Patent Application
20140291882
The present invention relates to a processing method of natural cellulose fiber intrinsically with enhanced antiseptic, deodorant and negative-ion features from bamboo, particularly for one regarding bamboo pulp with eco-friendly biodegradable feature. The product of the bamboo cellulose fiber produced by the present invention, either in filament or staple status, do really has effects in antiseptic and deodorant capability as well as anion retentiveness so that it can be used in textile, medical or health-care and bioscience fields as well as wafer-cleaning in semiconductor.
Currently, for raw materials used in producing chemical synthetic fiber, the consumption is polypropylene (PP), polyester (PET), polyethylene (PE) and Nylon in quantity order with overall consumed quantity 96%. However, the wasted fabric of chemical synthetic fiber after having been used incurs a malignant impact to the environment because they are un-biodegradable by natural environment. Nowadays, the manufacturers of the natural cellulose fabric gradually divert to use natural materials such as pulp with suitable solution become a mainstream to substitute for raw materials of chemical synthetic fiber so that it is so called as eco-friendly fiber or Lyocell fiber as the wasted fabric thereof is biodegradable.
Basing on the article in title of “The technological development and application for bamboo charcoal used in textile” publicized by the domestic “Forestry Research Institute in the Council of Agriculture” and research thesis in title of “new regenerated cellulose fiber—bamboo fiber” publicized in the issue 2 of year 2003 of “scientific and technical journals/periodicals” by the “Shandong Province Textile Industry Association” in the Mainland China, it testifies that the bamboo fiber intrinsically has enhanced antiseptic, moisture-absorbing, air-permeating, deodorant and negative-ion health-care features. Moreover, bamboo belong to rapid-growing plant having strong fertility with crop rate to cut down in 2-3 year span and good recycling resource with re-cultivating easiness without any severe ecological destruction to the forest land, which usually happened in cutting down of the timber. Besides, the cost of the bamboo pulp is only one third in the cost of the wood pulp. Therefore, the productions of bamboo fiber by means of solvent means in Lyocell fiber process have been publicized in many patent documents such as Mainland China Invention Patent in Patent Numbers of CN1129680, CN1190531, CN1315624 and CN100395384. However, the common drawback of foregoing Mainland China Invention Patents is lack of deodorant feature and effect on the basis of disclosed specifications thereof.
According to statistical information from the “Tariff Bureau of the Ministry of Finance in Taiwan”, it displays that the annual overall imported quantity of the fresh coffee beans in year 2011 is 17,685 metric tons. The annual overall quantity of wasted coffee residue for the imported fresh coffee beans after it having baked and spent is over 8,842 metric tons suppose the ratio of the wasted coffee residue to the fresh coffee beans is ½ normally. So far, most portion of the wasted coffee residue in 8,842 metric tons is disposed by incineration or being buried under ground while only few portions is used as deodorant, nutrition of the plants or cleaning additive. Besides, someone take the wasted coffee residue to fabricate a coffee yarn product such as Taiwan Invention Patent in Number of 1338729, which discloses the process as following.
(a): By selecting raw material from polypropylene (PP), polyester (PET), polyethylene (PE) and Nylon to prepare high polymer granules;
(b): By using wasted coffee residue to serve as property modifier;
(c): By blending foregoing high polymer granules and wasted coffee residue to become granular additive masterbatch; and
(d): Spin the granular additive masterbatch into yarns.
The drawback of the foregoing coffee yarn product is that it still incurs a malignant impact to the environment because they are un-biodegradable by natural environment since the high polymer granules also selected from polypropylene (PP), polyester (PET), polyethylene (PE) and Nylon.
Other than the wasted coffee residue in 8,842 metric tons mentioned above, there are bamboo forests of 15 hectares area, which is approximately 7.2% of overall tree forest area, in Taiwan too. Having realized foregoing issues, the applicant of the present invention take a long time hard study to perform penetrating and profound research and development in how to take advantages of the biodegradable, antiseptic and negative-ion health care features in the bamboo fiber and the deodorant feature in the wasted coffee residue as well as how to integrate these favorable features into a contemplated ideal natural cellulose fiber from bamboo. Eventually, an expected processing method of natural cellulose fiber intrinsically with enhanced antiseptic, deodorant and negative-ion features from bamboo of the present invention is worked out successfully after many times of experimental tests in trial implements.
