Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of an anti-ultraviolet flame-retardant polyester filament.
The technical scheme of the invention is as follows:
a preparation method of an anti-ultraviolet flame-retardant polyester filament yarn comprises the following steps:
A. grinding the PET slices and the PBT slices into powder, sieving the powder by a 80-mesh sieve, and taking undersize products to obtain polyester powder;
B. mixing nano titanium dioxide and modified nano silicon dioxide, and then dispersing at a high speed to obtain mixed nano powder;
C. carrying out vacuum pre-crystallization drying treatment on the polyester powder and the mixed nano powder;
D. mixing and dispersing polyester powder, mixed nano powder and flame-retardant powder, mixing by using a double screw, cooling and granulating to obtain an ultraviolet-resistant flame-retardant polyester fiber master batch;
E. uniformly mixing 2-5 wt% of the ultraviolet-resistant flame-retardant polyester fiber master batch with polyester chips, and shearing at high temperature of 285 ℃ for 270 DEG to obtain a spinning melt;
F. extruding the spinning melt into a spinning assembly, circularly blowing air in a constant-temperature and constant-humidity environment, and cooling to obtain nascent fiber; and subjecting the nascent fiber to primary drawing by hot oil at the temperature of 180-.
Preferably, in the step a, the mass ratio of the PET slices to the PBT slices is (18-25): 1.
preferably, in the step a, the mass ratio of the nano titanium dioxide to the modified nano silicon dioxide is (2-5): 1.
preferably, in the step B, the preparation method of the modified nano-silica comprises: mixing the nano-silica and the organic solvent in a container to form a mixed solution, refluxing and dehydrating the mixed solution, dropwise adding isocyanate into the mixed solution after moisture removal in the presence of protective gas, and reacting.
Preferably, in the step C, the process conditions of the vacuum pre-crystallization drying treatment are as follows: the vacuum degree is less than 0.1-0.3MPa, the temperature is 85-95 ℃, the temperature is kept for 2-3h, and then the temperature is raised by 8-10 ℃ in turn every hour until 130-;
preferably, in the step D, the flame retardant powder is antimony trioxide.
Preferably, in the step D, the ultraviolet-resistant flame-retardant polyester fiber master batch comprises the following raw materials in percentage by weight: 1.2 to 2.2 percent of mixed nano powder, 3 to 8 percent of flame retardant powder and the balance of polyester powder.
Preferably, in the step F, the draft ratio after the secondary draft is 6 to 8 times.
The invention has the advantages that: the preparation method of the anti-ultraviolet flame-retardant polyester filament yarn comprises the following steps: grinding the PET slices and the PBT slices into powder, and sieving to obtain polyester powder; mixing nano titanium dioxide and modified nano silicon dioxide, and then dispersing at a high speed to obtain mixed nano powder; carrying out vacuum pre-crystallization and drying; mixing and dispersing polyester powder, mixed nano powder and flame-retardant powder, mixing by a double screw, cooling and granulating to obtain modified master batch; uniformly mixing the modified master batch and the polyester chips, and then shearing at high temperature to obtain a spinning melt; extruding the spinning melt into a spinning assembly, blowing air and cooling to obtain nascent fiber; and then subjecting the nascent fiber to hot oil primary drafting and boiling water secondary drafting, heat setting, washing, drying and winding to obtain the anti-ultraviolet flame-retardant polyester filament. According to the anti-ultraviolet flame-retardant polyester fiber, the antimony trioxide is used as a flame retardant, and the nano titanium dioxide, the modified nano silicon dioxide and the antimony trioxide are used as a mixed anti-ultraviolet agent, so that the anti-ultraviolet flame-retardant polyester fiber has a very good anti-ultraviolet effect.
