CN101275289A - Frozen-irradiated auxiliary degumming process for china-hemp fibers - Google Patents
Frozen-irradiated auxiliary degumming process for china-hemp fibers Download PDFInfo
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- CN101275289A CN101275289A CNA2008100549865A CN200810054986A CN101275289A CN 101275289 A CN101275289 A CN 101275289A CN A2008100549865 A CNA2008100549865 A CN A2008100549865A CN 200810054986 A CN200810054986 A CN 200810054986A CN 101275289 A CN101275289 A CN 101275289A
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Abstract
The invention discloses a hemp fiber freezing radiation auxiliary de-gumming technique, comprising the following steps of undergoing UV radiation, quenching, and heating treatment after hot bath, acid pre-etching, and pre-chlorination, and then undergoing base oxygen-mechanical associative de-gumming treatment, finally adding a softener for secondary scouring. The hemp fiber surface de-gumming effect treated by the technique is prior to ordinary base oxygen method and mechanical de-gumming, and the former meets the requirement of product of national first grade; the lignin content meets requirement of finishing technique after spinning, which obtains good whiteness and flexibility, and controls breaking strength and tensile stretch of fiber in requirement of spinnability, with improved length and fineness of fiber is improved, greatly improved serviceability, and less pollutant effluents discharged, so that the invention is environment-friendly.
Description
Technical field
The present invention relates to a kind of Chinese fiber crops (being hemp) fiber degumming tech, particularly at alkali oxygen--on the basis of mechanically combining degumming method, be aided with a kind of frozen-irradiated auxiliary degumming process for china-hemp fibers of freezing heating and intensive ultraviolet radiation.
Background technology
The Degumming method of existing Chinese fiber crops (being hemp) fiber, as: traditional quick-fried method of pond Process of retting flax with, chemical degumming law, bacterial degumming method, enzymatic degumming, sudden strain of a muscle, alkali oxygen method, ultrasonic wave degumming method and mechanical-chemical degumming method etc.
The Feng Xinxing of Institutes Of Technology Of Zhejiang, Chen Jianyong etc. are CN1851062 at publication number, name is called in the patent of invention of " a kind of hemp degumming process ", adopt method that normal temperature and pressure and High Temperature High Pressure combine to the china-hemp fibers processing of coming unstuck, comparing general degumming tech saved time more than 1.5 hour, alkali concn reduces greatly, and content of lignin is lower than 0.5% in the fiber crops of processing back, the powerful basic free of losses of fiber, degummed ramie is pure white loose, and quality is good.But residual gum content of not mentioned in the present invention Chinese fiber crops and content of lignin may exist the still high problem of residual gum content and content of lignin.
The Chen Hongzhang of Beijing Saiterui Science ﹠ Technology Development Co., Ltd. etc. are CN1772976 at publication number, name is called in the patent of invention of " a kind of Degumming method of flax fibre and the flax fibre of production thereof ", earlier flax fibre was soaked in water 40-80 minute, then moisture flax fibre is put into the gas explosion jar, at pressure is 1.3-1.7MPa, dwell time is that vapour is quick-fried under 3-8 minute condition, takes out washing, oven dry.Can appropriateness come unstuck like this, can avoid again polluting, improved degumming rate and branch fiber number greatly and do not damaged fiber again, the spinnability of hemp is improved greatly, saved cost 1/3.But fibre whiteness and flexibility are not enough, and residual gum content and content of lignin may be still higher.
The Jiang Guohua of Hunan Institute Of Engineering has inquired into the influence of pre-chlorine treatment process parameter to Chinese fiber crops process of fiber quality, obtained the best pre-chlorine technological parameter of Chinese fiber crops: effective chlorine density is 1.5g/L, the pre-chlorine time is 10mim; bath raio is 1: 15; pH value is 3.0 (normal temperature); the residual gum content of the china-hemp fibers after this PROCESS FOR TREATMENT is 3.49%; do not reach the technological requirement about 2%; residual lignin is 0.94%; be higher than 0.8%; to spinning post-finishing, and especially the dyeing processing has adverse effect, and fibre whiteness and flexibility are lower.
