CN102127842A - Method for preparing natural cellulose nonwoven fabric in wet-type meltblown mode - Google Patents
Method for preparing natural cellulose nonwoven fabric in wet-type meltblown mode Download PDFInfo
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Abstract
The invention provides a method for preparing a natural cellulose nonwoven fabric in a wet-type meltblown mode, which comprises the following steps: adding an N-methylmorpholine N-oxide solvent into pulp which is used as a raw material, mixing to dissolve the pulp so as to obtain a dope, extruding the dope out of a spinning port in a meltblown mode to form a cellulose filament, solidifying and regenerating the cellulose filament through water spraying, washing with water, carrying out spunlace, drying, coiling and the like, thereby obtaining the natural cellulose fiber nonwoven fabric in a continuous long fiber shape.
Description
[technical field]
The invention relates to a kind of method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens, especially refer to a kind of environmental protection processing procedure that has low manufacturing cost and can not cause environmental pollution, the Nonwovens finished product that it makes belongs to the long fiber kenel, and have rerum naturas such as air permeability and good and water absorption rate, can be applied on the purposes such as textiles, medical and health, filtering material, biotechnology material and the wiping of photoelectricity wafer.
[background technology]
The present made Nonwovens of artificial synthetic fiber, it is high molecular polymerization raw material by fusion, with direct extrusion molding (spunlaid) through extruding extend to form continuous long fiber after, again it being stacked into net form forms, therefore this long fiber can be given Nonwovens and has rerum naturas such as air permeability and good and water absorption rate, so be widely used in large quantities such as on the fields such as amenities, wiping material, medical protection and filter material; The Nonwovens output that other aforementioned direct extrusion molding is produced, its city accounts for the statistics of rate according to U.S. Nonwovens TIA (INDA), grown to 43.7% (first) in 2009 from 33.5% (second) in 1994, whole output also reaches annual 2.7 hundred ten thousand tons, and employed maximum raw material in its production, be polypropylene (PP) in regular turn, polyester (PET), polyethylene (PE) and nylon (Nylon), account for 96% of total use amount altogether, so when these a large amount of artificial synthetic fiber's Nonwovenss become discarded object after using, owing to can't be decomposed by natural environment, on the contrary environment is produced huge bad impact results, moreover, these artificial synthetic fibers' raw material is also non-inexhaustible, be accompanied by the shortage of petrochemical material, its cost of obtaining also can raise gradually, recently produce the dealer of Nonwovens, be and then turn to gradually and use natural material to replace artificial synthetic fiber's raw material, but but find the mode of Nonwovens that this natural material is manufactured, just can reach because of adopting processing procedure long damp process or liquid drugs injection method, except that the direct extrusion molding of cost is the height, its fiber kenel belongs to staple fibre again, cause performances such as the gas permeability of Nonwovens product and water absorption rate to be weakened, therefore, make the Nonwovens product of long fiber kenel as how natural fabric raw material and low-cost processing procedure, just become important business anxious to be broken through.
[summary of the invention]
Main purpose of the present invention is providing a kind of method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens, it is to be that raw material adds oxidation methyl agate beautiful jade (N-methylmorpholineN-oxide with wood pulp (pulp), be called for short NMMO) solvent, make its phase mixed dissolution become mucus (dope), in the mode of melting and spraying (meltbrown) this mucus is formed cellulose tow from spinning mouthful to push out again, and via the ejection water smoke make cellulose tow solidify regeneration, after washing, liquid drugs injection rolls, dry and batch supervisor after, and make native cellulose fibre Nonwovens with continuous fiber kenel, because this processing procedure weak point makes manufacturing cost reduce, and because of using avirulent oxidation methyl agate beautiful jade, and become not the environmental protection processing procedure that can pollute environment as solvent and fully recycling.
Another object of the present invention is that a kind of method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens is being provided, according to the prepared native cellulose fibre Nonwovens of this method, belong to the continuous fiber kenel, except that having rerum naturas such as good gas permeability identical and water absorption rate with artificial synthetic fiber's Nonwovens, when becoming discarded object after it uses, can be in environment natural decomposition, and can not damage environment.
