CN112030550A - A kind of flame retardant, hydrophobic, oleophobic, ice-repellent finishing agent for fabric and preparation and application method thereof - Google Patents
A kind of flame retardant, hydrophobic, oleophobic, ice-repellent finishing agent for fabric and preparation and application method thereof Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 89
- 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 87
- 239000004744 fabric Substances 0.000 title claims abstract description 61
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 55
- 239000005871 repellent Substances 0.000 title claims abstract description 54
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 27
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 27
- 230000002940 repellent Effects 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000012948 isocyanate Substances 0.000 claims abstract description 11
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 10
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 9
- 239000011737 fluorine Substances 0.000 claims abstract description 9
- 239000002981 blocking agent Substances 0.000 claims abstract description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 125000001261 isocyanato group Chemical group *N=C=O 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000675 fabric finishing Substances 0.000 description 3
- 238000009962 finishing (textile) Methods 0.000 description 3
- -1 Phosphorus (phosphonate) ester Chemical class 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 206010019345 Heat stroke Diseases 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- TULILQAUNXZTQQ-UHFFFAOYSA-N N=C=O.O=C=NCCCCCCN=C=O Chemical compound N=C=O.O=C=NCCCCCCN=C=O TULILQAUNXZTQQ-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000008642 heat stress Effects 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/2246—Esters of unsaturated carboxylic acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
- D06M13/447—Phosphonates or phosphinates containing nitrogen atoms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
- D06M13/453—Phosphates or phosphites containing nitrogen atoms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明提供了一种织物用阻燃、疏水、疏油、疏冰整理剂及其制备和应用方法，该整理剂由包括如下重量份数的原料制备得到：水100份、防泼水剂2‑5份、交联剂0.5‑4份；其中，所述交联剂为由阻燃剂、多异氰酸酯和封端剂制备得到的封闭型阻燃多异氰酸酯。本发明通过具有低表面能特性的含氟防泼水剂的引入，赋予织物防泼水、疏油和疏冰的优异性能；同时，将阻燃剂与异氰酸酯反应制备封闭型阻燃多异氰酸酯，用于防泼水剂的交联剂，在提高织物阻燃性能的同时，提升了其耐水洗性能。本发明中整理剂处理后的织物将同时具备阻燃、疏水、疏油、疏冰、耐水洗等多种功能，可在消防员防护服装领域得到广泛应用，从而有效提升消防员的个人防护能力和救援效率。The invention provides a flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics and a preparation and application method thereof. The finishing agent is prepared from the following raw materials in parts by weight: 100 parts of water, and 2 parts of a water repellent agent. 5 parts, and 0.5-4 parts of a crosslinking agent; wherein, the crosslinking agent is a closed flame retardant polyisocyanate prepared from a flame retardant, a polyisocyanate and a blocking agent. The invention provides the fabric with excellent properties of water repellency, oleophobicity and ice repellency through the introduction of a fluorine-containing water repellent agent with low surface energy characteristics; at the same time, the flame retardant is reacted with an isocyanate to prepare a blocked flame retardant polyisocyanate, which is used for The cross-linking agent of the water repellent agent improves the fabric's flame retardant performance and also improves its washing resistance. The fabric treated with the finishing agent in the present invention will have various functions such as flame retardant, hydrophobic, oleophobic, ice-repellent, water-resistant, etc., and can be widely used in the field of firefighters' protective clothing, thereby effectively improving the personal protection ability of firefighters and rescue efficiency.
Description
技术领域technical field
本发明涉及织物整理技术领域，尤其是涉及一种织物用阻燃、疏水、疏油、疏冰整理剂及其制备和应用方法。The invention relates to the technical field of fabric finishing, in particular to a flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics and a preparation and application method thereof.
