CN117845372A - Flame-retardant polyester fabric and production process thereof - Google Patents
Flame-retardant polyester fabric and production process thereof Download PDFInfo
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- CN117845372A CN117845372A CN202410036771.XA CN202410036771A CN117845372A CN 117845372 A CN117845372 A CN 117845372A CN 202410036771 A CN202410036771 A CN 202410036771A CN 117845372 A CN117845372 A CN 117845372A
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- flame
- flame retardant
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- polyester fabric
- retardant
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000003063 flame retardant Substances 0.000 title claims abstract description 121
- 229920000728 polyester Polymers 0.000 title claims abstract description 114
- 239000004744 fabric Substances 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 47
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 30
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 30
- 229920001634 Copolyester Polymers 0.000 claims abstract description 27
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052698 phosphorus Inorganic materials 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 239000011574 phosphorus Substances 0.000 claims description 18
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 17
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 16
- 229940068041 phytic acid Drugs 0.000 claims description 16
- 239000000467 phytic acid Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004804 winding Methods 0.000 claims description 15
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 9
- DWSWCPPGLRSPIT-UHFFFAOYSA-N benzo[c][2,1]benzoxaphosphinin-6-ium 6-oxide Chemical compound C1=CC=C2[P+](=O)OC3=CC=CC=C3C2=C1 DWSWCPPGLRSPIT-UHFFFAOYSA-N 0.000 claims description 8
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000009960 carding Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010035 extrusion spinning Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000004753 textile Substances 0.000 abstract description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 24
- 239000005020 polyethylene terephthalate Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- -1 Polyethylene terephthalate Polymers 0.000 description 1
- 238000012863 analytical testing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of textile fabrics, and discloses a flame-retardant polyester fabric and a production process thereof, wherein the flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70-80 parts of PET, 35-40 parts of modified PET, 1.5-5 parts of composite flame retardant and 0.05-0.1 part of silane coupling agent, wherein the modified PET is organophosphorus flame retardant copolyester, and the composite flame retardant is prepared from aluminum hydroxide, melamine and bio-based flame retardant according to the mass ratio of 1:2:2, mixing, wherein the bio-based flame retardant is iron phytate, and the flame retardant performance of the flame retardant polyester fabric is improved by adding the modified PET and the composite flame retardant on the premise of not affecting the mechanical property, spinnability and durability of the material.
Description
Technical Field
The invention belongs to the technical field of textile fabrics, and particularly relates to a flame-retardant polyester fabric and a production process thereof.
Background
Polyethylene terephthalate (PET) is the most important commercial polyester polymer, and polyester fabric woven from polyester fibers is a chemical fiber garment fabric commonly used in daily life, and has the advantages of high strength, good flexibility, comfort in wearing, soft hand feeling, crease resistance and the like, and can be widely applied to garments and industrial fabrics, and can be also applied to outdoor articles such as various bags and tents. But because the polyester fabric is from the characteristic of synthetic material, so have very flammable characteristic, easy to produce the molten drop and cause the great threat to people's life and property security in the case of fire, this has limited the application field of the polyester fabric greatly.
At present, the preparation method of the flame-retardant polyester fabric mainly comprises the steps of immersing the polyester fabric in a prepared flame-retardant solution, so that the fabric has high-efficiency flame-retardant performance, and the flame retardant is attached to the surface of the fiber to absorb heat in a combustion area under the condition of fabric combustion, so that air is diluted and isolated, and combustion is prevented. However, after the fabric is washed for a plurality of times by soaking the fabric in the flame retardant, the flame retardant is washed off, the flame retardant capability of the fiber is weakened, and meanwhile, the flame retardant is added on the surface of the polyester fabric to ensure that the fabric is astringent in hand feeling and not soft.
Disclosure of Invention
In order to solve the defects in the background art, the invention aims to provide the flame-retardant polyester fabric and the production process thereof, and the flame-retardant performance of the flame-retardant polyester fabric is improved on the premise that the mechanical performance, spinnability and durability of the material are not affected by adding the modified PET and the composite flame retardant.
The aim of the invention can be achieved by the following technical scheme:
the flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70-80 parts of PET, 35-40 parts of modified PET, 1.5-5 parts of composite flame retardant and 0.05-0.1 part of silane coupling agent, wherein the modified PET is organic phosphorus flame-retardant copolyester.