Technical scheme of the present invention is: a kind of method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens, and its step comprises:
A. with the wood pulp raw material;
B. add oxidation methyl agate beautiful jade solvent (N-methylmorpholine N-oxide, be called for short NMMO) and oxazolyl phenyl stabilization agent (1,3-phenylene-bis 2-oxazoline, BOX) in wood pulp, carry out high speed with 50 ℃～80 ℃ low temperature and blend, in 5～10 minutes, evaporate the mixed moisture content of dissolving with 80 ℃～120 ℃ heating again and get rid of and form mucus (dope) to 5%～13%;
C. in the mode of melting and spraying (meltbrown) this mucus is formed cellulose tow from spinning mouthful to push out; And
D. spray water smoke and make this cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch supervisor, can make native cellulose Nonwovens with continuous fiber kenel.
Wherein, this raw material of wood pulp is to select wood pulp or the paper cellulose of alpha-cellulose content at the long and short fiber more than 65% for use, and its cellulosic degree of polymerization is between 500～1200.
Wherein, the concentration of this oxidation methyl agate beautiful jade solvent is 45%～75%.
Wherein, the content of cellulose of mucus is 6wt%～15wt% among this step b, and the viscosity of mucus is 300～3000 (poise), and the printing opacity index of mucus is 1.470～1.495, and the melt index of mucus is 200～1000.
Wherein, the coiling speed of this native cellulose Nonwovens is 2～200 meters of per minutes in the steps d.
Wherein, the basic weight of this native cellulose Nonwovens is 10g/m2～300g/m2 in the steps d.
Wherein, the operating direction of this native cellulose Nonwovens (MD) TENSILE STRENGTH is more than the 15kgf in the steps d, and the TENSILE STRENGTH of vertical direction (CD) is more than the 8kgf.
Wherein, the fibre number of this native cellulose Nonwovens is 1～15um in the steps d.
Wherein, the air permeability of this native cellulose Nonwovens is 100～3500 (cm3/cm2/min) in the steps d.
Wherein, the water absorption rate of this native cellulose Nonwovens is 300%～2000% in the steps d.
A kind of method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens of the present invention, its advantage and effect are: this method processing procedure weak point makes manufacturing cost reduce, and because of using avirulent oxidation methyl agate beautiful jade, and become not the environmental protection processing procedure that can pollute environment as solvent and fully recycling.According to the prepared native cellulose fibre Nonwovens of this method, belong to the continuous fiber kenel, except that having rerum naturas such as good gas permeability identical and water absorption rate, when becoming discarded object after it uses with artificial synthetic fiber's Nonwovens, can be in environment natural decomposition, and can not damage environment.
[description of drawings]
Fig. 1 is a manufacturing process calcspar of the present invention.
Fig. 2 is the oxidation methyl agate beautiful jade solvent used herein chemical structural drawing of (N-methylmorpholine N-oxide is called for short NMMO).
Fig. 3 is the illustrative view of the plain tow of meltblown fibers among the present invention.
Fig. 4 is a manufacturing process schematic diagram of the present invention.
Fig. 5 is the schematic appearance of the obtained native cellulose Nonwovens of the present invention.
Concrete label is as follows among the figure:
1-gear pump 2-mould
3-spins mouth pipe D-mucus
The H-hot-air
[specific embodiment]
Below in conjunction with drawings and Examples, technical scheme of the present invention is described further.
