CN102535161A - Processing method for jute fabric - Google Patents
Processing method for jute fabric Download PDFInfo
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- CN102535161A CN102535161A CN2011104509515A CN201110450951A CN102535161A CN 102535161 A CN102535161 A CN 102535161A CN 2011104509515 A CN2011104509515 A CN 2011104509515A CN 201110450951 A CN201110450951 A CN 201110450951A CN 102535161 A CN102535161 A CN 102535161A
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Abstract
The invention relates to a processing method for jute fabric, which comprises the following steps of: carrying out ultraviolet irradiation on the jute fabric, so that active macromolecular chains are produced on the surface of the jute fabric; spraying and coating flame retardant on the surface of the jute fabric; carrying out irradiation again; and drying after repeated operation, so that the processing for the jute fabric is realized. According to the processing method, allyl dimethyl phosphate ester is adopted as a grafted flame retardant monomer of the jute fabric, so that the jute fabric has better flame retardant property, has afterflame time, afterglow time and damaged length meeting national requirements on flame retardant indicators of fabrics, is low in cost in a finishing and using process, and is nontoxic and environment-friendly.
Description
Technical field
The present invention is relevant with the processing method of megila, a kind of method that adopts ultraviolet irradiation and surface spraying propenyl dimethyl phosphate to handle megila of saying so further.
Background technology
The principle of uv-light polymerization thing material surface photo-grafting modification and method are proposed the 1950's by people such as Oster the earliest; Up to the eighties; The surface light grafting method just causes material scholar's attention gradually, and Application Areas also progressively develops into surface-functionalized, high performance and grafting forming technique etc. by initial simple surfaces graft modification.The fiber surface grafting is to utilize ultraviolet irradiation to cause fiber and monomer generation graft polymerization reaction, follows radical polymerization mechanism.Ultraviolet irradiation is that than the advantage of other grafting method the ultraviolet light wavelength can select; Reaction condition requires lower.Active ultraviolet radiation graft technology is meant and has reversible termination (reversibly inactivated) reaction; Be the growing chain free radical can with the reversible spike that is combined into dormancy of other material (as the free radical that adds); Chain propagation reaction can be proceeded, and such radical polymerization process is " activity " radical polymerization.At present; The surface of handling generally is simple flat surface in the surface light grafting method; Be that the surface can be exposed under the ultraviolet light fully or the material printing opacity allows ultraviolet light to reach, the processing that is difficult for the direct surface that arrives for some character instability, labile macromolecular material and ultraviolet lights under ultraviolet lighting is then limited to.For this reason, when Zhang Zhengdong etc. have proposed/empty separated light crosslinking technology, adopt special means that one complete photo-grafting is reflected on time and the space and separate, be divided into multistep and carry out, thereby realize the graft modification on not illumination surface.As the time/empty separated light grafting intermittently reaches in the process of continuous coupling BP; Excitation state BP except in the hole of nucleopore membranes outer surface capture the active hydrogen and can also capture active hydrogen at internal surface of hole; Promptly in the hole, all there is spike to generate with the film surface; Hot joining branch reaction back all has grafted chain to occur with the film surface in the hole, thereby realizes the graft modification on not illumination surface.
Summary of the invention
Problem of the present invention is the fire retardant monomer propenyl dimethyl phosphate that contains active function groups is introduced in the flame treatment of megila; And the processing method that ultraviolet irradiation and surface spraying combine handled megila, and a kind of processing method that is used for megila is provided.
It is a kind of processing method that is used for megila that the present invention addresses the above problem the measure of being taked; This method is the megila ultraviolet irradiation to be handled with surperficial spray coated flame retardant agent combine; Select baking temperature; The fire retardant monomer propenyl dimethyl phosphate that will contain active function groups is again introduced in the megila, and its concrete steps are following:
(1) megila preliminary treatment
It is in 5% the neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, is heated to 60 ℃ then, stirs after 20 minutes and takes out, and uses washed with de-ionized water, dries;
(2) megila ultraviolet irradiation
The megila that step (1) is cleaned irradiation 3-5 minutes in the ultraviolet case; Ultraviolet source is the straight pipe type Iodine gallium light, and power is: 3000W, and ultraviolet wavelength is: 270-420nm; Make C-C, C=O or the c h bond of megila rupture, the surface produces active macromolecular chain;
(3) megila surface spraying
With the spray coated flame retardant agent of the surface of the megila after above-mentioned steps (2) radiation, said fire retardant is a propenyl dimethyl phosphate, and its consumption is 30-80% of a megila weight, and spraying temperature is 28-35 ℃, and relative air humidity remains on 30-35%RH; During the spraying fabric, spray gun is fabric face vertically, keeps 50 centimeters distance, all back and forth sprayings of speed;
(4) repeating above-mentioned steps (2) and step (3) is 3-10 times, and the megila after will handling then is dry down at 110-130 ℃.
