CN105088763A - Production process for flame-retarding textile - Google Patents
Production process for flame-retarding textile Download PDFInfo
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- CN105088763A CN105088763A CN201510562921.1A CN201510562921A CN105088763A CN 105088763 A CN105088763 A CN 105088763A CN 201510562921 A CN201510562921 A CN 201510562921A CN 105088763 A CN105088763 A CN 105088763A
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Abstract
The invention relates to a production process for flame-retarding textile. The production process is characterized by comprising the steps of textile padding sorting, drying, baking, alkali cleaning, water washing, stoving and the like. The textile processed through the production process is good in flame-retarding property and has higher limit oxygen index.
Description
Technical field
The present invention relates to a kind of textile production technique, especially relate to a kind of production technology of flame retardant textiles.
Background technology
Fire retardant is that a class can stop polymeric material to ignite or suppress the additive of flame propagation.The cellulose fire retardant produced both at home and abroad at present or study is many, wherein a part is phosphorous and fire retardant that is halogen, the Tetrakis hydroxymethyl phosphonium chloride (THPC) such as developed by Britain's Albright-Wilson's (Albright & Wilson) company's nineteen fifty-five, this fire retardant has good flame retardant effect for cellulose, but in use Diazolidinyl Urea, and halogen-containing flame retardant can produce toxic gas in the process of decomposes; Also have not halogen-containing, the fire retardant containing phosphorus, nitrogen, the N-dihydroxymethyl phosphono acrylamide (NMDPPA, i.e. PyrovatexCP) of such as Ciba Co., Ltd exploitation, domestic like product has the FRC-2 of Changzhou Chemical Engineering Inst..The flame retardant effect of the cellulose base fiber fabrics such as bamboo, cotton, fiber crops, viscose glue after this based flame retardant arranges can reach the B1 level in GB, and flame retardant effect has good washability, but the fabric after arranging can discharge free formaldehyde, and fabric feeling can harden.Therefore these fire retardants do not meet the requirement of ecological textile, and treated fabric feeling is not soft yet.
For this reason, researcher begins one's study exploitation low toxicity, halogen, meet environmental protection and efficient cellulose fire retardant, the fire retardant mulberry De Fulanmu (Sandoflam) 5060 of the STR-27 fire retardant that such as Shanghai Textile research institute successfully synthesizes and the exploitation of Lenzin (Lenzing) company, these two kinds of fire retardants contain sulphur P elements, not halogen-containing, be in existing at present cellulose fire retardant preferably, but in the preparation process of fire resistant cellulose product, the flame retardant additives amount needed is larger (is generally more than 20% of cellulose, or it is higher, just flame-retardancy requirements can be reached), therefore flame retarding efficiency is not high, cost is also larger, simultaneously, the fire retardant addition of vast scale also can make the hydraulic performance decline of product crude oil.
Therefore, for cellulose base fiber fabric, developing a kind of durable fire retardant meeting ecological textile requirement, is the key solving current problem.If one can be provided both to have had good durable flame-retardant effect, suitably can improve again the environment friendly flame retardant of fabric feeling, good prospect will be had for applying of product.
Along with the progress of science and technology, the raising of people's living standard; the demand of fire-retardant weaving face fabric is increasing; in numerous COTTON FABRIC antiflaming finishing agent, tetra methylol based flame retardant (THPC or THPOH) and N-methylol-3-dimethoxy phosphoryl Propionamides fire retardant (trade name PyrovatexCP) are current the most frequently used fire retardant kinds, but this two based flame retardant all exists the release And Spread of Solute of free formaldehyde.What Chinese invention patent application CN103321044A disclosed a kind of Flame Retarded Silk Fibers the invention discloses a kind of flame-retardant pure silk and preparation method thereof, adopt electrostatic self-assembled technology by dipping shitosan and sodium phytate solution prepare flame-retardant pure silk successively, sodium phytate is deposited on real silk by the electrostatic attraction between sodium phytate and shitosan by the method, and the method needs repeatedly repeated impregnations shitosan and sodium phytate solution.
As from the foregoing, the fire retardant of current successful market is the chemicals of synthesis, and there is the problem of release free formaldehyde; New disclosed natural fire retardant sodium phytate, to real silk, there is good flame retardant effect, but be to be combined with the electrostatic attraction of sodium phytate by shitosan to realize between fire retardant with silk, its washability is unknown, and the preparation of this conduction silk broadcloth needs repeatedly repeatedly to flood shitosan and sodium phytate, operation bothers relatively.