What the Qu Lijun of University Of Qingdao and Guo Xiaoqing etc. had studied a kind of fully " environmental protection " revolves roll-type physical mechanical Degumming method, and Chinese fiber crops colloid and unsticking form tested and analyze, set up under the physical mechanical degumming method about Chinese fiber crops colloid and fiber unsticking mechanical model, but can only effectively dispel in the raw ramie 30% colloid, and fibre whiteness is lower.
The Qu Lijun of University Of Qingdao and Guan Yunling carry out the research of the short flow process degumming and bleaching of alkaline oxygen bath one-step method new technology to Chinese fiber crops, the soda boiling and two step of the bleaching operation of routine are shortened to a step, and the optimal processing parameter of having determined the alkaline oxygen bath degumming method is: NaOH concentration 10.5g/L, H
2O
29.8g/L, processing time 127min, the ultimate strength of these PROCESS FOR TREATMENT Later Han Dynasty fiber crops is 29.6cN, residual gum content is 3.82%, be higher than 2%, do not reach the requirement that appropriateness is come unstuck, residual lignin is 3.25%, is higher than 0.8%, to spinning post-finishing, especially it is 45.7 that the processing of dyeing has adverse effect, whiteness, still on the low side;
The Li Jie of Wenzhou Vocational ﹠ Technical College adopts anacidity preliminary treatment and heavy two to boil the Chinese fiber crops raw ramie of PROCESS FOR TREATMENT high lignin, obtains good effect.The Zhou Yang of Dalian Polytechnic College weaving light industry institute and a large amount of experiments of processes such as Hao Xinmin of General Logistics Department quartermaster equipment exhibition area research institute draw, and the alkali consumption of the most suitable china-hemp fibers high temperature scouring is 14% under the certain condition.But the degumming effect that these two kinds of technologies still exist is undesirable, the residual gum content problem of higher, and also whiteness and flexibility are not good enough.
Summary of the invention
The purpose of this invention is to provide a kind of frozen-irradiated auxiliary degumming process for china-hemp fibers, have to solve that to exist residual gum content in Chinese retting process higher now, problem such as undesirable and whiteness of lignin removal effect and flexibility are lower; Two of purpose is that the Chinese fiber crops after handling reach the requirement of national Grade A, and meets the demand of spinning post-finishing technology.
The present invention realizes above-mentioned purpose and the technical scheme that the solves the problems of the technologies described above processing method that comprises that the processed by hot bath, preimpregnation acid treatment of fiber, pre-chlorine are handled and alkali oxygen-mechanically combining comes unstuck, be characterized in after pre-chlorine is handled, carry out following steps (in the following steps, the proportioning of fiber and solution is soaks 25 gram fibers in every liter of solution, promptly the concentration of china-hemp fibers in solution is 25g/L):
(1) UV radiation: will soak the china-hemp fibers of 25g/L, the hydrogen peroxide of 10-14g/L, the NaOH of 10-14g/L and the magnesium sulfate MgSO of 3-4g/L
4Mixed solution placed under the ultraviolet light of 280-350nm radiation 30-50 minute;
(2) quenching is freezed to thaw with high temperature: fiber after the radiation and mixed solution are stirred in the lump, and quenching places its taking-up 100 ℃-120 ℃ constant temperature boiling water to thaw fully until ice cube to freezing then;
(3) alkali oxygen-mechanical kiering: in the fiber after thawing, adding the boiling-off auxiliary agent stirs, kiering 150min-200min in 100 ℃-120 ℃ water bath with thermostatic control, and the NaOH, hydrogen peroxide and the magnesium sulfate MgSO that in 20min-30min adding above-mentioned steps (1), configure
4The state of mixed solution before kiering, to carry out mechanical agitation simultaneously, stir speed (S.S.) is 150-200r/min, alr mode be every 20min-30min suitable/stir counterclockwise alternately;
(4) during the secondary kiering, add the softener of 20-40g/L.