(5) megila after the above-mentioned grafting processing is spent deionised water, extract 24h with acetone Suo Shi, to remove the monomer and the homopolymers of megila surface adsorption, spend deionised water again, low temperature drying is to constant weight.
In above-mentioned a kind of processing method kind that is used for megila, the consumption of its said fire retardant is further elected 50% of megila weight as, and spraying temperature is further elected 33 ℃ as, and relative air humidity remains on 30%RH.Its use to such an extent that the preparation method of propenyl dimethyl phosphate flame retardant is following:
(1) in agitated reactor, adds ether and POCl3 for 4:1 in molar ratio;
(2) in agitated reactor, dripping mol ratio again is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and the control temperature is 0 ℃; The mixed liquor that the reaction back drips methyl alcohol and triethylamine reacted 3 hours again, left standstill 12 hours; Suction filtration obtains filtrating, and saturated NaCO is used in the back
3It is 7 that solution is regulated filtrating pH value, obtains propenyl dimethyl phosphate 50-70 ℃ of evaporations;
(3) reaction back suction filtration separates, and removes supernatant liquor, and the back distillation makes the Halogen fire retardant of polyphosphate.
A kind of megila processing method that is used for provided by the present invention; Compared with prior art; This method at first is that the megila behind ultraviolet irradiation can produce a large amount of active macromolecular chains; Graft polymerization reaction takes place in the C=C in these macromolecular chains and the fire retardant, and the form combination with valence link makes flame retardant effect more lasting; Next is at megila surface spraying monomer propenyl dimethyl phosphate flame retardant, has avoided fabric in treatment fluid, to pad technology, and the direct grafting megila of fire retardant surface, not only environmental protection but also practice thrift cost.
Compare with existing megila treatment technology, megila is immersed in the fire-retardant treatment liquid it is carried out irradiation, it is more that the required raw material of graft reaction takes place, and cost is higher; The method that the present invention adopts ultraviolet irradiation to combine with surperficial spray coated flame retardant agent is painted on the megila surface behind ultraviolet irradiation with fire retardant, does not need the participation of other reaction reagent; Both graft polymerization reaction can take place, simple to operate, equipment investment is few; Be convenient to control, pollution-free.
The present invention first with propenyl dimethyl phosphate as the fire-retardant monomer of the grafting of megila; Make it obtain fire resistance preferably; Its after flame time, glow time and char length are all through the fire-retardant index request of country to textiles, and limited oxygen index also can reach 30%, helps reducing casualties and property loss in the fire; Cost is low in arrangement and use, asepsis environment-protecting.
Description of drawings
Fig. 1 is the be untreated picture of former megila of the present invention;
Fig. 2 is the picture of the megila after the flame treatment of the present invention;
Fig. 3 is the present invention's former megila picture behind the 10s of in air, lighting a fire that is untreated;
Fig. 4 is the picture behind the 10s of in air, lighting a fire of the megila after the flame treatment of the present invention.
