CN115074853A - Flame-retardant polypropylene fabric and preparation method thereof - Google Patents

Flame-retardant polypropylene fabric and preparation method thereof Download PDF

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CN115074853A
CN115074853A CN202210728244.6A CN202210728244A CN115074853A CN 115074853 A CN115074853 A CN 115074853A CN 202210728244 A CN202210728244 A CN 202210728244A CN 115074853 A CN115074853 A CN 115074853A
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flame
retardant
polypropylene
preparation
reaction
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CN115074853B (en
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蔡亚君
卜凡童
陈旭
周凡雨
周建刚
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Wuhan Textile University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a flame-retardant polypropylene fabric and a preparation method thereof, which is characterized in that the fabric can be prepared by the following method: firstly, reacting melamine with formaldehyde to prepare a reaction solution; then, reacting the reaction liquid with dimethyl phosphate to prepare the nitrogen-phosphorus-containing flame retardant; blending nitrogen and phosphorus containing flame retardant with polypropylene particles, and spinning to prepare polypropylene fiber; and finally, spinning and weaving the polypropylene fiber to obtain the flame-retardant polypropylene fabric. The initial limit oxygen index of the flame-retardant polyester fabric prepared by the invention reaches more than 34 percent, and belongs to the range of flame-retardant materials; after 10 times of water washing, the limiting oxygen index is not obviously reduced and still reaches over 31 percent. The flame-retardant polypropylene fabric prepared by the method has strong flame retardance, and is simple in whole production process, low in price and small in environmental pollution in the production process.

Description

Flame-retardant polypropylene fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of fabric preparation, and particularly relates to a flame-retardant polypropylene fabric and a preparation method thereof.
Background
With the development of science and technology and the progress of society, the application range of textiles is gradually expanded. Meanwhile, the number of fires caused by the fire of the textiles or the spread of the fire caused by the absence of the flame retardant property of the textiles is also gradually increasing. Therefore, the flame retardant property and the safety of the textile are emphasized, and the textile has very important practical significance for reducing the harm of fire.
The polypropylene fiber fabric is a fabric woven by polypropylene fibers, the polypropylene fibers are known as polypropylene fibers, the raw material sources are rich, the production process is simple, and the product price is lower than that of other synthetic fibers. And the polypropylene fiber has light weight, high strength, good heat retention, strong wicking capability, obvious moisture absorption and sweat releasing effects and better chemical corrosion resistance. Therefore, the polypropylene fiber fabric has wide application range, can be used for manufacturing various clothes by pure spinning or blended and mixed weaving with wool, cotton or viscose fiber and the like, and can also be used as carpet, fishing net, canvas, hose, concrete reinforcing material, industrial fabric and non-woven fabric and the like. However, polypropylene fiber belongs to flammable fiber, the Limiting Oxygen Index (LOI) of the polypropylene fiber is only about 18%, petroleum smell can be emitted after combustion, the requirement of some fields on flame retardant performance cannot be met, the polypropylene fiber is very necessary to be subjected to flame retardance, and the polypropylene fiber has important practical significance and wide application prospect.
The research and study of the literature show that the flame retardant performance of the polypropylene fabric is concerned widely, such as: the Chinese patent application number 201210211082.5 discloses a preparation method of a halogen-free flame-retardant polypropylene bulked filament, which is prepared by the following steps: mixing the polypropylene chips and the flame-retardant particles in proportion, spinning by a BCF spinning unit, and obtaining the halogen-free flame-retardant polypropylene bulked filament by adopting the same spinning process as the conventional polypropylene bulked filament; the flame-retardant particles are prepared by premixing polypropylene slices, the composite halogen-free flame retardant and the solubilizing dispersant by a high-speed mixer, adding the premixed materials into a double-screw extruder, and then carrying out melting and mixing by the double-screw extruder. The preparation method effectively solves the environmental protection problem that a large amount of corrosive hydrogen halide gas and other toxic halides exist in the combustion process of the halogen-containing flame retardant; however, the method has relatively complex raw materials and complicated steps, and the flame retardant effect is gradually weakened along with the increase of the washing times of the polypropylene fabric. Therefore, the development of an economic and safe flame-retardant finishing technology is a constantly pursued goal of researchers to endow polypropylene fabrics with excellent flame-retardant performance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a flame-retardant polypropylene fabric and a preparation method thereof.
