CN102535161B - Processing method for jute fabric - Google Patents
Processing method for jute fabric Download PDFInfo
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- CN102535161B CN102535161B CN 201110450951 CN201110450951A CN102535161B CN 102535161 B CN102535161 B CN 102535161B CN 201110450951 CN201110450951 CN 201110450951 CN 201110450951 A CN201110450951 A CN 201110450951A CN 102535161 B CN102535161 B CN 102535161B
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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, says further a kind of method that adopts ultraviolet irradiation and surface spraying propenyl Dimethyl phosphate to process megila.
Background technology
The principle of uv-light polymerization thing material surface Modification of Photo-grafting Copolymerization and method are proposed the 1950's by people such as Oster the earliest, until 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 refers to exist reversible termination (reversibly inactivated) reaction, be that the growing chain free radical can become the spike of dormancy with other material (as the free radical that adds) Reversible binding, chain propagation reaction can be proceeded, and such radical polymerization process is " activity " radical polymerization.At present, the surface of processing is generally simple flat surface in the surface light grafting method, be that the surface can be exposed under ultraviolet light fully or the material printing opacity allows ultraviolet light to reach, limited to for unstable, the labile macromolecular material of some character under ultraviolet lighting and the difficult directly processing on the surface of arrival of ultraviolet light.For this reason, when Zhang Zhengdong etc. have proposed/empty separated light crosslinking technology, adopt any special measures that one complete UV-induced grafting is separated on time and space, be divided into multistep and carry out, thereby realize the not graft modification on illumination surface.As the time/empty separated light grafting intermittently reaches in the process of continuous coupling BP, excitation state BP is except capturing active hydrogen and can also capture active hydrogen at internal surface of hole at the hole of nucleopore membranes outer surface, namely in the hole and the film surface all have spike to generate, after hot joining branch reaction in the hole and the film surface have grafted chain to occur, thereby realize the not graft modification on 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 combines with surface spraying is processed megila, and provide a kind of processing method for megila.
It is a kind of processing method for megila that the present invention addresses the above problem institute's Adopts measure, the method is the megila ultraviolet irradiation to be processed with the surface spraying fire retardant combine, select baking temperature, the fire retardant monomer propenyl Dimethyl phosphate that will contain again active function groups is introduced in megila, and its concrete steps are as follows:
(1) megila preliminary treatment
It is in 5% neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, then is heated to 60 ℃, 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 fracture of megila, the surface produces active macromolecular chain;
(3) megila surface spraying
With the megila surface spraying fire retardant after above-mentioned steps (2) radiation, described fire retardant is the propenyl Dimethyl phosphate, and its consumption is 30-80% of 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 the distance of 50 centimeters, and average rate back and forth sprays;
(4) repeating above-mentioned steps (2) and step (3) is 3-10 times, and the megila after then processing is dry under 110-130 ℃.
(5) megila after above-mentioned grafting processing is washed with deionized water, extract 24h with the acetone Soxhlet, with monomer and the homopolymers of removal megila adsorption, then wash with deionized water, low temperature drying is to constant weight.
In above-mentioned a kind of processing method kind for megila, the consumption of its described 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.It uses to such an extent that the preparation method of propenyl Dimethyl phosphate fire retardant is as follows:
(1) add ether and phosphorus oxychloride for 4:1 in molar ratio in reactor;
(2) dripping mol ratio again in reactor is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and controlling temperature is 0 ℃, drip the mixed liquor of methyl alcohol and triethylamine after reaction, then reacted standing 12 hours 3 hours, suction filtration obtains filtrate, uses saturated NaCO afterwards
3It is 7 that solution is regulated filtrate pH value, obtains the propenyl Dimethyl phosphate 50-70 ℃ of evaporations;
(3) suction filtration after the reaction separates, and removes supernatant liquor, and rear distillation makes the Halogen fire retardant of polyphosphate.
Provided by the present invention a kind of for the megila processing method, compared with prior art, at first the method is that the megila after ultraviolet irradiation can produce a large amount of active macromolecular chains, graft polymerization reaction occurs in the C=C in these macromolecular chains and fire retardant, form combination with valence link makes flame retardant effect more lasting; Next is at megila surface spraying monomer propenyl Dimethyl phosphate fire retardant, has avoided fabric to pad technique in treatment fluid, and the direct grafting megila of fire retardant surface, not only environmental protection but also save cost.
Compare with existing megila treatment technology, megila is immersed in fire-retardant treatment liquid it is carried out irradiation, the required raw material of graft reaction occurs more, cost is higher; The method that the present invention adopts ultraviolet irradiation to combine with the surface spraying fire retardant, the megila that fire retardant is painted on after ultraviolet irradiation is surperficial, do not need the participation of other reaction reagent, both graft polymerization reaction can occur, simple to operate, equipment investment is few, be convenient to control, pollution-free.