Further preferably, the preparation method of the organophosphorus flame retardant copolyester comprises the following steps:
(1) Adding terephthalaldehyde, DOPO and N, N-dimethylformamide into a reactor with a condensing reflux device, then introducing nitrogen, heating to 100-120 ℃, stirring for reaction for 6-8 hours, cooling, distilling under reduced pressure to remove N, N-dimethylformamide, washing for 1-3 times by ethanol and deionized water in sequence, and vacuum drying for 10-12 hours at 70-80 ℃ to obtain a phosphorus-containing monomer A;
(2) Terephthalic acid, ethylene glycol and phosphorus-containing monomer A, sb 2 O 3 Adding nitrogen into a reaction kettle, charging nitrogen until the pressure is 0.3-0.5 MPa, heating to 210-220 ℃ for reaction for 2-4 h, heating to 260-270 ℃ for reaction for 6-8 h, and finally extruding and water-cooling the reacted polyester to obtain the organophosphorus flame-retardant copolyester.
Further preferably, the molar ratio of terephthalaldehyde to DOPO in step (1) is 1:3 to 5.
Further preferably, the mass ratio of terephthalic acid, ethylene glycol and phosphorus-containing monomer A in the step (2) is 10:14:0.5.
further preferably, the composite flame retardant consists of aluminum hydroxide, melamine and a bio-based flame retardant according to a mass ratio of 1:2:2 mixing.
Further preferably, the bio-based flame retardant is iron phytate, and the preparation method of the iron phytate comprises the following steps:
A. fe (NO) 3 ) 3 ·9H 2 O is dissolved by ionized water, and then a certain volume of phytic acid aqueous solution is added and fully stirred to generate white floccules;
B. and regulating the pH value of the solution to be neutral by using a sodium hydroxide solution, transferring the solution into a hydrothermal kettle, reacting for 8-12 hours at 75-85 ℃, and vacuum drying at 40-50 ℃ after suction filtration to obtain the phytic acid iron.
Further preferably, in step A the phytic acid and Fe (NO 3 ) 3 ·9H 2 The molar ratio of O is 2:1.
a production process of flame-retardant polyester fabric comprises the following steps:
s1, uniformly mixing all the raw materials of the flame-retardant polyester fabric, adding the mixture into an internal mixer, regulating the temperature to 260-270 ℃, banburying for 5-10 min, extruding, water-cooling, slicing, and drying to obtain polyester slices;
s2, placing the polyester chips into a screw, then carrying out melt extrusion on the polyester chips through a screw melt extrusion process, carrying out extrusion spinning at the temperature of 280-295 ℃, and then cooling, oiling and winding the spinning to obtain polyester POY fibers;
s3, sequentially carrying out processes of opening and picking, cotton carding, first drawing, second drawing, roving, spinning, winding and shaping on the polyester POY fibers to obtain polyester yarns;
s4, respectively taking the polyester yarns prepared in the step S3 as warp yarns and weft yarns, and weaving by interweaving to obtain the flame-retardant polyester fabric.
It is further preferable that the cooling temperature in step S2 is 20 to 30 ℃, the oil application rate is 0.42 to 1.5wt%, and the winding speed is 2700 to 3200m/min.
Further preferably, the warp yarn is a polyester yarn of 50 to 150D/30 to 600F, and the weft yarn is a polyester yarn of 100 to 800D/30 to 600F.
The invention has the beneficial effects that:
according to the flame-retardant polyester fabric, the flame retardant performance of the polyester fabric can be obviously improved by adding the modified PET and the composite flame retardant. The modified PET is an organic phosphorus flame-retardant copolyester, a high-phosphorus flame-retardant monomer is obtained by polymerizing terephthalaldehyde and DOPO, and then a phosphorus-containing monomer is introduced into a PET framework through a copolymerization method, so that the organic phosphorus flame-retardant copolyester and the PET substrate can be uniformly dispersed, and the mechanical properties of the material are not affected. The composite flame retardant adopts the combination of aluminum hydroxide, melamine and phytic acid, so that the flame retardant effect of external flame retardance is improved, the consumption of the external flame retardant is reduced, and the spinnability and the durability of the polyester fiber are further improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to those skilled in the art that other drawings can be obtained according to these drawings without inventive effort.
