CN115074853B - Flame-retardant polypropylene fabric and preparation method thereof - Google Patents

Flame-retardant polypropylene fabric and preparation method thereof Download PDF

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Publication number
CN115074853B
CN115074853B CN202210728244.6A CN202210728244A CN115074853B CN 115074853 B CN115074853 B CN 115074853B CN 202210728244 A CN202210728244 A CN 202210728244A CN 115074853 B CN115074853 B CN 115074853B
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flame
retardant
polypropylene
reaction
fabric
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CN115074853A (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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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, and is characterized in that the fabric can be prepared by the following method: firstly, melamine reacts with formaldehyde to prepare a reaction solution; then, reacting the reaction solution with dimethyl phosphate to prepare the nitrogen and phosphorus containing flame retardant; blending the nitrogen and phosphorus containing flame retardant with polypropylene particles, and spinning to obtain polypropylene fiber; and finally spinning and weaving the polypropylene fiber to obtain the flame-retardant polypropylene fabric. The initial limiting oxygen index of the flame-retardant polyester fabric prepared by the method reaches more than 34%, and the flame-retardant polyester fabric belongs to the flame-retardant material range; after 10 times of water washing, the limiting oxygen index is not obviously reduced, and still reaches more than 31 percent. The flame-retardant polypropylene fabric prepared by the method has strong flame retardance, and has the advantages of simple whole production process, low price and small 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 ignition of textiles or the spread of fire due to the lack of flame retardant properties of textiles is also increasing. Therefore, the flame retardant performance and the safety of the textile are emphasized, and the flame retardant fabric has very important practical significance for reducing the hazard of fire.
The polypropylene fabric is made of polypropylene fibers, the polypropylene fibers are named as polypropylene fibers, the raw material sources are rich, the production process is simple, and the product price is relatively lower than that of other synthetic fibers. The polypropylene fiber has light texture, high strength, good heat retention, strong wicking capability, obvious moisture absorption and sweat release effects and good chemical corrosion resistance. Therefore, the polypropylene fabric has wide application range, can be used for manufacturing various clothes by pure spinning or blended spinning with wool, cotton or viscose fiber and the like, and can also be used as carpets, fishing nets, canvases, hose belts, concrete reinforcing materials, industrial fabrics, non-woven fabrics and the like. However, polypropylene fibers belong to inflammable fibers, have a Limiting Oxygen Index (LOI) of only about 18%, emit petroleum smell after burning, cannot meet the requirements of some fields on flame retardance, are very necessary to be flame-retarded, and have important practical significance and wide application prospects.
The literature research shows that the flame retardant property of polypropylene fabrics is widely concerned, such as: the Chinese patent application No. 201210211082.5 discloses a preparation method of halogen-free flame-retardant polypropylene bulked filaments, which is prepared by the following steps: mixing polypropylene slices with flame-retardant particles in proportion, spinning by a BCF spinning machine set, and obtaining halogen-free flame-retardant polypropylene bulked filaments by adopting the same spinning process as that of conventional polypropylene bulked filaments; the flame-retardant particles are prepared by premixing polypropylene slices, a composite halogen-free flame retardant and a solubilizing dispersant by a high-speed mixer, adding the premixed polypropylene slices, the composite halogen-free flame retardant and the solubilizing dispersant into a double-screw extruder, and carrying out melt mixing by the double-screw extruder. The preparation method effectively solves the environmental protection problem of a large amount of corrosive hydrogen halide gas and other toxic halides 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 gradually weakens along with the increase of the washing times of the polypropylene fabric. Therefore, developing an economic and safe flame-retardant finishing technology, and endowing the polypropylene fabric with excellent flame-retardant performance is a constantly pursuing target of researchers.
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 steps: firstly, melamine reacts with formaldehyde to prepare a reaction solution; then, reacting the reaction solution with dimethyl phosphate to prepare the nitrogen and phosphorus containing flame retardant; blending the nitrogen and phosphorus containing flame retardant with polypropylene particles, and spinning to obtain polypropylene fiber; and finally spinning and weaving the polypropylene fiber to obtain the flame-retardant polypropylene fabric.
The invention further aims at providing a preparation method of the flame-retardant polypropylene fabric, which comprises the following steps:
(1) Melamine with formaldehyde: adding melamine and formaldehyde aqueous solution into dimethylformamide solution, stirring and reacting, setting the reaction temperature to be 110-120 ℃, and reacting for the following time: the reaction solution is prepared after 24 to 26 hours.
Preferably, the usage ratio of melamine (g), dimethylformamide (mL) and formaldehyde aqueous solution (mL) is: 1:10-20:1-2.
Preferably, the formaldehyde aqueous solution comprises the following components in percentage by mass: 10-20%.