Summary of the invention
The applicant, for above-mentioned market demand, is studied improvement, provides a kind of production technology of flame retardant textiles.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A production technology for flame retardant textiles, is characterized in that comprising the steps:
(1) preliminary treatment of textiles: pending textiles is dipped in clear water, ultrasonic 10-30min, takes out, and dries at 60-80 DEG C, stand-by;
(2) fire retarding treating liquid is prepared: join in the organic solvent of 30 ~ 200ml by 0.05 ~ 0.1mol formula I, 0.01 ~ 0.03mol crosslinking agent N hydroxymethyl acrylamide, 0.01 ~ 0.02mol dispersant lauryl sodium sulfate, at 50 ~ 80 DEG C, stirring reaction 0.5 ~ 2h, obtains fire retarding treating liquid; Described formula I is as follows:
(3) flame-proof treatment: after textiles is flooded 15 ~ 20 minutes in above-mentioned fire retarding treating liquid, two leachings two are rolled, pick-up 80 ~ 105%, then by textiles drying 5 ~ 10 minutes at 60 ~ 90 DEG C, then cures 2 ~ 8 minutes at 150 ~ 180 DEG C;
(4) post-drying of alkali cleaning, washing.
Preferably, described organic solvent is at least one in methyl alcohol, ethanol, isopropyl alcohol, n-butanol, acetone, espeleton, methylisobutylketone, acetonitrile, pyridine, phenol, DMF.
Preferably, described textiles is COTTON FABRIC.
The multiple flat wash trough of described caustic scrubbing step, the sodium carbonate of the first groove perfusion 10g/L, the sodium carbonate of the second groove perfusion 5g/L, the sodium carbonate of the 3rd groove perfusion 5g/L.
The invention also discloses the compound shown in a kind of formula I, it can be used for textile treatment.
The present invention has following beneficial effect:
1, the present invention first utilizes Cement Composite Treated by Plasma textiles, and the textiles after process loosens, and containing various active group.
2, novel formula I is adopted to form water proof fire retardant dressing liquid, when textiles after Cement Composite Treated by Plasma is transferred to and arranges in water proof fire retardant finishing agent, finishing agent can better be combined with textiles by crosslinking agent, and it is more firm, textiles soft comfortable after arrangement, has excellent water proof fire retardant performance.
3, in addition, in water proof fire retardant finishing agent, fire retardant, under the effect of dispersant, can realize well dispersion, thus better be cross-linked with textiles, and the fire retardant of the present invention's employing is asepsis environment-protecting shaped material, is conducive to environmental protection.
Embodiment
Below by embodiment, the invention will be further described.The method described in the embodiment of the present invention that it should be understood that is only used for the present invention is described, instead of limitation of the present invention, under concept thereof of the present invention, all belong to the scope of protection of present invention to the simple modifications of preparation method of the present invention.The all raw materials used in embodiment and solvent are all purchased from SigmaBiochemicalandOrganicCompoundsforResearchandDiagnos ticClinicalReagents company.
The preparation embodiment of formula I:
(1) cinnolines-3-ketone (1mmol), p-methyl benzenesulfonic acid (2mmol), N-bromo-succinimide (2mmol) are placed in round-bottomed flask, add DMF10mL, 100 DEG C are reacted 2 hours, and TLC display reaction is complete, stops reaction, add saturated sodium thiosulfate solution, extraction into ethyl acetate, merges organic phase, crosses silica gel chromatography, obtain white solid powder, yield 44%.
(2) product (1mmol) of step (1), thio-oxamide ethyl ester (3mmol) are placed in round-bottomed flask, add 10mL methyl alcohol, stirring at room temperature 24 hours, TLC display reaction is complete, stops reaction, add 20mL water, extraction into ethyl acetate, merges organic phase, crosses silica gel chromatography, obtain Tan solid powder, yield 63%.
(3) step (2) product (1mmol), hydrazine hydrate (2mmol) are placed in round-bottomed flask, add 10mL ethanol, back flow reaction, TLC display reaction is complete, stops reaction, cool to room temperature, filter, obtain white solid powder, yield 72%.
(4) step (3) product (1mmol), P-methoxybenzal-dehyde (1.5mmol) are placed in round-bottomed flask, add 10mL ethanol, back flow reaction 5 hours, TLC display reaction is complete, cool to room temperature, steaming desolventizes, and crosses silica gel chromatographic column and is separated, obtain the formula I of white solid powder, yield 79%.
1HNMR(d
6-DMSO,400MHz)δ:3.81(s,CH
3,3H),7.11(d,2CH,2H),7.27(d,CH,H),7.43(m,CH,H),7.66(d,2CH,2H),7.81(m,CH,H),8.07(d,CH,H),8.16(m,CH,H),8.61(s,CH,H),9.93(s,CH,H),12.26(s,NH,H).
