of cooling, crystallizing and drying the nylon salt mixed solution to obtain the nylon salt;
the cooling crystallization treatment is as follows: concentrating the mixed solution of the chinlon salt under reduced pressure by 4-5 times at 55-60 ℃ and 110-150 mmHg to obtain a concentrated solution; then cooling the concentrated solution to 0-5 ℃, centrifuging to obtain crystal precipitation, and filtering to obtain crystals of the chinlon salt;
the drying adopts reduced pressure drying;
the 1, 5-pentamethylene diamine mixed fermentation liquor is obtained by preparing 1, 5-pentamethylene diamine by a biological method;
2) Carrying out polymerization reaction on the aqueous solution of the nylon salt and a molecular weight regulator to obtain a nylon 5X polymer;
3) And (3) spraying the melt of the nylon 5X polymer through a spinneret plate to obtain melt trickle, cooling and solidifying the melt trickle to form filaments, and performing fiber post-processing on the solidified filaments to obtain the bio-based nylon 5X fiber material.
2. The production method according to claim 1, characterized in that: the mass ratio of the 1, 5-pentanediamine mixed fermentation liquor to the dibasic acid is 1:0.5 to 1.5;
the dibasic acid is at least one of succinic acid, adipic acid, azelaic acid, sebacic acid, terephthalic acid and dodecanedioic acid;
the conditions of the mixing reaction in step 1) are as follows: heating to 40-50 ℃ for reaction, and stirring for 0.5-1 hour;
and/or the presence of a gas in the gas,
in the step 2), the mass percentage concentration of the aqueous solution of the nylon salt is 30-70%;
the addition amount of the molecular weight regulator is 0.05-0.15% of the mass of the chinlon salt;
the molecular weight regulator is at least one of aliphatic or aromatic monobasic acid, dibasic acid, aliphatic or aromatic amine, hydrochloric acid, sodium hydroxide and hydrochloride of amino acid.
3. The production method according to claim 1 or 2, characterized in that: the step 2) also comprises a step of adding an auxiliary agent into the aqueous solution of the chinlon salt for polymerization reaction;
and/or the presence of a gas in the gas,
the auxiliary agent comprises at least one of a molecular weight regulator, a flame retardant, an antistatic agent, an antibacterial finishing agent and an anti-ultraviolet finishing agent;
the addition mass of the auxiliary agent is 0.05-0.15% of the mass of the polyamide salt.
4. The production method according to claim 1 or 2, characterized in that: in the step 2), the polymerization reaction comprises a prepolymerization reaction, a prepolymerization reaction and a post-polymerization reaction;
the prepolymerization conditions are as follows: the temperature is 240-265 ℃, the pressure is 1.68-1.85 MPa, and the time is 1-3 h;
after the prepolymerization reaction, releasing the pressure in the reaction system, raising the temperature to 280-290 ℃, and then carrying out the pre-polymerization reaction;
the conditions of the pre-polymerization reaction are as follows: the temperature is 280-290 ℃, and the time is 1-2 h;
the conditions of the postpolymerization are as follows: the temperature is 280-290 ℃, and the time is 5-20 min.
5. The production method according to claim 1 or 2, characterized in that: in the step 3), the process that the melt of the chinlon 5X polymer is sprayed out by a spinneret plate to obtain melt trickle is as follows: the method is carried out in a spinning box, and the temperature of the spinning box is as follows: the temperature of a first area of the spinning box body is 260-300 ℃, the temperature of a second area is 260-300 ℃, the temperature of a third area is 250-295 ℃, the temperature of a metering pump is 250-295 ℃, and the temperature of a spinning assembly is 270-290 ℃; the rotating speed of a metering pump is 12-15 rpm/min, and the nylon 5X polymer melt is distributed through a pipeline and conveyed to each spinning nozzle with equal residence time and pressure drop; the spinning speed is 300-4200 m/min;
the melt thin stream is cooled and formed by a side blowing device under the following conditions: the side blowing wind speed is 0.30-0.80 m/min; the wind temperature is 21-26 ℃; the side blowing pressure is 420-480 Pa.
6. The production method according to claim 1 or 2, characterized in that: the fiber post-processing comprises drawing, heat setting and curling and/or winding of the incompletely crystallized formed strand;
the drafting is two-stage drafting;
the conditions of the drawing were as follows: the temperature of one roller is 60-80 ℃; the temperature of the two rollers is 150-230 ℃; the temperature of the three rollers is 150-230 ℃; the drafting multiplying power is 2.01 to 3.50 times of the first grade and 1.01 to 1.10 times of the second grade;
the heat setting is steam heat setting, hot plate setting or water bath heat setting; the heat setting is carried out at the temperature of 150-230 ℃;
when the nylon long fiber is prepared, the fiber post-processing comprises the steps of winding and oiling solidified strand silk, then winding, cooling, drying and packaging; wherein the first winding speed is 500-4000 m/min; the concentration of the oiling oil agent is 2-15%, and the second winding speed is 500-1000 m/min.
When the nylon short fiber is prepared, the post-processing of the fiber comprises curling, cooling, drying, cutting and packaging, wherein the curling speed is 300-350 m/min, and the number of curls is 10-30.
7. The production method according to claim 1 or 2, characterized in that: the bio-based nylon 5X fiber material comprises at least one of bio-based nylon 54, bio-based nylon 56, bio-based nylon 59, bio-based nylon 510, bio-based nylon 5T and bio-based nylon 512.
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| CN202010927932.6A CN112111803B (en) | 2020-09-07 | 2020-09-07 | Preparation method of bio-based chinlon 5X fiber material |
| PCT/CN2021/116657 WO2022048662A1 (en) | 2020-09-07 | 2021-09-06 | Preparation method for bio-based nylon 5x fiber material |
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| CN202010927932.6A CN112111803B (en) | 2020-09-07 | 2020-09-07 | Preparation method of bio-based chinlon 5X fiber material |
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| DE602004000428T2 (en) * | 2003-05-26 | 2006-10-19 | Ajinomoto Co., Inc. | Process for the preparation of cadaverine dicarboxylate and its use for the production of nylon |
| JP5454191B2 (en) * | 2010-02-09 | 2014-03-26 | 東レ株式会社 | Crimped yarn and fiber structure |
| CN105885038A (en) * | 2015-05-12 | 2016-08-24 | 上海凯赛生物技术研发中心有限公司 | Method for preparing polyamide |
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| CN106637471B (en) * | 2017-02-24 | 2018-10-30 | 上海凯赛生物技术研发中心有限公司 | A kind of polyamide 5X Blulked continuous Filaments and its preparation method and application |
| CN110616471B (en) * | 2017-02-24 | 2022-11-01 | 上海凯赛生物技术股份有限公司 | Polyamide 5X medium-strength yarn and preparation method thereof |
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| CN108129329B (en) * | 2018-01-10 | 2020-06-30 | 山东寿光巨能金玉米开发有限公司 | Nylon 5X salt and preparation method thereof |
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