CN105113231A - Fabric with expansive type flame retardant coatings on surfaces and preparation method of fabric - Google Patents
Fabric with expansive type flame retardant coatings on surfaces and preparation method of fabric Download PDFInfo
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- CN105113231A CN105113231A CN201510594672.4A CN201510594672A CN105113231A CN 105113231 A CN105113231 A CN 105113231A CN 201510594672 A CN201510594672 A CN 201510594672A CN 105113231 A CN105113231 A CN 105113231A
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Abstract
The invention discloses a fabric with expansive type flame retardant coatings on surfaces and a preparation method of the fabric. Two surfaces of the fabric are coated with at least one composite coating formed by a polyelectrolyte complexe layer and an ammonium polyphosphate layer, and the polyelectrolyte complexe layer and the ammonium polyphosphate layer in the composite coating are taken as an inner layer and an outer layer respectively. The preparation method of the fabric comprises that a polyelectrolyte complexe solution and an ammonium polyphosphate solution are prepared. The fabric is soaked in enough polyelectrolyte complexe solution thoroughly, cleaned in ionized water and dried in vacuum; then the fabric is soaked in enough ammonium polyphosphate solution thoroughly, cleaned in ionized water and dried in vacuum; the above steps are repeated for a plurality of time, and the fabric with the expansive type flame retardant coatings on the surfaces is obtained. The preparation method is simple, easy to implement and high in efficiency, and the flame retardant property of the processed fabric is excellent; and the fabric has a wide application prospect and a practical value in the aspect of improving textile fire safety.
Description
Technical field
The present invention relates to a kind of fabric and preparation method thereof, especially relate to a kind of surface fabric with expansion type flame-retardant coatings and preparation method thereof.
Background technology
Cotton and fiber crops wait fabric to play key player in people's daily life.But this kind fabric is easy to burning, and flame propagation speed after burning, thus constrain its extensive use.Therefore, wait fabric to carry out flame treatment to cotton and fiber crops and there is certain theory and practical value.Usually, to cotton and fiber crops wait fabric carry out flame treatment often adopt pad-bake, the method such as sol-gel or graft modification, need special instrument and equipment or the preparation technology of complexity.In recent years, layer assembly method due to easy and simple to handle, flexibly and good stability, the application in fabrics flame resistance process causes great interest in the industry.But the expansion type flame-retardant coatings built based on layer assembly method of report, often operates consuming time at present, only good flame retardant effect could be shown when assembling the number of plies and being larger.Often molecular dimension is less for the module units for layer assembly of current report, and operating efficiency is low, could show good flame retardant effect when being only assembled to about 20 layers.Therefore, how adopting simple and efficient way to prepare expansion type flame-retardant coatings is fast a problem demanding prompt solution.
Summary of the invention
In order to overcome Problems existing in background technology, the object of the present invention is to provide a kind of surface fabric with expansion type flame-retardant coatings and preparation method thereof.The present invention utilizes layer assembly method to build Intumscent Flame Retardant System, is because of its good flame retardation effect and environmental protection.
For achieving the above object, the technical scheme that the present invention solves the employing of its technical problem is:
One, a kind of surface has the fabric of expansion type flame-retardant coatings:
Be covered with the combination coating that at least one deck is formed by polyelectrolyte complex compound layer and APP layer on two surfaces of fabric, in combination coating, polyelectrolyte complex compound layer and APP layer are respectively as internal layer and skin.
Described fabric is cotton fiber or hemp fabric.
Described polyelectrolyte complex compound is the polyelectrolyte complex compound of polyphosphoric acids and polymine, and in polyelectrolyte complex compound, the mass ratio of polyphosphoric acids and polymine is 4-0.25:1.
Two, surface has a preparation method for the fabric of expansion type flame-retardant coatings, comprises the following steps:
1) polyelectrolyte complex compound solution and APP solution is prepared;
2) fabric is fully soaked 1 ~ 5min in enough polyelectrolyte complex compound solution, clean 2 times in deionized water, vacuumize; Then in enough APP solution, fully soak 1 ~ 5min, clean 2 times in deionized water, vacuumize;
3) step 2 is repeated) several times, obtain the fabric that described surface has expansion type flame-retardant coatings.