The composition of boiling-off auxiliary agent and content are described in the frozen-irradiated auxiliary degumming process for china-hemp fibers of the present invention: waterglass sodium metasilicate (Na
2SiO
3) 0.1-0.3g/L, vulcanized sodium (Na
2S) 1-3g/L, sodium phosphate trimer (Na
5P
3O
10) 1-3g/L, sodium sulfite (Na
2SO
3) 0.7-0.9g/L; Described softener is that fiber crops are used nanometer softener MS-2, weave with the soft and graceful T20 of powerful film, high-hydroscopicity softener SF8800 or super soft environment-protective adhesive TEP.
During the technical scheme of the above-mentioned frozen-irradiated auxiliary degumming process for china-hemp fibers of the invention process, its main process characteristics are: (1) is at the pretreatment stage of china-hemp fibers, adopt hot bath, pre-pickling and special pre-chlorine to handle, so not only make fiber loose, remove the part water-solubility impurity, be beneficial to and come unstuck, and make fiber obtain preliminary oxidation bleaching and abundant swollen, the most important thing is to overcome the shortcoming that simple pickling processes makes lignin be difficult to remove; (2) china-hemp fibers is before a kiering, add NaOH, hydrogen peroxide and stabilizing agent magnesium sulfate in advance, and be placed on radiation under the intensive ultraviolet, make its fiber surface gelatinous layer be subjected to etching and destruction, increase and expanded crack, and most of cellulose of oxidation and part lignin, fibre whiteness is increased, the easier dissolving of lignin comes off; (3) fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing, take out then and put into the heating of constant temperature boiling water and thaw, in this process, rapid pucker ﹠ bloat in various degree takes place in fiber and colloid matrix simultaneously, cause its positive and negative drawing power effect that is subjected to vertical and horizontal, make colloid further destroy even come off; When (4) fiber after thawing being carried out the boiling-off of alkali oxygen method together with original mixed solution, add boiling-off additive, and take the circumstances into consideration to replenish the mixed solution of hydrogen peroxide, NaOH and the magnesium sulfate of evaporating loss, simultaneously with suitable/mechanical agitation of replacing counterclockwise, make that china-hemp fibers is easier to come unstuck; (5) to the fiber after the kiering, can repeat above-mentioned radiation-freezing-steps such as heating-kiering, carry out the secondary kiering, make its degumming effect better; (6) operation after the kiering and conventional chemical come unstuck consistently, obtain comparatively desirable china-hemp fibers.
Compare with the Chinese fiber crops that prior art is handled through the Chinese fiber crops that process of the present invention is handled, the present invention is at alkali oxygen--on the basis of mechanically combining degumming method, further be aided with freezing heating and intensive ultraviolet radiation treatment protocols, solved not only that to exist residual gum content in the existing Chinese retting process higher, problems such as the undesirable and serious environment pollution of lignin removal effect, and the Chinese fiber crops after handling have reached the requirement of national Grade A, meet the demand of spinning post-finishing technology.Simultaneously when the present invention obtains good whiteness and flexibility, also the ultimate strength of fiber and percentage elongation are controlled at and spin within the requirement; The length and the fineness of fiber also are improved, and wearability improves greatly.Its concrete beneficial effect also is (1) china-hemp fibers smooth surface after this PROCESS FOR TREATMENT, does not have remaining colloid substantially, as shown in Figures 1 and 2.(2) infared spectrum before and after coming unstuck shows that this technology is more thorough to the removal of lignin, hemicellulose and pectic substance, and especially the clearance to lignin is very high, and its characteristic peak disappears substantially; And part fiber macromolecular chain is terminal oxidized, illustrates that the oxidation bleaching degree of fiber is higher, sees accompanying drawing 3 and accompanying drawing 4.(3) come unstuck before and after the every performance indications of china-hemp fibers relatively as table 1.