The present invention provides a processing method of natural cellulose fiber intrinsically with enhanced antiseptic, deodorant and negative-ion features from bamboo. The processing method firstly blends a selected bamboo pulp with wasted coffee residue as raw material into a mixture. Secondly, put N-methylmorpholine N-oxide (NMMO) as primary dissolving solvent and 1,3-phenylene-bis 2-oxazoline (BOX) as additive stabilizer into prepared bamboo pulp mixture obtained previously for blending and dissolving via rapid grinding of a horizontal dope blending machine; then, dehydrate it via heating up to temperature between 80 degree of Celsius and 120 degree of Celsius (80° C.-120° C.) by vacuum thin film evaporator (VTFE) for 5 minutes to decrease water content thereof down to in range down of 5-13% so that a homogenized mucilaginous dope is formed. Thirdly, spin the dope obtained previously by dry-jet wet spinning method to form into threads. Finally, rinse, desiccate and lubricate the regenerated threads obtained previously as well as wind it up to produce reeled natural bamboo cellulose fiber with enhanced antiseptic, deodorant and negative-ion features such that the resultant fiber product can be either wound into continuous filament yarn or cut into staple fiber in accordance with the requirements specified. The overall process is simplified and shortened by using dry-jet wet spinning method with nontoxic N-methylmorpholine N-oxide (NMMO) as primary dissolving solvent, which is easily recovered and recycled via bleach, filtration, condensation and refinement processes. Besides, by combination the intrinsic antiseptic and negative-ion features of the bamboo cellulose with the deodorant feature of the wasted coffee residue, the fabric product become biodegradable in natural environment without any harmful effect.
For further disclose the fabricating process and efficacy, detailed description for some preferred exemplary embodiments with associated drawings is presented below. Please refer to
a. Material Selection and Preparation: Select bamboo pulp and wasted coffee residue as raw material to blend together mutually into a mixture, preferably the cellulose content of the bamboo pulp being over 80% and the range for degree of polymerization (DP) being 400-800 while the wasted coffee residue having been ground into range of 500 nm-1000 nm (nano-meter) granules in high speed mode;
b. Dope Blending and Dissolution: By putting N-methylmorpholine N-oxide (NMMO), whose chemical structure as shown in ) a rapid grinding of a horizontal dope blending machine; and, by means of cellulose features of high expanding, moistening and dissolving ability as well as high rate of dissolving speed affected by the N-methylmorpholine N-oxide (NMMO) to expedite mutually blending and dissolving effect for forming a slurry; then, dehydrate it via heating up to temperature between 80 degree of Celsius and 120 degree of Celsius (80°-
) vacuum thin film evaporator (VTFE) for 5 minutes to decrease water content thereof down to in range down of 5-13% so that a homogenized mucilaginous dope is formed;
c. Spinning and Thread Formation: Spin the dope obtained from previous step b by dry-jet wet spinning method, wherein the dope is fed into a die assembly and forcedly extruded out of spinnerets into the spinning machine for spinning and coagulation bath for coagulating and regenerating via a quantitative metering gear pump to form thread bundle of bamboo cellulose, wherein certain hot air is continuously fed therein for circulation around peripheral thereof then discharged out via surrounding of the spinnerets; and
d. Finishing and Fiber Formation: The thread bundle obtained from previous step c is orderly treated by water rinsing, desiccating, lubricating, winding-up and the like to produce reeled natural bamboo cellulose fiber with enhanced antiseptic, deodorant and negative-ion features such that the resultant fiber product can be either wound into continuous filament yarn or cut into staple fiber in accordance with the requirements specified, wherein, desiccating process is undertaken with temperature range in 100 degree of Celsius and 150 degree of Celsius (100° C.-150 winding speed in the winding process is in range of 200-800 meter per minute while the produced bamboo cellulose fiber has property that the range of fiber tenacity is 1.5 g/d-4.0 g/d, the range of fiber elongation rate is 4.0%-8.0% and the range of fiber Young's modulus is 50 g/d-150 g/d.
Wherein, the weight content of the wasted coffee residue in the prepared bamboo pulp mixture of step a aforesaid is in a range of 0.5 wt %-5 wt %.