背景技术Background technique
在实际救援过程中，消防服极易受到水流冲击，如若被水渍沾污，消防服装整体重量会增加，从而增大消防员负荷，影响消防员的战斗力。在高温环境下，浸湿的消防服装还会加剧其厚重闷热的缺点，更易导致消防员发生中暑等热应激现象，威胁消防员生命安全；在低温环境下，消防服表面的水分将很快冻结成冰，冻结的消防服将大大影响消防员的行动，这不但会影响消防员的救援效率，也会危及消防员的生命安全。同时，消防服在实际使用过程中还会面临火焰灼烧和清洗后双疏性能变差的问题。因此，需对消防服的疏水、疏冰、阻燃、耐水洗等性能进行提升。织物整理剂是常用的解决这些问题的方法，整理剂处理后的织物由于拒水的特性很容易让水从其表面滚落，而难以迅速结冰。同时由于具有高度疏水特性，织物表面即便结冰，冰也很容易从表面脱落。In the actual rescue process, fire-fighting clothing is very vulnerable to the impact of water flow. If it is stained by water, the overall weight of the fire-fighting clothing will increase, thereby increasing the load of firefighters and affecting the combat effectiveness of firefighters. In a high temperature environment, the wet fire clothing will also aggravate its thick and sultry shortcomings, and it is more likely to cause firefighters to suffer from heat stress such as heatstroke, threatening the life safety of firefighters; in a low temperature environment, the surface of the fire clothing will quickly become wet. Frozen into ice, the frozen fire suit will greatly affect the action of firefighters, which will not only affect the rescue efficiency of firefighters, but also endanger the lives of firefighters. At the same time, fire-fighting clothing will also face the problem of flame burning and poor amphiphobic performance after cleaning in the actual use process. Therefore, it is necessary to improve the performance of fire-fighting clothing such as hydrophobicity, ice-repellent, flame-retardant, and water-washing resistance. Fabric finishing is a common solution to these problems. The fabric treated with the finishing agent can easily allow water to roll off its surface due to its water-repellent properties, and it is difficult to freeze quickly. At the same time, due to its highly hydrophobic properties, even if the surface of the fabric freezes, the ice is easily detached from the surface.
市面上的织物防泼水剂所形成的涂层已经有较好的防泼水效果(如日本大金DAIKIN优尼恩防泼水整理TG-410)，但这些涂层在受到洗涤、磨损或水流冲击后容易失去防泼水效果，达不到消防服持久防泼水的要求。同时，由于这些涂层基本没有阻燃效果，有的甚至还有助燃效果，故无法应用到阻燃要求很高的消防服表面。有些涂层能做到表面超疏水、阻燃，但制备过程复杂，成本高(中国发明专利201510053494.4；陈珊珊，吉林大学，硕士论文，2014)。目前，市面上还没有见到能兼顾阻燃、疏水、疏油、疏冰、耐水洗的水性织物整理剂。The coatings formed by the fabric water repellent agents on the market already have a good water repellent effect (such as Japan's Daikin DAIKIN Union Water Repellent Finishing TG-410), but these coatings are washed, worn or impacted by water flow. It is easy to lose the water-repellent effect, and it cannot meet the requirements of durable water-repellent fire protection clothing. At the same time, since these coatings basically have no flame retardant effect, and some even have a combustion-supporting effect, they cannot be applied to the surface of fire-fighting clothing with high flame retardant requirements. Some coatings can achieve super-hydrophobicity and flame retardant surface, but the preparation process is complicated and the cost is high (China Invention Patent 201510053494.4; Chen Shanshan, Jilin University, Master Thesis, 2014). At present, there is no water-based fabric finishing agent on the market that can take into account flame retardancy, hydrophobicity, oleophobicity, ice repellency, and washing resistance.
发明内容SUMMARY OF THE INVENTION
有鉴于此，本发明旨在提出一种织物用阻燃、疏水、疏油、疏冰整理剂，通过含氟防泼水剂的低表面能以及封闭型阻燃多异氰酸酯交联剂的阻燃和交联特性，赋予织物阻燃、疏水、疏油、疏冰、耐水洗等优异性能。In view of this, the present invention aims to propose a flame-retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabrics, through the low surface energy of the fluorine-containing water repellent agent and the flame retardant and The cross-linking properties endow the fabric with excellent properties such as flame retardant, hydrophobic, oleophobic, ice-repellent, and water-washable.