Table 1
As can be seen from Table 1, adopt this technology one boil with two boil come unstuck after, 1. lignin, pectin content and residual gum content have all had tangible reduction, especially lignin boils one and is reduced to 0.75% and 0.73% respectively after boiling with two, residual gum content is reduced to 2.58% and 2.44% respectively, compare with the conventional chemical Degumming method, degumming effect is excellent to be obviously, meets the process requirements of spinning post-finishing; 2. the whiteness of fiber and softness are greatly improved, and the outward appearance of its stipe part and root fiber and feel all become pure white smooth, and be soft fine and smooth, sees accompanying drawing 5, Fig. 6, Fig. 7 and Fig. 8; Though 3. fiber row yielding and ultimate strength decrease, but still can guarantee the needs of spinning post-finishing; 4. after this PROCESS FOR TREATMENT, the average diameter of fiber and average length number value diminish, and wearability makes moderate progress.(4) this technology is to be aided with freezing heating and intensive ultraviolet radiation means on alkali oxygen-mechanically combining degumming tech basis again, and the pollutant effluents discharging is less, is a kind of relatively new technology of environmental protection.
Description of drawings
Fig. 1 is the untreated Chinese fiber crops of a present invention raw ramie SEM picture
Among the figure: the gum level of Chinese fiber crops raw ramie is higher, covers thicklyer, and covers dense evenly, and vertically is continuous band-shaped distribution along fiber.
Fig. 2 is come unstuck a Chinese fiber crops sem photomicrograph after handling of the present invention
Among the figure: fiber surface is smooth, does not have remaining colloid and impurity, can see many darker longitudinal grooves and part micropore.
Fig. 3 is Chinese fiber crops raw ramie of the present invention and the infared spectrum figure (local 1) that comes unstuck and handle Later Han Dynasty fiber crops
Among the figure: 1683.99cm
-1The stretching vibration absworption peak of C=O among the representative-CH=CH-CHO of place, china-hemp fibers after this PROCESS FOR TREATMENT has bigger enhancing at this place, peak, this just shows in the process of coming unstuck, the terminal oxidized degree of china-hemp fibers strand is higher, because oxidized bleaching of fiber so that whiteness increase are apparent in view.1734.02cm
-1What the place represented is C=O stretching vibration peak (xylan), and this is the characteristic peak of hemicellulose, handles the vibration peak of back china-hemp fibers at this place and is tending towards disappearing, and shows that the removal of hemicellulose is more thorough when coming unstuck.1629.40cm
-1What the place represented also is the C=O stretching vibration, but it is the characteristic absorption peak of lignin, and this peak also disappears substantially after the processing of coming unstuck, and the removal of lignin is more thorough.
Fig. 4 is Chinese fiber crops raw ramie of the present invention and the infared spectrum figure (local 2) that comes unstuck and handle Later Han Dynasty fiber crops,
Among the figure: 1319.98cm
-1The place is C=O stretching vibration in the lignin, and after coming unstuck, this peak disappears substantially, illustrates that this processing is very obvious to the removal effect of lignin.
Fig. 5 is a Chinese fiber crops raw ramie stipe part fiber shape appearance figure of the present invention
Among the figure: fiber colour is dark yellow, and there are many impurity and spot in the surface, and fiber is parallel closely is arranged in many elongated sheet strips, is wound in the reunion shape each other.
Fig. 6 is the present invention's Later Han Dynasty fiber crops stipe part fiber shape appearance figure that comes unstuck
Among the figure: fibre whiteness is significantly improved, and colloid and impurity are removed substantially, and flexibility is fine, and the fiber exquisiteness is shinny, is separated into many tuftlets and twines agglomerating each other.
Fig. 7 is a Chinese fiber crops raw ramie root fiber shape appearance figure of the present invention
Among the figure: fiber is parallel sheet or the strip of closely being arranged in the colloid matrix, and separation property each other is relatively poor, and color is dark yellow, and impurity is more, and fibre sheet is stronger and strong, and flexibility and crimpiness are relatively poor.
Fig. 8 is the present invention's snippings portion of Later Han Dynasty fiber shape appearance figure that comes unstuck
Among the figure: fiber becomes pure white shinny, soft fine and smooth, and separation property is better between fiber and the fiber, and surface impurity and colloid are removed substantially, and fiber forms certain curling.
The specific embodiment
The present invention can further describe by the specific embodiment in the technical scheme described in the foregoing invention content, and its described beneficial effect also can reach its described effect by specific embodiment.
Embodiment 1
The detailed process step of frozen-irradiated auxiliary degumming process for china-hemp fibers of the present invention is as follows:
One, processed by hot bath
Under 80 ℃, soak fiber 100min fully with deionized water (concentration of fiber in solution is 25g/L), and with agitator every 10min suitable/stir counterclockwise alternately it soaked evenly.Washing several times with clear water, is 7 until its soak pH value.
