WO2023184954A1 - Molybdenum disulfide coating for fireproof flame-retardant cotton fabric and coating method therefor - Google Patents
Molybdenum disulfide coating for fireproof flame-retardant cotton fabric and coating method therefor Download PDFInfo
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- WO2023184954A1 WO2023184954A1 PCT/CN2022/127626 CN2022127626W WO2023184954A1 WO 2023184954 A1 WO2023184954 A1 WO 2023184954A1 CN 2022127626 W CN2022127626 W CN 2022127626W WO 2023184954 A1 WO2023184954 A1 WO 2023184954A1
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- molybdenum disulfide
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- cotton fabric
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 68
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000576 coating method Methods 0.000 title claims abstract description 46
- 229920000742 Cotton Polymers 0.000 title claims abstract description 32
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 239000004744 fabric Substances 0.000 title claims abstract description 32
- 239000003063 flame retardant Substances 0.000 title claims abstract description 23
- 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 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 21
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 12
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 12
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 12
- 229940033123 tannic acid Drugs 0.000 claims abstract description 12
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 12
- 229920002258 tannic acid Polymers 0.000 claims abstract description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 14
- 238000003618 dip coating Methods 0.000 claims description 6
- 230000009970 fire resistant effect Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- -1 hydrogen Sodium oxide Chemical class 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 239000000779 smoke Substances 0.000 abstract description 4
- 238000003763 carbonization Methods 0.000 abstract description 3
- 231100000481 chemical toxicant Toxicity 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 3
- 230000001629 suppression Effects 0.000 abstract description 3
- 239000003440 toxic substance Substances 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 239000000428 dust Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910052961 molybdenite Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000007706 flame test Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
-
- 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
- D06M13/238—Tannins, e.g. gallotannic acids
Definitions
- the molybdenum disulfide described in the above technical solution is a powder with a lamella size of 0.2 to 10 microns.
- the concentration of tannic acid in the molybdenum disulfide ink described in the above technical solution is 4 grams per liter.
- the thermal decomposition of these cotton fabrics in high temperature environments can be characterized by thermogravimetric analysis.
- T 10% The temperature at which 10% of the weight is lost
- T max the temperature at which the maximum thermal decomposition rate is (T max ) and the char formation rate at 800°C are shown in Figure 1 .
- T 10% and T max of Cotton-MoS 2 (4s) shows that it has higher thermal stability.
- Molybdenum disulfide contributes to the formation of char, and the yield is about 4% higher than cotton fabric without molybdenum disulfide coating.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
A molybdenum disulfide coating for a fireproof flame-retardant cotton fabric and a coating method therefor. The coating comprises molybdenum disulfide ink, and the molybdenum disulfide ink comprises the following components: molybdenum disulfide, tannic acid, and a solvent, the solvent being isopropyl alcohol and water. The method comprises the following steps: S1, preparing molybdenum disulfide ink and carrying out ultrasonic treatment; S2, cyclically soaking a cotton fabric into the molybdenum disulfide ink of S1 for a certain period of time, and then carrying out drying treatment; and S3, adding a sodium hydroxide coating. No highly toxic chemical is not used, but environmentally friendly tannic acid is used. Molybdenum disulfide provides good smoke suppression performance during combustion, can implement effective embedment of gas and smoke/dust by means of sulfur defects, voids, edges and the like of molybdenum disulfide, and can also be used for catalysis of carbonization. The sodium hydroxide coating added can solve the technical problem of self-extinguishing.
Description
本发明涉及棉织物材料技术领域,具体涉及一种用于防火阻燃棉织物的二硫化钼涂层及其涂覆方法。The invention relates to the technical field of cotton fabric materials, and in particular to a molybdenum disulfide coating for fireproof and flame-retardant cotton fabrics and a coating method thereof.