Detailed Description
Example 1
A preparation method of an anti-ultraviolet flame-retardant polyester filament yarn comprises the following steps:
A. grinding the PET slices and the PBT slices into powder, sieving the powder by a 80-mesh sieve, and taking undersize products to obtain polyester powder;
B. mixing nano titanium dioxide and modified nano silicon dioxide, and then dispersing at a high speed to obtain mixed nano powder;
C. carrying out vacuum pre-crystallization drying treatment on the polyester powder and the mixed nano powder;
D. mixing and dispersing polyester powder, mixed nano powder and flame-retardant powder, mixing by using a double screw, cooling and granulating to obtain an ultraviolet-resistant flame-retardant polyester fiber master batch;
E. uniformly mixing the ultraviolet-resistant flame-retardant polyester fiber master batch with polyester chips according to the weight ratio of 3%, and shearing at the high temperature of 270-plus 285 ℃ to obtain a spinning melt;
F. extruding the spinning melt into a spinning assembly, circularly blowing air in a constant-temperature and constant-humidity environment, and cooling to obtain nascent fiber; and subjecting the nascent fiber to primary drawing with hot oil of 3200m/min and secondary drawing with boiling water of 5500m/min at 185 ℃, heat setting, washing, drying and winding.
In the step A, the mass ratio of the PET slices to the PBT slices is 22.8: 1.
in the step A, the mass ratio of the nano titanium dioxide to the modified nano silicon dioxide is 3.5: 1.
in the step B, the preparation method of the modified nano silicon dioxide comprises the following steps: mixing the nano-silica and the organic solvent in a container to form a mixed solution, refluxing and dehydrating the mixed solution, dropwise adding isocyanate into the mixed solution after moisture removal in the presence of protective gas, and reacting.
In the step C, the process conditions of the vacuum pre-crystallization drying treatment are as follows: keeping the temperature at 92 ℃ for 2.5h under the vacuum degree of less than 0.2MPa, and then sequentially increasing the temperature by 8.5 ℃ per hour until the temperature reaches 132 ℃;
in the step D, the flame-retardant powder is antimony trioxide.
In the step D, the ultraviolet-resistant flame-retardant polyester fiber master batch comprises the following raw materials in percentage by weight: 1.5 percent of mixed nano powder, 7 percent of flame-retardant powder and the balance of polyester powder.
In the step F, the draft ratio after the secondary draft is 6.5 times.
Example 2
A preparation method of an anti-ultraviolet flame-retardant polyester filament yarn comprises the following steps:
A. grinding the PET slices and the PBT slices into powder, sieving the powder by a 80-mesh sieve, and taking undersize products to obtain polyester powder;
B. mixing nano titanium dioxide and modified nano silicon dioxide, and then dispersing at a high speed to obtain mixed nano powder;
C. carrying out vacuum pre-crystallization drying treatment on the polyester powder and the mixed nano powder;
D. mixing and dispersing polyester powder, mixed nano powder and flame-retardant powder, mixing by using a double screw, cooling and granulating to obtain an ultraviolet-resistant flame-retardant polyester fiber master batch;
E. uniformly mixing the ultraviolet-resistant flame-retardant polyester fiber master batch with polyester chips according to the weight ratio of 5%, and then shearing at the high temperature of 285 ℃ to obtain a spinning melt;
F. extruding the spinning melt into a spinning assembly, circularly blowing air in a constant-temperature and constant-humidity environment, and cooling to obtain nascent fiber; and subjecting the nascent fiber to 4000m/min hot oil primary drafting and 5000m/min boiling water secondary drafting at 180 ℃, heat setting, washing, drying and winding.
In the step A, the mass ratio of the PET slices to the PBT slices is 25: 1.
in the step A, the mass ratio of the nano titanium dioxide to the modified nano silicon dioxide is 2: 1.
in the step B, the preparation method of the modified nano silicon dioxide comprises the following steps: mixing the nano-silica and the organic solvent in a container to form a mixed solution, refluxing and dehydrating the mixed solution, dropwise adding isocyanate into the mixed solution after moisture removal in the presence of protective gas, and reacting.