Described polyelectrolyte complex compound solution is prepared in the following ways: under normal temperature, with stirring, be 1.0-4.0wt% by concentration, pH value is that dropwise to drop to concentration be in the polyethylenimine solution of 1.0-4.0wt% for the poly phosphoric acid solution of 5.0-10.0, adopt hydrochloric acid or acetic acid dilute solution that pH value is adjusted to 5.0-10.0, obtain the polyelectrolyte complex compound solution of polyphosphoric acids that total soluble matters concentration is 0.5-2.0wt% and polymine, in polyelectrolyte complex compound, the mass ratio of polyphosphoric acids and polymine is 4-0.25:1.
Described APP solution is prepared in the following ways: under normal temperature, with stirring, the ammonium polyphosphate powder of drying is scattered in deionized water, add the sodium hydroxide solution of 1mol/L to transparent glutinous fluid, add the glacial acetic acid solution of 1mol/L to clear solution, adopt acid solution or aqueous slkali that pH value is adjusted to 5.0-10.0, obtain the APP solution that concentration is 0.5-2.0wt%.
Described acid solution adopts hydrochloric acid solution or acetum, and described aqueous slkali adopts sodium hydroxide solution.
The solution quality of described sodium hydroxide solution is identical with the solution quality of glacial acetic acid solution, and 5-20 is doubly to APP quality.
Described fabric is cotton fiber or hemp fabric.
Compared with background technology, the invention has the beneficial effects as follows:
Preparation method of the present invention is simple and operating efficiency is high.The present invention given full play to the large advantage of polyelectrolyte complex compound size, and rapid build expansion type flame-retardant coatings, the fabric after process has good fire resistance.The present invention has broad application prospects and practical value in the fire safety improving textiles.
Accompanying drawing explanation
Fig. 1 is the heat release rate curve of the pure ramie fabric without flame treatment.
Fig. 2 is the heat release rate curve that the ramie fabric of expansion type flame-retardant coatings is contained on surface that embodiment 1 prepares.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Embodiments of the invention are as follows:
The polyphosphoric acids adopted in embodiment, polymine, hydrochloric acid, APP, NaOH, COTTON FABRIC and ramie fabric are commercial material.Wherein, polyphosphoric acids, P
2o
5content>=85%; Polymine is branching type, M
w=25000, M
n=10000; APP, degree of polymerization >1000, phosphorus content: 28.0-30.0wt%.
Embodiment 1:
(1) under normal temperature, be under the magnetic agitation of 1000r/min in speed, be 1.0wt% by 100mL concentration, pH value be 10.0 poly phosphoric acid solution dropwise to drop to 100mL concentration be in the polyethylenimine solution of 1.0wt%, add deionized water, adopt hydrochloric acid or acetum that pH value is adjusted to 10.0, obtain the polyelectrolyte complex compound solution of polyphosphoric acids that 400mL concentration is 0.5wt% and polymine;
(2) under normal temperature, be under the mechanical agitation of 500r/min in speed, the ammonium polyphosphate powder of 4g drying is scattered in 200mL deionized water, add the 1mol/L sodium hydroxide solution of 40g to transparent glutinous fluid, add the 1mol/L hydrochloric acid solution of 40g to clear solution, add deionized water, adopt hydrochloric acid solution or sodium hydroxide solution that pH value is adjusted to 10.0, obtain the APP solution that 400mL concentration is 1.0wt%;
(3) 1min is soaked in the polyphosphoric acids formed in step (1) by ramie fabric (length x width: 400mm × 90mm) and the polyelectrolyte complex compound solution of polymine, by 500mL washed with de-ionized water 2 times, vacuumize at 60 DEG C; 1min is soaked in the APP solution formed in the step (2), by 500mL washed with de-ionized water 2 times, vacuumize at 60 DEG C;
(4) repeat step (3) 4 times, obtain the fabric that described surface has expansion type flame-retardant coatings, its clean quality increment is 15wt%.
