CN112663160A - Preparation method of flame-retardant cool cellulose fiber for summer curtain - Google Patents
Preparation method of flame-retardant cool cellulose fiber for summer curtain Download PDFInfo
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- CN112663160A CN112663160A CN202011405762.1A CN202011405762A CN112663160A CN 112663160 A CN112663160 A CN 112663160A CN 202011405762 A CN202011405762 A CN 202011405762A CN 112663160 A CN112663160 A CN 112663160A
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- 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 82
- 239000003063 flame retardant Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 51
- 238000009987 spinning Methods 0.000 claims abstract description 51
- 239000003094 microcapsule Substances 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000002826 coolant Substances 0.000 claims abstract description 28
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 24
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 24
- -1 rare earth lanthanum chloride Chemical class 0.000 claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 229910021389 graphene Inorganic materials 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- 239000004964 aerogel Substances 0.000 claims description 19
- 239000002270 dispersing agent Substances 0.000 claims description 19
- 239000010445 mica Substances 0.000 claims description 18
- 229910052618 mica group Inorganic materials 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 229920000877 Melamine resin Polymers 0.000 claims description 16
- 239000002775 capsule Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000001112 coagulating effect Effects 0.000 claims description 9
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- 239000004640 Melamine resin Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 230000005070 ripening Effects 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 239000000835 fiber Substances 0.000 abstract description 21
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 241000588724 Escherichia coli Species 0.000 abstract description 6
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000000227 grinding Methods 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 229920000297 Rayon Polymers 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 4
- 230000023556 desulfurization Effects 0.000 description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 4
- 235000011180 diphosphates Nutrition 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000004383 yellowing Methods 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920001410 Microfiber Polymers 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 239000003658 microfiber Substances 0.000 description 2
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention provides a preparation method of a flame-retardant cool cellulose fiber for summer curtains, which comprises the steps of preparation of composite flame retardant slurry, preparation of ice coolant slurry, preparation of blended spinning solution and spinning. The flame retardant contains magnesium hydroxide microcapsules, and the rare earth lanthanum chloride microcapsules are added into the composite flame retardant, so that the flame retardant effect of the flame retardant can be enhanced, and lanthanum chloride has a good antibacterial effect, so that a curtain prepared from the fiber has a good antibacterial effect. The dry breaking strength of the prepared fiber is 1.86-2.13cN/dtex, the wet breaking strength is 0.95-1.16cN/dtex, the limiting oxygen index is 28.3-30.6%, the bacteriostasis rate to staphylococcus aureus is 99.2-99.9%, the bacteriostasis rate to escherichia coli is 98.6-99.9%, the UPF value is 42-44, and the UVA value is 3.92-4.65%.
Description
Technical Field
The invention relates to a flame-retardant cool cellulose fiber and a preparation method thereof, in particular to a composite cellulose fiber which takes the cellulose fiber as a substrate and has the functions of flame retardance, coolness and ultraviolet resistance, is particularly suitable for summer curtains and belongs to the technical field of textiles.
Background
In summer, the sunlight is dazzling, and the curtain is pulled up, so that the irradiation of strong light is blocked, and a part of heat is isolated. If the curtain is thin, the light blocking effect is poor, and glare may occur across the curtain. The strong light penetrates through the curtain, and people in the room can obviously feel the temperature rise. If the curtain is thick, although the light blocking effect is good, the curtain is made of more materials, the weight of the curtain is heavy, and the disassembly, the assembly and the cleaning are not as convenient as thin materials.
Common curtains are inflammable, and certain flame retardant performance is inevitably required along with the improvement of the safety of the state to public facilities and household articles. The curtain can not be cleaned frequently, and bacteria can grow after a long time, so that the curtain with certain antibacterial performance is beneficial to the health of human bodies.