Two, preimpregnation acid treatment
Under 60 ℃, adopting concentration is that the dilute sulfuric acid of 9.8g/L soaks Gansu Chinese fiber crops raw ramie (concentration of fiber in solution is 25g/L) 100min fully, every 10min suitable/alternately stir counterclockwise it soaked evenly.Washing several times with clear water, is 7 until its soak pH value.
Three, pre-chlorine is handled
At normal temperatures, regulating pH value is 4, and adopting effective chlorine density is that the clorox of 1g/L soaks Gansu Chinese fiber crops raw ramie (concentration of fiber in solution is 25g/L) 40min fully, every 10min suitable/stir alternately counterclockwise that it is soaked is even.Washing several times with clear water, is 7 until its soak pH value.
Four, UV radiation
With preliminary treatment Later Han Dynasty fiber crops, put into the hydrogen peroxide of 12g/L, the NaOH of 12g/L and the magnesium sulfate mixed solution of 3.5g/L and soak (fiber is 25g/L in the concentration of solution) fully, and place radiation 40min under the ultraviolet light of wavelength 300nm, during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.
Five, quenching is freezed
Fiber and mixed solution after the taking-up radiation stir, and again it are put into plastic cup in the lump, place suddenly and freeze the freezing 240min of case, freeze fully until it.
Six, high temperature thaws
Taking-up is freezed Later Han Dynasty fiber crops and is placed 100 ℃ constant temperature boiling water to thaw fully until ice cube.
Seven, alkali oxygen-mechanical boiling-off
In the fiber after thawing, adding mixes and consoluet self-control boiling-off auxiliary agent (waterglass sodium metasilicate (Na
2SiO
3) 0.2g/L, vulcanized sodium (Na
2S) 2g/L, sodium phosphate trimer (Na
5P
3O
10) 2g/L, sodium sulfite (Na
2SO
3) 0.8g/L) stir, in 100 ℃ water bath with thermostatic control, heat 180min, and take the circumstances into consideration to add the mixed solution of a spot of NaOH, hydrogen peroxide and magnesium sulfate, to remedy the evaporation loss in the boiling-off process every 20min.During water-bath, must be 180r/min also with the agitator speed governing, every 25min suitable/stir counterclockwise alternately and make its boiling-off even.Take out fiber at last, the dilute sulfuric acid with 9.8g/L soaks 5min earlier, and cleaning until its soak pH value with clear water is 7 again.
Eight, secondary kiering
With the Chinese fiber crops after the kiering, the fiber crops of putting into the magnesium sulfate of NaOH, 3.5g/L of hydrogen peroxide, the 12g/L of 12g/L and 30g/L are soaked (fiber is 25g/L in the concentration of solution) fully with the mixed solution of nanometer softener MS-2, and place radiation 40min under the ultraviolet light of wavelength 300nm, during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.And then repeat above-mentioned 5-7 step.
Nine, scutching-dehydration-oil supply-de-oiled water-dry/dry.
Embodiment 2
According to the process of embodiment 1, the difference of embodiment 2 is:
One, when the UV radiation, hydrogen peroxide concentration is 10g/L, and naoh concentration is 10g/L, and magnesium sulfate concentration is 3g/L, and the ultraviolet radiation wavelength is 280nm, and radiated time is 30min.
Two, when the kiering of alkali oxygen, the kiering time is 150min, and the kiering temperature is 100 ℃, and agitator speed is 150r/min, alr mode be every 30min suitable/stir counterclockwise alternately.
Three, during the secondary kiering, the fiber crops that add 20g/L are with nanometer softener MS-2.
Embodiment 3
According to the process of embodiment 1, the difference of embodiment 3 is:
One, when the UV radiation, hydrogen peroxide concentration is 14g/L, and naoh concentration is 14g/L, and magnesium sulfate concentration is 4g/L, and the ultraviolet radiation wavelength is 350nm, and radiated time is 50min.