为达到上述目的，本发明的技术方案是这样实现的：In order to achieve the above object, the technical scheme of the present invention is achieved in this way:
一种织物用阻燃、疏水、疏油、疏冰整理剂，该整理剂由包括如下重量份数的原料制备得到：水100份、防泼水剂2-5份、交联剂0.5-4份；其中，所述交联剂为由阻燃剂、多异氰酸酯和封端剂制备得到的封闭型阻燃多异氰酸酯。A flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics, the finishing agent is prepared from the following raw materials by weight: 100 parts of water, 2-5 parts of water repellent agent, and 0.5-4 parts of cross-linking agent ; wherein, the crosslinking agent is a blocked flame retardant polyisocyanate prepared from a flame retardant, a polyisocyanate and a blocking agent.
织物用该织物用阻燃、疏水、疏油、疏冰整理剂所形成的涂层由于具有低表面能特性，能够赋予织物优异的拒水、疏油、疏冰性能，而封闭型阻燃多异氰酸酯交联剂本身具有较好的阻燃性能，同时还可与防泼水剂发生交联反应，在不影响拒水、疏油、疏冰性能的同时，为涂层提供了阻燃和耐水洗功能。The coating formed by the flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabric can endow the fabric with excellent water-repellent, oil-repellent and ice-repellent properties due to its low surface energy characteristics, while the closed type flame retardant is mostly used. Isocyanate cross-linking agent itself has good flame retardant performance, and at the same time, it can also cross-link with anti-water repellent agent, which provides flame retardant and washing resistance for the coating without affecting the water repellent, oleophobic and ice repellent properties. Function.
进一步，所述防泼水剂为含氟丙烯酸酯；含氟丙烯酸酯的大分子主链上既含有可供交联的侧羟基，又含有较长的碳氟侧链。Further, the water repellent agent is a fluorine-containing acrylate; the macromolecular main chain of the fluorine-containing acrylate contains both side hydroxyl groups available for crosslinking and longer fluorocarbon side chains.
进一步，所述封闭型阻燃多异氰酸酯的结构如下：Further, the structure of the closed flame retardant polyisocyanate is as follows:
其中，A代表封端剂，B代表多异氰酸酯，C代表阻燃剂。Among them, A represents blocking agent, B represents polyisocyanate, and C represents flame retardant.
进一步，所述阻燃剂的结构为：Further, the structure of the flame retardant is:
磷(膦)酸酯和三聚氰胺磷酸盐类阻燃剂本身阻燃性能较好，然后两端含有羟基或氨基可以与异氰酸酯反应，选择这种阻燃结构兼顾了阻燃和能与异氰酸酯反应。Phosphorus (phosphonate) ester and melamine phosphate flame retardants have better flame retardant properties, and then both ends contain hydroxyl or amino groups to react with isocyanates. This flame retardant structure is selected to take into account both flame retardancy and reaction with isocyanates.
进一步，所述R1、R2、R3、R4的结构如下：Further, the structures of the R 1 , R 2 , R 3 and R 4 are as follows:
进一步，所述封端剂中R的结构为：Further, the structure of R in the end capping agent is:
进一步，所述封闭型阻燃多异氰酸酯由包括如下步骤的制备方法制备得到：Further, the closed flame retardant polyisocyanate is prepared by a preparation method comprising the following steps:
(1)将阻燃剂和多异氰酸酯分别溶于溶剂，按照羟基或氨基与异氰酸根摩尔比为1:1，将阻燃剂溶液逐滴滴加到异氰酸酯溶液中，搅拌30-60min，制得阻燃多异氰酸酯；(1) Dissolve the flame retardant and the polyisocyanate in the solvent respectively, and add the flame retardant solution dropwise to the isocyanate solution according to the molar ratio of hydroxyl or amino group to isocyanate group of 1:1, and stir for 30-60 min to prepare Obtain flame retardant polyisocyanate;
(2)氮气保护下，将阻燃多异氰酸酯逐滴加入到封端剂溶液中，升温至80℃，反应30min，干燥，即得封闭型阻燃多异氰酸酯。(2) Under the protection of nitrogen, the flame retardant polyisocyanate is added dropwise to the blocking agent solution, the temperature is raised to 80° C., the reaction is performed for 30 minutes, and dried to obtain a blocked flame retardant polyisocyanate.