See also Fig. 1 to shown in Figure 5, the present invention uses the wet type mode of melting and spraying to prepare the method for native cellulose Nonwovens, and its step comprises:
A. be raw material with wood pulp (pulp); Select the wood pulp cellulose of alpha-cellulose content at the long and short fiber more than 65% for use, its cellulosic degree of polymerization (degree of polymerization is called for short DP) is between 500～1200;
B. add oxidation methyl agate beautiful jade solvent (N-methylmorpholine N-oxide, be called for short NMMO, its chemical constitution is as shown in Figure 2) and the oxazolyl phenyl stabilization agent (1,3-phenylene-bis 2-oxazoline, BOX) in wood pulp, make its phase mixed dissolution become mucus (dope); It is to utilize horizontal paste mixer, after this wood pulp cellulose, oxidation methyl agate beautiful jade solvent and oxazolyl phenyl additive inserted together, carrying out high speed with 60 ℃～80 ℃ low temperature blends, and by effect such as oxidation methyl agate beautiful jade is big to the cellulose swelling, dissolubility is high and rate of dissolution is fast, reach fast mutual mixed dissolution, utilize the vacuum film evaporimeter with 80 ℃～120 ℃ heating again, the mixed moisture content of evaporation dissolving is got rid of to 5～13% in 5 minutes, can form mucus (dope);
C. in the mode of melting and spraying (meltbrown) mucus is formed cellulose tow from spinning mouthful to push out; As shown in Figure 3, this mucus D is squeezed into by gear pump 1 and spins in mouthful mould 2, enter again and spin the spinning in the mouth pipe 3 of mouthful mould 2, by hot-air H continue to pour into spin mouthful mould 2 after, and, force mucus D from spin mouth pipe 3, to be melted and sprayed and squeeze out the outside cellulose tow that forms from spinning the air-flow effect of discharging around the mouth pipe 3; And
D. spray water smoke and make cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch supervisor (as shown in Figure 4), promptly make native cellulose fibre Nonwovens (as shown in Figure 5) with continuous fiber kenel.
Wherein, the oxazolyl phenyl stabilization agent (1 that step b added, 3-phenylene-bis 2-oxazoline, BOX) can reduce the color and luster of cellulose mucus and the decline of the degree of polymerization, and the concentration of this oxidation methyl agate beautiful jade solvent is 45%～75% and is the avirulence solvent, after in water-washing process, being washed out, can be recovered after more after filtration, decolouring and decompression concentrate and distill and re-use, low and the rate of recovery of its proportion of goods damageds can reach more than 99.5%, not only can reduce manufacturing cost, also can not cause the pollution of environment, meet the standard of environmental protection processing procedure fully.
The content of cellulose of this mucus is 6wt%～15wt% among the step b again, and the viscosity of its mucus is 300～3000 (poise), and the printing opacity index of mucus be 1.470～1.495 and the melt index of mucus be 200～1000.
In addition among the step a employed wood pulp also more alpha-cellulose content at the paper pulp of the long and short fiber more than 65%.
Being further proof characteristics of the present invention and enforcement effect, is to finish every test examples also to illustrate as the back:
At first, form shown in the table as sample in the table one 1 to the mucus of sample 10, it is to be respectively 650～1050 wood pulp cellulose and oxidation methyl agate beautiful jade (NMMO) solvent with the degree of polymerization, become slurries in 60 ℃～80 ℃ following high-speed stirred, utilize the unnecessary moisture content of vacuum film evaporator evaporation then, with 80 ℃～120 ℃ heating, get rid of moisture to 5%～13% in 5 minutes, cellulose dissolution can be become mucus (dope), then, in the mode of melting and spraying (meltbrown) mucus is formed cellulose tow through spinning a mouthful extruding, spraying water smoke again makes cellulose tow solidify regeneration, and wash in regular turn, liquid drugs injection rolls, dry and batch after, promptly finish in the table one sample 1 to each mucus composition table of sample 10.