The present invention is first with the grafting flame-retardant monomer of propenyl Dimethyl phosphate as megila, make it obtain fire resistance preferably, its after flame time, glow time and char length are all by the fire-retardant index request of country to textiles, limited oxygen index also can reach 30%, be conducive to reduce casualties and property loss in fire, cost is low in arrangement and use procedure, 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 flame treatment of the present invention;
Fig. 3 is the present invention's light a fire in air picture after 10s of former megila that is untreated;
Fig. 4 is light a fire in air picture after 10s of the megila after flame treatment of the present invention.
The specific embodiment
Implementing the processing method of a kind of megila of the present invention, is at first a kind of fire retardant for megila of preparation, and its described fire retardant is the propenyl Dimethyl phosphate, and its preparation method is as follows:
(1) add ether and phosphorus oxychloride in reactor, its mol ratio is 4:1, and ether is solvent;
(2) dripping mol ratio again in reactor is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and controlling temperature is 0 ℃, obtains compound (1) by shown in reaction equation (1),
Reaction equation (1) compound (1)
(3) mixed liquor of compound (1) with methyl alcohol and triethylamine reacted 3 ~ 6 hours by reaction equation (2); Standing 12 hours, suction filtration obtained filtrate, obtained 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 for megila, and the method follows these steps to carry out:
(1) megila preliminary treatment
It is in 5% neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, then is heated to 60 ℃, 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 fracture of megila, the surface produces active macromolecular chain;
(3) megila surface spraying
With the megila surface spraying fire retardant after above-mentioned steps (2) radiation, described fire retardant is the propenyl Dimethyl phosphate, and its consumption is 30-80% of 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 the distance of 50 centimeters, and average rate back and forth sprays;
(4) repeating above-mentioned steps (2) and step (3) is 3-5 times, and the megila after then processing is dry under 110-130 ℃.
(5) megila after above-mentioned grafting processing is washed with deionized water, extract 24h with the acetone Soxhlet, with monomer and the homopolymers of removal megila adsorption, then wash with deionized water, low temperature drying is to constant weight.
The megila ultraviolet irradiation to be processed with the surface spraying fire retardant combine in the above-mentioned embodiment of the present invention, select various parameters and baking temperature in technical process, then will contain in the fire retardant monomer propenyl Dimethyl phosphate introducing megila of active function groups.After megila is processed by the method for ultraviolet irradiation and spray coated flame retardant agent, by national standard, the combustibility of the megila after processing 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 the time and charcoal long.Oxygen index method is measured: measure by GB/T 5455-1997 " textile combustion performance test oxygen index method " test method that sample is just kept the required minimum oxygen concentration of burning (also claiming limited oxygen index), the megila that the present invention processed is detected, its testing result is: the after flame time of megila reaches: 13.64s, the time of glowing reaches 6.04s, char length reaches 184.5mm, and limited oxygen index reaches 30%.Be golden yellow as megila in Fig. 1, the surface is without capillary fiber; In Fig. 2: fire-retardant megila is through after repeatedly washing, and fabric is subjected to External Force Acting, and interfibrous winding becomes loose, and color and luster slightly shoals, and some capillary fibers are scattered on the surface; In Fig. 3: below former megila, after contact burning things which may cause a fire disaster (alcohol blast burner), burning, after naked light extinguishes, continue to glow rapidly, and the residue after burning is canescence, and weight is about 1% of former megila; In Fig. 4: below fire-retardant megila, after contact burning things which may cause a fire disaster (alcohol blast burner), burning is slow, and the residue after burning is black, is about 20 ~ 30% of fire-retardant megila weight.The fire retardant rear strong dehydrating agent that generated that is heated is described, makes fiber be dehydrated into rapidly charcoal, form the carbon-coating starvation, thereby reach fire-retardant purpose.
The below is further detailed the specific embodiment of the present invention by embodiment:
Embodiment 1
Step 1: it is in 5% neopelex cleaning fluid 10 minutes that the numb sheet that megila is cut into 6.5 * 20cm is inserted mass fraction, then stirs 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, and is as follows;
Step 3: at fabric face spraying propenyl Dimethyl phosphate fire 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 spraying process, and keep the distance of 50 centimeters left and right, average rate back and forth sprays; The living radical on jute this moment surface and the reaction of the carbon-carbon double bond in fire retardant are opened two keys, and fire retardant is grafted on jute, and is as follows:
Step 4: repeating step two and step 36 times, jute accumulative total irradiation is 24 minutes, fire-retardant treatment liquid accumulative total quantity for spray is that 50.6%(is to the weight of jute), this moment, the fire retardant that the jute surface grafting is a large amount of has anti-flaming function, and was as follows under ultraviolet irradiation:
Step 5: it is dry that the jute after spraying is put into air dry oven, and temperature setting is set to 120 ℃, and the time is 60min.Dried fabric is fully washed with deionized water, extract 24h with the acetone Soxhlet, to remove monomer and the homopolymers of sample surfaces absorption.Fully wash with deionized water, low temperature drying namely 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%.
