CN105133285A - Method for performing durable flame-retardant grafting modification on fabric through cooperation of low-temperature plasma with electron beam irradiation - Google Patents
Method for performing durable flame-retardant grafting modification on fabric through cooperation of low-temperature plasma with electron beam irradiation Download PDFInfo
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- CN105133285A CN105133285A CN201510601493.9A CN201510601493A CN105133285A CN 105133285 A CN105133285 A CN 105133285A CN 201510601493 A CN201510601493 A CN 201510601493A CN 105133285 A CN105133285 A CN 105133285A
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Abstract
The invention discloses a method for performing durable flame-retardant grafting modification on fabric through cooperation of low-temperature plasma with electron beam irradiation. The method comprises steps as follows: firstly, the fabric is placed in a low-temperature plasma device for low-temperature plasma pretreatment; then the fabric is treated with a sodium hydroxide solution, and impurities such as colloid and the like in the fabric are removed; the fabric is taken out and fully washed with water, after residual sodium hydroxide is removed, the fabric is placed in an oven to be dried, and then the fabric is taken out and weighed; the dried fabric is soaked in a grafting monomer solution, then the fabric is taken out, the redundant liquid is rolled out by the aid of a padder, the fabric is wrapped with a plastic film and placed in a valve bag, and both the fabric and the valve bag are placed under a high-power electron beam for irradiation; after irradiation, the grafted fabric is washed with deionized water, and homopolymers and unreacted grafting monomers on the surface of the fabric are removed; then the washed fabric is placed in the oven to be dried for 24 h, and a product is obtained. The method has the advantages that the fabric has the lasting flame-retardant effect and the higher washing resistance.
Description
Technical field
The present invention relates to a kind of fabric graft modified method, be specially the durable flame-retardant graft-modification method of a kind of low-temperature plasma synergistic electron beam irradiation to fabric.
Background technology
Lower temperature plasma technology is the plasma treated material surface utilizing inert gas or reacting gas, and the large molecule activation in surface decomposes.The monomer be decomposed again in material surface polymerization, also may may generate gaseous volatilization and fall.The former can make material obviously roughened, and the latter has corrasion to material surface.Lower temperature plasma technology may be used for the numerous areas such as the starching of fabric, the coming unstuck of destarch and flax fibre, the calendering of fabric, the hydrophilic treatment of synthetic fiber, its Be very effective, and the superficial layer only acting on fabric can not affect the performance of fabric itself, thus has great importance in the application of textile industry.
Electron beam irradiation crosslinking technology is exactly the high electron beam irradiation material utilizing high voltage electric field to accelerate, and makes material produce excited state molecule and causes various chemical reaction, thus change or improve the performance of material by high energy electron.Pass through irradiation, make to be connected to form network structure by the chemical bond of certain forms between the long linear molecule between macromolecular material, it can make the binding force between macromolecule greatly strengthen, and then the heat endurance of reinforcing material, anti-flammability, chemical stability etc.Simultaneously high-energy electron beam irradiation technology have to have compared with the irradiance method such as gamma-rays can district's pack that is wider, electron beam better, capacity usage ratio is higher, danger that radiation leaks can not occur, do not need to process the advantages such as radiation source refuse.When high-power electron beam acts on material, the chemical bond of material can be destroyed, produce active ion or free radical, material is destroyed or is cross-linked.The advantage adopting high-power electron beam to carry out graft reaction is: operation is simple for which, without any need for initator and do not need to carry out Final finishing, utilizing charged particle to carry out modification to material, non-secondary pollution, is efficient a, environmental protection, low cost and other advantages.
Textiles is widely used in the every field such as clothes, decoration, but very easily burns due to fiber, therefore in use can increase unsafe factor.Therefore, the flame-proof treatment of textiles is become to the problem of people's concern.The anti-flaming function of fabric to elimination disaster hidden-trouble, delay fire spreading, to reduce people life property loss very important.Flame-retarded technology is adopted to be improve one of fire safety level, the strategic measure reducing fire damage.And more and more stricter flame-retardant standard and the enforcement of environmental regulation, make fire proofing must meet the requirement of these two aspects simultaneously.Therefore, attach great importance to the research that fabric novel flame-retardant is arranged both at home and abroad, require that fabric not only will have good fire resistance, and want environmental protection, so carry out graft modification to strengthen the focus that its flame retardant effect becomes a research to fabric face.
