CN109930225B - Chlorine-bleaching-free high-whiteness viscose fiber and preparation method thereof - Google Patents
Chlorine-bleaching-free high-whiteness viscose fiber and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 144
- 229920000297 Rayon Polymers 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004061 bleaching Methods 0.000 claims abstract description 94
- 238000009987 spinning Methods 0.000 claims abstract description 70
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 34
- 239000006185 dispersion Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 13
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000007547 defect Effects 0.000 claims abstract description 11
- 239000011593 sulfur Substances 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims description 78
- 239000000243 solution Substances 0.000 claims description 41
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 37
- 239000002253 acid Substances 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 238000006477 desulfuration reaction Methods 0.000 claims description 25
- 230000023556 desulfurization Effects 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 20
- 239000012190 activator Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 230000001112 coagulating effect Effects 0.000 claims description 14
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 230000005070 ripening Effects 0.000 claims description 8
- 239000011550 stock solution Substances 0.000 claims description 8
- 238000004383 yellowing Methods 0.000 claims description 8
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 7
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 4
- 239000007844 bleaching agent Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 3
- -1 amide compound Chemical class 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 125000000373 fatty alcohol group Chemical group 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000460 chlorine Substances 0.000 abstract description 10
- 229910052801 chlorine Inorganic materials 0.000 abstract description 10
- 150000001805 chlorine compounds Chemical class 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000004745 nonwoven fabric Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 2
- 229910052760 oxygen Inorganic materials 0.000 abstract 2
- 239000001301 oxygen Substances 0.000 abstract 2
- 230000004913 activation Effects 0.000 abstract 1
- 150000002926 oxygen Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 36
- 239000003513 alkali Substances 0.000 description 12
- 229910052979 sodium sulfide Inorganic materials 0.000 description 11
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 6
- 235000017491 Bambusa tulda Nutrition 0.000 description 6
- 241001330002 Bambuseae Species 0.000 description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 239000011425 bamboo Substances 0.000 description 6
- 150000002191 fatty alcohols Chemical class 0.000 description 6
- ZBJVLWIYKOAYQH-UHFFFAOYSA-N naphthalen-2-yl 2-hydroxybenzoate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=C(C=CC=C2)C2=C1 ZBJVLWIYKOAYQH-UHFFFAOYSA-N 0.000 description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 description 6
- 235000011152 sodium sulphate Nutrition 0.000 description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 6
- 229960001763 zinc sulfate Drugs 0.000 description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 description 6
- 150000001408 amides Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- 239000005708 Sodium hypochlorite Substances 0.000 description 3
- 239000006081 fluorescent whitening agent Substances 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 235000018167 Reynoutria japonica Nutrition 0.000 description 1
- 240000001341 Reynoutria japonica Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- FRPJTGXMTIIFIT-UHFFFAOYSA-N tetraacetylethylenediamine Chemical compound CC(=O)C(N)(C(C)=O)C(N)(C(C)=O)C(C)=O FRPJTGXMTIIFIT-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to the technical field of chemical fiber processing, in particular to chlorine-free bleaching high-whiteness viscose and a preparation method thereof, wherein chlorine-free bleaching dissolving wood pulp is selected as a raw material to prepare a viscose spinning solution, and the viscose spinning solution is uniformly mixed with a titanium dioxide dispersion solution and then sent into a spinning machine to be solidified and regenerated to obtain nascent fiber; the nascent fiber is drafted and oriented to form fiber with certain strength, the fiber is cut off and then enters a fluff tank and a refiner, and the chlorine-free bleached high-whiteness viscose fiber is prepared by adopting a low-temperature activation oxygen bleaching process. The prepared chlorine-free bleaching high-whiteness viscose fiber has higher whiteness, extremely low defect content and extremely low residual sulfur content, and can be used in the fields of various non-woven fabrics and medical sanitary materials; by adopting the low-temperature activated oxygen bleaching process, the pollution problem of chlorine compounds in the wastewater caused by the chlorine bleaching process is avoided; compared with the high-temperature oxygen bleaching process, the method is favorable for reducing energy consumption, reducing the damage of the mechanical property of the fiber and realizing the comprehensive balance of the mechanical property and whiteness of the fiber.