The invention aims to provide a flame-retardant polypropylene fabric, which can be prepared by the following method: firstly, reacting melamine with formaldehyde to prepare a reaction solution; then, reacting the reaction liquid with dimethyl phosphate to prepare the nitrogen-phosphorus-containing flame retardant; blending nitrogen and phosphorus containing flame retardant with polypropylene particles, and spinning to prepare polypropylene fiber; and finally, spinning and weaving the polypropylene fiber to obtain the flame-retardant polypropylene fabric.
The invention also aims to provide a preparation method of the flame-retardant polypropylene fabric, which comprises the following steps:
(1) reaction of melamine with formaldehyde: adding melamine and formaldehyde aqueous solution into dimethylformamide solution, stirring and reacting, wherein the reaction temperature is set to be 110-120 ℃, and the reaction time is as follows: and (3) preparing a reaction solution after 24-26 hours.
Preferably, the melamine (g), the dimethylformamide (mL) and the aqueous formaldehyde solution (mL) are used in the following ratio: 1: 10-20: 1-2.
Preferably, the mass fraction of the formaldehyde aqueous solution is: 10 to 20 percent.
(2) Reaction with dimethyl phosphate: adding dimethyl phosphate and triethylamine into the reaction solution prepared in the step (1), stirring and reacting, regulating and controlling the reaction temperature to be 110-120 ℃, and controlling the reaction time to be: and (3) after 24-26 hours, adding the reaction liquid into a petroleum ether solvent after the reaction is finished, stirring and mixing, standing for layering, taking petroleum ether on the upper layer, distilling under reduced pressure, and drying to obtain the nitrogen and phosphorus containing flame retardant.
Preferably, the reaction solution (mL), dimethyl phosphate (mL) and triethylamine (mL) prepared in step (1) are used in the following ratio: 1: 0.1-0.2.
Preferably, the ratio of the amount of the reaction solution (mL) to the amount of the petroleum ether solvent (mL) is: 1: 10-20.
(3) Blending: and (3) blending the nitrogen and phosphorus containing flame retardant prepared in the step (2) with polypropylene particles at a certain temperature, and then spinning to prepare the polypropylene fiber.
Preferably, the blending temperature is: 150 to 180 ℃.
Preferably, the dosage ratio of the nitrogen-phosphorus containing flame retardant (g) to the polypropylene particles (g) is as follows: 1: 100-200.
(4) Preparing the fabric: spinning and weaving the polypropylene fiber prepared in the step (3) to prepare the flame-retardant polypropylene fabric.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention realizes the blending of the nitrogen-phosphorus-containing flame retardant and the polypropylene particles, and the method obviously improves the flame retardant property of the polypropylene fabric.
(2) The inventor of the application unexpectedly finds that the initial limit oxygen index of the flame-retardant polypropylene fabric prepared by the invention reaches more than 34 percent, and the flame-retardant polypropylene fabric belongs to the range of flame-retardant materials; after 10 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 31 percent; in addition, after the polypropylene fiber fabric is washed by water for 10 times, the flame retardant property of the flame retardant polypropylene fiber fabric prepared by the invention exceeds that of the purchased flame retardant polypropylene fiber fabric.
(3) The compound containing nitrogen and phosphorus elements has good flame retardant effect, and the flame retardant containing nitrogen and phosphorus is prepared by reacting melamine with dimethyl phosphate. The inventor of the application unexpectedly finds that the nitrogen-phosphorus-containing flame retardant has good compatibility with polypropylene particles, and can realize uniform mixing of the nitrogen-phosphorus-containing flame retardant and the polypropylene particles; further found that: after the polypropylene fiber fabric is washed by water for many times, the flame retardant property of the polypropylene fiber fabric is not weakened.