本发明还提供了一种如上述所述的织物用阻燃、疏水、疏油、疏冰整理剂的制备方法，该方法包括如下步骤：The present invention also provides a preparation method of the above-mentioned flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics, the method comprising the following steps:
室温下，将防泼水剂和交联剂加入到水中，在500转速下搅拌30min，停止搅拌，静置2h去除气泡，制得织物用阻燃、疏水、疏油、疏冰整理剂。At room temperature, add the water repellent agent and crosslinking agent to the water, stir at 500 revolutions for 30 minutes, stop stirring, and let stand for 2 hours to remove air bubbles to prepare a flame retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabrics.
本发明还提供了一种如上述所述的织物用阻燃、疏水、疏油、疏冰整理剂的应用方法，该方法包括如下步骤：The present invention also provides a method for applying the above-mentioned flame retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics, the method comprising the following steps:
(1)将织物于室温下浸渍于织物用阻燃、疏水、疏油、疏冰整理剂中1-2min，取出后置于浸轧机中浸轧，浸轧压力为0.25Mpa；(1) Immerse the fabric in a flame-retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabric at room temperature for 1-2min, take it out and place it in a padding mill for padding, and the padding pressure is 0.25Mpa;
(2)将步骤(1)得到的织物置于120-170℃烘箱中烘烤1-10min。(2) The fabric obtained in step (1) is placed in an oven at 120-170° C. for 1-10 min.
本发明还提供了一种如上述所述的织物用阻燃、疏水、疏油、疏冰整理剂在消防员防护服装上的应用。The present invention also provides the application of the above-mentioned flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics to firefighters' protective clothing.
相对于现有技术，本发明所述的织物用阻燃、疏水、疏油、疏冰整理剂及其制备和应用方法具有以下优势：Compared with the prior art, the flame-retardant, hydrophobic, oleophobic, ice-repellent finishing agent for fabrics of the present invention and its preparation and application methods have the following advantages:
(1)本发明所述的织物用阻燃、疏水、疏油、疏冰整理剂通过具有低表面能特性的含氟防泼水剂的引入，赋予织物防泼水、疏油和疏冰的优异性能，从而确保消防员在高温和低温环境下能够舒适和高效的进行救援工作。在整理剂中引入阻燃剂，赋予织物优异的阻燃性能，为消防员的安全提供进一步的保障；同时，将阻燃剂反应到多异氰酸酯交联剂上，避免直接将阻燃剂添加至整理剂时，织物正常使用和清洗过程中造成的阻燃剂损失和织物阻燃性能下降。(1) The flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics of the present invention imparts excellent properties of water-repellent, oleophobic and ice-repellent to the fabric through the introduction of a fluorine-containing water-repellent agent with low surface energy properties. , so as to ensure that firefighters can carry out rescue work comfortably and efficiently in high and low temperature environments. The flame retardant is introduced into the finishing agent to endow the fabric with excellent flame retardant performance and provide further protection for the safety of firefighters; at the same time, the flame retardant is reacted to the polyisocyanate crosslinking agent to avoid adding the flame retardant directly to the When the finishing agent is used, the loss of flame retardant and the flame retardant performance of the fabric caused by the normal use and cleaning of the fabric.
(2)本发明所述的织物用阻燃、疏水、疏油、疏冰整理剂对织物的处理方法简便易行，并且整理剂对织物的视觉和手感影响较小。(2) The flame-retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabrics of the present invention is simple and easy to handle, and the finishing agent has little effect on the visual and hand feeling of the fabric.
具体实施方式Detailed ways
需要说明的是，在不冲突的情况下，本发明中的实施例及实施例中的特征可以相互组合。It should be noted that the embodiments of the present invention and the features of the embodiments may be combined with each other under the condition of no conflict.