Description
Technical Field
The invention relates to the technical field of chemical fiber processing, in particular to a chlorine-free bleaching high-whiteness viscose fiber and a preparation method thereof.
Background
Clean high-whiteness viscose fibers are a type of differential viscose fibers and are widely used in the fields of non-woven fabrics, medical sanitary materials and the like. Whiteness is an important evaluation index of clean high-whiteness viscose fibers. In order to improve the whiteness of the fiber, the fiber is bleached mainly by using sodium hypochlorite or hydrogen peroxide in the production of viscose fiber, but the chlorine or chlorine compound bleaching is adopted, so that the pollution problem of the chlorine compound exists in bleaching waste water, and the problems of fiber whiteness insufficiency, high hydrogen peroxide consumption, fiber mechanical property damage and the like exist only by adopting hydrogen peroxide bleaching. In the prior art, in order to improve the whiteness of fibers, a patent with the application number of CN 201010501442.6 discloses a preparation method of totally chlorine-free high-whiteness cellulose fibers, wherein the whiteness of the fibers is improved mainly by adding a fluorescent whitening agent, and a hydrogen peroxide bleaching technology is not involved.
The patent with the application number of CN201610743740.3 discloses a high-whiteness viscose staple fiber and a preparation method thereof, wherein the high-whiteness viscose staple fiber is prepared by adopting a twice bleaching process of a sodium hypochlorite alkaline solution and an activated hydrogen peroxide alkaline solution, the whiteness can reach more than 92%, the strength and elongation and the handfeel softness of the fiber are not affected, and the activating agent used in the application is tetraacetylethylenediamine.
The patent with the application number of CN 201210469572.5 discloses a method for bleaching cotton bast cellulose fibers, which adopts two bleaching processes of sodium hydrosulfite bleaching and hydrogen peroxide bleaching, so that the prepared cotton bast cellulose fibers have good whiteness, the hand feeling and the flexibility of the fibers are improved, the spinning performance of the fibers is improved, the auxiliary agents used in the application comprise urea, magnesium sulfate, penetrant and the like, and the bleaching time is 45-55 min.
In the above patent applications, some use sodium hypochlorite for bleaching, and some use hydrogen peroxide for bleaching, but the bleaching time is long. Because some fluorescent whitening agents are added into medical sanitary materials and have potential risks to human bodies, in order to meet market demands, a preparation process of the chlorine-free high-whiteness viscose fiber without the fluorescent whitening agents needs to be further developed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the chlorine-free bleaching high-whiteness viscose fiber and the preparation method thereof are provided, wherein the whiteness of the fiber is high, and the damage to the mechanical property of the fiber is less.
In order to solve the problems, the specific technical scheme of the invention is as follows:
the chlorine-free bleached high-whiteness viscose fiber is prepared by the following preparation method, and specifically comprises the following steps:
(1) preparing a viscose spinning solution: selecting chlorine-free bleached and dissolved wood pulp as a raw material, preparing a viscose spinning solution by the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 4-1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.5: 100-1.0: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform. The spinning speed of the spinning machine is 45-60 m/min.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent to a refiner and is subjected to the working procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying to prepare the chlorine-free bleaching high-whiteness viscose fiber. The first washing temperature is 70-75 ℃, the second washing temperature is 60-80 ℃, the third washing temperature is 55-70 ℃, and the final washing temperature is 70-75 ℃; the desulfurizer used in the desulfurization process is one or two of sodium hydroxide and sodium sulfide, the concentration of the desulfurizer is 2-5 g/L, and the desulfurization temperature is 65-80 ℃; the bleaching agent is hydrogen peroxide, and the addition amount of the bleaching agent is 3-16 g/L; an activator and a penetrant assistant are used in the bleaching process, wherein the addition amount of the activator is 0.6-4 g/L, and the addition amount of the penetrant is 0.2-1 g/L; the bleaching temperature is 60-80 ℃, the PH value of bleaching liquid is controlled to be 9-12, and the bleaching time is 3-4 min. The activator is an amide compound. The penetrating agent is fatty alcohol polyether surfactant containing carboxylic group and sulfonic group.