Wherein, in step b above, additive stabilizer 1,3-phenylene-bis 2-oxazoline (BOX) functions to subdue the declining recession for the color and degree of polymerization (DP) of bamboo cellulose while the primary dissolving solvent N-methylmorpholine N-oxide (NMMO) is nontoxic with concentration range of 50%-75% so that it can be recycled with low consumption rate after having been drained out in water rinse process with a range for rate of recovery up to over 99.7%. Thereby, it completely complies with the eco-friendly criteria of the environmental protection because it not only can reduce the manufacturing cost but also will not incur any harmful pollution to the environment.
Furthermore, in the steps d above, the primary NMMO dissolving solvent used in the process of the present invention will be liberated after coagulating, regenerating in coagulation bath and water rinsing process. The actual procedure of the primary NMMO dissolving solvent recovery includes steps as below:
1. Bleach: adopting absorption method of the suspended active carbon. Put 0.05%-0.10% active carbon powder of good absorptivity and suspension ability into the solution of NMMO solvent to be de-colored, then alternate the air-blast mixing absorption and the stationary suspending absorption treatments in treating time ratio is 1:3 to 1:6 for 8 hours to finish the bleaching procedure so that not only the related equipments can be simplified but also the energy can be saved as well as the bleaching effect can be promoted.
2. Filtration: adopting two filtering stages. First coarse filtering stage: for simplifying the equipment, general cartridge filter is used together with the auxiliary filtering agent, which is pre-coated over the surface of the cartridge filter, and put 0.03%-0.05% of leavening agents into the liquid to be filtrated for not only preventing the active carbon from accumulating on the surface thereof in hindering the filtering speed but also regularly maintaining filtering effect of high performance without decay. The composition of said auxiliary filtering agent is preferably made of diatomite and cellulose in ratio of 4:1. After completion of the coarse filtering stage, the filtering dregs and residual liquid are centrifugal and dehydrating treated for recovery so that the residual auxiliary filtering agent dehydrated is reused as auxiliary filtering effect being remained. Second fine filtering stage: by means of fine filter UF, the purity of the filtered liquid is the same as fresh NMMO solvent. The features of this two filtering stages in coarse filtering stage and fine filtering stage are low equipment cost, low consumption rate, high treating quantity and high purity.
3. Condensation: concurrently combining two condensing methods. To recover the rinsing liquid in the present invention, the condensing load in dehydration is very large in manner of approximately 90 tons per ton of fiber as solvent concentration must be condensed from range of 6.5%-8.0% to range of 50%-55%. For low yield quantity of fiber, the tri-effect condensing method is adopted to dehydrate per ton of rinsing liquid in using 0.5 ton of steam (high steam consumption, low electric power consumption); For high yield quantity of fiber, the Mechanical Vapor Recompression (MVR) condensing method is adopted to dehydrate per ton of rinsing liquid in using 0.003-0.03 ton of steam (low steam consumption, high electric power consumption); The yield condensed solvent and water in both foregoing condensing methods are also completely recovered for reusing though each condensing method is only suitable for different specific yield quantity of fiber. Wherein, the yield condensed solvent is reused as processing solvent and yield condensed water is reused to rinse fiber.
4. Refinement: adopting oxidation and neutralizing reduction under low temperature of 80 degree of Celsius (80° C.): Using 35% hydrogen peroxide (H2O2) as oxidant and 85% hydrazine hydrate (N2H4.H2O) as neutralizing reductant, the result is measured by electric potential titrating method; the NMMO content is decreased down below 10 ppm so that not only the purity of NMMO is promoted but also the NMMO consumption is decreased.
For further understanding the efficacy of the present invention, the experimental embodiments with different compositions, conditions and parameters in accordance with process thereof are described in detail as below.