棉织物在当今纺织工业以及人们的日常生活当中扮演了举足轻重的作用,但是由于其阻燃效果不佳,因此发生火灾时会在全时间范围内产生巨大的损失。这一缺点对于目前新兴的以织物为基础的智能穿戴电子产品来说更是一个巨大的挑战。目前常用的阻燃添加剂是以卤素,磷或者甲醛等化合物为基础的,这些阻燃添加剂在制造或者使用的过程当中会释放出有毒的化学物品。并且它们和正在新兴发展的智能穿戴行业并不匹配,因为阻燃添加剂只能提供阻燃性能而不是多功能特性。这就意味基底织物需要进行多次处理才能够满足不同的应用,例如导电性等。Cotton fabric plays a pivotal role in today's textile industry and people's daily lives. However, due to its poor flame retardant effect, huge losses will occur throughout the entire time in the event of a fire. This shortcoming is a huge challenge for the current emerging smart wearable electronic products based on fabrics. Currently commonly used flame retardant additives are based on compounds such as halogens, phosphorus or formaldehyde. These flame retardant additives will release toxic chemicals during the manufacturing or use process. And they do not match the emerging smart wear industry because flame retardant additives can only provide flame retardant properties rather than multifunctional properties. This means that the base fabric needs to be processed multiple times to meet different applications, such as conductivity.
二维材料的发展为智能穿戴行业提供了方向,其能够同时满足阻燃以及其他方面的应用,包括高比表面积,灵活性,高机械稳定性,高导电性,高导热性以及阻隔性能。目前处在研究开发阶段的二维材料包括还原氧化石墨烯以及六方氮化硼,但是其在防火方面的性能并不显着,例如不能有效地提供阻烟性能,炭催化性能以及形成有效的物理屏障。除此之外,它们的热稳定性并不优异,这就使得其在燃烧的过程当中容易出现分解。The development of two-dimensional materials provides a direction for the smart wearable industry, which can simultaneously meet flame retardant and other applications, including high specific surface area, flexibility, high mechanical stability, high electrical conductivity, high thermal conductivity and barrier properties. Two-dimensional materials currently in the research and development stage include reduced graphene oxide and hexagonal boron nitride, but their performance in fire protection is not significant. For example, they cannot effectively provide smoke suppression properties, carbon catalytic properties, and form effective physical properties. barrier. In addition, their thermal stability is not excellent, which makes them prone to decomposition during the combustion process.
发明内容Contents of the invention
本发明的目的是克服现有技术的缺陷,提供一种用于防火阻燃棉织物的二硫化钼涂层及其涂覆方法。The purpose of the present invention is to overcome the shortcomings of the prior art and provide a molybdenum disulfide coating for fire-proof and flame-retardant cotton fabrics and a coating method thereof.
实现本发明目的的技术方案是:一种用于防火阻燃棉织物的二硫化钼涂层,包括二硫化钼墨水,所述二硫化钼墨水具有以下组分:二硫化钼、鞣酸、溶剂,所述溶剂为异丙醇和水。The technical solution to achieve the object of the present invention is: a molybdenum disulfide coating for fire-proof and flame-retardant cotton fabrics, including molybdenum disulfide ink, the molybdenum disulfide ink has the following components: molybdenum disulfide, tannic acid, solvent , the solvent is isopropyl alcohol and water.
上述技术方案所述二硫化钼为片层大小0.2~10微米的粉体。The molybdenum disulfide described in the above technical solution is a powder with a lamella size of 0.2 to 10 microns.
上述技术方案所述二硫化钼墨水中二硫化钼的浓度为2~20克每升。The concentration of molybdenum disulfide in the molybdenum disulfide ink described in the above technical solution is 2 to 20 grams per liter.
上述技术方案所述二硫化钼墨水中鞣酸的浓度为4克每升。The concentration of tannic acid in the molybdenum disulfide ink described in the above technical solution is 4 grams per liter.