FIG. 1 is an infrared spectrum of an organophosphorus flame retardant copolyester prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
An organic phosphorus flame-retardant copolyester has the following structural formula:
the preparation method of the organophosphorus flame retardant copolyester comprises the following steps:
(1) Adding 1.5mol of terephthalaldehyde, 6mol of DOPO and 250ml of N, N-dimethylformamide into a reactor with a condensing reflux device, then introducing nitrogen, heating to 100 ℃, stirring for reaction for 8 hours, cooling, distilling under reduced pressure to remove the N, N-dimethylformamide, washing for 1-3 times by ethanol and deionized water in sequence, and vacuum drying at 70 ℃ for 12 hours to obtain a phosphorus-containing monomer A, wherein the structural formula is as follows:
(2) 18.5g of terephthalic acid, 26g of ethylene glycol and 0.9g of phosphorus-containing monomer A are added into a reaction kettle, and a catalyst Sb is added 2 O 3 And (3) charging nitrogen until the pressure is 0.3MPa, heating to 220 ℃ for reaction for 2 hours, heating to 270 ℃ for reaction for 6 hours, and finally extruding the polyester after the reaction into water-cooled slices to obtain the organophosphorus flame-retardant copolyester.
And grinding and tabletting the prepared powder after the organophosphorus flame-retardant copolyester is crushed with KBr powder, and testing the chemical structure of the organophosphorus flame-retardant copolyester by adopting a Fourier infrared spectrometer to obtain an infrared spectrum of the organophosphorus flame-retardant copolyester, wherein the infrared spectrum is shown in figure 1. As can be seen, 3430cm -1 Is characterized by that it is a stretching vibration peak of-OH in-COOH on polyester main chain, 2950cm -1 Nearby is-CH 2 -a telescopic vibration absorption peak, 1720cm -1 The absorption peak of-C=O on the main chain of the polyester is 830cm -1 The vicinity is a benzene ring stretching vibration absorption peak. Furthermore, 1245cm -1 The absorption peaks of the telescopic vibration with the vicinity of P=O are located at 1090 cm and 970cm -1 The absorption peaks of P-O-C are nearby, and the P-O-C are characteristic absorption peaks of the structure of the organophosphorus flame retardant, which indicates that the organophosphorus flame retardant copolyester is successfully prepared.
Example 2
The preparation method of the organophosphorus flame retardant copolyester comprises the following steps:
(1) Adding 1.5mol of terephthalaldehyde, 4.5mol of DOPO and 200ml of N, N-dimethylformamide into a reactor with a condensing reflux device, then introducing nitrogen, heating to 110 ℃, stirring for reaction for 7 hours, cooling, distilling under reduced pressure to remove the N, N-dimethylformamide, washing for 1-3 times by ethanol and deionized water in sequence, and vacuum drying at 75 ℃ for 11 hours to obtain a phosphorus-containing monomer A;
(2) 20g of terephthalic acid, 28.3g of ethylene glycol and 1.2g of phosphorus-containing monomer A are added into a reaction kettle, and a catalyst Sb is added 2 O 3 And (3) charging nitrogen until the pressure is 0.4MPa, heating to 215 ℃ for reaction for 3 hours, heating to 265 ℃ for reaction for 7 hours, and finally extruding the polyester after the reaction into water-cooled slices to obtain the organophosphorus flame-retardant copolyester.
Example 3
The preparation method of the organophosphorus flame retardant copolyester comprises the following steps:
(1) Adding 1.5mol of terephthalaldehyde, 7.5mol of DOPO and 300ml of N, N-dimethylformamide into a reactor with a condensing reflux device, then introducing nitrogen, heating to 120 ℃, stirring for reaction for 6 hours, cooling, distilling under reduced pressure to remove the N, N-dimethylformamide, washing for 1-3 times by ethanol and deionized water in sequence, and vacuum drying at 80 ℃ for 102 hours to obtain a phosphorus-containing monomer A;
(2) 15.2g of terephthalic acid, 21.3g of ethylene glycol and 0.8g of phosphorus-containing monomer A are added into a reaction kettle, and a catalyst Sb is added 2 O 3 And (3) charging nitrogen to the pressure of 0.5MPa, heating to 210 ℃ for reaction for 4 hours, heating to 260 ℃ for reaction for 8 hours, and finally extruding the polyester after the reaction to water-cooled slices to obtain the organophosphorus flame-retardant copolyester.
