CN112647144A - Preparation method of sweet wormwood cellulose fiber - Google Patents
Preparation method of sweet wormwood cellulose fiber Download PDFInfo
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- CN112647144A CN112647144A CN202011493796.0A CN202011493796A CN112647144A CN 112647144 A CN112647144 A CN 112647144A CN 202011493796 A CN202011493796 A CN 202011493796A CN 112647144 A CN112647144 A CN 112647144A
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- artemisinin
- liquid
- artemisia apiacea
- solution
- cellulose
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 45
- 235000001405 Artemisia annua Nutrition 0.000 title claims abstract description 30
- 240000000011 Artemisia annua Species 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- BLUAFEHZUWYNDE-NNWCWBAJSA-N artemisinin Chemical compound C([C@](OO1)(C)O2)C[C@H]3[C@H](C)CC[C@@H]4[C@@]31[C@@H]2OC(=O)[C@@H]4C BLUAFEHZUWYNDE-NNWCWBAJSA-N 0.000 claims abstract description 99
- 229960004191 artemisinin Drugs 0.000 claims abstract description 99
- 229930101531 artemisinin Natural products 0.000 claims abstract description 99
- 239000000835 fiber Substances 0.000 claims abstract description 19
- 229920000223 polyglycerol Polymers 0.000 claims abstract description 13
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008117 stearic acid Substances 0.000 claims abstract description 12
- 241000049464 Artemisia apiacea Species 0.000 claims abstract 15
- 235000011570 Artemisia caruifolia var apiacea Nutrition 0.000 claims abstract 15
- 229920000297 Rayon Polymers 0.000 claims description 42
- 238000009987 spinning Methods 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 30
- 238000004132 cross linking Methods 0.000 claims description 25
- 239000006185 dispersion Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 18
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 18
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 18
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- AFOSIXZFDONLBT-UHFFFAOYSA-N divinyl sulfone Chemical compound C=CS(=O)(=O)C=C AFOSIXZFDONLBT-UHFFFAOYSA-N 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 4
- RQFLGKYCYMMRMC-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O RQFLGKYCYMMRMC-UHFFFAOYSA-N 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 abstract description 7
- 239000001913 cellulose Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 230000001112 coagulating effect Effects 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 229930003944 flavone Natural products 0.000 description 3
- 235000011949 flavones Nutrition 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004627 regenerated cellulose Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- 238000002166 wet spinning Methods 0.000 description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 3
- 229960001763 zinc sulfate Drugs 0.000 description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 description 3
- XMIIGOLPHOKFCH-UHFFFAOYSA-N 3-phenylpropionic acid Chemical compound OC(=O)CCC1=CC=CC=C1 XMIIGOLPHOKFCH-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229930004069 diterpene Natural products 0.000 description 2
- 150000004141 diterpene derivatives Chemical class 0.000 description 2
- 150000002212 flavone derivatives Chemical class 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 229930004725 sesquiterpene Natural products 0.000 description 2
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- GOLORTLGFDVFDW-UHFFFAOYSA-N 3-(1h-benzimidazol-2-yl)-7-(diethylamino)chromen-2-one Chemical compound C1=CC=C2NC(C3=CC4=CC=C(C=C4OC3=O)N(CC)CC)=NC2=C1 GOLORTLGFDVFDW-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- -1 coumarin, flavone Chemical class 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 201000004792 malaria Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Abstract
The invention discloses a preparation method of artemisia apiacea cellulose fibers, which solves the technical problem that after the existing artemisinin and cellulose fibers are compounded, the compound content in the cellulose and the strength of the fibers are required to be further improved so as to meet the requirements of higher requirements. The invention comprises dispersing artemisinin dissolving solution by polyglycerol monoester stearic acid and cyclohexane to obtain artemisinin dispersing solution. The sweet wormwood cellulose fiber prepared by the invention has the advantages of high sweet wormwood content, high breaking strength and the like.