The specific embodiment
The processing method of a kind of megila of embodiment of the present invention at first is a kind of fire retardant that is used for megila of preparation, and its said fire retardant is a propenyl dimethyl phosphate, and its preparation method is following:
(1) in agitated reactor, add ether and POCl3, its mol ratio is 4:1, and ether is a solvent;
(2) in agitated reactor, dripping mol ratio again is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and the control temperature is 0 ℃, obtains compound (1) through shown in the reaction equation (1),
Reaction equation (1) compound (1)
(3) mixed liquor of compound (1) with methyl alcohol and triethylamine reacted 3 ~ 6 hours through reaction equation (2); Left standstill 12 hours, suction filtration obtains filtrating, obtains compound (2)-propenyl dimethyl phosphate at 50 ~ 70 ℃ of rotary evaporations;
Reaction equation (2) compound (2)
Next is to implement a kind of processing method that is used for megila, and this method follows these steps to carry out:
(1) megila preliminary treatment
It is in 5% the neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, is heated to 60 ℃ then, stirs after 20 minutes and takes out, and uses washed with de-ionized water, dries;
(2) megila ultraviolet irradiation
The megila that step (1) is cleaned irradiation 3-5 minutes in the ultraviolet case; Ultraviolet source is the straight pipe type Iodine gallium light, and power is: 3000W, and ultraviolet wavelength is: 270-420nm; Make C-C, C=O or the c h bond of megila rupture, the surface produces active macromolecular chain;
(3) megila surface spraying
With the spray coated flame retardant agent of the surface of the megila after above-mentioned steps (2) radiation, said fire retardant is a propenyl dimethyl phosphate, and its consumption is 30-80% of a megila weight, and spraying temperature is 28-35 ℃, and relative air humidity remains on 30-35%RH; During the spraying fabric, spray gun is fabric face vertically, keeps 50 centimeters distance, all back and forth sprayings of speed;
(4) repeating above-mentioned steps (2) and step (3) is 3-5 times, and the megila after will handling then is dry down at 110-130 ℃.
(5) megila after the above-mentioned grafting processing is spent deionised water, extract 24h with acetone Suo Shi, to remove the monomer and the homopolymers of megila surface adsorption, spend deionised water again, low temperature drying is to constant weight.
Be the megila ultraviolet irradiation to be handled with surperficial spray coated flame retardant agent combine in the above-mentioned embodiment of the present invention; Select various parameters and baking temperature in the technical process, the fire retardant monomer propenyl dimethyl phosphate that will contain active function groups is again introduced in the megila.After megila is handled through the method for ultraviolet irradiation and spray coated flame retardant agent; By national standard the combustibility of the megila after handling is tested, concrete mode adopts the vertical combustion method to measure: press GB/T 5455-1997 " textile combustion performance test normal beam technique "; Probe temperature is 10-30 ℃, and relative humidity is 30-80%; Measure afterflame after fabric is lighted 12s, glow time and charcoal be long.Oxygen index method is measured: measure the test method that sample is just kept the required minimum oxygen concentration of burning (also claiming limited oxygen index) by GB/T 5455-1997 " textile combustion performance test oxygen index method "; Megila to the present invention handled detects; Its testing result is: the after flame time of megila reaches: 13.64s; The time of glowing reaches 6.04s, and char length reaches 184.5mm, and limited oxygen index reaches 30%.Be golden yellow like megila among Fig. 1, the no capillary fiber in surface; In Fig. 2: fire-retardant megila is through after repeatedly washing, and fabric receives the external force effect, and interfibrous winding becomes loose, and color and luster shoals slightly, and some capillary fibers are scattered on the surface; In Fig. 3: former megila below is behind contact burning things which may cause a fire disaster (alcohol blast burner), and burning after naked light extinguishes, continues to glow rapidly, and the residue after the burning is canescence, and weight is about 1% of former megila; In Fig. 4: fire-retardant megila below is behind contact burning things which may cause a fire disaster (alcohol blast burner), and burning is slow, and the residue black in color after the burning is about 20 ~ 30% of fire-retardant megila weight.Explain to have generated strong dehydrating agent after fire retardant is heated, make fiber be dehydrated into charcoal rapidly, form the carbon-coating starvation, thereby reach fire-retardant purpose.
Make further detailed description by the embodiment specific embodiments of the invention below:
Embodiment 1
Step 1: it is in 5% the neopelex cleaning fluid 10 minutes that the numb sheet that megila is cut into 6.5 * 20cm is inserted mass fraction, stirs then after 20 minutes and takes out, and with washed with de-ionized water repeatedly, dries;
Step 2: with cleaned megila irradiation 4 minutes in the ultraviolet case, ultraviolet wavelength is 350nm, this moment megila C-C, C=O or c h bond fracture, the surface produces active macromolecular chain, as follows;
Step 3: at fabric face spraying propenyl dimethyl phosphate flame retardant, spraying temperature is 33 ℃ with the spray machine, and relative air humidity remains on 30%RH; The vertically fabric face of rifle of disputing in the spraying process, and keep the distance about 50 centimeters, all back and forth sprayings of speed; This moment, the living radical and the carbon-carbon double bond in the fire retardant on jute surface reacted, and two keys are opened, and fire retardant is grafted on the jute, as follows:
Step 4: repeating step two and step 36 times, then jute accumulative total irradiation is 24 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 50.6% (to the weight of jute), and this moment, the fire retardant that the jute surface grafting is a large amount of had anti-flaming function under ultraviolet irradiation, as follows:
Step 5: it is dry that the jute after will spraying is put into air dry oven, and temperature is set to 120 ℃, and the time is 60min.Dried fabric is fully washed with deionized water, extract 24h, to remove the monomer and the homopolymers of sample surfaces absorption with acetone Suo Shi.Fully wash with deionized water, low temperature drying promptly gets fire-retardant megila to constant weight again.Through detecting, the after flame time of fire-retardant megila is 13.64s, and the time of glowing is 6.04s, char length 184.5mm, limited oxygen index 28%.