Fire resistance test result is in table 1 and Fig. 2.Contrast the pure ramie fabric (fire resistance test result is in table 1 and Fig. 1) without flame treatment, can find out, the expansion type flame-retardant coatings of described structure significantly reduces HRR peak value (PHRR) and total heat release (THR), demonstrates good flame retardant effect.
Embodiment 2:
(1) under normal temperature, be under the magnetic agitation of 1000r/min in speed, be 3.0wt% by 200mL concentration, pH value be 7.0 poly phosphoric acid solution dropwise to drop to 50mL concentration be in the polyethylenimine solution of 3.0wt%, add deionized water, adopt hydrochloric acid or acetum that pH value is adjusted to 7.0, obtain the polyelectrolyte complex compound solution of polyphosphoric acids that 750mL concentration is 1.0wt% and polymine;
(2) under normal temperature, be under the mechanical agitation of 500r/min in speed, the ammonium polyphosphate powder of 3g drying is scattered in 200mL deionized water, add the 1mol/L sodium hydroxide solution of 15g to transparent glutinous fluid, add the 1mol/L hydrochloric acid solution of 15g to clear solution, add deionized water, adopt hydrochloric acid solution or sodium hydroxide solution that pH value is adjusted to 5.0, obtain the APP solution that 600mL concentration is 0.5wt%;
(3) 2min is soaked in the polyphosphoric acids formed in step (1) by ramie fabric (length x width: 400mm × 90mm) and the polyelectrolyte complex compound solution of polymine, by 750mL washed with de-ionized water 2 times, vacuumize at 60 DEG C; 2min is soaked in the APP solution formed in the step (2), by 600mL washed with de-ionized water 2 times, vacuumize at 60 DEG C;
(4) repeat step (3) 3 times, obtain the fabric that described surface has expansion type flame-retardant coatings, its clean quality increment is 14wt%.
Fire resistance test result is in table 1.
Embodiment 3:
(1) under normal temperature, be under the magnetic agitation of 1000r/min in speed, be 4.0wt% by 50mL concentration, pH value be 5.0 poly phosphoric acid solution dropwise to drop to 200mL concentration be in the polyethylenimine solution of 4.0wt%, add deionized water, adopt hydrochloric acid or acetum that pH value is adjusted to 5.0, obtain the polyelectrolyte complex compound solution of polyphosphoric acids that 500mL concentration is 2.0wt% and polymine;
(2) under normal temperature, be under the mechanical agitation of 500r/min in speed, the ammonium polyphosphate powder of 10g drying is scattered in 50mL deionized water, add the 1mol/L sodium hydroxide solution of 200g to transparent glutinous fluid, add the 1mol/L hydrochloric acid solution of 200g to clear solution, add deionized water, adopt hydrochloric acid solution and sodium hydroxide solution that pH value is adjusted to 7.0, obtain the APP solution that 500mL concentration is 2.0wt%;
(3) 5min is soaked in the polyphosphoric acids formed in step (1) by ramie fabric (length x width: 400mm × 90mm) and the polyelectrolyte complex compound solution of polymine, by 500mL washed with de-ionized water 2 times, vacuumize at 60 DEG C; 5min is soaked in the APP solution formed in the step (2), by 500mL washed with de-ionized water 2 times, vacuumize at 60 DEG C.
(4) repeat step (3) 2 times, obtain the fabric that described surface has expansion type flame-retardant coatings, its clean quality increment is 17wt%.
Fire resistance test result is in table 1.
Each embodiment of the present invention has all carried out fire resistance test, and the ramie fabric fire resistance test result of gained surface containing expansion type flame-retardant coatings is as shown in table 1, and its empty sample is not containing the pure ramie fabric of expansion type flame-retardant coatings.Fire resistance method of testing: miniature calorimeter (GovmarkMCC-2, the U.S.), oxygen gas flow rate: 20mL/min, nitrogen flow rate: 80mL/min, sample is constant temperature 5min at 100 DEG C first, is then warming up to 700 DEG C with the speed of 1 DEG C/sec.