(2) Reaction with dimethyl phosphate: adding dimethyl phosphate into the reaction liquid prepared in the step (1), adding triethylamine, stirring for reaction, regulating the reaction temperature to be 110-120 ℃, and controlling the reaction time to be: and (3) after the reaction is finished for 24 to 26 hours, adding the reaction solution into petroleum ether solvent, stirring and mixing, standing until the reaction solution is layered, taking upper petroleum ether, distilling under reduced pressure, and drying to obtain the nitrogen and phosphorus-containing flame retardant.
Preferably, the ratio of the amount of the reaction solution (mL), the amount of the dimethyl phosphate (mL) and the amount of the triethylamine (mL) prepared in the step (1) is: 1:0.1-0.2:0.1-0.2.
Preferably, the ratio of the amount of the reaction solution (mL) to 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 spinning to prepare the polypropylene fiber.
Preferably, the blending temperature is: 150-180 ℃.
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 a 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 and 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 surprisingly discovers that the initial limiting oxygen index of the flame-retardant polypropylene fabric prepared by the application reaches more than 34 percent, and the flame-retardant polypropylene fabric belongs to the flame-retardant material range; after 10 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 31 percent; in addition, after 10 times of water washing, the flame retardant property of the flame retardant polypropylene fabric prepared by the method exceeds the flame retardant property of the purchased flame retardant polypropylene fabric.
(3) The compound containing nitrogen and phosphorus has good flame retardant effect, and the melamine and the dimethyl phosphate react to prepare the flame retardant containing nitrogen and phosphorus. The inventor of the present application surprisingly found that the nitrogen-phosphorus-containing flame retardant has good compatibility with polypropylene particles, and can achieve uniform mixing of the two; it was further found that: the flame retardant property of the polypropylene fabric is not weakened after the polypropylene fabric is washed by water for many times.
(4) The flame-retardant polypropylene fabric prepared by the method has strong flame retardance, and has the advantages of simple whole production process, low price and small environmental pollution in the production process.
Detailed Description
The examples and comparative examples described below illustrate the invention in detail.
Example 1
The preparation method of the flame-retardant polypropylene fabric comprises the following steps:
(1) Melamine with formaldehyde: to 15mL of dimethylformamide solution, 1g of melamine and 1.5mL of 15wt% aqueous formaldehyde solution were added, and the reaction was stirred and carried out at 115℃for a period of time: the reaction solution was prepared for 25 hours.
(2) Reaction with dimethyl phosphate: adding 1.5mL of dimethyl phosphate into 10mL of the reaction solution prepared in the step (1), adding 1.5mL of triethylamine, stirring for reaction, regulating the reaction temperature to 115 ℃, and reacting for the following time: and (3) after the reaction is finished for 25 hours, adding the reaction solution into petroleum ether solvent with 15 times of volume, stirring and mixing, standing until the reaction solution is layered, taking upper petroleum ether, distilling under reduced pressure, and drying to obtain the nitrogen and 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 spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen and phosphorus containing flame retardant to the polypropylene particles is as follows: 1:150.
(4) Preparing a 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) Melamine with formaldehyde: to 10mL of dimethylformamide solution, 1g of melamine and 1mL of 10wt% aqueous formaldehyde solution were added, and the reaction was stirred and carried out at 110℃for a period of time: 24 hours, a reaction solution was obtained.
(2) Reaction with dimethyl phosphate: adding 1mL of dimethyl phosphate into 10mL of the reaction solution prepared in the step (1), adding triethylamine, stirring for reaction, regulating the reaction temperature to 110 ℃, and controlling the reaction time to be: and (3) after the reaction is finished for 24 hours, adding the reaction solution into petroleum ether solvent with the volume of 10 times, stirring and mixing, standing until the reaction solution is layered, taking upper petroleum ether, distilling under reduced pressure, and drying to obtain the nitrogen and 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 spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen and phosphorus containing flame retardant to the polypropylene particles is as follows: 1:100.
(4) Preparing a 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) Melamine with formaldehyde: to 20mL of dimethylformamide solution, 1g of melamine and 1mL of 20wt% aqueous formaldehyde solution were added, and the reaction was stirred and carried out at 120℃for a period of time: the reaction solution was obtained after 26 hours.
(2) Reaction with dimethyl phosphate: adding 2mL of dimethyl phosphate into 10mL of the reaction solution prepared in the step (1), adding 2mL of triethylamine, stirring for reaction, regulating the reaction temperature to 120 ℃, and controlling the reaction time to be: and (2) after the reaction is finished for 26 hours, adding the reaction solution into petroleum ether solvent with the volume of 20 times, stirring and mixing, standing until the reaction solution is layered, taking upper petroleum ether, distilling under reduced pressure, and drying to obtain the nitrogen and 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 spinning to prepare polypropylene fibers; the dosage ratio of the nitrogen and phosphorus containing flame retardant to the polypropylene particles is as follows: 1:200.