Example 4
The preparation of the phytic acid iron comprises the following steps:
A. 0.05mol of Fe (NO) 3 ) 3 ·9H 2 O is dissolved by 50ml of ionized water, 40ml of 2.5mol/L phytic acid aqueous solution is added, and the mixture is fully stirred to generate white floccules;
B. and regulating the pH value of the solution to be neutral by using a sodium hydroxide solution, transferring the solution into a hydrothermal kettle, reacting for 8 hours at the temperature of 85 ℃, and drying the solution at the temperature of 50 ℃ under vacuum after suction filtration to obtain the iron phytate.
The iron phytate powder prepared in example 4 was subjected to EDS analytical testing and the results are shown in table 1. As can be seen from Table 1, the content of P, fe element is 16.44% and 19.47%, respectively, indicating that the phytic acid ligand and Fe in the phytic acid iron 3+ The coordination is successful.
TABLE 1 results of the iron phytate EDS test
| Element type | Element mass fraction (%) |
| C | 11.36 |
| O | 43.18 |
| P | 16.44 |
| Fe | 19.47 |
| Na | 9.55 |
Example 5
The preparation of the phytic acid iron comprises the following steps:
B. 0.1mol of Fe (NO) 3 ) 3 ·9H 2 O is dissolved by 100ml of ionized water, and 80ml of 2.5mol/L phytic acid aqueous solution is added and fully stirred to generate white floccule;
B. and regulating the pH value of the solution to be neutral by using a sodium hydroxide solution, transferring the solution into a hydrothermal kettle, reacting for 10 hours at 70 ℃, and vacuum-drying at 45 ℃ after suction filtration to obtain the iron phytate.
Example 6
The preparation of the phytic acid iron comprises the following steps:
C. 0.08mol of Fe (NO) 3 ) 3 ·9H 2 O is dissolved by 50ml of ionized water, 60ml of 2.5mol/L phytic acid aqueous solution is added, and the mixture is fully stirred to generate white floccules;
B. and regulating the pH value of the solution to be neutral by using a sodium hydroxide solution, transferring the solution into a hydrothermal kettle, reacting for 12 hours at the temperature of 75 ℃, and vacuum-drying at the temperature of 40 ℃ after suction filtration to obtain the iron phytate.
Example 7
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70 parts of PET, 40 parts of modified PET, 0.5 part of aluminum hydroxide, 0.5 part of melamine, 0.5 part of bio-based flame retardant and 0.1 part of silane coupling agent, wherein the modified PET is the organophosphorus flame retardant copolyester prepared in example 1, and the bio-based flame retardant is the iron phytate prepared in example 4.
The production process of the flame-retardant polyester fabric comprises the following steps:
s1, uniformly mixing all the raw materials of the flame-retardant polyester fabric, adding the mixture into an internal mixer, regulating the temperature to 260 ℃, carrying out internal mixing for 10min, extruding, water-cooling, slicing, and drying to obtain polyester slices;
s2, placing the polyester chips in a screw, then carrying out melt extrusion on the polyester chips through a screw melt extrusion process, carrying out extrusion spinning at the temperature of 280 ℃, and then cooling, oiling and winding the spinning to obtain the polyester POY fiber, wherein the cooling temperature is 30 ℃, the oiling rate is 0.42wt%, and the winding speed is 3200m/min;
s3, sequentially carrying out processes of opening and picking, cotton carding, first drawing, second drawing, roving, spinning, winding and shaping on the polyester POY fibers to obtain polyester yarns;
s4, taking the polyester yarns prepared in the step S3 as warp yarns and weft yarns respectively, wherein the warp yarns are 50/600F polyester yarns, and the weft yarns are 100D/600F polyester yarns, and weaving the polyester yarns through interweaving to obtain the flame-retardant polyester fabric.
Example 8
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 75 parts of PET, 38 parts of modified PET, 1 part of aluminum hydroxide, 1 part of melamine, 1 part of bio-based flame retardant and 0.08 part of silane coupling agent, wherein the modified PET is the organophosphorus flame retardant copolyester prepared in example 1, and the bio-based flame retardant is the iron phytate prepared in example 4.