Summary of the invention
The object of the invention is to provide a kind of low-temperature plasma synergistic electron beam irradiation to the durable flame-retardant graft-modification method of fabric.
The object of the invention is to be achieved through the following technical solutions.
Low-temperature plasma synergistic electron beam irradiation, to a durable flame-retardant graft-modification method for fabric, the steps include:
(1) first fabric is placed in low-temperature plasma device and carries out low temperature plasma preliminary treatment;
(2) then fabric sodium hydroxide solution is processed 30min under the condition of 95-100 DEG C, the impurity such as the colloid in removing fabric;
(3) wash fully after being taken out by fabric, putting into baking oven after removing residual hydrogen sodium oxide molybdena under the condition of 80-90 DEG C dries 1-3h, and taking-up is weighed;
(4) fabric of oven dry is immersed in 1-3 hour in grafted monomers solution, takes out subsequently and shut out surplus liquid through padding machine, fabric plastic sheeting is wrapped, puts into valve bag, under fabric is put into high-power electron beam together with valve bag, carry out irradiation;
(5) after irradiation terminates, by the fabric washed with de-ionized water after grafting, the homopolymers of removing fabric face and unreacted grafted monomers; Then the fabric after cleaning is put into baking oven to dry 24 hours, obtain product.
In step (1), described fabric comprises crudefiber crop, cotton fiber and the bamboo fibres such as flax, ramie, jute, fabric made by the various novel cellulosic fibre of lotus fiber and textiles.
In step (1), the pretreated process conditions of described low temperature plasma are: the working gas of employing is the mist of one or more gases in argon gas, nitrogen, oxygen and air; Operating pressure is 10-150Pa, and discharge power is 10-300W, and the processing time is 1-20min.
In step (2), described concentration of sodium hydroxide solution is 15-30g/L.
In step (4), described high-energy electron beam irradiation reaction condition is: irradiation dose is 0-100kGy and other radiation unit's transforming numericals corresponding.
In step (4), atmosphere during described electron beam irradiation, temperature conditions all do not limit, and atmosphere can be divided into atmospheric environment, vacuum environment or contain the inert gas environment of nitrogen and/or helium.
In step (4), in described grafted monomers solution, solute is the one in the vinyl monomers such as acrylamide, Methacrylamide, acrylic acid and methacrylic acid, and its concentration is 0.1-10mol/L; Solvent is water.
Described grafted monomers solvent can with the composite use of other functional finishing agent, the effect not affecting other functional finishing agent.
The invention has the advantages that:
Compared with existing top finish, impregnating flame-retardant finishing method, these traditional fire-retardant modes often do not have durability for the flame-proof treatment of fabric, and technological process is longer, process equipment complicated operation, uncontrollable factor is a lot, causes fabrics flame resistance effect wayward.Meanwhile, these method for sorting can increase the processing cost for sewage.
Compared with the technology of existing irradiation grafting process fabric, by the method generation graft reaction of fabric ultraviolet light irradiation, its irradiation dose is less, and the free radical quantity thus produced is relatively few, percent grafting can be caused lower, and then affect the flame retardant effect of fabric.
Lower temperature plasma technology and high energy electron beams process are used for the durable flame-retardant graft modification aspect of fabric by the present invention first, and after low temperature plasma preliminary treatment, the percent grafting of fabric is had greatly improved, thus fire resistance is significantly improved.
The method that the vinyl monomers such as acrylamide are used for the high-power electron beam of fabric by the present invention first carries out grafting with this to improve the fire resistance of fabric.The later fabrics flame resistance performance of modification significantly improves, and testing vertical flammability shows, its after flame time and time of glowing obviously reduce.And monomer is connected by covalent bond with fabric, the flame retardant effect of the fabric therefore after graft modification has certain water-wash resistance, and effect is lasting.
