CN112030550A - Flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for fabric and preparation and application methods thereof - Google Patents
Flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for fabric and preparation and application methods thereof Download PDFInfo
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- CN112030550A CN112030550A CN202010920395.2A CN202010920395A CN112030550A CN 112030550 A CN112030550 A CN 112030550A CN 202010920395 A CN202010920395 A CN 202010920395A CN 112030550 A CN112030550 A CN 112030550A
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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
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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
- D06M13/322—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
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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
- D06M13/322—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
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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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
- 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
The invention provides a flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for fabrics and a preparation method and an application method thereof, wherein the finishing agent is prepared from the following raw materials in parts by weight: 100 parts of water, 2-5 parts of water repellent agent and 0.5-4 parts of cross-linking agent; the cross-linking agent is blocked flame-retardant polyisocyanate prepared from a flame retardant, polyisocyanate and a blocking agent. The invention endows the fabric with excellent water repellent, oleophobic and ice repellent performance by introducing the fluorine-containing water repellent with low surface energy characteristic; meanwhile, the flame retardant and isocyanate react to prepare the closed flame-retardant polyisocyanate which is used as a cross-linking agent of a water splashing preventive agent, so that the flame retardance of the fabric is improved, and the water washing resistance of the fabric is improved. The fabric treated by the finishing agent has multiple functions of flame retardance, hydrophobicity, oleophobicity, ice-phobicity, water-washing resistance and the like, and can be widely applied to the field of protective clothing of firemen, so that the personal protection capability and the rescue efficiency of the firemen are effectively improved.
Description
Technical Field
The invention relates to the technical field of fabric finishing, in particular to a flame-retardant, hydrophobic, oleophobic and deicing finishing agent for fabric and a preparation method and an application method thereof.
Background
In the actual rescue process, the firefighter uniform is extremely easy to be impacted by water flow, if the firefighter uniform is polluted by water stain, the whole weight of the firefighter uniform can be increased, so that the load of a firefighter is increased, and the fighting capacity of the firefighter is influenced. In a high-temperature environment, the defect of thick and stuffy fire-fighting clothing is also aggravated by the soaked fire-fighting clothing, so that the heat stress phenomenon such as heatstroke and the like of a fireman is more easily caused, and the life safety of the fireman is threatened; under the low temperature environment, moisture on the surface of the firefighter uniform can be frozen into ice quickly, the action of a firefighter can be greatly influenced by the frozen firefighter uniform, the rescue efficiency of the firefighter can be influenced, and the life safety of the firefighter can be endangered. Meanwhile, the firefighter uniform can also face the problem that the amphiphobic performance of the firefighter uniform is poor after flame burning and cleaning in the actual use process. Therefore, the performances of the fire-fighting clothing such as hydrophobicity, ice-phobicity, flame retardance, water washing resistance and the like need to be improved. The fabric finishing agent is a commonly used method for solving the problems, and the fabric treated by the finishing agent is difficult to freeze quickly because the water repellent property of the fabric is easy to roll off the surface of the fabric. Meanwhile, due to the highly hydrophobic characteristic, even if the surface of the fabric is frozen, ice can easily fall off from the surface.
The coatings formed by the fabric water-repellent agents on the market already have better water-repellent effect (such as Japanese DAIKIN Younnien water-repellent finishing TG-410), but the coatings easily lose the water-repellent effect after being washed, abraded or impacted by water flow, and cannot meet the requirement of the fire-fighting clothes on lasting water-repellent effect. Meanwhile, the coatings basically have no flame retardant effect, and some coatings even have combustion-supporting effect, so the coatings cannot be applied to the surface of the firefighter uniform with high flame retardant requirement. Some coatings can achieve super-hydrophobic and flame-retardant surface, but the preparation process is complex and the cost is high (Chinese invention patent 201510053494.4; Chenshangshan, Jilin university, Master thesis 2014). At present, no water-based fabric finishing agent which can resist flame, water, oil and ice and can resist washing is available in the market.
