CN117737876A - Preparation method of nitrogen-phosphorus flame-retardant viscose fiber - Google Patents
Preparation method of nitrogen-phosphorus flame-retardant viscose fiber Download PDFInfo
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- CN117737876A CN117737876A CN202311530524.7A CN202311530524A CN117737876A CN 117737876 A CN117737876 A CN 117737876A CN 202311530524 A CN202311530524 A CN 202311530524A CN 117737876 A CN117737876 A CN 117737876A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 104
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000000835 fiber Substances 0.000 title claims abstract description 63
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229920000297 Rayon Polymers 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000009987 spinning Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000004061 bleaching Methods 0.000 claims abstract description 11
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 11
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- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 42
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 239000002002 slurry Substances 0.000 claims description 27
- 238000007598 dipping method Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 22
- 229910052759 nickel Inorganic materials 0.000 claims description 21
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000001112 coagulating effect Effects 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- 238000004383 yellowing Methods 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 229920002678 cellulose Polymers 0.000 claims description 10
- 239000001913 cellulose Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 10
- 229960001763 zinc sulfate Drugs 0.000 claims description 10
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 10
- 239000007844 bleaching agent Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 230000003009 desulfurizing effect Effects 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 244000261422 Lysimachia clethroides Species 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 230000005070 ripening Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 abstract description 21
- 238000002347 injection Methods 0.000 abstract description 11
- 239000007924 injection Substances 0.000 abstract description 11
- 238000010790 dilution Methods 0.000 description 8
- 239000012895 dilution Substances 0.000 description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000012946 outsourcing Methods 0.000 description 4
- 239000008234 soft water Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 239000012991 xanthate Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 description 1
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- -1 alkoxy cyclotriphosphazene Chemical compound 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000003292 glue Substances 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- VMGAPWLDMVPYIA-HIDZBRGKSA-N n'-amino-n-iminomethanimidamide Chemical compound N\N=C\N=N VMGAPWLDMVPYIA-HIDZBRGKSA-N 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- BOLDJAUMGUJJKM-LSDHHAIUSA-N renifolin D Natural products CC(=C)[C@@H]1Cc2c(O)c(O)ccc2[C@H]1CC(=O)c3ccc(O)cc3O BOLDJAUMGUJJKM-LSDHHAIUSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention provides a preparation method of nitrogen-phosphorus flame-retardant viscose fiber, which adopts a pre-spinning injection method to blend a novel flame-retardant system with viscose to prepare a flame-retardant fiber product with better physical and mechanical properties and washing resistance. Comprises (1) preparing a flame retardant solution; (2) preparing a spinning primary solution; (3) blending spinning; (4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product. The invention endows the finished product with excellent flame retardance and spinnability.
Description
Technical Field
The invention belongs to the technical field of textile, and particularly relates to a preparation method of nitrogen-phosphorus flame-retardant viscose fiber.
Background
The viscose fiber comprises cellulose as main component, and has a zigzag skin-core structure in transverse section and a groove structure distributed on longitudinal surface. The preparation method comprises the steps of taking natural fibers as raw materials, preparing soluble cellulose xanthate through the procedures of alkalization, aging, yellowing and the like, preparing viscose liquid by dissolving the soluble cellulose xanthate in dilute alkali solution, and preparing the viscose liquid through wet spinning.
The selection of the flame retardant in the research and development process of the flame retardant viscose fiber has important significance. Currently, flame retardants that find application in the viscose field include: DDPS, THPX, alkoxy cyclotriphosphazene, MDPA and the like, but the flame retardant performance, physical and mechanical properties, environmental protection, toxicity, water resistance and the like are irregular. For example, in the CN103643334a patent, zinc oxide is selected as a flame retardant, and the zinc oxide exists in the form of particles in the viscose solution, so that the phenomenon of blocking the spinneret orifices is easy to occur, and the spinning uniformity is affected; in the patent CN106884310B, a mode of adding a microcapsule flame retardant into a spinning coagulating bath is selected, metal powder is used as a flame-retardant matrix, the addition of the flame retardant into the coagulating bath has great influence on industrial production, and meanwhile, the flame retardance and the water washing resistance of the fiber are poor.