下面将结合实施例来详细说明本发明。The present invention will be described in detail below with reference to the embodiments.
实施例1：Example 1:
封闭型阻燃多异氰酸酯的制备方法：The preparation method of the closed flame retardant polyisocyanate:
(1)将膦酸酯阻燃剂(结构式如表1)和六亚甲基二异氰酸酯按照羟基和异氰酸酯摩尔比为1:1分别溶于甲苯溶剂，在200转速搅拌下将膦酸酯阻燃剂溶液逐滴滴加到异氰酸酯六亚甲基二异氰酸酯溶液中，继续搅拌30min，干燥，制得阻燃多异氰酸酯；(1) Dissolve the phosphonate flame retardant (structural formula as shown in Table 1) and hexamethylene diisocyanate in a toluene solvent according to the molar ratio of hydroxyl and isocyanate of 1:1, and stir the phosphonate ester flame retardant at 200 revolutions. The agent solution was added dropwise to the isocyanate hexamethylene diisocyanate solution, continued to stir for 30 min, and dried to obtain flame retardant polyisocyanate;
(2)氮气保护下，将阻燃多异氰酸酯逐滴加入到苯酚类封端剂溶液中，升温至80℃，反应30min，干燥，即得封闭型阻燃多异氰酸酯。(2) Under nitrogen protection, the flame retardant polyisocyanate is added dropwise to the phenolic blocking agent solution, the temperature is raised to 80° C., the reaction is performed for 30 minutes, and dried to obtain a blocked flame retardant polyisocyanate.
一种织物用阻燃、疏水、疏油、疏冰整理剂的制备方法，该方法包括如下步骤：A preparation method of a flame retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics, the method comprises the following steps:
取C8型防泼水剂(日本大金公司TG-581，固含量30wt％)2份、封闭型阻燃多异氰酸酯0.5份、水100份，室温下，将防泼水剂和交联剂加入到水中，在500转速下搅拌30min，停止搅拌，静置2h去除气泡，制得织物用阻燃、疏水、疏油、疏冰整理剂。Take 2 parts of C8 type water repellent agent (TG-581 of Japan's Daikin company, solid content 30wt%), 0.5 part of closed flame retardant polyisocyanate, and 100 parts of water, at room temperature, add the water repellent agent and crosslinking agent to the water , stir at 500 revolutions for 30 minutes, stop stirring, let stand for 2 hours to remove air bubbles, and prepare a flame retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabrics.
一种织物用阻燃、疏水、疏油、疏冰整理剂的应用方法，该方法包括如下步骤：An application method of a flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agent for fabrics, the method comprises the following steps:
(1)将芳纶织物于室温下浸渍于织物用阻燃、疏水、疏油、疏冰整理剂中1min，取出后置于浸轧机中浸轧，浸轧压力为0.25Mpa；(1) Immerse the aramid fabric in a flame-retardant, hydrophobic, oleophobic, and ice-repellent finishing agent for fabric at room temperature for 1 min, take it out and place it in a padding mill for padding, and the padding pressure is 0.25Mpa;
(2)重复浸渍和浸轧步骤2次；(2) Repeat the dipping and padding steps twice;
(3)将浸轧后的织物置于120℃烘箱中5min，即制得具有阻燃、疏水、疏油、疏冰功能的织物。(3) The fabric after padding was placed in an oven at 120° C. for 5 minutes, to obtain a fabric with flame-retardant, hydrophobic, oleophobic and ice-repellent functions.
实施例2-5以及对比例1-3与实施例1相比，制备步骤基本相同，仅阻燃剂、异氰酸酯、防泼水剂、封端剂种类和含量不同，各实施例和对比例中阻燃剂、异氰酸酯、防泼水剂、封端剂具体种类和含量见表1。Compared with Example 1, the preparation steps of Examples 2-5 and Comparative Examples 1-3 are basically the same, and only the types and contents of flame retardants, isocyanates, water repellent agents, and end-capping agents are different. See Table 1 for the specific types and contents of burning agent, isocyanate, water repellent agent, and end-capping agent.