(4) The flame-retardant polypropylene fabric prepared by the method has strong flame retardance, and is simple in whole production process, low in price and small in environmental pollution in the production process.
Detailed Description
The following examples and comparative examples illustrate the present invention in detail.
Example 1
The preparation method of the flame-retardant polypropylene fabric comprises the following steps:
(1) reaction of melamine with formaldehyde: 1g of melamine and 1.5mL of a 15 wt% aqueous formaldehyde solution were added to 15mL of a dimethylformamide solution, and the mixture was stirred to react at 115 ℃ for the following reaction time: after 25 hours, a reaction solution was obtained.
(2) Reaction with dimethyl phosphate: adding 1.5mL of dimethyl phosphate into 10mL of reaction liquid prepared in the step (1), adding 1.5mL of triethylamine, stirring for reaction, regulating and controlling the reaction temperature to be 115 ℃, and controlling the reaction time to be: and (3) after 25 hours, adding the reaction solution into 15 times of petroleum ether solvent after the reaction is finished, stirring and mixing, standing for layering, taking petroleum ether on the upper layer, distilling under reduced pressure, and drying to obtain the nitrogen-phosphorus-containing flame retardant.
(3) Blending: blending the nitrogen and phosphorus-containing flame retardant prepared in the step (2) with polypropylene particles at 160 ℃, and then spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen-phosphorus containing flame retardant to the polypropylene particles is as follows: 1: 150.
(4) Preparing the fabric: spinning and weaving the polypropylene fiber prepared in the step (3) to prepare the flame-retardant polypropylene fabric.
Example 2
The preparation method of the flame-retardant polypropylene fabric comprises the following steps:
(1) reaction of melamine with formaldehyde: adding 1g of melamine and 1mL of 10 wt% aqueous formaldehyde solution into 10mL of dimethylformamide solution, stirring and reacting, wherein the reaction temperature is set to be 110 ℃, and the reaction time is as follows: after 24 hours, a reaction solution was obtained.
(2) Reaction with dimethyl phosphate: adding 1mL of dimethyl phosphate into 10mL of reaction liquid prepared in the step (1), adding triethylamine, stirring for reaction, regulating and controlling the reaction temperature to be 110 ℃, and controlling the reaction time to be: and (3) after 24 hours, adding the reaction solution into a petroleum ether solvent with the volume of 10 times of that of the reaction solution, stirring and mixing, standing for layering, taking petroleum ether on the upper layer, distilling under reduced pressure, and drying to obtain the nitrogen-phosphorus-containing flame retardant.
(3) Blending: blending the nitrogen and phosphorus containing flame retardant prepared in the step (2) with polypropylene particles at 150 ℃, and then spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen-phosphorus containing flame retardant to the polypropylene particles is as follows: 1: 100.
(4) Preparing the fabric: spinning and weaving the polypropylene fiber prepared in the step (3) to prepare the flame-retardant polypropylene fabric.
Example 3
The preparation method of the flame-retardant polypropylene fabric comprises the following steps:
(1) reaction of melamine with formaldehyde: adding 1g of melamine and 1mL of 20 wt% aqueous formaldehyde solution into 20mL of dimethylformamide solution, stirring and reacting, wherein the reaction temperature is set to be 120 ℃, and the reaction time is as follows: after 26 hours, a reaction solution was obtained.
(2) Reaction with dimethyl phosphate: adding 2mL of dimethyl phosphate and 2mL of triethylamine into 10mL of the reaction solution prepared in the step (1), stirring for reaction, regulating and controlling the reaction temperature to be 120 ℃, and controlling the reaction time to be: and (3) after 26 hours, adding the reaction solution into a 20-time volume of petroleum ether solvent after the reaction is finished, stirring and mixing, standing for layering, taking petroleum ether at the upper layer, distilling under reduced pressure, and drying to obtain the nitrogen-phosphorus-containing flame retardant.