Blend wasted coffee residue with selected bamboo pulp in 500 degree of polymerization (DP) together with primary dissolving solvent N-methylmorpholine N-oxide (NMMO) and various additive ratios of stabilizer 1,3-phenylene-bis 2-oxazoline (BOX) to form a slurry via blending, dissolving and rapid grinding processes; then, dehydrate it via heating up to temperature in range of 80 degree of Celsius and 120 degree of Celsius (80° C.-120) vacuum thin film evaporator (VTFE) for 5 minutes to decrease water content thereof down to range of 5%-13% so that a homogenized mucilaginous dope is formed; spin the dope obtained by dry-jet wet spinning method, which is processed by forcing the dope to spinning machine via quantitative metering pump for extruding the dope out of the spinnerets into the coagulation bath for coagulating and regenerating to form into threads; and rinse, desiccate, lubricate and wind up the regenerated threads obtained to produce reeled natural bamboo cellulose fiber with enhanced antiseptic, deodorant and negative-ion features. The resultant data for samples 1-6 of bamboo cellulose fiber obtained from foregoing embodiment are listed in the Table 1 in sub-title “Embodiment 1:Samples 1-6, which is nested in title of “Dope Constituent Table for Samples 1-12 of bamboo cellulose fiber”.
Blend wasted coffee residue with selected bamboo pulp in 750 degree of polymerization (DP) together with primary dissolving solvent N-methylmorpholine N-oxide (NMMO) and various additive ratios of stabilizer 1,3-phenylene-bis 2-oxazoline (BOX) to form a slurry via blending, dissolving and rapid grinding processes, then, dehydrate it via heating up to temperature between 80 degree of Celsius and 120 degree of Celsius (80°-) vacuum thin film evaporator (VTFE) for 5 minutes to decrease water content thereof down to 5%-13% so that a homogenized mucilaginous dope is formed; spin the dope obtained by dry-jet wet spinning method, which is processed by forcing the dope to spinning machine via quantitative metering pump for extruding the dope out of the spinnerets into the coagulation bath for coagulating and regenerating to form into threads; and rinse, desiccate, lubricate and wind up the regenerated threads obtained to produce reeled natural bamboo cellulose fiber with enhanced antiseptic, deodorant and negative-ion features. The resultant data for samples 1-6 of bamboo cellulose fiber obtained from foregoing embodiment are listed in the Table 1 in sub-title “Embodiment 2:Samples 7-12, which is nested in title of “Dope Constituent Table for Samples 1-12 of bamboo cellulose fiber”.
Usually, bamboo grows in natural wild-field instead of greenhouse. In this natural environment, the reason why bamboo can be free from moth and mildewed is that it has intrinsic anti-bacteria organic compound named “bamboo quinone”, which has antiseptic capability. In this embodiment, we try to test and assay whether the antiseptic capability of the intrinsic “bamboo quinone” can be maintained to what degree if the bamboo is transformed into bamboo cellulose fiber as well as whether the produced bamboo cellulose fiber still possesses such antiseptic capability. The testing bacteria in this embodiment adopt type (A) bacteria: Methicillin Resistant Staphyloccous Aureus (MRSA) (ATCC 6538P) and type (B) bacteria: Klebsiella Pheumoniae (ATCC 4352) as two testing strains or bacteria species.
The experiment is performed in accordance with JIS L1902-1998 Quantitative Method. The incubated bacteria concentration within 1.0±0.3 E+5 (number/ml) means valid for the experiment. And, the numerical (1.3 E+4) denotes 13,000 with analog and so on.
Ma is bacteria number of un-processed sample in immediate count upon cleansing without incubation.
Mb is bacteria number of un-processed sample after being incubated for 18-24 hours.
Mc is bacteria number of processed sample after being incubated for 18-24 hours.
The growing activity value of the bacteria (BGA) is computed by following calculating formula such that BGA>1.5 means valid of the experiment.
Growing Activity value of the Bacteria: BGA=log (Mb)−log (Ma)
Bacteriostatic value of the sampie: BSN=log (Mb)−log (Mc)
Bactericidal value of the sampie: BKN=log (Ma)−log (Mc)
According to the evaluating criterion from the “Japan Association of Fiber Evaluating Technology for new function” (JAFET), the antiseptic function is that the testing sample has bacteriostatic effect if its bacteriostatic value BSN>2.2 while the testing sample has bactericidal effect if its bactericidal value BKN>0. The resultant data in the test for assaying of the antiseptic capability for samples 1-12 of bamboo cellulose fiber obtained from foregoing embodiment are listed in the Table 2 and Table 3.
As shown in the Tables 2 and 3 above, the sample bamboo cellulose fiber of the present invention has excellent antiseptic capability both in bacteriostatic and bactericidal effects for both of bacteria of Methicillin Resistant Staphyloccous Aureus (MRSA) (ATCC 6538P) and Klebsiella Pheumoniae (ATCC 4352).