一种用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,具有以下步骤:A coating method of molybdenum disulfide coating for fire-resistant and flame-retardant cotton fabrics, which has the following steps:
S1,制备二硫化钼墨水,将二硫化钼、鞣酸溶于异丙醇和水,将混合后的混合溶液进行超声处理,得到二硫化钼墨水;S1, prepare molybdenum disulfide ink, dissolve molybdenum disulfide and tannic acid in isopropyl alcohol and water, and perform ultrasonic treatment on the mixed solution to obtain molybdenum disulfide ink;
S2,将棉织物浸渍到S1的二硫化钼墨水一定时间后,进行烘干处理,以此作为一次浸渍涂覆循环;循环三次;In S2, the cotton fabric is immersed in the molybdenum disulfide ink of S1 for a certain period of time, and then dried, as a dip coating cycle; cycle three times;
S3,将经过浸渍涂覆循环后的棉织物添加氢氧化钠涂层。S3, add sodium hydroxide coating to the cotton fabric after the dip coating cycle.
上述技术方案所述S1中,所述超声处理是在超声频率37kHz、超声功率820W、室温20℃、大气压1atm的超声池中进行,超声处理2个小时。In S1 of the above technical solution, the ultrasonic treatment is performed in an ultrasonic pool with an ultrasonic frequency of 37 kHz, an ultrasonic power of 820 W, a room temperature of 20°C, and an atmospheric pressure of 1 atm, and the ultrasonic treatment lasts for 2 hours.
上述技术方案所述S2中,烘干处理的温度是120℃,时间是30分钟。In S2 of the above technical solution, the temperature of the drying process is 120°C and the time is 30 minutes.
上述技术方案所述S3中,所述氢氧化钠涂层使用的是1wt%的氢氧化钠溶液。In S3 of the above technical solution, the sodium hydroxide coating uses a 1wt% sodium hydroxide solution.
采用上述技术方案后,本发明具有以下积极的效果:After adopting the above technical solution, the present invention has the following positive effects:
本发明二硫化钼涂层的配方有效地解决了当前涂层配方的一些短板。The formula of the molybdenum disulfide coating of the present invention effectively solves some shortcomings of the current coating formula.
(1)不使用剧毒化学品,使用的是从植物当中提取的、环保的鞣酸。(1) No highly toxic chemicals are used, only environmentally friendly tannic acid extracted from plants is used.
(2)与其它应用于二维材料的防火涂层相比,二硫化钼在燃烧过程中提供了更好的阻烟性能,并且可以通过自身的硫缺陷,空隙以及边缘等进行有效地气体及烟尘镶嵌,还可以用于炭化的催化。同时,它还具有比还原氧化石墨烯和六方氮化硼更高的热稳定性。(2) Compared with other fire-retardant coatings applied to two-dimensional materials, molybdenum disulfide provides better smoke suppression performance during the combustion process, and can effectively carry out gas and fire protection through its own sulfur defects, voids and edges. Soot inlay can also be used as a catalyst for carbonization. At the same time, it also has higher thermal stability than reduced graphene oxide and hexagonal boron nitride.
(3)添加的氢氧化钠涂层,相比于一般的二维材料来说,可以解决自熄灭的技术问题。(3) The added sodium hydroxide coating can solve the technical problem of self-extinguishing compared to general two-dimensional materials.
图1为不同织物的T
10%,T
max以及800℃时的炭生成率;
Figure 1 shows the T 10% , T max and char formation rate of different fabrics at 800°C;
图2为在垂直火焰测试中确定的不同样品的余焰时间、余辉时间和炭化长度。Figure 2 shows the afterflame time, afterglow time and char length of different samples determined in the vertical flame test.
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。通常在此处附图中描述和示出的本发明实施例的组件可以以各种不同的配置来布置和设计。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments These are some embodiments of the present invention, rather than all embodiments. The components of the embodiments of the invention generally described and illustrated in the figures herein may be arranged and designed in a variety of different configurations.
一种用于防火阻燃棉织物的二硫化钼涂层,包括二硫化钼墨水,所述二硫化钼墨水具有以下组分:二硫化钼、鞣酸、溶剂,所述溶剂为异丙醇和水。所述二硫化钼为片层大小0.2~10微米的粉体。案所述二硫化钼墨水中二硫化钼的浓度为2~20克每升。所述二硫化钼墨水中鞣酸的浓度为4克每升。A molybdenum disulfide coating for fireproof and flame-retardant cotton fabrics, including molybdenum disulfide ink, the molybdenum disulfide ink has the following components: molybdenum disulfide, tannic acid, solvent, the solvent is isopropyl alcohol and water . The molybdenum disulfide is a powder with a lamella size of 0.2 to 10 microns. The concentration of molybdenum disulfide in the molybdenum disulfide ink described in the case is 2 to 20 grams per liter. The concentration of tannic acid in the molybdenum disulfide ink is 4 grams per liter.