Description
Technical Field
The invention relates to the technical field of functional cellulose fibers, and particularly relates to a preparation method of sweet wormwood herb cellulose fibers.
Background
The sweet wormwood herb is a common traditional Chinese medicine, mainly contains various chemical components such as sesquiterpene, diterpene, flavone, phenylpropionic acid, coumarin, flavone and volatile oil, and has pharmacological activities of resisting malaria, resisting tumors, inhibiting bacteria, killing insects, relieving fever, resisting inflammation, regulating immunity and the like. The sweet wormwood herb has various chemical components, including sesquiterpene, diterpene, flavone, phenylpropionic acid, coumarin, volatile oil and the like. The sesquiterpenoids are not only the main component of the sweet wormwood herb, but also the important effective component, and have wide pharmacological action.
The regenerated cellulose fiber is produced by using natural cellulose (cotton, hemp, bamboo, tree, shrub) as a raw material, and only changing the physical structure of the natural cellulose without changing the chemical structure of the natural cellulose. Active hydroxyl exists on cellulose molecules, so that each link in the production of the regenerated cellulose fiber can be grafted and copolymerized with other molecules for combined modification.
The artemisinin is compounded with the regenerated cellulose fiber to obtain a spinning product which is beneficial to human health, and the spinning product is popular with the public, but at present, the binding force of the artemisinin and the cellulose fiber and the strength of the fiber compounded with the artemisinin need to be further improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: after the existing artemisinin is compounded with cellulose fiber, the compounding content in the cellulose and the strength of the fiber are required to be further improved so as to meet the requirements of higher requirements.
The invention is realized by the following technical scheme:
a method for preparing herba Artemisiae Annuae cellulose fiber comprises dispersing artemisinin solution with polyglycerol monoester stearic acid and cyclohexane to obtain artemisinin dispersion.
The invention considers that the sweet wormwood is added into the cellulose fiber and needs to be fully dispersed to ensure that the sweet wormwood is uniformly mixed with the fiber spinning solution and obtain a fiber product with better performance, therefore, the artemisinin solution is dispersed by adopting different dispersing agents twice in sequence, wherein polyglycerol monoester stearic acid is a nonionic surfactant, is relatively stable and has good dispersion effect under alkaline, acidic and neutral environments, and is also a good defoaming agent, which is beneficial to defoaming when the artemisinin dispersion solution and the viscose spinning solution are mixed at the later stage, and cyclohexane is taken as a dispersing phase to further disperse the artemisinin, thereby obtaining the artemisinin dispersion solution with good dispersion effect, and being beneficial to compounding with the cellulose fiber at the later stage.
The invention preferably discloses a preparation method of sweet wormwood cellulose fiber, which comprises the steps of treating artemisinin dispersion liquid by using hydroxypropyl methyl cellulose and carrying out crosslinking modification by using divinyl sulfone to obtain sweet wormwood crosslinking liquid.
The added cyclohexane has a good dispersing effect, but also has a certain diluting effect, and the composite effect is poor under the condition that the artemisinin dispersion liquid is too thin, so that the hydroxypropyl methyl cellulose is added into the artemisinin dispersion liquid to play a thickening effect, the artemisinin dispersion liquid is more favorably reacted with the cellulose, and in order to further improve the reaction of the artemisinin with the cellulose fiber, the divinyl sulfone is also adopted to modify the artemisinin so that the artemisinin is more easily reacted with the cellulose fiber, and the content of the artemisinin in the cellulose fiber is improved.
The invention preferably discloses a preparation method of sweet wormwood cellulose fiber, which comprises the following steps: dissolving artemisinin in organic alcohol solution and purifying.
Further, the organic alcohol solution is 20-80% of ethanol solution, the dissolving temperature is 40-70 ℃, and the dissolving and heat preservation time is 0.5-2 h.
The invention preferably discloses a preparation method of sweet wormwood herb cellulose fibers, which comprises the following purification steps: firstly, carrying out suction filtration to primarily remove impurities, and then centrifuging to carry out secondary impurity removal.