The production process of the flame-retardant polyester fabric comprises the following steps:
s1, uniformly mixing all the raw materials of the flame-retardant polyester fabric, adding the mixture into an internal mixer, regulating the temperature to 265 ℃, carrying out internal mixing for 8min, extruding, water-cooling, slicing, and drying to obtain polyester slices;
s2, placing the polyester chips into a screw, then carrying out melt extrusion on the polyester chips through a screw melt extrusion process, carrying out extrusion spinning at the temperature of 285 ℃, and then cooling, oiling and winding the spinning to obtain the polyester POY fiber, wherein the cooling temperature is 25 ℃, the oiling rate is 1.12wt%, and the winding speed is 2950m/min;
s3, sequentially carrying out processes of opening and picking, cotton carding, first drawing, second drawing, roving, spinning, winding and shaping on the polyester POY fibers to obtain polyester yarns;
s4, respectively taking the polyester yarns prepared in the step S3 as warp yarns and weft yarns, wherein the warp yarns are 100D/350F polyester yarns, and the weft yarns are 500D/350F polyester yarns, and weaving the polyester yarns through interweaving to obtain the flame-retardant polyester fabric.
Example 9
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 80 parts of PET, 35 parts of modified PET, 1.5 parts of aluminum hydroxide, 1.5 parts of melamine, 1.5 parts of bio-based flame retardant and 0.05 part of silane coupling agent, wherein the modified PET is the organophosphorus flame retardant copolyester prepared in example 1, and the bio-based flame retardant is the iron phytate prepared in example 4.
The production process of the flame-retardant polyester fabric comprises the following steps:
s1, uniformly mixing all the raw materials of the flame-retardant polyester fabric, adding the mixture into an internal mixer, regulating the temperature to 270 ℃, carrying out internal mixing for 5min, extruding, water-cooling, slicing, and drying to obtain polyester slices;
s2, placing the polyester chips in a screw, then carrying out melt extrusion on the polyester chips through a screw melt extrusion process, carrying out extrusion spinning at the temperature of 295 ℃, and then cooling, oiling and winding the spinning to obtain the polyester POY fiber, wherein the cooling temperature is 20 ℃, the oiling rate is 1.5wt%, and the winding speed is 2700m/min;
s3, sequentially carrying out processes of opening and picking, cotton carding, first drawing, second drawing, roving, spinning, winding and shaping on the polyester POY fibers to obtain polyester yarns;
s4, taking the polyester yarns prepared in the step S3 as warp yarns and weft yarns respectively, wherein the warp yarns are the polyester yarns with the density of 150D/50F, and the weft yarns are the polyester yarns with the density of 800D/50F, and weaving the polyester yarns through interweaving to obtain the flame-retardant polyester fabric.
Comparative example 1
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70 parts of PET, 0.5 part of aluminum hydroxide, 0.5 part of melamine, 0.5 part of bio-based flame retardant and 0.1 part of silane coupling agent, wherein the bio-based flame retardant is the iron phytate prepared in example 4.
The production process of the flame-retardant polyester fabric is the same as that of example 7
Comparative example 2
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70 parts of PET, 40 parts of modified PET, 0.5 part of aluminum hydroxide, 0.5 part of melamine and 0.1 part of silane coupling agent, wherein the modified PET is the organophosphorus flame retardant copolyester prepared in example 1.
The production process of the flame-retardant polyester fabric is the same as that of example 7
Comparative example 3
The flame-retardant polyester fabric comprises the following raw materials in parts by weight: 70 parts of PET, 0.5 part of aluminum hydroxide, 0.5 part of melamine and 0.1 part of silane coupling agent.
The production process of the flame-retardant polyester fabric is the same as that of example 7
Performance detection
The flame retardant properties of the flame retardant polyester fabrics prepared in examples 7 to 9 and comparative examples 1 to 3 were tested according to the standard GB/T5455-2014, the flame retardant polyester fabrics were fixed on a vertical burning tester, and after a certain time, the damage length, smoldering time and continuous burning time of the flame retardant polyester fabrics in the vertical direction were measured to obtain the data shown in Table 2 below.