一种用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,具有以下步骤:A coating method of molybdenum disulfide coating for fire-resistant and flame-retardant cotton fabrics, which has the following steps:
S1,制备二硫化钼墨水,将二硫化钼、鞣酸溶于异丙醇和水,将混合后的混合溶液进行超声处理,得到二硫化钼墨水;超声处理是在超声频率37kHz、超声功率820W、室温20℃、大气压1atm的超声池中进行,超声处理2个小时。S1, prepare molybdenum disulfide ink, dissolve molybdenum disulfide and tannic acid in isopropyl alcohol and water, and conduct ultrasonic treatment on the mixed solution to obtain molybdenum disulfide ink; the ultrasonic treatment is performed at an ultrasonic frequency of 37kHz, an ultrasonic power of 820W, It was carried out in an ultrasonic pool at room temperature of 20°C and atmospheric pressure of 1 atm, and the ultrasonic treatment was carried out for 2 hours.
S2,将棉织物浸渍到S1的二硫化钼墨水一定时间后,进行烘干处理,以此作为一次浸渍涂覆循环;循环三次;烘干处理的温度是120℃,时间是30分钟。In S2, the cotton fabric is immersed in the molybdenum disulfide ink of S1 for a certain period of time, and then dried, as a dip coating cycle; cycle three times; the temperature of the drying process is 120°C and the time is 30 minutes.
S3,将经过浸渍涂覆循环后的棉织物添加氢氧化钠涂层。氢氧化钠涂层使用的是1wt%的氢氧化钠溶液。S3, add sodium hydroxide coating to the cotton fabric after the dip coating cycle. The sodium hydroxide coating uses a 1wt% sodium hydroxide solution.
根据上面的方法按下表进行样本的制作:According to the above method, make the sample according to the following table:
| 二硫化钼涂层Molybdenum disulfide coating | 氢氧化钠涂层sodium hydroxide coating | 添加重量(%)Added weight (%) |
CottonCotton | 无none | 无none | 无none |
Cotton-NCotton-N | 无none |
一次涂层one |
12%12% |
Cotton-MoS2(4s)Cotton-MoS2(4s) | 三次涂层(小片层,16g/L)Three coatings (small flake layer, 16g/L) | 无none | 19%19% |
Cotton-MoS2(4s)-NCotton-MoS2(4s)-N | 三次涂层(小片层,16g/L)Three coatings (small flake layer, 16g/L) | 一次涂层one coat | 32%32% |
Cotton-MoS2(4b)-NCotton-MoS2(4b)-N | 三次涂层(大片层,16g/L)Three coats (large layer, 16g/L) | 一次涂层one coat | 31%31% |
Cotton-MoS2(0.5s)-NCotton-MoS2(0.5s)-N | 三次涂层(小片层,2g/L)Three coatings (small flake layer, 2g/L) | 一次涂层one coat | 19%19% |
见图1,以上6种样本,检测T
10%,T
max以及800℃时的炭生成率。
See Figure 1. The above 6 samples were tested for T 10% , T max and the carbon formation rate at 800°C.