The technical parameters of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: the fineness is 1.32-1.75 dtex; the length is 32-40 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is more than or equal to 87.0 percent; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
The present invention uses chlorine-free bleaching to dissolve wood pulp to ensure that the fibers contain no chlorine-containing chemical components. The whiteness of the chlorine-free bleaching-dissolved wood pulp is more than 89%, and the content of methyl cellulose is more than 90%.
The invention is beneficial to improving the whiteness of the fiber by adding the titanium dioxide delustering agent with high whiteness.
The invention optimizes the spinning speed to obtain proper bleaching time and ensure the balance of yield and quality index.
Steam pressure at the inlet of the fluff tank is 1.0-1.5bar, steam bubbles are sprayed out from small holes of a steam spraying pipe at the bottom of the fluff tank and burst on the liquid surface under the action of the steam pressure, and fibers are dispersed to make the thickness of the fiber layer uniform. In addition, the high-temperature steam can remove the acid gas and CS in the fiber2And the steam is discharged and enters a condensation recovery system, so that the residual sulfur content in the fiber is greatly reduced.
In the desulfurization process, the desulfurizer with proper concentration is added for desulfurization, so that the desulfurization effect is enhanced, and the whiteness of the fiber before bleaching is improved.
The penetrant of the fatty alcohol polyether surfactant containing carboxylic acid groups and sulfonic acid groups is added in the bleaching process, is an efficient and environment-friendly surfactant, is beneficial to reducing the surface tension of a solution, accelerates the penetration of the bleaching agent into fibers, and has a synergistic effect on improving the whiteness of the fibers.
According to the invention, a certain proportion of the activating agent containing amide groups is added in the bleaching process, and the activating agent can react with hydrogen peroxide to generate a substance with higher oxidation activity, so that the bleaching can be carried out at a lower temperature, and the damage to the mechanical property of the fiber can be reduced.
The invention is beneficial to reducing the temperature fluctuation of the bleaching solution by increasing the water temperature of the secondary washing so as to improve the bleaching effect.
The invention reduces the impurity content of metal compounds and adjusts the PH value of the fiber by an acid washing process.
The special oil for non-woven fabric used in the invention is a Japanese bamboo oil, has antistatic and smoothing effects, and is safe and nontoxic to human bodies.
The chlorine-free bleaching high-whiteness viscose fiber and the preparation method thereof provided by the invention have the following beneficial effects:
(1) the novel chlorine-bleaching-free high-whiteness viscose fiber prepared by the invention has the advantages of extremely low defect content, extremely low residual sulfur content, less surface active substances and low water-soluble substance content, and can be used in the fields of various non-woven fabrics and medical sanitary materials.
(2) The invention adopts the hydrogen peroxide bleaching process, thereby avoiding the pollution problem of chlorine compounds in the wastewater caused by adopting chlorine or chlorine compound bleaching.
(3) Compared with the traditional high-temperature hydrogen peroxide bleaching process, the low-temperature activated bleaching process is favorable for reducing energy consumption, reducing fiber performance damage and improving the bleaching effect.