The Chinese patent with the application number of CN201410354049.7 discloses a flame-retardant cool regenerated polyester filament fiber and a production method thereof, wherein the fiber skin layer is obtained by melt spinning of cool master batches and regenerated polyester chips, the core layer is obtained by melt spinning of the flame-retardant master batches and the regenerated polyester chips, and the fiber prepared by the technology has cool and flame-retardant properties. The cool powder with the cool function of the fiber consists of jade, zinc oxide and titanium dioxide, the three substances have the cool and ultraviolet-proof functions, but have the defects of poor heat insulation effect and poor antibacterial performance when being used for curtains, and the fiber is synthetic fiber, so that the source of raw materials is not as wide as that of cellulose fiber, and the product cannot be naturally decomposed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a flame-retardant cool cellulose fiber for summer curtains, which realizes the following purposes:
the flame retardant property of the fiber is improved;
meanwhile, the fabric has the performances of cool feeling, antibiosis and ultraviolet resistance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of flame-retardant cool cellulose fibers for summer curtains comprises the steps of preparation of composite flame retardant slurry, preparation of ice-cooling agent slurry, preparation of blended spinning solution and spinning.
The preparation method comprises the following specific steps:
1. preparation of composite flame retardant slurry
The composite flame retardant consists of a flame retardant and rare earth lanthanum chloride microcapsules, and is prepared into slurry to ensure that the composite flame retardant and spinning glue can be quickly and uniformly mixed, wherein the slurry contains 15.0-25.0 wt% of the flame retardant, 1.0-3.0 wt% of the rare earth lanthanum chloride microcapsules, 0.5-2.0 wt% of a dispersing agent and the balance of deionized water.
The flame retardant is a mixture of one or more of a phosphorus flame retardant, a silicon nitrogen flame retardant and a melamine resin flame retardant and magnesium hydroxide microcapsules, and the mixing mass ratio is 15: 1-2.
The wall material of the magnesium hydroxide microcapsule is melamine formaldehyde resin, and the content of magnesium hydroxide in the capsule is 60-80 wt%.
The capsule wall material of the rare earth lanthanum chloride microcapsule is melamine formaldehyde resin, and the content of the rare earth lanthanum chloride in the capsule is 60-80 wt%.
The dispersant is preferably one or more of NNO, sodium hexametaphosphate and peregal.
The particle size D90 of the composite flame retardant slurry is less than or equal to 2.0 mu m.
2. Preparation of a Coolant slurry
The cooling agent consists of mica powder, graphene aerogel and an ultraviolet-proof agent. The ultraviolet-proof agent has the functions of blocking and reflecting ultraviolet rays, can block partial ultraviolet rays and reduces the heating effect of light rays on indoor air. The graphene aerogel has a large number of cavities, has a good adsorption effect, and simultaneously, the graphene and the flame retardant are used together, so that the flame retardant property can be enhanced.
Further, the cooling agent slurry comprises 10.0-15.0 wt% of mica powder, 15.0-20.0 wt% of graphene aerogel, 6.0-8.0 wt% of an ultraviolet-proof agent, 0.5-2.0 wt% of a dispersing agent and the balance of deionized water.
The ultraviolet-proof agent is one or more of titanium dioxide, talcum powder and argil.
The particle size D90 of the mica powder is not more than 0.9 mu m, the particle size D90 of the graphene aerogel is 1-2 mu m, and the particle size D90 of the ultraviolet-proof agent is not more than 1 mu m.
The dispersing agent is one or more of sodium dodecyl benzene sulfonate, sodium hexametaphosphate and silane coupling agent.
The preparation method of the cooling agent slurry comprises the following steps: adding deionized water into a preparation tank, adding a dispersing agent, uniformly stirring, adding graphene aerogel, stirring for 0.5-1.5 hours, adding mica powder and an ultraviolet-proof agent, and rotating the stirrer at 1500-2000 r/min. Grinding for 2.0-4.0 hours by using a grinder, wherein the rotating speed of the grinder is 3000-5000 r/min, then performing ultrasonic treatment for 20-40 min by using ultrasonic waves, the ultrasonic power is 900-1000 w, the cold agent slurry is kept in a stirring state before adding the spinning solution, and the rotating speed of a stirrer is 1000-1500 r/min.