The experiment for evaluating deodorant effect is on the testing basis in absorption of the ammonia odor. The testing method is performed in following steps.
Step 1: fill the ammonia gas of specific concentration into the air-tight bottle;
Step 2: put the sample Lyocell processed bamboo cellulose fiber of the present invention in specific quantity into the same bottle aforesaid to absorb ammonia gas for 15 minutes; and
Step 3: measure the gas concentration in the sample Lyocell processed bamboo cellulose fiber before and after putting into the bottle by gas chromatograph (GC).
The ratio of the deodorant property (DOP) for ammonia absorption rate test is calculated by following formula.
(DOP) for ammonia absorption rate test: DOP=(Ca−Cr)/Ca
Where, Ca is the gas concentration in the sample fiber before absorbing ammonia while Cr is the gas concentration in the sample fiber after absorbing ammonia.
As shown in the Table 4 above, the sample bamboo cellulose fiber of the present invention has excellent deodorant capability.
Negative ion, which is also called anion, has been recognized as “the vitamin of the air”, confirming its health effect on human. Ions can be generated when a large amount of energy is applied to an atom or a molecule so that negative ions are created in nature with air molecules broken apart by UV radiation from sunlight, cosmic radiation, radioactive substances and thunderstorm as well as water splashing from waterfalls, jetting river, ejecting fountain and raging sea waves. Plants that carry out photosynthesis are also able to generate negative ions. Numerous studies have established the health benefits and therapeutic effect of negative ions that covers at least the following aspects such as (1): Regulating nervous system; (2): Promote the health of cardiovascular system; (3): Enhance the function of respiratory system; (4): Strengthen the function of immune system; (5): Inhibiting oxygen radicals and preventing oxidation; (6): Detoxifying function; (7): Delay aging and enhancing beauty; and (8): Strengthen on the emotional and mental wellness.
The experiment for evaluating anion retentiveness adopts digital air cation/anion ion counter made by specific American manufacturer. The testing method is performed via firstly rub, crumple and knead the sample bamboo cellulose fiber of the present invention by hands; and then count the number of the negative ions by the ion counter. The resultant data for samples 1-12 of bamboo cellulose fiber obtained from foregoing embodiment in evaluating anion retentiveness are listed in the Table 5.
As shown in the Table 5 above, the sample bamboo cellulose fiber of the present invention has excellent anion retentiveness in exceeding normal anion content of 430 (ions/cc) for atmosphere on earth surface.
Put samples 1-12 of bamboo cellulose fiber to launder under condition in 70 degree of Celsius (70° C.) hot water with 5 g/L laundry detergent for 45 minutes. The experimental results for testing by foregoing laundering method for 10 times are shown in the Tables 6, 7 and 8 below.
As the experimental results for testing antiseptic and deodorant capability shown in the Tables 6 and 7, even to launder for 10 times under condition of 70 degree of Celsius (70)° C. hot water with 5 g/L laundry detergent for about 45 minutes, the antiseptic and deodorant capability for the sample bamboo cellulose fiber in the present invention can still keep 95% approximately. Thereby, it really is a natural cellulose fiber with long-lasting persistence in antiseptic and deodorant capability, which is far better than that of marketing antiseptic and/or deodorant fibers processed by surface treatment or antiseptic addition. Besides, from the experimental results for testing anion retentiveness shown in the Table 8, even to launder for 10 times under condition of n 70 degree of Celsius (70° C.) hot water with 5 g/L laundry detergent for 45 minutes, the anion retentiveness for the sample bamboo cellulose fiber in the present invention can still keep obvious anion retentiveness effectively. Thereby, it really is a natural cellulose fiber with long-lasting persistence in anion retentiveness without harmful spoil.
In conclusion the disclosure heretofore, the bamboo cellulose fiber produced by the present invention do really has effects in antiseptic and deodorant capability as well as anion retentiveness so that it can be used in textile, medical or health-care and bioscience fields as well as wafer-cleaning in semiconductor. Thus, it really has innovative novelty beyond obviousness of the prior arts and practical industrial application, which meet the basic criterion of the patentability. Accordingly, we submit the patent application in accordance with the related patent law.
| Number | Date | Country | Kind |
|---|---|---|---|
| 102110616 | Mar 2013 | TW | national |