由图1可知,这些棉织物在高温环境下的热分解可以被热重分析所表征。其损失10%重量所处的温度(T
10%),最大热分解速率所处的温度(T
max)以及800℃时的炭生成率显示在图一中。Cotton-MoS
2(4s)更高的T
10%and T
max,显示其具有更高的热稳定性。二硫化钼有助于炭的形成,其产量比未经二硫化钼涂层的棉织物高约4%。作为比较,尽管经过氢氧化钠处理的Cotton-N拥有与Cotton-MoS
2(4s)相似的炭产率,但它削弱了织物的热稳定性,因为T
10%和T
max均降低。Cotton-N的最大分解速率仍然低于Cotton和Cotton-MoS
2(4s),这表明氢氧化钠涂层所带来的膨胀炭化的催化作用能够防止织物在高温下进一步分解。如Cotton-MoS
2(4s)-N所示,结合二硫化钼和氢氧化钠涂层显示出协同效应,其最大分解速率比Cotton-N或Cotton-MoS
2(4s)显著降低。其炭产率的增加甚至超过了Cotton-N和Cotton-MoS
2(4s)之和。
As can be seen from Figure 1, the thermal decomposition of these cotton fabrics in high temperature environments can be characterized by thermogravimetric analysis. The temperature at which 10% of the weight is lost (T 10% ), the temperature at which the maximum thermal decomposition rate is (T max ) and the char formation rate at 800°C are shown in Figure 1 . The higher T 10% and T max of Cotton-MoS 2 (4s) shows that it has higher thermal stability. Molybdenum disulfide contributes to the formation of char, and the yield is about 4% higher than cotton fabric without molybdenum disulfide coating. For comparison, although Cotton-N treated with sodium hydroxide possesses similar char yield to Cotton- MoS2 (4s), it weakens the thermal stability of the fabric as both T 10% and T max are reduced. The maximum decomposition rate of Cotton-N is still lower than that of Cotton and Cotton-MoS 2 (4s), which indicates that the catalytic effect of expansion carbonization brought about by the sodium hydroxide coating can prevent further decomposition of the fabric at high temperatures. As shown for Cotton-MoS 2 (4s)-N, combining molybdenum disulfide and sodium hydroxide coatings shows a synergistic effect with a significantly lower maximum decomposition rate than Cotton-N or Cotton-MoS 2 (4s). The increase in carbon yield even exceeds the sum of Cotton-N and Cotton-MoS 2 (4s).
见图2,以上6种样本,在垂直火焰测试中确定的不同样品的余焰时间、余辉时间和炭化长度。See Figure 2 for the above six samples. The afterflame time, afterglow time and char length of different samples were determined in the vertical flame test.
在垂直火焰测试中,Cotton-N已完全燃烧,而余焰时间减少了约50%,从Cotton的12秒减少到约6秒。这显示出氢氧化钠促进了自熄灭特性。火焰熄灭后,余辉时间明显增加至Cotton的近7倍。Cotton-MoS
2(4s)也已完全燃烧,但余焰时间和余辉时间都只略有增加。在Cotton-MoS
2(4s)-N中可以看到显着的改进,其中余焰时间、余辉时间和炭化长度都已减少。与Cotton相比,尤其是余辉时间和炭化长度减少了约80%。二硫化钼薄片增强了膨胀炭的机械性能。
In the vertical flame test, Cotton-N burned completely while afterflame time was reduced by about 50%, from Cotton's 12 seconds to about 6 seconds. This shows that sodium hydroxide promotes self-extinguishing properties. After the flame is extinguished, the afterglow time is significantly increased to nearly 7 times that of Cotton. Cotton-MoS 2 (4s) also burned completely, but the afterflame time and afterglow time only increased slightly. Significant improvements are seen in Cotton-MoS 2 (4s)-N, where afterflame time, afterglow time and char length have all been reduced. In particular, afterglow time and char length are reduced by approximately 80% compared to Cotton. Molybdenum disulfide flakes enhance the mechanical properties of expanded carbon.
以上所述的具体实施例,对本发明的目的、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above-mentioned specific embodiments further describe the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above-mentioned are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.
Claims (8)
- 一种用于防火阻燃棉织物的二硫化钼涂层,其特征在于,包括二硫化钼墨水,所述二硫化钼墨水具有以下组分:二硫化钼、鞣酸、溶剂,所述溶剂为异丙醇和水。A molybdenum disulfide coating for fireproof and flame-retardant cotton fabrics, characterized in that it includes molybdenum disulfide ink, and the molybdenum disulfide ink has the following components: molybdenum disulfide, tannic acid, and a solvent, and the solvent is Isopropyl alcohol and water.