3. Preparing a blended spinning solution: cellulose pulp is used as a raw material, and the viscose is prepared through the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, mixing, filtering, defoaming and the like, a pre-spinning injection system is utilized, composite flame retardant slurry with the content of alpha cellulose of 15-20 wt% calculated according to the effective components of a composite flame retardant is added into spinning glue, ice cooling agent slurry with the content of alpha cellulose of 3-5 wt% calculated according to the effective components of the ice cooling agent (the effective components of the composite flame retardant and the ice cooling agent do not contain a dispersing agent) is added, and the mixture is uniformly mixed through a dynamic mixer to obtain a blending spinning solution.
The indexes of the spinning glue are as follows: 9.2-9.6% of alpha-cellulose, 5.2-6.0% of alkali, 40-50 s of viscosity (falling ball method), and 12-18 ml of ripening degree (10% ammonium chloride value).
4. Spinning and post-treatment: and (3) the blended spinning solution enters a coagulating bath for spinning, and the tows are subjected to multi-stage drafting to obtain formed tows. The obtained tows are subjected to post-treatment processes of cutting, desulfurization, washing, oiling, drying and the like to obtain the cellulose fiber with the flame-retardant and cool functions.
Preferably, the coagulating bath contains 110-130 g/L of sulfuric acid, 10-15 g/L of zinc sulfate and 300-320 g/L of sodium sulfate.
By adopting the technical scheme, the prepared fiber has the limiting oxygen index of more than or equal to 28 percent, the bacteriostatic rate on staphylococcus aureus of more than or equal to 99 percent, the bacteriostatic rate on escherichia coli of more than or equal to 98 percent, the UPF value of more than 40 and the UVA of less than 5 percent.
Compared with the prior art, the invention has the following beneficial effects:
(1) the dry breaking strength of the prepared fiber is more than or equal to 1.80cN/dtex, the wet breaking strength is more than or equal to 0.90cN/dtex, the limiting oxygen index is more than or equal to 28%, the bacteriostasis rate to staphylococcus aureus is more than or equal to 99%, the bacteriostasis rate to escherichia coli is more than or equal to 98%, the UPF value is more than 40, and the UVA value is less than 5%.
(2) The flame retardant contains magnesium hydroxide microcapsules, and the rare earth lanthanum chloride microcapsules are added into the composite flame retardant, so that the flame retardant effect of the flame retardant can be enhanced, and lanthanum chloride has a good antibacterial effect, so that a curtain prepared from the fiber has a good antibacterial effect.
The cooling agent consists of mica, graphene aerogel and an ultraviolet-proof agent, and the mica provides a good cooling feeling and also has a synergistic flame-retardant effect. The graphene aerogel has more cavities, mica and an ultraviolet-proof agent can be adsorbed in the cavities, and the slurry is prevented from being lost in the fiber forming process. The graphene aerogel and the flame retardant act together, so that the flame retardant property of the material can be improved.
The added anti-ultraviolet agent can prevent ultraviolet rays from entering a room, so that the cooling agent has better effects on light resistance, heat insulation and ultraviolet ray resistance of the curtain.
The present invention will be described in detail with reference to examples.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1:
1. preparation of composite flame retardant slurry
Adding pyrophosphate powder with the particle size of less than 0.6 mu m into deionized water at the temperature of 40 ℃, adding a dispersant NNO, stirring for 2 hours at the rotating speed of 1000r/min of a stirrer, grinding for 4 hours at the rotating speed of 4000r/min by using a grinder, then adding magnesium hydroxide microcapsules and rare earth lanthanum chloride microcapsules, continuously stirring for 1 hour at the rotating speed of 2000r/min of the stirrer, and detecting that the particle size D90 of the slurry is 1.967 mu m.