Table 2 flame retardant polyester fabric flame retardant property test
As can be seen from the data in Table 2, the flame retardant properties of the flame retardant polyester fabrics in examples 7 to 9 and comparative example 2 are obviously superior to those of comparative examples 1 and 3, and the difference is that the flame retardant polyester fabrics in examples 7 to 9 and comparative example 2 both adopt the organophosphorus flame retardant copolyester prepared by the invention, which shows that the organophosphorus flame retardant copolyester of the invention has good flame retardant effect, and in addition, the flame retardant effect of comparative example 1 is slightly higher than that of comparative example 3, and the flame retardant effect is higher than that of pure aluminum hydroxide and melamine due to the compounding of the added phytic acid with aluminum hydroxide and melamine.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (10)
1. The flame-retardant polyester fabric is characterized by comprising the following raw materials in parts by weight: 70-80 parts of PET, 35-40 parts of modified PET, 1.5-5 parts of composite flame retardant and 0.05-0.1 part of silane coupling agent, wherein the modified PET is organophosphorus flame retardant copolyester, and has the following structural formula:
2. the flame retardant polyester fabric of claim 1, wherein the preparation method of the organophosphorus flame retardant copolyester comprises the following steps:
(1) Adding terephthalaldehyde, DOPO and N, N-dimethylformamide into a reactor with a condensing reflux device, then introducing nitrogen, heating to 100-120 ℃, stirring for reaction for 6-8 hours, cooling, distilling under reduced pressure to remove N, N-dimethylformamide, washing for 1-3 times sequentially by ethanol and deionized water, and vacuum drying for 10-12 hours at 70-80 ℃ to obtain a phosphorus-containing monomer A, wherein the structural formula is as follows:
(2) Terephthalic acid, ethylene glycol and phosphorus-containing monomer A, sb 2 O 3 Adding nitrogen into a reaction kettle, charging nitrogen until the pressure is 0.3-0.5 MPa, heating to 210-220 ℃ for reaction for 2-4 h, heating to 260-270 ℃ for reaction for 6-8 h, and finally extruding and water-cooling the reacted polyester to obtain the organophosphorus flame-retardant copolyester.
3. The flame retardant polyester fabric according to claim 1, wherein the molar ratio of terephthalaldehyde to DOPO in the step (1) is 1:3 to 5.
4. The flame retardant polyester fabric according to claim 1, wherein the mass ratio of terephthalic acid, ethylene glycol and phosphorus-containing monomer A in the step (2) is 10:14:0.5.
5. the flame-retardant polyester fabric according to claim 1, wherein the composite flame retardant comprises aluminum hydroxide, melamine and a bio-based flame retardant according to a mass ratio of 1:2:2 mixing.
6. The flame retardant polyester fabric according to claim 5, wherein the bio-based flame retardant is iron phytate, and the preparation method of the iron phytate comprises the following steps:
A. fe (NO) 3 ) 3 ·9H 2 O is dissolved by ionized water, and then a certain volume of phytic acid aqueous solution is added and fully stirred to generate white floccules;
B. and regulating the pH value of the solution to be neutral by using a sodium hydroxide solution, transferring the solution into a hydrothermal kettle, reacting for 8-12 hours at 75-85 ℃, and vacuum drying at 40-50 ℃ after suction filtration to obtain the phytic acid iron.
7. The flame retardant polyester fabric according to claim 6, wherein the phytic acid and Fe (NO 3 ) 3 ·9H 2 The molar ratio of O is 2:1.
8. the production process of the flame retardant polyester fabric according to any one of claims 1 to 7, which is characterized by comprising the following steps:
s1, uniformly mixing all the raw materials of the flame-retardant polyester fabric, adding the mixture into an internal mixer, regulating the temperature to 260-270 ℃, banburying for 5-10 min, extruding, water-cooling, slicing, and drying to obtain polyester slices;
s2, placing the polyester chips into a screw, then carrying out melt extrusion on the polyester chips through a screw melt extrusion process, carrying out extrusion spinning at the temperature of 280-295 ℃, and then cooling, oiling and winding the spinning to obtain polyester POY fibers;
s3, sequentially carrying out processes of opening and picking, cotton carding, first drawing, second drawing, roving, spinning, winding and shaping on the polyester POY fibers to obtain polyester yarns;
s4, respectively taking the polyester yarns prepared in the step S3 as warp yarns and weft yarns, and weaving by interweaving to obtain the flame-retardant polyester fabric.
9. The process for producing flame-retardant polyester fabric according to claim 8, wherein the cooling temperature in the step S2 is 20-30 ℃, the oiling rate is 0.42-1.5 wt%, and the winding speed is 2700-3200 m/min.
10. The process for producing flame-retardant polyester fabric according to claim 8, wherein the warp is polyester yarn with 50-150D/30-600F and the weft is polyester yarn with 100-800D/30-600F.
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