Said method at first is that the megila behind ultraviolet irradiation can produce a large amount of active macromolecular chains, and graft polymerization reaction takes place the C=C in these macromolecular chains and the fire retardant, and the form combination with valence link makes flame retardant effect more lasting; Next is at megila surface spraying monomer propenyl dimethyl phosphate flame retardant, has avoided fabric in treatment fluid, to pad technology, and the direct grafting megila of fire retardant surface, not only environmental protection but also practice thrift cost.
Embodiment 2
The megila that cleans up was put into ultraviolet case irradiation 3 minutes, and ultraviolet wavelength is 270nm, sprays propenyl dimethyl organic phosphate flame-retardant treatment fluid with the spray machine at fabric face then, and spraying temperature is 35 ℃, and relative air humidity remains on 35%RH; The vertically fabric face of rifle of disputing in the spraying process, and keep the distance about 50 centimeters, all back and forth sprayings of speed; Repeat above-mentioned steps 5 times, then megila accumulative total irradiation is 24 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 30%, (to the weight of megila).It is dry that megila after the spraying is put into air dry oven, 80 ℃ of preliminary drying temperature, and 1 hour time, temperature is set to 120 ℃ then, and the time is 80min.Dried fabric is fully washed with deionized water, extract 24h, to remove the monomer and the homopolymers of sample surfaces absorption with acetone Suo Shi.Fully wash with deionized water, low temperature drying is to constant weight again.Through detecting, the limited oxygen index of the fire-retardant megila that makes is 26%.
Embodiment 3
The megila that cleans up was put into ultraviolet case irradiation 5 minutes; Ultraviolet wavelength is 400nm, sprays propenyl dimethyl organic phosphate flame-retardant treatment fluid with the spray machine at fabric face then, and spraying temperature is 28 ℃; Relative air humidity remains on 30%RH; The vertically fabric face of rifle of disputing in the spraying process, and keep the distance about 50 centimeters, all back and forth sprayings of speed; Repeat above-mentioned steps 6 times, then megila accumulative total irradiation is 30 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 70%, (to the weight of megila).It is dry that megila after the spraying is put into air dry oven, 80 ℃ of preliminary drying temperature, and 1 hour time, temperature is set to 130 ℃ then, and the time is 100min.Dried fabric is fully washed with deionized water, extract 24h, to remove the monomer and the homopolymers of sample surfaces absorption with acetone Suo Shi.Fully wash with deionized water, low temperature drying is to constant weight again.Through detecting, the limited oxygen index of the fire-retardant megila that makes is 29%.
Embodiment 4
The megila that cleans up was put into ultraviolet case irradiation 5 minutes, and ultraviolet wavelength is 420nm, sprays propenyl dimethyl organic phosphate flame-retardant treatment fluid with the spray machine at fabric face then, and spraying temperature is 30 ℃, and relative air humidity remains on 35%RH; The vertically fabric face of rifle of disputing in the spraying process, and keep the distance about 50 centimeters, all back and forth sprayings of speed; Repeat above-mentioned steps 8 times, then megila accumulative total irradiation is 40 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 80% (to the weight of megila).It is dry that megila after the spraying is put into air dry oven, 80 ℃ of preliminary drying temperature, and 2 hours time, temperature is set to 130 ℃ then, and the time is 2 hours.Dried fabric is fully washed with deionized water, extract 24h, to remove the monomer and the homopolymers of sample surfaces absorption with acetone Suo Shi.Fully wash with deionized water, low temperature drying is to constant weight again.Through detecting, the limited oxygen index of the fire-retardant megila that makes is 30%.