(3) Blending: blending the nitrogen and phosphorus containing flame retardant prepared in the step (2) with polypropylene particles at 180 ℃, and then spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen-phosphorus containing flame retardant to the polypropylene particles is as follows: 1: 200.
(4) Preparing the fabric: spinning and weaving the polypropylene fiber prepared in the step (3) to prepare the flame-retardant polypropylene fabric.
Comparative example A
In this comparative example, "1 g of melamine" in step (1) was reduced to "0.1 g of melamine" by way of comparison with example 1, and the other preparation process was carried out in accordance with the preparation process of example 1.
Comparative example B
In this comparative example, "1.5 mL of dimethyl phosphate" in step (2) was reduced to "0.15 mL of dimethyl phosphate" by way of comparison with example 1, and the other preparation method was carried out in the same manner as in example 1.
Comparative example C
In this comparative example, using example 1 as a comparison, the "ratio of the amount of the nitrogen-phosphorus-containing flame retardant to the amount of the polypropylene particles in step (3) was: 1: 150 "is changed into that the dosage ratio of the nitrogen-phosphorus-containing flame retardant to the polypropylene particles is as follows: 0.1: 150 ", the other preparation was carried out according to the preparation of example 1.
Performance evaluation examples:
in order to better detect the flame retardance of the polypropylene fabric prepared in the invention, the flame retardance of the polypropylene fabric prepared in the specific embodiments 1-3 and the comparative examples A-C in the invention and the flame retardant performance of the purchased flame retardant polypropylene fabric are tested, and the test method adopts an oxygen index test method, namely, the polypropylene fabric is subjected to standard washing according to GB/T5454-1997 textile combustion performance test oxygen index method, and reference GB/T20944.1-2007 washing fastness tester washing method. The test results are shown in table 1.
Table 1 flame retardant test results of polypropylene fabrics prepared in examples 1 to 3 and comparative examples a to C and polypropylene fabrics purchased without and after 10 times of water washing
Figure BDA0003711592030000051
The limiting oxygen index LOI is one of important indexes of flame-retardant materials, and materials with the limiting oxygen index of more than 28 percent are flame-retardant materials generally. As can be seen from Table 1, the initial limit oxygen index of the flame-retardant polypropylene fabric prepared by the invention reaches more than 34 percent, and the flame-retardant polypropylene fabric belongs to the range of flame-retardant materials; after 10 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 31 percent; in addition, the flame retardant property of the flame retardant polypropylene fabric prepared by the invention exceeds the flame retardant property of the purchased flame retardant polypropylene fabric. In addition, the inventors of the present application further found that the limiting oxygen index of the polypropylene face fabrics prepared in comparative examples a-C were all small, indicating that: the dosage of melamine, the dosage of dimethyl phosphate and the dosage ratio of the nitrogen-phosphorus containing flame retardant to the polypropylene particles all have important influence on the flame retardant property of the polypropylene fabric. The flame retardant property test shows that: the flame-retardant polypropylene fabric prepared by the invention has a good flame-retardant effect, and is a qualified flame-retardant polypropylene fabric.

Claims (7)

1. The preparation method of the flame-retardant polypropylene fabric is characterized by comprising the following steps of:
(1) blending: blending nitrogen and phosphorus containing flame retardant and polypropylene particles at a certain temperature, and then spinning to prepare polypropylene fiber;
(2) preparing the fabric: spinning and weaving the polypropylene fiber prepared in the step (1) to prepare the flame-retardant polypropylene fabric; the initial limit oxygen index of the flame-retardant polypropylene fabric is higher than 34%, and after 10 times of washing, the limit oxygen index is higher than 31%.