The flame retardant in the slurry is pyrophosphate and magnesium hydroxide microcapsules, the ratio of the pyrophosphate to the magnesium hydroxide microcapsules is 15:1, the wall material of the magnesium hydroxide microcapsules is melamine formaldehyde resin, and the content of magnesium hydroxide in the capsules is 60 wt%. The content of the flame retardant in the composite slurry is 15.0wt%, the content of the rare earth lanthanum chloride microcapsule is 1.0wt%, and the content of the dispersant NNO is 0.5 wt%.
In order to prevent the lanthanum chloride from losing, the lanthanum chloride is prepared into a microcapsule with a melamine formaldehyde resin as a capsule wall, and the content of the lanthanum chloride in the capsule is 80 wt%.
2. Preparation of a Coolant slurry
Adding deionized water into a preparation tank, adding dispersant sodium dodecyl benzene sulfonate, stirring uniformly, adding graphene aerogel with the particle size D90 of 1.865 mu m, stirring for 0.5 hour, adding mica powder and an ultraviolet-proof agent titanium dioxide, and rotating the stirrer at 2000 r/min. Grinding for 2.0 hours by a grinder, wherein the rotation speed of the grinder is 5000r/min, then carrying out ultrasonic treatment for 20min, the power of the ultrasonic machine is 1000w, and the detected particle size D90 is 1.932 mu m. The cooling agent slurry is kept in a stirring state before the spinning solution is added, and the rotating speed of the stirrer is 1500 r/min.
Wherein, the slurry contains 10.0wt% of mica powder, 15.0wt% of graphene aerogel, 6.0wt% of titanium dioxide and 0.5wt% of sodium dodecyl benzene sulfonate.
3. Preparing a blended spinning solution: cellulose pulp is used as a raw material, and viscose is prepared by the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, mixing, filtering, defoaming and the like, wherein the index of the spinning glue is as follows: microfiber content 9.58%, alkali content 5.94%, viscosity 48.8s (falling ball method), and ripening degree 15.6ml (10% ammonium chloride value).
By utilizing a pre-spinning injection system, adding composite flame retardant slurry with the content of alpha cellulose of 15.0wt% calculated according to the effective components of the composite flame retardant into spinning dope, adding cooling agent slurry with the content of alpha cellulose of 5.0wt% calculated according to the effective components of the cooling agent into the spinning dope, and uniformly mixing the mixture by a dynamic mixer to obtain the blended spinning dope.
4. Spinning and post-treatment: and (3) feeding the blended spinning solution into a coagulating bath for spinning, wherein the coagulating bath contains 128.56g/L sulfuric acid, 318.24g/L sodium sulfate and 11.24g/L zinc sulfate. And (4) performing multistage drafting on the tows to obtain the formed tows. The obtained tows are subjected to post-treatment processes of cutting, desulfurization, washing, oiling, drying and the like to obtain the cellulose fiber with the flame-retardant and cool functions.
The detection fiber indexes are as follows: the dry breaking strength of the fiber is 2.13cN/dtex, the wet breaking strength is 1.16cN/dtex, the limiting oxygen index is 28.3 percent, the bacteriostasis rate to staphylococcus aureus is 99.2 percent, the bacteriostasis rate to escherichia coli is 98.6 percent, the UPF value is 44, and the UVA value is 3.92 percent.
Example 2:
1. preparation of composite flame retardant slurry
Adding silicon-ammonium pyrophosphate with the particle size of less than 0.6 mu m into deionized water at 50 ℃, adding a dispersing agent sodium hexametaphosphate, stirring for 1.0 hour at the rotating speed of 2000r/min of a stirrer, grinding for 3 hours at the rotating speed of 4500r/min by using a grinding machine, adding magnesium hydroxide microcapsules and lanthanum chloride microcapsules, continuously stirring for 80 minutes at the rotating speed of 1500r/min of the stirrer, and detecting the particle size D90 of the slurry to be 1.876 mu m.
The flame retardant in the slurry is silicon-ammonium pyrophosphate and magnesium hydroxide microcapsules, the ratio of the silicon-ammonium pyrophosphate to the magnesium hydroxide microcapsules is 15:2, the wall material of the magnesium hydroxide microcapsules is melamine formaldehyde resin, and the content of magnesium hydroxide in the capsules is 80 wt%. In the composite slurry, the content of the flame retardant is 25.0wt%, the content of the rare earth lanthanum chloride microcapsule is 3.0wt%, and the content of the dispersant sodium hexametaphosphate is 2.0 wt%.