Furthermore, the aperture of the filter cloth of the filter is 600-1200 meshes, the rotation speed of the centrifugation is 2000-6000 rpm, and the time of the centrifugation is 2-10 minutes.
The invention obtains the artemisinin solution with higher content through multiple purifications.
The invention preferably discloses a preparation method of sweet wormwood herb cellulose fibers, wherein the addition amount of polyglycerol monoester stearic acid is 0.5-1 per mill of the artemisinin liquid, and the addition amount of cyclohexane is 0.2-15% of the artemisinin liquid.
The invention preferably discloses a preparation method of sweet wormwood herb cellulose fibers, wherein the addition amount of the hydroxypropyl methyl cellulose is 2-8% of the artemisinin dispersion liquid.
The invention preferably relates to a preparation method of sweet wormwood herb cellulose fibers, wherein the addition amount of the divinyl sulfone is 2-10% of the artemisinin dispersion liquid.
The invention preferably discloses a preparation method of sweet wormwood cellulose fiber, wherein the sweet wormwood cross-linking solution and the viscose spinning solution are firstly subjected to primary defoaming respectively, and then are mixed and subjected to secondary defoaming.
According to the invention, through the combined action of defoaming twice and defoaming action of the polyglycerol monoester stearic acid added in the early stage, bubbles in the mixed spinning solution are completely removed, and the obtained fiber has high strength.
The invention preferably discloses a preparation method of sweet wormwood cellulose fiber, wherein the sweet wormwood cross-linking liquid and the viscose spinning liquid are mixed according to the mass ratio of the artemisinin to the viscose spinning liquid of 1-40: mixing at a ratio of 60-99.
The invention preferably discloses a preparation method of sweet wormwood cellulose fiber, which is characterized in that sweet wormwood cross-linking liquid and viscose spinning liquid are mixed for spinning, and then are solidified, solidified and post-treated to obtain sweet wormwood viscose fiber.
The invention adopts a two-bath wet spinning method, the defoamed artemisinin-containing viscose is fed into a spinning machine through a viscose supply pipeline, is quantitatively fed through a metering pump, is filtered again for particle impurities through a candle filter, and is fed into a spinneret assembly through a bent pipe. The adhesive is passed under pressure through a plurality of orifices to form a plurality of adhesive streamlets.
After the viscose flows out, the viscose enters a coagulating bath and is coagulated and formed into primary filaments by the coagulating bath with the sodium sulfate of 250-360g/L, the sulfuric acid of 80-130g/L, the zinc sulfate of 10-50g/L, the aluminum sulfate of 8-25g/L, the specific gravity of 1.25-1.32 and the temperature of 40-60 ℃. The primary filament is sent by a godet to be bundled and drawn, in a curing bath, the primary filament is drawn and simultaneously finally finishes the decomposition and regeneration process, the structure and the performance of the fiber are basically shaped, and a stable sheath-core structure is formed.
Cutting the fiber bundle according to a certain specification, and then carrying out acid pickling, desulfurization, water washing, acid pickling, water washing, oiling, dehydration and drying to obtain the artemisinin viscose fiber.
The invention has the following advantages and beneficial effects:
1. the invention adopts polyglycerol monoester stearic acid and cyclohexane to disperse the artemisinin liquid, the hydroxypropyl methyl cellulose is thickened to strengthen the crosslinking effect, and then the divinyl sulfone is adopted to carry out crosslinking modification, so that the obtained artemisinin crosslinking liquid has good bonding property with the cellulose fiber and high fiber breaking strength.