(4) Preparing a 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, by way of comparison with example 1, the "1g melamine" in step (1) was reduced to "0.1g melamine", and the other preparation methods were carried out in accordance with the preparation method of example 1.
Comparative example B
In this comparative example, with reference to example 1, the "1.5mL of dimethyl phosphate" in step (2) was reduced to "0.15mL of dimethyl phosphate", and the other production methods were carried out in accordance with the production method of example 1.
Comparative example C
In this comparative example, with example 1 as a comparison, the "amount ratio of the nitrogen-phosphorus-containing flame retardant to the polypropylene particles in step (3) was: 1:150 'is changed into' the dosage ratio of the nitrogen-phosphorus-containing flame retardant to the polypropylene particles is: 0.1:150 ", the other preparation methods being carried out as in example 1.
Performance evaluation example:
In order to better detect the flame retardance of the polypropylene fabrics prepared in the invention, the polypropylene fabrics prepared in the specific examples 1-3 and the comparative examples A-C and the purchased flame-retardant polypropylene fabrics are tested for flame retardance, and the test method adopts an oxygen index test method, namely, the standard washing of the polypropylene fabrics is carried out according to GB/T5454-1997 oxygen index method for textile combustion performance test and referring to a washing method of a GB/T20944.1-2007 washing fastness tester. The test results are shown in Table 1.
Table 1 flame retardant test results of the polypropylene fabrics and the purchased polypropylene fabrics prepared in examples 1 to 3 and comparative examples a to C after not being washed with water and washed with water for 10 times
The limiting oxygen index LOI is one of important indexes of flame retardant materials, and materials with the limiting oxygen index higher than 28% are flame retardant materials. As can be seen from Table 1, the initial limiting oxygen index of the flame-retardant polypropylene fabric prepared by the application reaches more than 34%, and the flame-retardant polypropylene fabric belongs to the flame-retardant material range; 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 method exceeds the flame retardant property of the purchased flame retardant polypropylene fabric. In addition, the inventors of the present application further found that the polypropylene fabrics prepared in comparative examples a to C were smaller in limiting oxygen index, indicating that: the amount of melamine, the amount of dimethyl phosphate and the ratio of the nitrogen-phosphorus-containing flame retardant to the polypropylene particles have important influence on the flame retardant property of the polypropylene fabric. The flame retardant property experiment test shows that: the flame-retardant polypropylene fabric prepared by the method has good flame-retardant effect, and is a qualified flame-retardant polypropylene fabric.

Claims (4)

1. The preparation method of the flame-retardant polypropylene fabric is characterized by comprising the following steps of:
(1) Blending: blending the nitrogen and phosphorus containing flame retardant with polypropylene particles at a certain temperature, and spinning to obtain polypropylene fibers;
(2) Preparing a fabric: spinning and weaving the polypropylene fiber prepared in the step (1) to prepare flame-retardant polypropylene fabric; wherein the initial limiting oxygen index of the flame-retardant polypropylene fabric is higher than 34%, and the limiting oxygen index of the flame-retardant polypropylene fabric is higher than 31% after 10 times of water washing;
The preparation method of the nitrogen and phosphorus containing flame retardant comprises the following steps: adding dimethyl phosphate into the reaction solution 1, adding triethylamine, stirring for reaction, regulating the reaction temperature to be 110-120 ℃ and the reaction time to be 24-26 hours, adding the reaction solution 2 into 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 and phosphorus-containing flame retardant;
The preparation method of the reaction liquid 1 comprises the following steps: adding melamine and formaldehyde aqueous solution into dimethylformamide solution, stirring and reacting, setting the reaction temperature to be 110-120 ℃ and the reaction time to be 24-26 hours, and preparing reaction solution 1;
The dosage ratio of the melamine to the dimethylformamide to the formaldehyde aqueous solution is 1g to (10-20) mL to (1-2) mL; the mass fraction of the formaldehyde aqueous solution is 10-20%.
2. The method for preparing the flame retardant polypropylene fabric according to claim 1, wherein the blending temperature is 150-180 ℃; the dosage ratio of the nitrogen and phosphorus containing flame retardant to the polypropylene particles is 1g to (100-200 g).
3. The preparation method of the flame-retardant polypropylene fabric according to claim 2, wherein the dosage ratio of the reaction solution 1 to the dimethyl phosphate to the triethylamine is 1mL to (0.1-0.2) mL; the dosage ratio of the reaction liquid 2 to the petroleum ether solvent is 1mL to (10-20 mL).
4. A flame retardant polypropylene fabric, characterized in that the flame retardant polypropylene fabric is prepared by the preparation method of any one of claims 1-3.
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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