Disclosure of Invention
Conventional halogen-based flame retardants are considered to be efficient flame retardants for cellulose, but the halogen-based flame retardants are increasingly limited in use by toxic and corrosive substances released during use. Instead, a halogen-free flame retardant is used. The halogen-free flame retardant mainly comprises phosphate, phosphorus nitrogen compound, phosphorus silicon compound, nitrogen silicon compound, silicon boron compound and the like. Among them, nitrogen-phosphorus system flame retardants are the most effective flame retardants for cellulose.
The invention adopts the nitrogen-phosphorus flame retardant as the flame-retardant matrix, and the prepared finished fiber has the advantages of excellent physical and mechanical properties, good washability, no generation of toxic gas and the like, and can effectively overcome the defects of the existing flame-retardant viscose fiber.
The nitrogen-phosphorus flame-retardant viscose fiber prepared by the invention adopts a pre-spinning injection method to blend a novel flame-retardant system with viscose, and prepares a flame-retardant fiber product with better physical and mechanical properties and washing resistance. On the basis of having the traditional viscose fiber which is skin-friendly, soft, easy to dye and renewable, the flame retardant and spinnability of the finished product are endowed.
The specific technical scheme of the invention is as follows:
the nitrogen-phosphorus flame-retardant viscose fiber is prepared by blending a nitrogen-phosphorus flame retardant, wherein the linear density of the finished fiber is 1.10-2.20dtex, the dry breaking strength is more than or equal to 2.15cN/dtex, the wet breaking strength is more than or equal to 1.20cN/dtex, the dry breaking elongation is 15.0-20.0%, the dry breaking strength variation coefficient is less than or equal to 18%, the whiteness is 70-80%, and the limiting oxygen index is more than or equal to 30%.
The preparation method of the nitrogen-phosphorus flame-retardant viscose fiber comprises the following steps:
(1) Preparing a flame retardant solution: diluting the nitrogen-phosphorus flame retardant concentrated solution to a solid content of 10-20%, filtering by a nickel screen to remove large particles in the solution, and uniformly stirring for later use;
(2) Preparing a spinning primary solution: soaking, squeezing, crushing, ageing, yellowing, dissolving, grinding, filtering and defoaming cellulose pulp to obtain spinning primary liquid, namely the spinning primary liquid A fiber: 8.0-9.0%, alkali: 4.0-6.0%, ripening degree: 10-15ml (ammonium chloride method), viscosity: 35-50 seconds (ball drop method);
(3) Blend spinning: uniformly mixing a flame retardant and a spinning primary liquid, and feeding the flame retardant into a coagulating bath for spinning and forming through a metering pump, a candle filter, a gooseneck and a spinneret to form a primary tow;
(4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product.
The nitrogen-phosphorus flame retardant is an outsourcing flame retardant, the main component of the nitrogen-phosphorus flame retardant is a halogen-free dioxanitrogen-phosphorus heterocyclic compound (molecular weight is 1500-3000), the solid content of a mother liquor slurry is 40%, the granularity is less than or equal to 1000nm, the viscosity of the slurry is less than or equal to 300 mPa.s (room temperature is 20 ℃), and the pH value is 10.
The dilution step adopts soft water and slurry to mix and dilute, and the slurry dilution is carried out to a certain extent, so that the dispersion efficiency of the slurry can be effectively improved.
The addition amount of the nitrogen-phosphorus flame retardant is 5-15% of the weight of the corresponding alpha-fiber.
The aperture of the nickel screen is 2-5um, the nickel screen is made of pure nickel, and the nickel content is 99.5%.
The said dipping adopts one dipping, the concentration of dipping alkali solution is 210-240g/L, the dipping temperature is 50-60 ℃ and the dipping time is 30-60min.