Adopt low temperature plasma to carry out colloid to fabric face and produce corrasion, part colloid on fiber is occurred loosening, broken, be easy to remove, again through the high temperature scouring of sodium hydroxide solution, thus make coming unstuck of fiber surface more thorough, Impurity removal obtains also cleaner, thus is conducive to the carrying out of follow-up graft reaction.
The low temperature plasma preliminary treatment adopted in the present invention is a kind of physical method, does not need to use water, steam and chemicals etc., thus can reduce sewage discharge, reduction energy loss, is a kind of preprocess method of environmental protection.
Use high-power electron beam to carry out graft reaction to fabric in the present invention, the ray energy of high-power electron beam is high, and penetration capacity is strong, and reaction can be deep into fabric, and fabric grafting is even.And without any need for initator in the process of high-power electron beam process fabric, have reaction speed fast, operation is simple, do not need to carry out the advantages such as Final finishing, non-secondary pollution.
The textile field such as flame-retardant textile of the present invention goes for clothes, decoration, family are spun, and be there is the flame retardant effect of durability, comfortable feel by the fabric that the method produces.
Detailed description of the invention
Technical characterstic of the present invention is set forth further below in conjunction with specific embodiment.
Embodiment one
First sodolin being placed in working gas is N
2operating pressure is 10Pa, discharge power is preliminary treatment 120s in the low-temperature plasma device of 100W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric drying is taken out later and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 22KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of gained sodolin is 12.58%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 4s and 3s respectively, and limited oxygen index is 31%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 5s and 4s, limited oxygen index is 30%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Embodiment two
First sodolin being placed in working gas is N
2operating pressure is 10Pa, discharge power is preliminary treatment 150s in the low-temperature plasma device of 100W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric drying is taken out later and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 43KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of sodolin is 24.20%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 3s and 2s respectively, and limited oxygen index is 34%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 4s and 3s, limited oxygen index is 31%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Embodiment three
First sodolin being placed in working gas is N
2operating pressure is 10Pa, discharge power is preliminary treatment 180s in the low-temperature plasma device of 100W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric is taken out and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 65KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of sodolin is 36.78%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 2s and 1s respectively, and limited oxygen index is 37%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 3s and 3s, limited oxygen index is 34%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Embodiment four
First sodolin being placed in working gas is N
2operating pressure is 15Pa, discharge power is preliminary treatment 180s in the low-temperature plasma device of 100W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric is taken out and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 65KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of sodolin is 37.43%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 2s and 1s respectively, and limited oxygen index is 38%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 2s and 3s, limited oxygen index is 35%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Embodiment five
First sodolin being placed in working gas is N
2operating pressure is 20Pa, discharge power is preliminary treatment 180s in the low-temperature plasma device of 100W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric is taken out and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 65KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of sodolin is 38.21%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 2s and 1s respectively, and limited oxygen index is 38.5%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 3s and 2s, limited oxygen index is 36%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Embodiment six
First sodolin being placed in working gas is N
2operating pressure is 10Pa, discharge power is preliminary treatment 180s in the low-temperature plasma device of 150W, then by fabric sodium hydroxide solution preliminary treatment 30min under the condition of 95-100 DEG C, remove impurity, then fabric is washed fully, after removing residual alkali, fabric is put into baking oven and dry at the temperature of 80-90 DEG C.Fabric is taken out and weighs the quality of sodolin.Then be soak 2.5h in the acrylamide monomer solution of 2mol/l in concentration by fabric, then fabric is rolled (padding machine rotating speed 1m/min through a leaching one, pressure 0.1Mpa) after, irradiation is carried out under putting into high-power electron beam, irradiation dose is 65KGy, after completion of the reaction, by fabric taking-up washed with de-ionized water, to remove the homopolymers of fabric face and unreacted grafted monomers, finally dry in an oven to constant weight.The surface grafting rate of sodolin is 38.89%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 1s and 1s respectively, and limited oxygen index is 38.7%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 2s and 2s, limited oxygen index is 36.5%.Illustrate that the durable flame-retardant sodolin of gained has the flame retardant effect of good durability.