表1实施例和对比例具体配方(各组分的单位为重量份数)Table 1 embodiment and the specific formula of comparative example (the unit of each component is parts by weight)
按照GB/T 4745-2012《纺织品防水性能的检测和评价沾水法》，测试整理剂处理后芳纶织物的沾水等级，使用平推法(塑料套模内水预冷2h)测试织物表面与冰之间的结合力；同时，分别取处理好的织物进行机洗和水流冲击一段时间，烘干后再次测量织物表面的沾水等级和推冰剪切力；机洗是将织物放入洗衣机内加入一定量的自来水(浸没织物)洗涤30分钟，共计50次；水流冲击试验是将织物放于冲击力为105.3kPa的水流下冲击2h；通过测试织物的极限氧指数表征其阻燃性能，极限氧指数按照GB/T 5454-1997《纺织品燃烧性能试验氧指数法》进行测试。According to GB/T 4745-2012 "Testing and Evaluation of Waterproofing Performance of Textiles", test the water-wetting grade of aramid fabrics treated with the finishing agent, and use the flat push method (water pre-cooling in the plastic mold for 2h) to test the surface of the fabric The binding force with ice; at the same time, the treated fabrics were machine washed and impacted by water for a period of time, and after drying, the water level of the fabric surface and the ice pushing shear force were measured again; machine washing is to put the fabric in Add a certain amount of tap water (submerged the fabric) into the washing machine for 30 minutes, a total of 50 times; the water impact test is to place the fabric under a water flow with an impact force of 105.3kPa for 2 hours; test the fabric's limit oxygen index to characterize its flame retardant performance , the limiting oxygen index is tested according to GB/T 5454-1997 "Textile Combustion Performance Test Oxygen Index Method".
表2给出了实施例和对比例中的测试结果，包括沾水等级、冰柱结合力、机洗和水流冲击后沾水等级、机洗和水流冲击后冰柱结合力、极限氧指数等。Table 2 presents the test results in the Examples and Comparative Examples, including the wet grade, icicle binding force, water wet grade after machine washing and water impact, icicle binding force after machine washing and water impact, limiting oxygen index, etc. .
表2实施例1-5和对比例1-3的测试结果Table 2 Test results of Examples 1-5 and Comparative Examples 1-3
结果分析：Result analysis:
综上可以看出，未处理的织物样品亲水性强，易结冰且冰的结合力强，较难清除；使用含氟丙烯酸酯处理后的织物疏水、疏冰性能得到明显提升，但是由于其粘附力较弱，水洗后含氟丙烯酸酯流失，导致其疏水、疏冰性能明显降低；当进一步引入异氰酸酯后，处理后的织物样品的耐水洗性能得到明显提升，洗涤后织物的疏水、疏冰性能基本保持不变；封闭型阻燃异氰酸酯的引入能够进一步提升织物的阻燃性能；同时，随着阻燃、疏水、疏油、疏冰整理剂含量的提高，处理后织物的疏水、疏冰、阻燃、和耐水洗等性能逐渐提升。In summary, it can be seen that the untreated fabric samples have strong hydrophilicity, are easy to freeze, and have strong ice binding force, making them difficult to remove; the hydrophobic and ice-repellent properties of the fabrics treated with fluorine-containing acrylate are significantly improved, but due to Its adhesion is weak, and the fluorine-containing acrylate is lost after washing, resulting in a significant decrease in its hydrophobic and ice-repellent properties; when isocyanate is further introduced, the water-washing resistance of the treated fabric samples is significantly improved. The ice-repellent performance remains basically unchanged; the introduction of blocked flame-retardant isocyanate can further improve the flame-retardant performance of the fabric; at the same time, with the increase in the content of flame-retardant, hydrophobic, oleophobic and ice-repellent finishing agents, the hydrophobicity, Ice-repellent, flame-retardant, and water-washable properties are gradually improved.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the scope of the present invention. within the scope of protection.
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