Table 1
In table 1: PHRR: HRR peak value, unit W/g; THR: total heat release, unit kJ/g.
In analytical table 1, data are known, expansion type flame-retardant coatings of the present invention serves good fire retardation to ramie fabric, and simple operating efficiency is high, and technique effect is given prominence to, have broad application prospects and practical value in the fire safety improving textiles.
Above-described embodiment is only used for explaining the present invention, instead of limits the scope of the invention.Any equivalence change made in Spirit Essence of the present invention and claims or modification, be all considered as in protection scope of the present invention.
Claims (9)
1. a surface has the fabric of expansion type flame-retardant coatings, it is characterized in that: be covered with the combination coating that at least one deck is formed by polyelectrolyte complex compound layer and APP layer on two surfaces of fabric, in combination coating, polyelectrolyte complex compound layer and APP layer are respectively as internal layer and skin.
2. a kind of surface according to claim 1 has the fabric of expansion type flame-retardant coatings, it is characterized in that: described fabric is cotton fiber or hemp fabric.
3. a kind of surface according to claim 1 has the fabric of expansion type flame-retardant coatings, it is characterized in that: described polyelectrolyte complex compound is the polyelectrolyte complex compound of polyphosphoric acids and polymine, in polyelectrolyte complex compound, the mass ratio of polyphosphoric acids and polymine is 4-0.25:1.
4. surface has a preparation method for the fabric of expansion type flame-retardant coatings, it is characterized in that comprising the following steps:
1) polyelectrolyte complex compound solution and APP solution is prepared;
2) fabric is fully soaked 1 ~ 5min in enough polyelectrolyte complex compound solution, clean 2 times in deionized water, vacuumize; Then in enough APP solution, fully soak 1 ~ 5min, clean 2 times in deionized water, vacuumize;
3) step 2 is repeated) several times, obtain the fabric that described surface has expansion type flame-retardant coatings.
5. a kind of surface according to claim 4 has the preparation method of the fabric of expansion type flame-retardant coatings, it is characterized in that: described polyelectrolyte complex compound solution is prepared in the following ways: under normal temperature, with stirring, be 1.0-4.0wt% by concentration, pH value is that dropwise to drop to concentration be in the polyethylenimine solution of 1.0-4.0wt% to the poly phosphoric acid solution of 5.0-10.0, adopt hydrochloric acid or acetic acid dilute solution that pH value is adjusted to 5.0-10.0, obtain the polyelectrolyte complex compound solution of polyphosphoric acids that total soluble matters concentration is 0.5-2.0wt% and polymine, in polyelectrolyte complex compound, the mass ratio of polyphosphoric acids and polymine is 4-0.25:1.
6. a kind of surface according to claim 4 has the preparation method of the fabric of expansion type flame-retardant coatings, it is characterized in that: described APP solution is prepared in the following ways: under normal temperature, with stirring, the ammonium polyphosphate powder of drying is scattered in deionized water, add the sodium hydroxide solution of 1mol/L to transparent glutinous fluid, add the glacial acetic acid solution of 1mol/L to clear solution, adopt acid solution or aqueous slkali that pH value is adjusted to 5.0-10.0, obtain the APP solution that concentration is 0.5-2.0wt%.
7. a kind of surface according to claim 6 has the preparation method of the fabric of expansion type flame-retardant coatings, it is characterized in that: described acid solution adopts hydrochloric acid solution or acetum, and described aqueous slkali adopts sodium hydroxide solution.
8. a kind of surface according to claim 6 has the preparation method of the fabric of expansion type flame-retardant coatings, it is characterized in that: the solution quality of described sodium hydroxide solution is identical with the solution quality of glacial acetic acid solution, and 5-20 is doubly to APP quality.