Disclosure of Invention
In view of the above, the invention aims to provide a flame-retardant, hydrophobic, oleophobic and deicing finishing agent for fabrics, which endows the fabrics with excellent performances such as flame retardance, hydrophobicity, oleophobicity, deicing and water washing resistance through the low surface energy of a fluorine-containing water repellent agent and the flame-retardant and crosslinking characteristics of a closed flame-retardant polyisocyanate crosslinking agent.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a flame-retardant, hydrophobic, oleophobic and deicing finishing agent for fabrics is prepared from the following raw materials in parts by weight: 100 parts of water, 2-5 parts of water repellent agent and 0.5-4 parts of cross-linking agent; the cross-linking agent is blocked flame-retardant polyisocyanate prepared from a flame retardant, polyisocyanate and a blocking agent.
The fabric is coated with the flame-retardant, hydrophobic, oleophobic and deicing finishing agent, so that the fabric has excellent water repellency, oleophobic and deicing performance due to the low surface energy characteristic, and the closed flame-retardant polyisocyanate crosslinking agent has good flame retardance and can perform crosslinking reaction with the water repellent agent, so that the flame retardance and water washing resistance are provided for the coating while the water repellency, oleophobic and deicing performance are not influenced.
Further, the anti-splashing agent is fluorine-containing acrylate; the macromolecular main chain of the fluorine-containing acrylate contains lateral hydroxyl groups for crosslinking and also contains longer fluorocarbon side chains.
Further, the structure of the blocked flame-retardant polyisocyanate is as follows:
wherein A represents a blocking agent, B represents polyisocyanate, and C represents a flame retardant.
Further, the flame retardant has the structure:
the flame retardant of the phosphate (phosphonate) ester and the melamine phosphate type flame retardant has good flame retardant property, and then hydroxyl or amino groups at two ends can react with isocyanate.
Further, R is1、R2、R3、R4The structure of (A) is as follows:
further, the structure of R in the end-capping agent is as follows:
Further, the blocked flame-retardant polyisocyanate is prepared by a preparation method comprising the following steps:
(1) respectively dissolving a flame retardant and polyisocyanate in a solvent, dropwise adding the flame retardant solution into an isocyanate solution according to the molar ratio of hydroxyl or amino to isocyanato of 1:1, and stirring for 30-60min to prepare the flame-retardant polyisocyanate;
(2) and (3) under the protection of nitrogen, dropwise adding the flame-retardant polyisocyanate into the blocking agent solution, heating to 80 ℃, reacting for 30min, and drying to obtain the closed flame-retardant polyisocyanate.
The invention also provides a preparation method of the flame-retardant, hydrophobic, oleophobic and anti-icing finishing agent for the fabric, which comprises the following steps:
adding the anti-splashing agent and the cross-linking agent into water at room temperature, stirring for 30min at the rotating speed of 500, stopping stirring, standing for 2h to remove bubbles, and preparing the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric.
The invention also provides an application method of the flame-retardant, hydrophobic, oleophobic and anti-icing finishing agent for the fabric, which comprises the following steps:
(1) soaking the fabric in the flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for 1-2min at room temperature, taking out, and padding in a padding machine under the padding pressure of 0.25 Mpa;
(2) and (3) placing the fabric obtained in the step (1) in an oven at the temperature of 120-170 ℃ for baking for 1-10 min.
The invention also provides application of the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric to protective clothing of firefighters.
Compared with the prior art, the flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for the fabric and the preparation and application methods thereof have the following advantages:
(1) the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric, disclosed by the invention, has the advantages that by introducing the fluorine-containing water splashing preventive agent with the characteristic of low surface energy, the fabric is endowed with excellent water splashing preventive, oleophobic and deicing performances, so that a fireman can be ensured to be capable of performing rescue work comfortably and efficiently in high-temperature and low-temperature environments. A flame retardant is introduced into the finishing agent, so that the fabric is endowed with excellent flame retardant property, and further guarantee is provided for the safety of firefighters; meanwhile, the flame retardant is reacted on the polyisocyanate crosslinking agent, so that the flame retardant loss and the reduction of the flame retardant performance of the fabric caused in the normal use and cleaning processes of the fabric when the flame retardant is directly added to the finishing agent are avoided.