The addition amount of the carbon disulfide in the yellowing process is 35-45% of the weight of the corresponding alpha-fiber.
The mixing of the viscose primary liquid and the flame-retardant slurry adopts a pre-spinning injection process, and a pre-spinning injection system consists of a homogenizing pump, a static mixer and a pressure-feeding pump.
The spinning glue composition after the blending of the adhesive primary liquid and the flame-retardant slurry is as follows: 8.0 to 9.0 percent of alpha-fiber, 4.0 to 6.0 percent of alkali, 10 to 15ml of ripening degree (ammonium chloride method) and 35 to 45 seconds of viscosity (falling ball method).
The coagulating bath comprises the following components: 95-115g/L of sulfuric acid, 8-15g/L of zinc sulfate, 320-340g/L of sodium sulfate and 45-55 ℃.
The two baths consist of: 25-40g/L of sulfuric acid, 1-5g/L of zinc sulfate, 150-250g/L of sodium sulfate, and the temperature: 75-85 ℃.
The temperature of sulfuric acid in the fluff tank is 5-20g/L and 90-100 ℃.
The desulfurization procedure adopts sodium hydroxide or sodium sulfite as a desulfurizing agent, and the concentration of the desulfurizing agent is 5-10g/L.
The bleaching process adopts sodium hypochlorite or hydrogen peroxide as bleaching agent, and the concentration of the bleaching agent is 5-10g/L.
The invention has the technical effects that:
(1) The invention adopts the injection technology before spinning, does not increase equipment, and has simple and easily controlled operation.
(2) The nitrogen-phosphorus flame retardant adopted by the invention has good high temperature resistance, oxidation resistance and acid and alkali resistance, the flame retardant property of the fiber is basically maintained unchanged along with the time, and the water washing resistance is excellent in the later application process.
(3) The nitrogen-phosphorus flame retardant adopted by the invention has low addition, small influence on fiber strength, better physical and mechanical properties, less possibility of blocking spinneret orifices in the preparation process, more uniform spinning and contribution to industrialization.
(4) The flame-retardant property of the nitrogen-phosphorus flame-retardant viscose fiber prepared by the invention is superior to that of industrial superior products, and the flame-retardant viscose fiber can be used for spinning flame-retardant yarns, so that the application field is widened to a certain extent.
(5) The flame-retardant fiber has the characteristics of anti-dripping and non-toxic smoke generation.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiments.
Example 1:
a preparation method of nitrogen-phosphorus flame-retardant viscose fiber comprises the following steps:
(1) Preparing a flame retardant solution: diluting the nitrogen-phosphorus flame retardant concentrated solution to a solid content of 10%, filtering by a nickel screen to remove large particles in the solution, and uniformly stirring for later use;
the nitrogen-phosphorus flame retardant is an outsourcing flame retardant, the main component of the nitrogen-phosphorus flame retardant is a halogen-free dioxanitrogen-phosphorus heterocyclic compound (molecular weight is 1500-3000), the solid content of a mother liquor slurry is 40%, the granularity is less than or equal to 1000nm, the viscosity of the slurry is less than or equal to 300 mPa.s (room temperature is 20 ℃), and the pH value is 10.
The addition amount of the nitrogen-phosphorus flame retardant is 7% of the weight of the corresponding formazan fiber.
The aperture of the nickel screen is 5um, the nickel screen is made of pure nickel, and the nickel content is 99.5%.
(2) Preparing a spinning primary solution: soaking, squeezing, crushing, ageing, yellowing, dissolving, grinding, filtering and defoaming cellulose pulp to obtain spinning primary liquid, namely the spinning primary liquid A fiber: 9.0%, alkali: 6.0%, ripening degree: 15ml (ammonium chloride method), viscosity: 50 seconds (ball drop method);
the dilution step adopts soft water and slurry to mix and dilute, and the slurry dilution is carried out to a certain extent, so that the dispersion efficiency of the slurry can be effectively improved.