Table one: sample 1 to the mucus of sample 10 is formed table
| Sample | Cellulosic degree of polymerization | Anti-degree of polymerization decline additive adding proportion (wt%) | Cellulosic degree of polymerization fading rate (%) | Content of cellulose (%) | Solvent (%) | Water content (%) | Mucus viscosity (poise) | Mucus printing opacity index | The |
| 1 | 650 | 0.05％ | 26.2 | 7.6 | 81.3 | 11.1 | 840 | 1.489 | 870 |
| 2 | 650 | 0.10％ | 20.5 | 8.5 | 81.9 | 9.6 | 980 | 1.482 | 820 |
| 3 | 650 | 0.15％ | 14.7 | 9.1 | 81.2 | 9.7 | 1240 | 1.486 | 810 |
| 4 | 650 | 0.20％ | 11.6 | 8.5 | 82.0 | 9.5 | 1060 | 1.481 | 820 |
| 5 | 650 | 0.25％ | 11.3 | 8.2 | 81.8 | 10.0 | 960 | 1.485 | 830 |
| 6 | 1050 | 0.05％ | 26.5 | 7.8 | 81.8 | 10.4 | 1240 | 1.481 | 750 |
| 7 | 1050 | 0.10％ | 21.7 | 7.5 | 81.1 | 11.4 | 1560 | 1.480 | 720 |
| 8 | 1050 | 0.15％ | 15.9 | 9.1 | 82.1 | 8.8 | 1420 | 1.482 | 700 |
| 9 | 1050 | 0.20％ | 13.8 | 8.2 | 82.0 | 9.8 | 1280 | 1.476 | 740 |
| 10 | 1050 | 0.25％ | 12.1 | 7.9 | 81.0 | 11.1 | 1320 | 1.479 | 710 |
Then, according to the fiber degree of polymerization in the table one and anti-degree of polymerization decline additive adding proportion, the sample 11 of making different Nonwovens basic weights is to sample 20, carry out the test of its Nonwovens intensity, its mode of carrying out detects according to the CNS5610 standard, method is as follows: respectively with operating direction (the Mechanical Direction of each sample, MD) and vertical direction (Cross Direction, CD), take off each 10 of extension test test pieces, its test piece length is at least 180mm, width is 2.54mm, uses omnipotent strength tester to test, and setting the folder distance is 76mm, rate of extension 300mm/min, sample 11 to the Nonwovens intensity of sample 20 test back gained is as shown in Table 2.
Table two: sample 11 is to the rerum natura table of sample 20
| Sample | Cellulosic degree of polymerization | Anti-degree of polymerization decline additive adding proportion (wt%) | Nonwovens basic weight g/m 2 | Nonwovens intensity MD direction kgf | Nonwovens intensity CD direction kgf | Fibre number um |
| 11 | 650 | 0.05％ | 75 | 15.1 | 8.3 | 4.2 |
| 12 | 650 | 0.10％ | 76 | 16.0 | 8.9 | 3.8 |
| 13 | 650 | 0.15％ | 75 | 16.1 | 8.2 | 4.5 |
| 14 | 650 | 0.20％ | 74 | 16.0 | 8.0 | 3.5 |
| 15 | 650 | 0.25％ | 75 | 15.5 | 8.8 | 4.7 |
| 16 | 1050 | 0.05％ | 75 | 15.8 | 8.8 | 5.5 |
| 17 | 1050 | 0.10％ | 74 | 15.2 | 9.1 | 5.8 |
| 18 | 1050 | 0.15％ | 76 | 16.7 | 9.4 | 6.2 |
| 19 | 1050 | 0.20％ | 75 | 16.2 | 9.5 | 5.9 |
| 20 | 1050 | 0.25％ | 75 | 16.1 | 9.5 | 7.2 |
At last, make sample 21 to sample 32 with the different fiber degree of polymerization and Nonwovens basic weight again, carry out the test of its Nonwovens air permeability and water absorption rate, its mode of carrying out detects according to the CNS5612 standard, is that sample is cut into 26 * 26cm
2Each four, with the air permeability testing machine: TEXTEST FX3300 is to 26 * 26cm
2Test piece carry out air permeability test, earlier Nonwovens is cut 5 vertical test pieces, the width of each test piece is 76mm, then (one the quality of test piece is 5.0 ± 0.1g) to decide to length on the quality of test piece, test piece and basket are immersed in the water, went through for 10 seconds, hold the again openend of basket, test piece and basket are taken out in water together, allow the basket openend up, dripped for 10 seconds, immediately this test piece and basket are put into together to know the glass of quality, taking by weighing the gross mass of test piece, basket and glass, accurately is 0.1g.The water absorption rate value formula of test piece is as follows:
Sample 21 to the Nonwovens air permeability and the water absorption rate of sample 32 test back gained is as shown in Table 3.