(2) The method for processing the fabric by using the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric is simple and easy to implement, and the finishing agent has small influence on the vision and hand feeling of the fabric.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail with reference to examples.
Example 1:
the preparation method of the closed flame-retardant polyisocyanate comprises the following steps:
(1) respectively dissolving phosphonate flame retardant (structural formula shown in table 1) and hexamethylene diisocyanate in a toluene solvent according to a molar ratio of hydroxyl to isocyanate of 1:1, dropwise adding the phosphonate flame retardant solution into an isocyanate hexamethylene diisocyanate solution under stirring at a rotating speed of 200, continuously stirring for 30min, and drying to prepare flame-retardant polyisocyanate;
(2) and (3) under the protection of nitrogen, dropwise adding the flame-retardant polyisocyanate into the phenol blocking agent solution, heating to 80 ℃, reacting for 30min, and drying to obtain the enclosed flame-retardant polyisocyanate.
A preparation method of a flame-retardant, hydrophobic, oleophobic and deicing finishing agent for fabrics comprises the following steps:
taking 2 parts of C8 type water repellent agent (TG-581, Japan Dajin company, with the solid content of 30 wt%), 0.5 part of closed flame-retardant polyisocyanate and 100 parts of water, adding the water repellent agent and a cross-linking agent into the water at room temperature, stirring for 30min at the rotating speed of 500, stopping stirring, standing for 2h to remove bubbles, and preparing the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric.
A method of applying a flame retardant, hydrophobic, oleophobic, icephobic finish to a fabric, the method comprising the steps of:
(1) soaking aramid fiber fabric in flame retardant, hydrophobic, oleophobic and ice-phobic finishing agent for fabric at room temperature for 1min, taking out, and padding in a padding machine under padding pressure of 0.25 Mpa;
(2) repeating the dipping and padding steps for 2 times;
(3) and (3) placing the padded fabric in an oven at 120 ℃ for 5min to obtain the fabric with the functions of flame retardance, hydrophobicity, oleophobicity and deicing.
Compared with the example 1, the preparation steps of the examples 2 to 5 and the comparative examples 1 to 3 are basically the same, and only the types and the contents of the flame retardant, the isocyanate, the water repellent agent and the blocking agent are different, and the specific types and the contents of the flame retardant, the isocyanate, the water repellent agent and the blocking agent in the examples and the comparative examples are shown in the table 1.
TABLE 1 examples and comparative example specific formulations (units of each component are parts by weight)
Testing the water-soaking grade of the aramid fiber fabric treated by the finishing agent according to GB/T4745 plus 2012 'method for detecting and evaluating the water-soaking performance of textiles', and testing the binding force between the surface of the fabric and ice by using a horizontal pushing method (precooling for 2h by water in a plastic sleeve mold); simultaneously, respectively taking the treated fabric, performing machine washing and water flow impact for a period of time, and measuring the water-dipping grade and ice-pushing shearing force of the fabric surface again after drying; the machine washing is to put the fabric into a washing machine and add a certain amount of tap water (submerge the fabric) to wash for 30 minutes, 50 times in total; the water flow impact test is to put the fabric under the water flow with the impact force of 105.3kPa for 2 h; the flame retardant performance of the fabric is characterized by testing the limit oxygen index of the fabric, and the limit oxygen index is tested according to GB/T5454-1997 textile combustion performance test oxygen index method.
Table 2 shows the test results in examples and comparative examples, including the water pick-up level, icicle bonding force, water pick-up level after machine washing and water flow impingement, icicle bonding force after machine washing and water flow impingement, limiting oxygen index, and the like.