The dipping adopts one-time dipping, the concentration of dipping alkali liquor is 240g/L, the dipping temperature is 60 ℃, and the dipping time is 60min.
The carbon disulfide addition amount in the yellowing process is 42% of the weight of the corresponding alpha-fiber.
(3) Blend spinning: uniformly mixing a flame retardant and a spinning primary liquid, and feeding the flame retardant into a coagulating bath for spinning and forming through a metering pump, a candle filter, a gooseneck and a spinneret to form a primary tow;
the mixing of the viscose primary liquid and the flame-retardant slurry adopts a pre-spinning injection process, and a pre-spinning injection system consists of a homogenizing pump, a static mixer and a pressure-feeding pump.
The coagulating bath comprises the following components: 95g/L sulfuric acid, 8g/L zinc sulfate, 320g/L sodium sulfate and 45 ℃.
(4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product.
The two baths consist of: 25g/L of sulfuric acid, 1g/L of zinc sulfate, 150g/L of sodium sulfate, and the temperature: 75 ℃.
The temperature of sulfuric acid in the fluff tank is 5g/L and 90 ℃.
The desulfurization procedure adopts sodium hydroxide as a desulfurizing agent, and the concentration of the sodium hydroxide is 5g/L.
The bleaching process adopts sodium hypochlorite as bleaching agent, and the concentration of the sodium hypochlorite is 5g/L.
The final fiber data are shown in Table 1:
TABLE 1
| Fiber properties | Example 1 | Example 2 | Example 3 |
| Linear density (dtex) | 1.33 | 1.35 | 1.32 |
| Dry break strength (cN/dtex) | 2.21 | 2.18 | 2.19 |
| Wet break strength (cN/dtex) | 1.23 | 1.28 | 1.24 |
| Elongation at Dry (%) | 19.1 | 19.4 | 19.3 |
| Coefficient of variation in dry break strength (%) | 17.3 | 17.2 | 16.9 |
| Whiteness (%) | 77.6 | 77.2 | 77.5 |
| Limiting oxygen index (%) | 30.9 | 30.8 | 30.6 |
Example 2:
a preparation method of nitrogen-phosphorus flame-retardant viscose fiber comprises the following steps:
(1) Preparing a flame retardant solution: diluting the nitrogen-phosphorus flame retardant concentrated solution to 15% of solid content, filtering by a nickel screen to remove large particles in the solution, and uniformly stirring for later use;
the nitrogen-phosphorus flame retardant is an outsourcing flame retardant, the main component of the nitrogen-phosphorus flame retardant is a halogen-free dioxanitrogen-phosphorus heterocyclic compound (molecular weight is 1500-3000), the solid content of a mother liquor slurry is 40%, the granularity is less than or equal to 1000nm, the viscosity of the slurry is less than or equal to 300 mPa.s (room temperature is 20 ℃), and the pH value is 10.
The addition amount of the nitrogen-phosphorus flame retardant is 9% of the weight of the corresponding alpha-fiber.
The aperture of the nickel screen is 4um, the nickel screen is made of pure nickel, and the nickel content is 99.5%.
(2) Preparing a spinning primary solution: soaking, squeezing, crushing, ageing, yellowing, dissolving, grinding, filtering and defoaming cellulose pulp to obtain spinning primary liquid, namely the spinning primary liquid A fiber: 8.5%, alkali: 5%, maturity: 13ml (ammonium chloride method), viscosity: 42 seconds (ball drop method);
the dilution step adopts soft water and slurry to mix and dilute, and the slurry dilution is carried out to a certain extent, so that the dispersion efficiency of the slurry can be effectively improved.
The dipping adopts one-time dipping, the concentration of dipping alkali liquor is 230g/L, the dipping temperature is 55 ℃, and the dipping time is 50min.
The carbon disulfide addition amount in the yellowing process is 40% of the weight of the corresponding alpha-fiber.