In the step C, the process conditions of the vacuum pre-crystallization drying treatment are as follows: keeping the temperature for 3h at the vacuum degree of less than 0.3MPa and the temperature of 85 ℃, and then sequentially increasing the temperature by 8 ℃ per hour until the temperature reaches 135 ℃;
in the step D, the flame-retardant powder is antimony trioxide.
In the step D, the ultraviolet-resistant flame-retardant polyester fiber master batch comprises the following raw materials in percentage by weight: 1.2 percent of mixed nano powder, 8 percent of flame retardant powder and the balance of polyester powder.
In the step F, the draft ratio after the secondary draft is 6 times.
Example 3
A preparation method of an anti-ultraviolet flame-retardant polyester filament yarn comprises the following steps:
A. grinding the PET slices and the PBT slices into powder, sieving the powder by a 80-mesh sieve, and taking undersize products to obtain polyester powder;
B. mixing nano titanium dioxide and modified nano silicon dioxide, and then dispersing at a high speed to obtain mixed nano powder;
C. carrying out vacuum pre-crystallization drying treatment on the polyester powder and the mixed nano powder;
D. mixing and dispersing polyester powder, mixed nano powder and flame-retardant powder, mixing by using a double screw, cooling and granulating to obtain an ultraviolet-resistant flame-retardant polyester fiber master batch;
E. uniformly mixing the ultraviolet-resistant flame-retardant polyester fiber master batch with polyester chips according to the weight ratio of 2%, and shearing at the high temperature of 270 ℃ to obtain a spinning melt;
F. extruding the spinning melt into a spinning assembly, circularly blowing air in a constant-temperature and constant-humidity environment, and cooling to obtain nascent fiber; and subjecting the nascent fiber to primary drawing with 3000m/min hot oil and secondary drawing with 6000m/min boiling water at 200 ℃, heat setting, washing, drying and winding.
In the step A, the mass ratio of the PET slices to the PBT slices is 18: 1.
in the step A, the mass ratio of the nano titanium dioxide to the modified nano silicon dioxide is 5: 1.
in the step B, the preparation method of the modified nano silicon dioxide comprises the following steps: mixing the nano-silica and the organic solvent in a container to form a mixed solution, refluxing and dehydrating the mixed solution, dropwise adding isocyanate into the mixed solution after moisture removal in the presence of protective gas, and reacting.
In the step C, the process conditions of the vacuum pre-crystallization drying treatment are as follows: keeping the temperature at 95 ℃ for 2h under the vacuum degree of less than 0.1MPa, and then sequentially increasing the temperature by 10 ℃ per hour until the temperature reaches 130 ℃;
in the step D, the flame-retardant powder is antimony trioxide.
In the step D, the ultraviolet-resistant flame-retardant polyester fiber master batch comprises the following raw materials in percentage by weight: 2.2 percent of mixed nano powder, 3 percent of flame retardant powder and the balance of polyester powder.
In the step F, the draft ratio after the secondary draft is 8 times.
Comparative example 1
The modified nano-silica in the embodiment 1 is replaced by the conventional unmodified nano-silica, and the rest proportion and the preparation method are not changed.
The following test results, specific results of which are shown in table 1, were obtained by testing the anti-ultraviolet flame-retardant polyester fiber filaments prepared in examples 1 to 3 and comparative example 1 according to the method of GB/T18830-2002.
Table 1: comparing the test results of examples 1-3 with that of comparative example 1;
| example 1 | Example 2 | Example 3 | Comparative example 1 |
| UVA transmittance% | ≤0.3 | ≤0.3 | ≤0.3 | 1.1 |
| UVB transmittance% | ≤0.1 | ≤0.1 | ≤0.1 | 0.4 |
| UPF value | ≥50 | ≥50 | ≥50 | ≥50 |
The test data show that the anti-ultraviolet flame-retardant polyester fiber filament prepared by the invention has very good anti-ultraviolet performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.