TABLE 2 test results of examples 1 to 5 and comparative examples 1 to 3
And (4) analyzing results:
in conclusion, untreated fabric samples are strong in hydrophilicity, easy to freeze, strong in ice binding force and difficult to remove; the hydrophobic and ice-shedding performance of the fabric treated by the fluorine-containing acrylate is obviously improved, but the hydrophobic and ice-shedding performance of the fabric is obviously reduced due to the loss of the fluorine-containing acrylate after washing because the adhesion force of the fabric is weaker; after further introducing isocyanate, the water washing resistance of the treated fabric sample is obviously improved, and the hydrophobic and ice-phobic properties of the washed fabric are basically kept unchanged; the flame retardant property of the fabric can be further improved by introducing the closed flame retardant isocyanate; meanwhile, with the improvement of the content of the flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent, the performances of hydrophobicity, ice-phobicity, flame retardance, water washing resistance and the like of the treated fabric are gradually improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric is characterized in that: the finishing agent is prepared from the following raw materials in parts by weight: 100 parts of water, 2-5 parts of water repellent agent and 0.5-4 parts of cross-linking agent; the cross-linking agent is blocked flame-retardant polyisocyanate prepared from a flame retardant, polyisocyanate and a blocking agent.
2. A flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 1, characterized in that: the anti-splashing agent is fluorine-containing acrylate; the macromolecular main chain of the fluorine-containing acrylate contains lateral hydroxyl groups for crosslinking and also contains longer fluorocarbon side chains.
3. A flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 1, characterized in that: the structure of the closed flame-retardant polyisocyanate is as follows:
wherein A represents a blocking agent, B represents polyisocyanate, and C represents a flame retardant.
4. A flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 3, characterized in that: the structure of the flame retardant is as follows:
5. a flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 4, characterized in that: the R is1、R2、R3、R4The structure of (A) is as follows:
6. a flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 3, characterized in that: the structure of the end-capping agent R is as follows:
7. A flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to claim 1, characterized in that: the blocked flame-retardant polyisocyanate is prepared by a preparation method comprising the following steps:
(1) respectively dissolving a flame retardant and polyisocyanate in a solvent, dropwise adding the flame retardant solution into an isocyanate solution according to the molar ratio of hydroxyl or amino to isocyanato of 1:1, and stirring for 30-60min to prepare the flame-retardant polyisocyanate;
(2) and (3) under the protection of nitrogen, dropwise adding the flame-retardant polyisocyanate into the blocking agent solution, heating to 80 ℃, reacting for 30min, and drying to obtain the closed flame-retardant polyisocyanate.
8. A process for the preparation of a flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics according to any of claims 1-7, characterized in that: the method comprises the following steps:
adding the anti-splashing agent and the cross-linking agent into water at room temperature, stirring for 30min at the rotating speed of 500, stopping stirring, standing for 2h to remove bubbles, and preparing the flame-retardant, hydrophobic, oleophobic and deicing finishing agent for the fabric.
9. A method of using a flame retardant, hydrophobic, oleophobic, and icephobic finish for a fabric according to any of claims 1-7, characterized by: the method comprises the following steps:
(1) soaking the fabric in the flame-retardant, hydrophobic, oleophobic and ice-phobic finishing agent for 1-2min at room temperature, taking out, and padding in a padding machine under the padding pressure of 0.25 Mpa;
(2) and (3) placing the fabric obtained in the step (1) in an oven at the temperature of 120-170 ℃ for baking for 1-10 min.
10. Use of a flame retardant, hydrophobic, oleophobic, icephobic finish for fabrics as defined in any of claims 1-7 on firefighter protective apparel.
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| CN114409697A (en) * | 2022-02-25 | 2022-04-29 | 青岛长荣化工科技有限公司 | Double-end hydroxyl reaction type flame retardant and preparation method thereof |
| CN114524843A (en) * | 2022-02-25 | 2022-05-24 | 青岛长荣化工科技有限公司 | Hydroxyl-terminated reactive flame retardant and preparation method thereof |
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