(3) Blend spinning: uniformly mixing a flame retardant and a spinning primary liquid, and feeding the flame retardant into a coagulating bath for spinning and forming through a metering pump, a candle filter, a gooseneck and a spinneret to form a primary tow;
the mixing of the viscose primary liquid and the flame-retardant slurry adopts a pre-spinning injection process, and a pre-spinning injection system consists of a homogenizing pump, a static mixer and a pressure-feeding pump.
The coagulating bath comprises the following components: 105g/L sulfuric acid, 12g/L zinc sulfate, 330g/L sodium sulfate and 50 ℃.
(4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product.
The two baths consist of: 30g/L of sulfuric acid, 3g/L of zinc sulfate, 200g/L of sodium sulfate, and the temperature: 80 ℃.
The temperature of sulfuric acid in the fluff tank is 12g/L and 95 ℃.
The desulfurization procedure adopts sodium sulfite as a desulfurizing agent, and the concentration of the sodium sulfite is 8g/L.
The bleaching process adopts sodium hypochlorite as bleaching agent, and the concentration of the sodium hypochlorite is 8g/L.
The final fiber data are shown in Table 1.
Example 3:
a preparation method of nitrogen-phosphorus flame-retardant viscose fiber comprises the following steps:
(1) Preparing a flame retardant solution: diluting the nitrogen-phosphorus flame retardant concentrated solution to a solid content of 20%, filtering by a nickel screen to remove large particles in the solution, and uniformly stirring for later use;
the nitrogen-phosphorus flame retardant is an outsourcing flame retardant, the main component of the nitrogen-phosphorus flame retardant is a halogen-free dioxanitrogen-phosphorus heterocyclic compound (molecular weight is 1500-3000), the solid content of a mother liquor slurry is 40%, the granularity is less than or equal to 1000nm, the viscosity of the slurry is less than or equal to 300 mPa.s (room temperature is 20 ℃), and the pH value is 10.
The addition amount of the nitrogen-phosphorus flame retardant is 11% of the weight of the corresponding alpha-fiber.
The aperture of the nickel screen is 5um, the nickel screen is made of pure nickel, and the nickel content is 99.5%.
(2) Preparing a spinning primary solution: soaking, squeezing, crushing, ageing, yellowing, dissolving, grinding, filtering and defoaming cellulose pulp to obtain spinning primary liquid, namely the spinning primary liquid A fiber: 8.0%, alkali: 4.0%, ripening degree: 10ml (ammonium chloride method), viscosity: 35 seconds (ball drop method);
the dilution step adopts soft water and slurry to mix and dilute, and the slurry dilution is carried out to a certain extent, so that the dispersion efficiency of the slurry can be effectively improved.
The dipping adopts one-time dipping, the concentration of dipping alkali liquor is 215g/L, the dipping temperature is 50 ℃, and the dipping time is 30min.
The addition amount of carbon disulfide in the yellowing process is 35% of the weight of the corresponding alpha-fiber.
(3) Blend spinning: uniformly mixing a flame retardant and a spinning primary liquid, and feeding the flame retardant into a coagulating bath for spinning and forming through a metering pump, a candle filter, a gooseneck and a spinneret to form a primary tow;
the mixing of the viscose primary liquid and the flame-retardant slurry adopts a pre-spinning injection process, and a pre-spinning injection system consists of a homogenizing pump, a static mixer and a pressure-feeding pump.
The coagulating bath comprises the following components: 110g/L of sulfuric acid, 14g/L of zinc sulfate, 335g/L of sodium sulfate and 53 ℃.
(4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product.
The two baths consist of: 38g/L of sulfuric acid, 4g/L of zinc sulfate, 245g/L of sodium sulfate, and the temperature: 81 ℃.
The temperature of sulfuric acid in the fluff tank is 18g/L and 98 ℃.
The desulfurization procedure adopts sodium sulfite as a desulfurizing agent, and the concentration of the sodium sulfite is 9g/L.
The bleaching process adopts hydrogen peroxide as bleaching agent, and the concentration of the bleaching agent is 9g/L.