2. The invention obtains high-content artemisinin solution through multiple purification.
3. The invention has the advantages that the polyglycerol monoester stearic acid is added for dispersion and has the defoaming effect, and the strength of the cellulose fiber is improved while the content of the artemisinin in the cellulose fiber is increased through twice defoaming.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
A preparation method of sweet wormwood cellulose fiber comprises the following steps:
step 1: preparation of artemisinin dissolving solution
Dissolving artemisinin powder in ethanol solution, stirring, adding ethanol to dissolve artemisinin powder completely, wherein the mass ratio of artemisinin powder to ethanol solution is 1:5, the dissolving temperature is 60 deg.C, the concentration of ethanol solution is 60%, and keeping the temperature for 2h to obtain artemisinin dissolving solution.
Step 2: purification of artemisinin
And (3) carrying out suction filtration on the artemisinin solution by using a suction filter, wherein the aperture of filter cloth is 800 meshes, removing impurities, and then filtering by using a centrifugal machine at the rotating speed of 5000 r/min for 8 min to obtain the artemisinin solution.
And step 3: preparation of artemisinin dispersion
Adding 0.8 ‰ polyglycerol monoester stearic acid into the solution, stirring, and adding 6% cyclohexane to obtain artemisinin dispersion.
And 4, step 4: preparation of artemisinin crosslinking solution
Preparing hydroxypropyl methyl cellulose into a 2% solution, adding a hydroxypropyl methyl cellulose solution according to the amount of 6% of the sweet wormwood herb dispersion solution, quantitatively and slowly adding the hydroxypropyl methyl cellulose solution into the artemisinin dissolving solution through a metering pump, continuously stirring, fully mixing the two solutions, standing for 3 hours, defoaming the artemisinin solution treated by the hydroxypropyl methyl cellulose, slowly adding 6% of divinyl sulfone of the artemisinin solution into the artemisinin solution containing the hydroxypropyl methyl cellulose to obtain an artemisinin crosslinking solution, ensuring uniform distribution, and defoaming again.
And 5: mixing artemisinin crosslinking solution and viscose spinning solution
And (2) defoaming the viscose for the first time, respectively conveying the artemisinin crosslinking solution and the viscose spinning solution to a pre-spinning process for static mixing by a metering pump and a supply system, and defoaming for the second time, wherein the mass ratio of the artemisinin dissolving solution to the viscose spinning solution is that the artemisinin accounts for 20%, and the mass ratio of the viscose spinning solution accounts for 80%.
Step 6: spinning
And (3) adopting a two-bath wet spinning method, feeding the defoamed artemisinin-containing viscose into a spinning machine through a viscose supply pipeline, quantitatively feeding the viscose into the spinning machine through a metering pump, filtering out particle impurities again through a candle filter, and feeding the viscose into a spinneret assembly through a bent pipe. The adhesive is passed under pressure through a plurality of orifices to form a plurality of adhesive streamlets.
And 7: solidification and solidification
After the viscose flows out, the viscose enters a coagulating bath, and is coagulated and formed into primary filaments by the coagulating bath with 300g/L of sodium sulfate, 110g/L of sulfuric acid, 35g/L of zinc sulfate, 20g/L of aluminum sulfate, 1.30 of specific gravity and 40-60 ℃ of temperature. The primary filament is sent by a godet to be bundled and drawn, in a curing bath, the primary filament is drawn and simultaneously finally finishes the decomposition and regeneration process, the structure and the performance of the fiber are basically shaped, and a stable sheath-core structure is formed.
And 8: post-treatment
Cutting the fiber bundle according to a certain specification, and then carrying out acid pickling, desulfurization, water washing, acid pickling, water washing, oiling, dehydration and drying to obtain the artemisinin viscose fiber.
Example 2
A preparation method of sweet wormwood cellulose fiber comprises the following steps:
step 1: preparation of artemisinin dissolving solution
Dissolving artemisinin powder in ethanol solution, stirring, adding ethanol to dissolve artemisinin powder completely, wherein the mass ratio of artemisinin powder to ethanol solution is 1:5, the dissolving temperature is 60 deg.C, the concentration of ethanol solution is 60%, and keeping the temperature for 1h to obtain artemisinin dissolving solution.