Claims (3)
1. processing method that is used for megila, this method follows these steps to carry out:
(1) megila preliminary treatment
It is in 5% the neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, is heated to 60 ℃ then, stirs after 20 minutes and takes out, and uses washed with de-ionized water, dries;
(2) megila ultraviolet irradiation
The megila that step (1) is cleaned irradiation 3-5 minutes in the ultraviolet case; Ultraviolet source is the straight pipe type Iodine gallium light, and power is: 3000W, and ultraviolet wavelength is: 270-420nm; Make C-C, C=O or the c h bond of megila rupture, the surface produces active macromolecular chain;
(3) megila surface spraying
With the spray coated flame retardant agent of the surface of the megila after above-mentioned steps (2) radiation, said fire retardant is a propenyl dimethyl phosphate, and its consumption is 30-80% of a megila weight, and spraying temperature is 28-35 ℃, and relative air humidity remains on 30-35%RH; During the spraying fabric, spray gun is fabric face vertically, keeps 50 centimeters distance, all back and forth sprayings of speed;
(4) repeating above-mentioned steps (2) and step (3) is 3-5 times, and the megila after will handling then is dry down at 110-130 ℃;
(5) megila after the above-mentioned grafting processing is spent deionised water, extract 24h with acetone Suo Shi, to remove the monomer and the homopolymers of megila surface adsorption, spend deionised water again, low temperature drying is to constant weight.
2. the method for claim 1, the consumption of its said fire retardant is 50% of a megila weight, and spraying temperature is 33 ℃, and relative air humidity remains on 30%RH.
3. the processing method that is used for megila as claimed in claim 1, the preparation method of its said propenyl dimethyl phosphate is following:
(1) in agitated reactor, adds ether and POCl3 for 4:1 in molar ratio;
(2) in agitated reactor, dripping mol ratio again is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and the control temperature is 0 ℃; The mixed liquor that the reaction back drips methyl alcohol and triethylamine reacted 3 hours again, left standstill 12 hours; Suction filtration obtains filtrating, and saturated NaCO is used in the back
3It is 7 that solution is regulated filtrating pH value, obtains propenyl dimethyl phosphate 50-70 ℃ of evaporations;
(3) reaction back suction filtration separates, and removes supernatant liquor, and the back distillation makes propenyl dimethyl phosphate flame retardant.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105133285A (en) * | 2015-09-18 | 2015-12-09 | 江南大学 | Method for performing durable flame-retardant grafting modification on fabric through cooperation of low-temperature plasma with electron beam irradiation |
| CN105463832A (en) * | 2015-03-12 | 2016-04-06 | 苏州摩维天然纤维材料有限公司 | Preparation method of hemp fibers with flame retardancy function and hemp fibers |
| CN107385884A (en) * | 2017-08-15 | 2017-11-24 | 马鞍山中港服饰有限公司 | A kind of modification processing method of knitwear ramee |
| CN107476047A (en) * | 2017-08-15 | 2017-12-15 | 马鞍山中港服饰有限公司 | A kind of technique for improving flax fiber and using characteristic |
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| CN1563550A (en) * | 2004-04-19 | 2005-01-12 | 太原理工大学 | Technique of nano crystallizing treatment on surface of fiber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463832A (en) * | 2015-03-12 | 2016-04-06 | 苏州摩维天然纤维材料有限公司 | Preparation method of hemp fibers with flame retardancy function and hemp fibers |
| CN105463832B (en) * | 2015-03-12 | 2017-11-10 | 苏州摩维天然纤维材料有限公司 | A kind of preparation method and its flaxen fiber of the flaxen fiber with anti-flaming function |
| CN105133285A (en) * | 2015-09-18 | 2015-12-09 | 江南大学 | Method for performing durable flame-retardant grafting modification on fabric through cooperation of low-temperature plasma with electron beam irradiation |
| CN107385884A (en) * | 2017-08-15 | 2017-11-24 | 马鞍山中港服饰有限公司 | A kind of modification processing method of knitwear ramee |
| CN107476047A (en) * | 2017-08-15 | 2017-12-15 | 马鞍山中港服饰有限公司 | A kind of technique for improving flax fiber and using characteristic |
| CN107476047B (en) * | 2017-08-15 | 2018-03-27 | 马鞍山中港服饰有限公司 | A kind of technique for improving flax fiber and using characteristic |
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