The final fiber data are shown in Table 1.
The spinneret hole blocking phenomenon does not occur in the production process of the embodiments 1 to 3, spinning is continuous and uniform, the prepared flame-retardant fiber cannot be melted and dripped when being burnt by fire, toxic gas cannot be generated, and the flame-retardant fiber can be automatically extinguished when leaving the flame.
Claims (10)
1. The preparation method of the nitrogen-phosphorus flame-retardant viscose fiber is characterized by comprising the following steps of:
(1) Preparing a flame retardant solution: diluting the nitrogen-phosphorus flame retardant concentrated solution to a solid content of 10-20%, filtering by a nickel screen to remove large particles in the solution, and uniformly stirring for later use;
(2) Preparing a spinning primary solution: soaking, squeezing, crushing, ageing, yellowing, dissolving, grinding, filtering and defoaming cellulose pulp to obtain spinning primary liquid, namely the spinning primary liquid A fiber: 8.0 to 9.0wt percent of alkali: 4.0 to 6.0wt%, ripening degree: 10-15ml, ammonium chloride method; viscosity: 35-50 seconds, falling ball method;
(3) Blend spinning: uniformly mixing a flame retardant and a spinning primary liquid, and feeding the flame retardant into a coagulating bath for spinning and forming through a metering pump, a candle filter, a gooseneck and a spinneret to form a primary tow;
(4) And (3) carrying out two-bath, drafting, cutting, fluff tank, water washing, desulfurization, bleaching, oiling, drying and packaging on the primary tows to obtain a nitrogen-phosphorus flame-retardant viscose fiber finished product.
2. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized in that: the nitrogen-phosphorus flame retardant is a halogen-free dioxanitrogen-phosphorus heterocyclic compound, the molecular weight is 1500-3000, the solid content of the mother liquor slurry is 40%, the granularity is less than or equal to 1000nm, the viscosity of the slurry is less than or equal to 300 mPa.s, the room temperature is 20 ℃, and the pH value is 10.
3. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized in that: the addition amount of the nitrogen-phosphorus flame retardant is 5-15% of the weight of the corresponding alpha-fiber.
4. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized in that: the said dipping adopts one dipping, the concentration of dipping alkali solution is 210-240g/L, the dipping temperature is 50-60 ℃ and the dipping time is 30-60min.
5. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized in that: the addition amount of the carbon disulfide in the yellowing process is 35-45% of the weight of the corresponding alpha-fiber.
6. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized by comprising the following steps: the coagulating bath comprises the following components: 95-115g/L of sulfuric acid, 8-15g/L of zinc sulfate, 320-340g/L of sodium sulfate and 45-55 ℃.
7. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized by comprising the following steps: the two baths consist of: 25-40g/L of sulfuric acid, 1-5g/L of zinc sulfate, 150-250g/L of sodium sulfate, and the temperature: 75-85 ℃.
8. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized by comprising the following steps: the temperature of sulfuric acid in the fluff tank is 5-20g/L and 90-100 ℃.
9. The method for preparing the nitrogen-phosphorus flame-retardant viscose fiber according to claim 1, which is characterized by comprising the following steps: the desulfurization procedure adopts sodium hydroxide or sodium sulfite as a desulfurizing agent, and the concentration of the desulfurizing agent is 5-10g/L; the bleaching process adopts sodium hypochlorite or hydrogen peroxide as bleaching agent, and the concentration of the bleaching agent is 5-10g/L.
10. A nitrogen-phosphorus flame retardant viscose fiber, characterized in that it is obtained by the preparation method according to any one of claims 1 to 9.
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| CN202311530524.7A CN117737876A (en) | 2023-11-16 | 2023-11-16 | Preparation method of nitrogen-phosphorus flame-retardant viscose fiber |
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| CN202311530524.7A CN117737876A (en) | 2023-11-16 | 2023-11-16 | Preparation method of nitrogen-phosphorus flame-retardant viscose fiber |
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