(4) The invention adds the environment-friendly penetrant auxiliary agent in the bleaching process to further improve the whiteness of the fiber.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Example 1
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 4; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 1.0: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 45 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 60 ℃, and the drafting rate of the two-bath is 30%. The steam pressure at the inlet of the fluff tank is 1.4 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.75dtex and the length of 40mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 70 ℃, the second washing temperature is 60 ℃, the third washing temperature is 55 ℃, and the final washing temperature is 70 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide and sodium sulfide, the concentration of the sodium hydroxide is 2g/L, the concentration of the sodium sulfide is 2g/L, and the desulfurization temperature is 65 ℃; respectively adding a penetrant containing fatty alcohol polyether surfactant components containing carboxylic acid groups and sulfonic acid groups, an amide activator and hydrogen peroxide into bleaching alkali liquor in a bleaching step, wherein the addition amount of the penetrant is 0.2g/L, the addition amount of the activator is 0.7g/L, and the addition amount of the hydrogen peroxide is 3 g/L; the bleaching temperature is 80 ℃, the pH value of bleaching alkali liquor is 9, and the bleaching time is 4 min. 3g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 4g/L, and the pH value of the oiled filament bundle is 7.1. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: fineness of 1.75 dtex; the length is 40 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 87.0 percent; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
Example 2
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.5: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 60 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 62 ℃, and the drafting rate of the two-bath is 35%. The steam pressure at the inlet of the fluff tank is 1.5 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.32dtex and the length of 32mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 75 ℃, the second washing temperature is 80 ℃, the third washing temperature is 70 ℃, and the final washing temperature is 75 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide, the concentration of the sodium hydroxide is 5g/L, and the desulfurization temperature is 75 ℃; respectively adding a penetrant of a fatty alcohol polyether surfactant containing carboxylic acid groups and sulfonic acid groups, an amide activator and hydrogen peroxide into bleaching alkali liquor in a bleaching step, wherein the adding amount of the penetrant is 1g/L, the adding amount of the activator is 4g/L, and the adding amount of the hydrogen peroxide is 16 g/L; the bleaching temperature is 60 ℃, the pH value of bleaching alkali liquor is 12, and the bleaching time is 3 min. 4g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 3.5g/L, and the pH value of the filament bundle after oiling is 7.2. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: fineness of 1.32 dtex; the length is 32 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 88.0%; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
Example 3
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 55 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 62 ℃, and the drafting rate of the two-bath is 35%. The steam pressure at the inlet of the fluff tank is 1.5 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.69dtex and the length of 38mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 75 ℃, the second washing temperature is 70 ℃, the third washing temperature is 65 ℃, and the final washing temperature is 70 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide and sodium sulfide, the concentration of the sodium hydroxide is 2g/L, the concentration of the sodium sulfide is 3g/L, and the desulfurization temperature is 75 ℃; respectively adding a penetrant containing fatty alcohol polyether surfactant components containing carboxylic acid groups and sulfonic acid groups, an amide activator and hydrogen peroxide into bleaching alkali liquor in a bleaching step, wherein the addition amount of the penetrant is 0.4g/L, the addition amount of the activator is 3g/L, and the addition amount of the hydrogen peroxide is 12 g/L; the bleaching temperature is 70 ℃, the pH value of bleaching alkali liquor is 11, and the bleaching time is 3.3 min. 4g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 3.5g/L, and the pH value of the filament bundle after oiling is 7.1. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: the fineness is 1.69 dtex; the length is 38 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 87.6 percent; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
Example 4
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 4; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 1.0: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 45 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 60 ℃, and the drafting rate of the two-bath is 30%. The steam pressure at the inlet of the fluff tank is 1.4 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.75dtex and the length of 40mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 70 ℃, the second washing temperature is 60 ℃, the third washing temperature is 55 ℃, and the final washing temperature is 70 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide and sodium sulfide, the concentration of the sodium hydroxide is 3g/L, the concentration of the sodium sulfide is 3g/L, and the desulfurization temperature is 80 ℃; respectively adding a penetrant containing fatty alcohol polyether surfactant components containing carboxylic acid groups and sulfonic acid groups, an amide activator and hydrogen peroxide into bleaching alkali liquor in a bleaching step, wherein the addition amount of the penetrant is 0.2g/L, the addition amount of the activator is 0.6g/L, and the addition amount of the hydrogen peroxide is 3 g/L; the bleaching temperature is 80 ℃, the pH value of bleaching alkali liquor is 9, and the bleaching time is 4 min. 3g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 4g/L, and the pH value of the oiled filament bundle is 7.1. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: fineness of 1.75 dtex; the length is 40 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 87.2%; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