Step 2: purification of artemisinin
And (3) carrying out suction filtration on the artemisinin solution by using a suction filter, wherein the aperture of filter cloth is 800 meshes, removing impurities, and then filtering by using a centrifugal machine at the rotating speed of 5000 r/min for 8 min to obtain the artemisinin solution.
And step 3: preparation of artemisinin dispersion
Adding 0.5 ‰ polyglycerol monoester stearic acid into the solution, stirring, and adding 0.2% cyclohexane to obtain artemisinin dispersion.
And 4, step 4: preparation of artemisinin crosslinking solution
Preparing 1% solution from hydroxypropyl methyl cellulose, adding a hydroxypropyl methyl cellulose solution according to the amount of 2% of the sweet wormwood herb dispersion liquid, quantitatively and slowly adding the hydroxypropyl methyl cellulose solution into the artemisinin dissolving solution through a metering pump, continuously stirring, fully mixing the two solutions, standing for 1h, defoaming the artemisinin solution treated by hydroxypropyl methyl cellulose, slowly adding 2% divinyl sulfone of the artemisinin solution into the artemisinin solution containing hydroxypropyl methyl cellulose to obtain the artemisinin crosslinking solution, ensuring uniform distribution, and defoaming again.
And 5: mixing artemisinin crosslinking solution and viscose spinning solution
And (2) defoaming the viscose for the first time, respectively conveying the artemisinin crosslinking solution and the viscose spinning solution to a pre-spinning process for static mixing by a metering pump and a supply system, and defoaming for the second time, wherein the mass ratio of the artemisinin dissolving solution to the viscose spinning solution is that the artemisinin accounts for 20%, and the mass ratio of the viscose spinning solution accounts for 80%.
Step 6: spinning
And (3) adopting a two-bath wet spinning method, feeding the defoamed artemisinin-containing viscose into a spinning machine through a viscose supply pipeline, quantitatively feeding the viscose into the spinning machine through a metering pump, filtering out particle impurities again through a candle filter, and feeding the viscose into a spinneret assembly through a bent pipe. The adhesive is passed under pressure through a plurality of orifices to form a plurality of adhesive streamlets.
And 7: solidification and solidification
After the viscose flows out, the viscose enters a coagulating bath, and is coagulated and formed into primary filaments by the coagulating bath which contains 250g/L of sodium sulfate, 80g/L of sulfuric acid, 10g/L of zinc sulfate and 8g/L of aluminum sulfate, has the specific gravity of 1.25 and is at the temperature of 50 ℃. The primary filament is sent by a godet to be bundled and drawn, in a curing bath, the primary filament is drawn and simultaneously finally finishes the decomposition and regeneration process, the structure and the performance of the fiber are basically shaped, and a stable sheath-core structure is formed.
And 8: post-treatment
Cutting the fiber bundle according to a certain specification, and then carrying out acid pickling, desulfurization, water washing, acid pickling, water washing, oiling, dehydration and drying to obtain the artemisinin viscose fiber.
Comparative example 1
This example differs from example 1 in that the dispersion was carried out without the addition of polyglycerol monoester stearic acid and cyclohexane after the purification of the artemisinin solution.
Comparative example 2
This example differs from example 1 in that the artemisinin dispersion was not viscosified with hydroxypropyl methylcellulose prior to crosslinking.
Comparative example 3
The difference between this example and example 1 is that only after mixing the artemisinin crosslinking solution and the viscose spinning solution, the deaeration is performed once, and the artemisinin crosslinking solution and the viscose spinning solution are not deaerated separately.
The protein content and the fiber breaking strength of the above examples and comparative examples were measured, and the results are shown in table 1 below:
TABLE 1 table of the performance test of samples obtained in different examples
As can be seen from table 1 above:
(1) after the purified artemisinin solution is dispersed by polyglycerol monoester stearic acid and cyclohexane, the obtained artemisinin cellulose fiber has high breaking strength and high artemisinin content.