Two, when the kiering of alkali oxygen, the kiering time is 200min, and the kiering temperature is 120 ℃, and agitator speed is 200r/min, alr mode be every 20min suitable/stir counterclockwise alternately.
Three, during the secondary kiering, the weaving that adds 40g/L is with the soft and graceful T20 of powerful film.
Embodiment 4
According to the process of embodiment 1, the difference of embodiment 4 is:
During first and second kiering, the mixed solution (fiber is 25g/L in the concentration of solution) of china-hemp fibers being put into the high-hydroscopicity softener SF8800 of the magnesium sulfate of NaOH, 4g/L of hydrogen peroxide, the 10g/L of 14g/L and 30g/L soaks fully, and place radiation 40min under the ultraviolet light of wavelength 300nm, during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.And then the 5-7 step in the repetition embodiment 1.
Embodiment 5
According to the process of embodiment 1, the difference of embodiment 5 is:
During first and second kiering, the mixed solution (fiber is 25g/L in the concentration of solution) of china-hemp fibers being put into the super soft environment-protective adhesive TEP of the magnesium sulfate of NaOH, 3g/L of hydrogen peroxide, the 14g/L of 10g/L and 40g/L soaks fully, and place radiation 40min under the ultraviolet light of wavelength 280nm, during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.And then the 5-7 step in the repetition embodiment 1.
Claims (3)
1. frozen-irradiated auxiliary degumming process for china-hemp fibers, the processing method that comprises that the processed by hot bath, preimpregnation acid treatment of fiber, pre-chlorine are handled and alkali oxygen-mechanically combining comes unstuck, it is characterized in that after pre-chlorine is handled, carry out following steps (in the following steps, the proportioning of fiber and solution is soaks 25 gram fibers in every liter of solution, promptly the concentration of china-hemp fibers in solution is 25g/L):
(1) UV radiation: will soak the china-hemp fibers of 25g/L, the hydrogen peroxide of 10-14g/L, the NaOH of 10-14g/L and the magnesium sulfate MgSO of 3-4g/L
4Mixed solution placed under the ultraviolet light of 280-350nm radiation 30-50 minute;
(2) quenching is freezed to thaw with high temperature: fiber after the radiation and mixed solution are stirred in the lump, and quenching places its taking-up 100 ℃-120 ℃ constant temperature boiling water to thaw fully until ice cube to freezing then;
(3) alkali oxygen-mechanical kiering: in the fiber after thawing, adding the boiling-off auxiliary agent stirs, kiering 150min-200min in 100 ℃-120 ℃ water bath with thermostatic control, and the NaOH, hydrogen peroxide and the magnesium sulfate MgSO that in 20min-30min adding step (1), configure
4The state of mixed solution before kiering, carry out mechanical agitation simultaneously, stir speed (S.S.) is 150-200r/min, alr mode be every 20min-30min suitable/stir counterclockwise alternately;
(4) during the secondary kiering, add the softener of 20-40g/L.
2. frozen-irradiated auxiliary degumming process for china-hemp fibers as claimed in claim 1 is characterized in that the composition of boiling-off auxiliary agent and content are: waterglass sodium metasilicate (Na
2SiO
3) 0.1-0.3g/L, vulcanized sodium (Na
2S) 1-3g/L, sodium phosphate trimer (Na
5P
3O
10) 1-3g/L, sodium sulfite (Na
2SO
3) 0.7-0.9g/L.
3. frozen-irradiated auxiliary degumming process for china-hemp fibers as claimed in claim 1 is characterized in that softener is that fiber crops are used nanometer softener MS-2, weave with the soft and graceful T20 of powerful film, high-hydroscopicity softener SF8800 or super soft environment-protective adhesive TEP.
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CN102330158A (en) * | 2011-08-09 | 2012-01-25 | 太原理工大学 | Hemp degumming and softening synchronous treatment process |
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DE265205C (en) * | 1911-11-11 | |||
GB166044A (en) * | 1920-07-06 | 1921-07-14 | Emil Claviez | Improved treatment of bast-fibres |
CN1036797C (en) * | 1994-06-17 | 1997-12-24 | 山东省东平大麻纺织总厂 | Technology for quickly hemp degumming |
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