Comparative example 1
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 55 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 62 ℃, and the drafting rate of the two-bath is 35%. The steam pressure at the inlet of the fluff tank is 1.5 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.69dtex and the length of 38mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 75 ℃, the second washing temperature is 70 ℃, the third washing temperature is 65 ℃, and the final washing temperature is 70 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide and sodium sulfide, the concentration of the sodium hydroxide is 2g/L, the concentration of the sodium sulfide is 3g/L, and the desulfurization temperature is 75 ℃; respectively adding penetrant containing fatty alcohol polyether surfactant components containing carboxylic acid groups and sulfonic acid groups and hydrogen peroxide into bleaching alkali liquor in a bleaching step, wherein the adding amount of the penetrant is 0.4g/L, and the adding amount of the hydrogen peroxide is 12 g/L; the bleaching temperature is 70 ℃, the pH value of bleaching alkali liquor is 11, and the bleaching time is 3.3 min. 4g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 3.5g/L, and the pH value of the filament bundle after oiling is 7.1. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: the fineness is 1.69 dtex; the length is 38 mm; the dry breaking strength is more than or equal to 2.0 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 86.4%; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
Comparative example 2
(1) Preparing a viscose spinning solution: preparing a viscose spinning solution by using chlorine-free bleaching and dissolving wood pulp with the whiteness of 89% and the content of methyl fibers of 90% as a raw material through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, ripening and the like, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the mixture into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100.
(2) viscose spinning:
the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; the coagulated and regenerated nascent fiber is gathered into a long strand of tows to a drafting machine through a godet roller and a two-bath tank, and the tows are drafted and oriented to form fiber with certain strength, and the fiber is cut off and then enters a fluff tank. The coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 7g/L zinc sulfate and 10g/L Berol Spin 653 surfactant. The temperature of the acid bath is 45 ℃; the spinneret consists of 45 small spinneret caps, each spinneret cap is provided with 2100 holes, and the diameter of each micropore is 0.06 mm. The spinning speed is 55 m/min. The two-bath comprises 30g/l of sulfuric acid, the temperature of the two-bath is 62 ℃, and the drafting rate of the two-bath is 35%. The steam pressure at the inlet of the fluff tank is 1.5 bar.
(3) Post-treatment of viscose fibers:
the viscose staple fiber from the fluff tank is sent into a refiner, and the chlorine-free bleached high-whiteness viscose fiber with the fineness of 1.69dtex and the length of 38mm is prepared after the procedures of primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying. The first washing temperature is 75 ℃, the second washing temperature is 70 ℃, the third washing temperature is 65 ℃, and the final washing temperature is 70 ℃; the desulfurizer used in the desulfurization process is sodium hydroxide and sodium sulfide, the concentration of the sodium hydroxide is 2g/L, the concentration of the sodium sulfide is 3g/L, and the desulfurization temperature is 75 ℃; in the bleaching step, an amide activator and hydrogen peroxide are respectively added into bleaching alkali liquor, wherein the addition amount of the activator is 3g/L, and the addition amount of the hydrogen peroxide is 12 g/L; the bleaching temperature is 70 ℃, the pH value of bleaching alkali liquor is 11, and the bleaching time is 3.3 min. 4g/L sulfuric acid is added in the acid washing process, the post agent used for oiling is a bamboo post agent, the addition amount of the oil agent is 3.5g/L, and the pH value of the filament bundle after oiling is 7.1. The drying temperature is 140 ℃, and after drying, the chlorine bleaching-free high-whiteness viscose fiber product is obtained, and the moisture regain of the product is controlled at 13%.
The quality indexes of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: the fineness is 1.69 dtex; the length is 38 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is 86.8%; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
From the viewpoint of the product properties, the whiteness in examples 1 to 4 was higher than that in comparative example. In comparison with example 3, comparative example 1, which did not use an activator, had lower fiber whiteness and lower dry breaking strength, and comparative example 2, which did not use a penetrant but did not use an activator, had lower fiber whiteness.