Table three: sample 21 is to the rerum natura table of sample 32
| Sample | Cellulosic degree of polymerization | Nonwovens basic weight (g/m 2) | Fibre number (um) | Nonwovens air permeability (Cm 3/cm 2/min) | Nonwovens water absorption rate (%) |
| 21 | 650 | 25 | 4.1 | 2650 | 450 |
| 22 | 650 | 75 | 3.6 | 605 | 520 |
| 23 | 650 | 125 | 4.6 | 219 | 610 |
| 24 | 650 | 175 | 3.4 | 195 | 750 |
| 25 | 650 | 225 | 4.6 | 182 | 920 |
| 26 | 650 | 300 | 4.2 | 145 | 1420 |
| 27 | 1050 | 25 | 5.2 | 2870 | 420 |
| 28 | 1050 | 75 | 5.6 | 627 | 550 |
| 29 | 1050 | 125 | 6.0 | 230 | 650 |
| 30 | 1050 | 175 | 5.9 | 211 | 730 |
| 31 | 1050 | 225 | 6.2 | 195 | 880 |
| 32 | 1050 | 300 | 5.8 | 158 | 1350 |
By the sample 21 of sample 11 in the above-mentioned table two to sample 20 and the table three to shown in the sample 32, native cellulose fibre Nonwovens according to the continuous fiber kenel that the present invention finished, no matter the intensity of its operating direction (MD) or vertical direction (CD) is all very desirable, air permeability under the different basic weights and water absorption rate performance, also all be better than existing known artificial synthetic fiber's Nonwovens and natural fabric Nonwovens, so meet required requirement condition on the purposes such as textiles, health care material, filter material, biotechnology material and the wiping of photoelectricity wafer fully.
Claims (10)
1. method of using the wet type mode of melting and spraying to prepare the native cellulose Nonwovens, it is characterized in that: its step comprises:
A. with the wood pulp raw material;
B. add oxidation methyl agate beautiful jade solvent and oxazolyl phenyl stabilization agent in wood pulp, carry out high speed with 50 ℃～80 ℃ low temperature and blend, in 5～10 minutes, evaporate the mixed moisture content of dissolving with 80 ℃～120 ℃ heating again and get rid of and form mucus to 5%～13%;
C. in the mode of melting and spraying this mucus is formed cellulose tow from spinning mouthful to push out; And
D. spray water smoke and make this cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch program, can make native cellulose Nonwovens with continuous fiber kenel.
2. method according to claim 1 is characterized in that: this raw material of wood pulp is to select wood pulp or the paper cellulose of alpha-cellulose content at the long and short fiber more than 65% for use, and its cellulosic degree of polymerization is between 500～1200.
3. method according to claim 1 is characterized in that: the concentration of this oxidation methyl agate beautiful jade solvent is 45%～75%.
4. method according to claim 1 is characterized in that: the content of cellulose of mucus is 6wt%～15wt% among this step b, and the viscosity of mucus is 300～3000, and the printing opacity index of mucus is 1.470～1.495, and the melt index of mucus is 200～1000.
5. method according to claim 1 is characterized in that: the coiling speed of this native cellulose Nonwovens is 2～200 meters of per minutes in the steps d.
6. method according to claim 1 is characterized in that: the basic weight of this native cellulose Nonwovens is 10g/m in the steps d
2～300g/m
2
7. method according to claim 1 is characterized in that: the operating direction TENSILE STRENGTH of this native cellulose Nonwovens is more than the 15kgf in the steps d, and the TENSILE STRENGTH of vertical direction is more than the 8kgf.
8. method according to claim 1 is characterized in that: the fibre number of this native cellulose Nonwovens is 1～15um in the steps d.
9. method according to claim 1 is characterized in that: the air permeability of this native cellulose Nonwovens is 100～3500cm in the steps d
3/ cm
2/ min.
10. method according to claim 1 is characterized in that: the water absorption rate of this native cellulose Nonwovens is 300%～2000% in the steps d.
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Effective date of registration: 20201021 Address after: Room 230, No. 415, Jiujiang Road, Shanghai, Huangpu District Patentee after: Zhang Wenbo Address before: Xiang Yong Le Cun Chinese Taiwan Changhua County Puyan Fan Jin Road No. 94 Patentee before: ACELON CHEMICAL AND FIBER Corp. |