2. The preparation method of the flame-retardant polypropylene fiber fabric according to claim 1, wherein the blending temperature is 150-180 ℃; the dosage ratio of the nitrogen-phosphorus-containing flame retardant to the polypropylene particles is 1g to (100-200).
3. The preparation method of the flame-retardant polypropylene fiber fabric according to claim 1, wherein the preparation method of the nitrogen and phosphorus containing flame retardant comprises the following steps: adding dimethyl phosphate into the reaction liquid, adding triethylamine, stirring for reaction, regulating the reaction temperature to be 110-120 ℃, controlling the reaction time to be 24-26 hours, adding the reaction liquid into a petroleum ether solvent after the reaction is finished, stirring and mixing, standing for layering, taking upper petroleum ether, distilling under reduced pressure, and drying to obtain the nitrogen-phosphorus-containing flame retardant.
4. The preparation method of the flame-retardant polypropylene fabric according to claim 3, wherein the usage ratio of the reaction solution, the dimethyl phosphate and the triethylamine is 1mL to (0.1-0.2) mL; the dosage ratio of the reaction liquid to the petroleum ether solvent is 1mL to (10-20) mL.
5. The preparation method of the flame-retardant polypropylene fabric according to claim 3, wherein the preparation method of the reaction solution comprises the following steps: and adding melamine and formaldehyde aqueous solution into the dimethylformamide solution, stirring and reacting, wherein the reaction temperature is set to be 110-120 ℃, and the reaction time is set to be 24-26 hours, so as to prepare the reaction solution.
6. The preparation method of the flame-retardant polypropylene fiber fabric according to claim 5, wherein the amount ratio of the melamine to the aqueous solution of the dimethylformamide to the formaldehyde is 1g to (10-20) mL to (1-2) mL; the mass fraction of the formaldehyde aqueous solution is 10-20%.
7. A flame-retardant polypropylene fabric is characterized by being prepared by the preparation method of the flame-retardant polypropylene fabric according to any one of claims 1 to 6.
CN202210728244.6A 2022-06-24 2022-06-24 Flame-retardant polypropylene fabric and preparation method thereof Active CN115074853B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB790663A (en) * 1954-11-05 1958-02-12 Geigy Ag J R Improvements relating to compositions for flame-proofing cellulose containing material, their use, and material treated therewith
CN101974166A (en) * 2010-09-16 2011-02-16 中科院广州化学有限公司 Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof
CN102732985A (en) * 2012-06-26 2012-10-17 常州灵达特种纤维有限公司 Preparation method of halogen free flame retardation polypropylene bulked filament
CN105199096A (en) * 2015-11-11 2015-12-30 江苏钟山化工有限公司 Preparation and application of nitrogen and phosphorus structured flame-retardant polyether polyol
CN111041610A (en) * 2020-01-07 2020-04-21 郑州中科新兴产业技术研究院 Melamine/cellulose flame-retardant material and preparation method thereof
CN113046890A (en) * 2020-05-09 2021-06-29 苏州才豪电子科技有限公司 Flame-retardant fabric for automotive vehicle interior

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB790663A (en) * 1954-11-05 1958-02-12 Geigy Ag J R Improvements relating to compositions for flame-proofing cellulose containing material, their use, and material treated therewith
CN101974166A (en) * 2010-09-16 2011-02-16 中科院广州化学有限公司 Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof
CN102732985A (en) * 2012-06-26 2012-10-17 常州灵达特种纤维有限公司 Preparation method of halogen free flame retardation polypropylene bulked filament
CN105199096A (en) * 2015-11-11 2015-12-30 江苏钟山化工有限公司 Preparation and application of nitrogen and phosphorus structured flame-retardant polyether polyol
CN111041610A (en) * 2020-01-07 2020-04-21 郑州中科新兴产业技术研究院 Melamine/cellulose flame-retardant material and preparation method thereof
CN113046890A (en) * 2020-05-09 2021-06-29 苏州才豪电子科技有限公司 Flame-retardant fabric for automotive vehicle interior

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