Comparative example one
In order to compare with the present invention, by sodolin without low-temperature plasma preprocessing technique, other conditions process with under the identical condition of embodiment 1.The surface grafting rate of gained sodolin is 9.64%, and testing vertical flammability shows that after flame time and time of glowing are reduced to 8s and 7s respectively, and limited oxygen index is 29%.Use the same method for 20 times in washing later and record after flame time and the time of glowing and be respectively 6s and 5s, limited oxygen index is 27%.
By comparing of embodiment 1 and comparative example 1, can find out that the percent grafting of the sodolin after low-temperature plasma preprocessing technique and flame retardant effect are all significantly improved, the persistence of its flame retardant effect is also better simultaneously.As can be seen here, the present invention has primacy.
Example cited by the present invention is only for purpose of explanation, and each reactive material and reaction condition can both realize the present invention in the bound value of each technological parameter, no longer distinguishes illustrative example at this.
The oher improvements and changes that those skilled in the art directly derive without departing from the spirit and concept in the present invention or associate, all should think within protection scope of the present invention.
Claims (7)
1. low-temperature plasma synergistic electron beam irradiation is to a durable flame-retardant graft-modification method for fabric, it is characterized in that: the steps include:
(1) first fabric is placed in low-temperature plasma device and carries out low temperature plasma preliminary treatment;
(2) then fabric sodium hydroxide solution is processed 30min under the condition of 95-100 DEG C, the impurity such as the colloid in removing fabric;
(3) wash fully after being taken out by fabric, putting into baking oven after removing residual hydrogen sodium oxide molybdena under the condition of 80-90 DEG C dries 1-3h, and taking-up is weighed;
(4) fabric of oven dry is immersed in 1-3 hour in grafted monomers solution, takes out subsequently and shut out surplus liquid through padding machine, fabric plastic sheeting is wrapped, puts into valve bag, under fabric is put into high-power electron beam together with valve bag, carry out irradiation;
(5) after irradiation terminates, by the fabric washed with de-ionized water after grafting, the homopolymers of removing fabric face and unreacted grafted monomers; Then the fabric after cleaning is put into baking oven to dry 24 hours, obtain product.
2. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (1), described fabric comprises crudefiber crop, cotton fiber and the bamboo fibres such as flax, ramie, jute, fabric made by the various novel cellulosic fibre of lotus fiber and textiles.
3. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (1), the pretreated process conditions of described low temperature plasma are: the working gas of employing is the mist of one or more gases in argon gas, nitrogen, oxygen and air; Operating pressure is 10-150Pa, and discharge power is 10-300W, and the processing time is 1-20min.
4. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (2), and described concentration of sodium hydroxide solution is 15-30g/L.
5. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (4), described high-energy electron beam irradiation reaction condition is: irradiation dose is 0-100kGy and other radiation unit's transforming numericals corresponding.
6. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (4), atmosphere during described electron beam irradiation, temperature conditions all do not limit, and atmosphere can be divided into atmospheric environment, vacuum environment or contain the inert gas environment of nitrogen and/or helium.
7. a kind of low-temperature plasma synergistic electron beam irradiation according to claim 1 is to the durable flame-retardant graft-modification method of fabric, it is characterized in that: in step (4), in described grafted monomers solution, solute is the one in acrylamide, Methacrylamide, acrylic acid and methacrylate vinyl base monomer, and its concentration is 0.1-10mol/L; Solvent is water.
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| CN105671952A (en) * | 2016-04-26 | 2016-06-15 | 江南大学 | Anti-aging modification method of polyester fabric based on electron irradiation |
| CN106592221A (en) * | 2016-12-07 | 2017-04-26 | 江南大学 | Preparation method of flame-retardant antistatic fabric |
| CN107964778A (en) * | 2017-11-27 | 2018-04-27 | 桐乡佳车科技有限公司 | A kind of cut pile fabric afterfinish method |
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| CN105671952A (en) * | 2016-04-26 | 2016-06-15 | 江南大学 | Anti-aging modification method of polyester fabric based on electron irradiation |
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| CN106592221A (en) * | 2016-12-07 | 2017-04-26 | 江南大学 | Preparation method of flame-retardant antistatic fabric |
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Application publication date: 20151209 |