Embodiment 1:
(1) preliminary treatment of textiles: pending COTTON FABRIC is dipped in clear water, ultrasonic 10min, takes out, and dries at 80 DEG C, stand-by;
(2) fire retarding treating liquid is prepared: join in the ethanol of 100ml by 0.05mol formula I, 0.01mol crosslinking agent N hydroxymethyl acrylamide, 0.01mol dispersant lauryl sodium sulfate, stirring reaction 1h, obtains fire retarding treating liquid at 80 DEG C;
(3) flame-proof treatment: after COTTON FABRIC is flooded 20 minutes in above-mentioned fire retarding treating liquid, two leachings two are rolled, pick-up 85%, then by COTTON FABRIC drying 10 minutes at 80 DEG C, then cures 2 minutes at 150 DEG C;
(4) post-drying of alkali cleaning, washing.
Embodiment 2:
(1) preliminary treatment of textiles: pending COTTON FABRIC is dipped in clear water, ultrasonic 30min, takes out, and dries at 80 DEG C, stand-by;
(2) fire retarding treating liquid is prepared: join in the acetone of 200ml by 0.1mol formula I, 0.03mol crosslinking agent N hydroxymethyl acrylamide, 0.02mol dispersant lauryl sodium sulfate, stirring reaction 2h, obtains fire retarding treating liquid at 80 DEG C;
(3) flame-proof treatment: after COTTON FABRIC is flooded 20 minutes in above-mentioned fire retarding treating liquid, two leachings two are rolled, pick-up 95%, then by textiles drying 10 minutes at 90 DEG C, then cures 8 minutes at 180 DEG C;
(4) post-drying of alkali cleaning, washing.
Embodiment 3:
(1) preliminary treatment of textiles: pending COTTON FABRIC is dipped in clear water, ultrasonic 20min, takes out, and dries at 70 DEG C, stand-by;
(2) fire retarding treating liquid is prepared: join in the organic solvent of 200ml by 0.08mol formula I, 0.03mol crosslinking agent N hydroxymethyl acrylamide, 0.02mol dispersant lauryl sodium sulfate, at 80 DEG C, stirring reaction 2h, obtains fire retarding treating liquid;
(3) flame-proof treatment: after COTTON FABRIC is flooded 20 minutes in above-mentioned fire retarding treating liquid, two leachings two are rolled, pick-up 90%, then by textiles drying 10 minutes at 90 DEG C, then cures 6 minutes at 180 DEG C;
(4) post-drying of alkali cleaning, washing.
The toxicity test of formula I:
The active detection by transfection of the PPAR δ of the compound represented by formula I of invention is confirmed.In addition, PPAR hypotype PPAR α and the selective of PPAR γ are also tested.Test cell toxicity is detected, by animal experiment study activity in vivo by MTT.
CV-1 cell is used in this detection.Described cell is seeded in 96 orifice plates containing the DMEM being added with 10%FBS, DBS (DBS, through degreasing) and 1% penicillin/streptomycin, and at 37 DEG C, 5%CO
2incubator in cultivate.Test and carry out according to the step of inoculation, transfection, sample administration and confirmation.Specifically, CV-1 cell is seeded to 96 orifice plates (5000 cells/well), transfection after 24 hours.By total length PPAR plasmid DNA, can confirm because having uciferase activity PPAR activity reporter dna, provide about the beta galactosidase DNA of transfection efficiency information and transfection reagent are used for transfection.By sample dissolution in methyl-sulfoxide (DMSO), by medium, it is administered in cell with variable concentrations.In incubator, cultured cell is after 24 hours, makes lysis by using lysis buffer.Photometer and ELIASA is used to measure uciferase activity and betagalactosidase activity.The value of the luciferase using the value correction of beta galactosidase to obtain.Utilize these value graphings, and calculate EC
50.
Compound of the present invention has high selectivity for PPAR δ as can be seen here.
Execution MTT detection is the cytotoxicity in order to test the compound represented by formula I of the present invention.MTT is water-soluble yellow substance, but can be become the insoluble crystal of purple by the dehydrogenase in mitochondria when it is introduced in living cells.MTT is being dissolved in after in methyl-sulfoxide and can confirming cytotoxicity by measuring OD550.Experiment is carried out as follows.
CV-1 cell is inoculated in (5000 cells/well) in 96 orifice plates.At 37 DEG C, 5%CO
2incubator in cultivate described cell 24 hours, and it is used to the sample of variable concentrations.Then, again by described cell chulture 24 hours, MTT reagent is added wherein.Cultivate after 15 minutes, the purple crystals of generation is dissolved in methyl-sulfoxide.ELIASA is used to measure optical density, to confirm cytotoxicity.
As a result, the compound represented by formula I is identified does not have cytotoxicity for PPAR, even if be EC in its concentration
50value 100 times ~ 1000 times time also like this.
The effect test of flame-proof cotton fabric:
COTTON FABRIC after embodiment 1-3 flame treatment, is tested it respectively as follows, and test result is in table 1.Wherein the COTTON FABRIC of comparative example is not through the fire retarding treating liquid process containing formula I, only passes through washing.