(2) After the artemisinin dispersion liquid is thickened by adding hydroxypropyl methyl cellulose, the crosslinking effect is better, and the obtained artemisinin cellulose fiber has higher breaking strength and higher artemisinin content.
(3) Through twice deaeration, the obtained sweet wormwood cellulose fiber has higher breaking strength, and the artemisinin content is slightly higher than that of once deaeration.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of sweet wormwood cellulose fiber is characterized in that polyglycerol monoester stearic acid and cyclohexane are adopted to disperse artemisinin dissolving solution to obtain artemisinin dispersing solution.
2. The method for preparing artemisia apiacea cellulose fibers according to claim 1, wherein the artemisia apiacea cross-linking liquid is obtained by treating the artemisinin dispersion liquid with hydroxypropyl methyl cellulose and performing cross-linking modification with divinyl sulfone.
3. The method for preparing artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the method for preparing the artemisinin liquid comprises the following steps: dissolving artemisinin in organic alcohol solution and purifying.
4. The method for preparing artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the purification step is: firstly, carrying out suction filtration to primarily remove impurities, and then centrifuging to carry out secondary impurity removal.
5. The method for preparing artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the addition amount of the polyglycerol monostearate stearic acid is 0.5-1 per thousand of the artemisinin liquid, and the addition amount of the cyclohexane is 0.2-15% of the artemisinin liquid.
6. The method for preparing Artemisia apiacea cellulose fiber according to claim 1 or 2, wherein the amount of the hydroxypropyl methylcellulose is 2-8% of the artemisinin dispersion.
7. The method for preparing artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the divinyl sulfone is added in an amount of 2-10% of the artemisinin dispersion.
8. The method for preparing artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the artemisia apiacea crosslinking liquid and the viscose spinning liquid are firstly subjected to primary defoaming respectively and then mixed and subjected to secondary defoaming.
9. The preparation method of the artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the artemisia apiacea crosslinking liquid and the viscose spinning liquid are mixed according to a mass ratio of the artemisinin to the viscose spinning liquid of 1-40: mixing at a ratio of 60-99.
10. The preparation method of the artemisia apiacea cellulose fibers according to claim 1 or 2, wherein the artemisia apiacea viscose fibers are obtained through solidification, solidification and post-treatment after the artemisia apiacea cross-linking liquid and the viscose spinning liquid are mixed and spun.
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| CN108754659A (en) * | 2018-06-04 | 2018-11-06 | 汕头市欣和棉麻纺织有限公司 | A kind of qinghaosu cellulose fibre and preparation method thereof |
| US20190203381A1 (en) * | 2017-12-29 | 2019-07-04 | Infinitus(China) Company Ltd. | A method for preparing regenerated cellulose fibers having anti-bacteria, anti-mite and anti-mould functions and the use thereof |
| CN110230112A (en) * | 2019-06-05 | 2019-09-13 | 罗莱生活科技股份有限公司 | A kind of antibiosis anti-acarien smelly eliminating viscose fiber and preparation method thereof |
| CN111719244A (en) * | 2020-06-18 | 2020-09-29 | 山东理工大学 | Preparation of polycaprolactone/collagen composite nanofiber membrane with artemisinin slow-release function |
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| US20190203381A1 (en) * | 2017-12-29 | 2019-07-04 | Infinitus(China) Company Ltd. | A method for preparing regenerated cellulose fibers having anti-bacteria, anti-mite and anti-mould functions and the use thereof |
| CN108754659A (en) * | 2018-06-04 | 2018-11-06 | 汕头市欣和棉麻纺织有限公司 | A kind of qinghaosu cellulose fibre and preparation method thereof |
| CN110230112A (en) * | 2019-06-05 | 2019-09-13 | 罗莱生活科技股份有限公司 | A kind of antibiosis anti-acarien smelly eliminating viscose fiber and preparation method thereof |
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