- 根据权利要求1所述的一种用于防火阻燃棉织物的二硫化钼涂层,其特征在于:所述二硫化钼为片层大小0.2~10微米的粉体。A molybdenum disulfide coating for fireproof and flame-retardant cotton fabrics according to claim 1, characterized in that: the molybdenum disulfide is a powder with a lamellar size of 0.2 to 10 microns.
- 根据权利要求1所述的一种用于防火阻燃棉织物的二硫化钼涂层,其特征在于:所述二硫化钼墨水中二硫化钼的浓度为2~20克每升。A molybdenum disulfide coating for fireproof and flame-retardant cotton fabric according to claim 1, characterized in that: the concentration of molybdenum disulfide in the molybdenum disulfide ink is 2 to 20 grams per liter.
- 根据权利要求1所述的一种用于防火阻燃棉织物的二硫化钼涂层,其特征在于:所述二硫化钼墨水中鞣酸的浓度为4克每升。A molybdenum disulfide coating for fire-proof and flame-retardant cotton fabric according to claim 1, characterized in that: the concentration of tannic acid in the molybdenum disulfide ink is 4 grams per liter.
- 一种如权1-4任一所述的用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,其特征在于,具有以下步骤:A coating method of molybdenum disulfide coating for fire-proof and flame-retardant cotton fabrics as described in any one of claims 1-4, characterized by having the following steps:S1,制备二硫化钼墨水,将二硫化钼、鞣酸溶于异丙醇和水,将混合后的混合溶液进行超声处理,得到二硫化钼墨水;S1, prepare molybdenum disulfide ink, dissolve molybdenum disulfide and tannic acid in isopropyl alcohol and water, and perform ultrasonic treatment on the mixed solution to obtain molybdenum disulfide ink;S2,将棉织物浸渍到S1的二硫化钼墨水一定时间后,进行烘干处理,以此作为一次浸渍涂覆循环;循环三次;In S2, the cotton fabric is immersed in the molybdenum disulfide ink of S1 for a certain period of time, and then dried, as a dip coating cycle; cycle three times;S3,将经过浸渍涂覆循环后的棉织物添加氢氧化钠涂层。S3, add sodium hydroxide coating to the cotton fabric after the dip coating cycle.
- [根据细则26改正 05.01.2023]
[Amended in accordance with Rule 26 05.01.2023]
根据权利要求5所述的一种用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,其特征在于:所述S1中,所述超声处理是在超声频率37kHz、超声功率820W、室温20℃、大气压1atm的超声池中进行,超声处理2个小时。A method for coating molybdenum disulfide coating on fire-resistant and flame-retardant cotton fabrics according to claim 5, characterized in that: in the S1, the ultrasonic treatment is performed at an ultrasonic frequency of 37 kHz and an ultrasonic power of 820 W. It was carried out in an ultrasonic pool at room temperature of 20°C and atmospheric pressure of 1 atm, and the ultrasonic treatment was carried out for 2 hours. - [根据细则26改正 05.01.2023]
根据权利要求5所述的一种用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,其特征在于:所述S2中,烘干处理的温度是120℃,时间是30分钟。 [Amended in accordance with Rule 26 05.01.2023]
The coating method of molybdenum disulfide coating for fire-proof and flame-retardant cotton fabric according to claim 5, characterized in that: in said S2, the temperature of the drying treatment is 120°C and the time is 30 minutes. - [根据细则26改正 05.01.2023]
根据权利要求5所述的一种用于防火阻燃棉织物的二硫化钼涂层的涂覆方法,其特征在于:所述S3中,所述氢氧化钠涂层使用的是1wt%的氢氧化钠溶液。 [Amended in accordance with Rule 26 05.01.2023]
A coating method of molybdenum disulfide coating for fire-proof and flame-retardant cotton fabric according to claim 5, characterized in that: in said S3, the sodium hydroxide coating uses 1wt% hydrogen Sodium oxide solution.
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