Claims (5)
1. A preparation method of chlorine-free bleached high-whiteness viscose is characterized by comprising the following steps:
(1) preparing a viscose spinning solution:
selecting chlorine-free bleached dissolving wood pulp as a raw material, preparing a viscose spinning solution by sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening, uniformly mixing with a titanium dioxide dispersion solution, and then feeding into a spinning machine; the mass ratio of titanium dioxide to pure water in the titanium dioxide dispersion liquid is 1: 4-1: 5; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.5: 100-0.7: 100, respectively;
(2) viscose spinning:
the mixed spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
sending the viscose staple fiber from the fluff tank into a refiner, and performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, acid washing, final washing, oiling, dehydration and drying to obtain the chlorine-free bleached high-whiteness viscose fiber; the bleaching agent used in the bleaching process is hydrogen peroxide, and the addition amount is 3-16 g/L; an activator and a penetrant assistant are used in the bleaching process, wherein the addition amount of the activator is 0.6-4 g/L, and the addition amount of the penetrant is 0.2-1 g/L; the bleaching temperature is 60-80 ℃, the pH value of bleaching liquid is controlled to be 9-12, and the bleaching time is 3-4 min; the activating agent is an amide compound; the penetrating agent is a fatty alcohol polyether surfactant containing carboxylic acid groups and sulfonic acid groups in the components;
the technical parameters of the obtained chlorine-free bleaching high-whiteness viscose fiber are as follows: the fineness is 1.32-1.75 dtex; the length is 32-40 mm; the dry breaking strength is more than or equal to 2.10 cN/dtex; the dry breaking elongation is 19.0 to 22.0 percent; the whiteness is more than or equal to 87.0 percent; the defect content is less than or equal to 1.5mg/100 g; the content of residual sulfur is less than or equal to 5mg/100 g; the surface active matter is less than or equal to 3 mm; the content of water soluble substances is less than or equal to 0.6 percent.
2. The method for preparing chlorine-free bleached high-whiteness viscose fiber according to claim 1, wherein the whiteness of the chlorine-free bleached dissolving wood pulp in the step (1) is more than 89%, and the content of methyl cellulose is more than 90%.
3. The method for preparing chlorine-free bleached high-whiteness viscose fibers according to claim 1, wherein the spinning speed of the spinning machine in the step (2) is 45-55 m/min.
4. The method for preparing the chlorine-free bleached high-whiteness viscose fiber according to claim 1, wherein the temperature of the secondary washing in the step (3) is 70-80 ℃, and the temperature of the tertiary washing is 55-70 ℃.
5. A chlorine-free bleached high-whiteness viscose fiber, which is obtained by the process of any one of claims 1 to 4.
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| CN111058185B (en) * | 2019-12-05 | 2021-02-09 | 湖北拓盈新材料有限公司 | High-strength viscose non-woven fabric and preparation method thereof |
| CN112981577A (en) * | 2019-12-12 | 2021-06-18 | 连津格股份公司 | Method for producing modal fibers completely chlorine-free |
| CN112575402B (en) * | 2020-12-03 | 2022-08-30 | 赛得利（福建）纤维有限公司 | Preparation method of low-odor viscose fibers |
| CN112522817A (en) * | 2020-12-04 | 2021-03-19 | 宜宾丝丽雅股份有限公司 | Production process of odorless viscose fiber |
| CN112553705A (en) * | 2020-12-09 | 2021-03-26 | 赛得利（福建）纤维有限公司 | Preparation method of flame-retardant viscose fibers |
| CN112575403A (en) * | 2020-12-29 | 2021-03-30 | 新疆中泰纺织集团有限公司 | Clean high-whiteness extinction viscose fiber and preparation method thereof |
| CN112813517A (en) * | 2021-01-04 | 2021-05-18 | 山东雅美科技有限公司 | Method for refining and post-treating nonwoven cellulose fibers and nonwoven cellulose fibers |
| CN114197210B (en) * | 2021-12-21 | 2024-03-19 | 赛得利（福建）纤维有限公司 | Hydrophobically modified viscose fiber and preparation method thereof |
| CN115262216B (en) * | 2022-08-29 | 2024-03-19 | 赛得利（福建）纤维有限公司 | Preparation method of high-whiteness antibacterial viscose fiber |
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