9. a kind of surface according to claim 4 has the preparation method of the fabric of expansion type flame-retardant coatings, it is characterized in that: described fabric is cotton fiber or hemp fabric.
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CN105566683A (en) * | 2015-12-25 | 2016-05-11 | 中国科学院宁波材料技术与工程研究所 | Supermolecular flame retardant based on ionic bonds and preparation method thereof |
CN105755836A (en) * | 2016-04-25 | 2016-07-13 | 浙江大学宁波理工学院 | Three-component layer-by-layer self-assembly flame-retardant modified ramie fabric and preparation method thereof |
WO2017091976A1 (en) * | 2015-12-01 | 2017-06-08 | 陈杰 | Expansion flame retardant system for mattress or pillow inner-sleeve filler flame retardation and method therefor |
CN109912804A (en) * | 2019-03-28 | 2019-06-21 | 南京林业大学 | A kind of preparation method of phosphorus nitrogen modified lignin resin base expansibility flame-proof agent |
CN110777531A (en) * | 2019-11-21 | 2020-02-11 | 闽江学院 | Modified wool fabric and preparation method thereof |
CN112359597A (en) * | 2020-12-07 | 2021-02-12 | 东华大学 | Organic/inorganic hybrid film-coated cotton textile and preparation method thereof |
CN114701230A (en) * | 2022-03-25 | 2022-07-05 | 龙岩东腾再生资源科技有限公司 | Needle cotton with good flame-retardant effect and processing method thereof |
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Cited By (11)
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WO2017091976A1 (en) * | 2015-12-01 | 2017-06-08 | 陈杰 | Expansion flame retardant system for mattress or pillow inner-sleeve filler flame retardation and method therefor |
CN105566683A (en) * | 2015-12-25 | 2016-05-11 | 中国科学院宁波材料技术与工程研究所 | Supermolecular flame retardant based on ionic bonds and preparation method thereof |
CN105566683B (en) * | 2015-12-25 | 2018-12-25 | 中国科学院宁波材料技术与工程研究所 | A kind of supermolecule fire retardant and preparation method thereof based on ionic bond |
CN105755836A (en) * | 2016-04-25 | 2016-07-13 | 浙江大学宁波理工学院 | Three-component layer-by-layer self-assembly flame-retardant modified ramie fabric and preparation method thereof |
CN105755836B (en) * | 2016-04-25 | 2017-11-28 | 浙江大学宁波理工学院 | A kind of three flame-retardant modified ramie fabrics of component LBL self-assembly and preparation method thereof |
CN109912804A (en) * | 2019-03-28 | 2019-06-21 | 南京林业大学 | A kind of preparation method of phosphorus nitrogen modified lignin resin base expansibility flame-proof agent |
CN109912804B (en) * | 2019-03-28 | 2021-04-02 | 南京林业大学 | Preparation method of phosphorus-nitrogen modified lignin-based intumescent flame retardant |
CN110777531A (en) * | 2019-11-21 | 2020-02-11 | 闽江学院 | Modified wool fabric and preparation method thereof |
CN112359597A (en) * | 2020-12-07 | 2021-02-12 | 东华大学 | Organic/inorganic hybrid film-coated cotton textile and preparation method thereof |
CN112359597B (en) * | 2020-12-07 | 2022-02-18 | 东华大学 | Organic/inorganic hybrid film-coated cotton textile and preparation method thereof |
CN114701230A (en) * | 2022-03-25 | 2022-07-05 | 龙岩东腾再生资源科技有限公司 | Needle cotton with good flame-retardant effect and processing method thereof |
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Effective date of registration: 20200901 Address after: 312000 Zhejiang Province, Shaoxing city Keqiao District Qianqing Town Village relic Patentee after: Zhejiang Pengyue Textile Co., Ltd Address before: 310018, No. 928, No. 2, Poplar Street, Jianggan Economic Development Zone, Hangzhou, Zhejiang Patentee before: Zhejiang University of Technology |