At first said method is that the megila after ultraviolet irradiation can produce a large amount of active macromolecular chains, and graft polymerization reaction occurs the C=C in these macromolecular chains and 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 fire retardant, has avoided fabric to pad technique in treatment fluid, and the direct grafting megila of fire retardant surface, not only environmental protection but also save cost.
Embodiment 2
The megila that cleans up was put into ultraviolet case irradiation 3 minutes, and ultraviolet wavelength is 270nm, then sprays propenyl Dimethyl phosphate fire-retardant treatment liquid with the spray machine at fabric face, and spraying temperature is 35 ℃, and relative air humidity remains on 35%RH; The vertically fabric face of rifle of disputing in spraying process, and keep the distance of 50 centimeters left and right, average rate back and forth sprays; Repeat above-mentioned steps 5 times, megila accumulative total irradiation is 24 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 30%, (to the weight of megila).Megila after spraying is put into air dry oven dry, 80 ℃ of preliminary drying temperature, 1 hour time, then temperature setting is set to 120 ℃, and the time is 80min.Dried fabric is fully washed with deionized water, extract 24h with the acetone Soxhlet, to remove monomer and the homopolymers of sample surfaces absorption.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, then spray propenyl Dimethyl phosphate fire-retardant treatment liquid with the spray machine at fabric face, spraying temperature is 28 ℃, relative air humidity remains on 30%RH, the vertically fabric face of rifle of disputing in spraying process, and keep the distance of 50 centimeters left and right, average rate back and forth sprays; Repeat above-mentioned steps 6 times, megila accumulative total irradiation is 30 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is 70%, (to the weight of megila).Megila after spraying is put into air dry oven dry, 80 ℃ of preliminary drying temperature, 1 hour time, then temperature setting is set to 130 ℃, and the time is 100min.Dried fabric is fully washed with deionized water, extract 24h with the acetone Soxhlet, to remove monomer and the homopolymers of sample surfaces absorption.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, then sprays propenyl Dimethyl phosphate fire-retardant treatment liquid with the spray machine at fabric face, and spraying temperature is 30 ℃, and relative air humidity remains on 35%RH; The vertically fabric face of rifle of disputing in spraying process, and keep the distance of 50 centimeters left and right, average rate back and forth sprays; Repeat above-mentioned steps 8 times, megila accumulative total irradiation is 40 minutes, and fire-retardant treatment liquid accumulative total quantity for spray is that 80%(is to the weight of megila).Megila after spraying is put into air dry oven dry, 80 ℃ of preliminary drying temperature, time 2 h, then temperature setting is set to 130 ℃, and the time is 2 hours.Dried fabric is fully washed with deionized water, extract 24h with the acetone Soxhlet, to remove monomer and the homopolymers of sample surfaces absorption.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, the method follows these steps to carry out:
(1) megila preliminary treatment
It is in 5% neopelex cleaning fluid 10 minutes that megila is immersed in mass fraction, then is heated to 60 ℃, 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 fracture of megila, the surface produces active macromolecular chain;
(3) megila surface spraying
With the megila surface spraying fire retardant after above-mentioned steps (2) radiation, described fire retardant is the propenyl Dimethyl phosphate, and its consumption is 30-80% of 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 the distance of 50 centimeters, at the uniform velocity back and forth spraying;
(4) repeat above-mentioned steps (2) and step (3) 3-5 times, the megila after then processing is dry under 110-130 ℃;
(5) megila after above-mentioned grafting processing is washed with deionized water, extract 24h with the acetone Soxhlet, with monomer and the homopolymers of removal megila adsorption, then wash with deionized water, low temperature drying is to constant weight.
2. the processing method for megila as claimed in claim 1, the consumption of its described fire retardant is 50% of megila weight, and spraying temperature is 33 ℃, and relative air humidity remains on 30%RH.
3. the processing method for megila as claimed in claim 1, the preparation method of its described propenyl Dimethyl phosphate is as follows:
(1) add ether and phosphorus oxychloride for 4:1 in molar ratio in reactor;
(2) dripping mol ratio again in reactor is propenyl and the triethylamine mixed liquor of 1:1, stirring reaction 6 hours, and controlling temperature is 0 ℃, drip the mixed liquor of methyl alcohol and triethylamine after reaction, then reacted standing 12 hours 3 hours, suction filtration obtains filtrate, uses saturated NaCO afterwards
3It is 7 that solution is regulated filtrate pH value, obtains the propenyl Dimethyl phosphate 50-70 ℃ of evaporations;
(3) suction filtration after the reaction separates, and removes supernatant liquor, and rear distillation makes propenyl Dimethyl phosphate fire retardant.
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| 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 |
| 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 |
| CN107385884B (en) * | 2017-08-15 | 2018-07-10 | 马鞍山中港服饰有限公司 | A kind of modification processing method of knitwear ramee |
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| CN1280474C (en) * | 2004-04-19 | 2006-10-18 | 太原理工大学 | Technique of nano crystallizing treatment on surface of fiber |
| CN101270545B (en) * | 2008-05-16 | 2010-06-02 | 太原理工大学 | Degumming flame-proof process technique for Han fibrilia |
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