1) charcoal damages length
The charcoal of finishing of cotton textiles damages length, glow time and after flame time foundation GB/T5455-1997 " textile combustion performance test normal beam technique " mensuration in M601 normal beam technique fabrics flame resistance ability meter (Qingdao Mount spins Instrument Ltd.);
2) limited oxygen index
The limited oxygen index (LOI) of finishing of cotton textiles is upper according to GB/T5454-1997 " textile combustion performance measurement oxygen index method " mensuration at M606A oxygen index measurer (Qingdao Mount spins Instrument Ltd.);
3) strength loss
Strength test measures on Nantong Hongda Experiment Instruments Co., Ltd. HD026H electronic fabric tensometer by GB/T3923-1997 " textile fabric tensile property part 1: the mensuration galley proof method of ultimate strength and extension at break ", and the strength loss after fabric bleaching calculates by formula (1):
In formula: S
1for the brute force before fabric fire-retardant finishing, S
2for the brute force after fabric fire-retardant finishing.
The test result of table 1 flame-retardant textile
As shown in Table 1, after flame retarding process process of the present invention, the limited oxygen index of COTTON FABRIC is higher, and charcoal damages contraction in length, and illustrate that the fire resistance of COTTON FABRIC improves, strength loss is less.As can be seen here, the flame-proof cotton fabric excellent flame retardancy that the present invention obtains, and there is certain washability.
Claims (6)
1. a production technology for flame retardant textiles, is characterized in that comprising the steps:
(1) preliminary treatment of textiles: pending textiles is dipped in clear water, ultrasonic 10-30min, takes out, and dries at 60-80 DEG C, stand-by;
(2) fire retarding treating liquid is prepared: join in the organic solvent of 30 ~ 200ml by 0.05 ~ 0.1mol formula I, 0.01 ~ 0.03mol crosslinking agent N hydroxymethyl acrylamide, 0.01 ~ 0.02mol dispersant lauryl sodium sulfate, at 50 ~ 80 DEG C, stirring reaction 0.5 ~ 2h, obtains fire retarding treating liquid; Described formula I is as follows:
(3) flame-proof treatment: after textiles is flooded 15 ~ 20 minutes in above-mentioned fire retarding treating liquid, two leachings two are rolled, pick-up 80 ~ 105%, then by textiles drying 5 ~ 10 minutes at 60 ~ 90 DEG C, then cures 2 ~ 8 minutes at 150 ~ 180 DEG C;
(4) post-drying of alkali cleaning, washing.
2. production technology according to claim 1, is characterized in that described organic solvent is at least one in methyl alcohol, ethanol, isopropyl alcohol, n-butanol, acetone, espeleton, methylisobutylketone, acetonitrile, pyridine, phenol, DMF.
3. production technology according to claim 1 and 2, is characterized in that described textiles is COTTON FABRIC.
4. production technology according to claim 1, is characterized in that the multiple flat wash trough of described caustic scrubbing step, the sodium carbonate of the first groove perfusion 10g/L, the sodium carbonate of the second groove perfusion 5g/L, the sodium carbonate of the 3rd groove perfusion 5g/L.
5. the compound shown in a formula I:
6. the application of formula I according to claim 5 in Fire-proof Finishing Agents for Textile process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103835131A (en) * | 2012-11-24 | 2014-06-04 | 无锡市银泰纺织品有限公司 | Production technology of flame-retardant textile |
| CN104264467A (en) * | 2014-09-15 | 2015-01-07 | 河南工程学院 | Preparation method of flame-retardant cotton fabric |
| CN104562683A (en) * | 2015-02-04 | 2015-04-29 | 湖州厉华妤婕联合纺织有限公司 | Preparation method of novel waterproof fire-resistant textile |
| CN104817552A (en) * | 2015-05-04 | 2015-08-05 | 吉首大学 | Preparing method of (E)-N'-arylmethylene-4-(coumarin-3-yl)thiazole-2-hydrazide compound and its application |
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2015
- 2015-09-07 CN CN201510562921.1A patent/CN105088763A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103835131A (en) * | 2012-11-24 | 2014-06-04 | 无锡市银泰纺织品有限公司 | Production technology of flame-retardant textile |
| CN104264467A (en) * | 2014-09-15 | 2015-01-07 | 河南工程学院 | Preparation method of flame-retardant cotton fabric |
| CN104562683A (en) * | 2015-02-04 | 2015-04-29 | 湖州厉华妤婕联合纺织有限公司 | Preparation method of novel waterproof fire-resistant textile |
| CN104817552A (en) * | 2015-05-04 | 2015-08-05 | 吉首大学 | Preparing method of (E)-N'-arylmethylene-4-(coumarin-3-yl)thiazole-2-hydrazide compound and its application |
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Application publication date: 20151125 |