In order to prevent the lanthanum chloride from losing, the lanthanum chloride is prepared into a microcapsule with a melamine formaldehyde resin as a capsule wall, and the content of the lanthanum chloride in the capsule is 60 wt%.
2. Preparation of a Coolant slurry
Adding deionized water into a preparation tank, adding a dispersing agent sodium hexametaphosphate, uniformly stirring, adding graphene aerogel with the particle size D90 of 1.543 mu m, stirring for 1.5 hours, adding mica powder and an ultraviolet-proof agent talcum powder, and rotating the stirrer at 1500 r/min. Grinding for 4 hours by a grinding machine at the rotating speed of 3000r/min, and then carrying out ultrasonic treatment for 40min by ultrasonic waves, wherein the power of the ultrasonic wave is 1000w, and the detected particle size D90 is 1.675 mu m. The cooling agent slurry is kept in a stirring state before the spinning solution is added, and the rotating speed of the stirrer is 1000 r/min.
Wherein, the slurry contains 15.0wt% of mica powder, 20.0wt% of graphene aerogel, 8.0wt% of talcum powder and 2.0wt% of sodium hexametaphosphate.
3. Preparing a blended spinning solution: cellulose pulp is used as a raw material, and viscose is prepared by the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, mixing, filtering, defoaming and the like, wherein the index of the spinning glue is as follows: the alpha-cellulose content was 9.20%, the alkali content was 5.28%, the viscosity was 45.7s (falling ball method), and the degree of ripening was 12.3ml (10% ammonium chloride value).
By utilizing a pre-spinning injection system, adding composite flame retardant slurry with the content of alpha cellulose of 20.0wt% calculated according to the effective components of the composite flame retardant into spinning dope, adding cooling agent slurry with the content of alpha cellulose of 3.0wt% calculated according to the effective components of the cooling agent into the spinning dope, and uniformly mixing the mixture by a dynamic mixer to obtain the blended spinning dope.
4. Spinning and post-treatment: and (3) feeding the blended spinning solution into a coagulating bath for spinning, wherein the coagulating bath contains 112.32g/L sulfuric acid, 306.53g/L sodium sulfate and 14.58g/L zinc sulfate. And (4) performing multistage drafting on the tows to obtain the formed tows. The obtained tows are subjected to post-treatment processes of cutting, desulfurization, washing, oiling, drying and the like to obtain the cellulose fiber with the flame-retardant and cool functions.
The detection fiber indexes are as follows: the dry breaking strength of the fiber is 1.86 cN/dtex, the wet breaking strength is 0.95 cN/dtex, the limiting oxygen index is 30.6 percent, the bacteriostasis rate to staphylococcus aureus is 99.9 percent, the bacteriostasis rate to escherichia coli is 99.9 percent, the UPF value is 42, and the UVA value is 4.65 percent.
Example 3:
1. preparation of composite flame retardant slurry
Adding melamine resin with the particle size of less than 0.6 mu m into deionized water at 45 ℃, adding a dispersant, adding the dispersant, stirring for 1.0 hour at the rotating speed of 1000r/min of a stirrer, grinding for 2 hours at the rotating speed of 5000r/min by using a grinder, adding magnesium hydroxide microcapsules and rare earth lanthanum chloride microcapsules, continuously stirring for 2 hours at the rotating speed of 1500r/min of the stirrer, and detecting the particle size D90 of the slurry to be 1.838 mu m.
The flame retardant in the slurry is melamine resin and magnesium hydroxide microcapsules, the ratio of the melamine resin to the magnesium hydroxide microcapsules is 15:1, the wall material of the magnesium hydroxide microcapsules is melamine formaldehyde resin, and the content of magnesium hydroxide in the capsules is 70 wt%. In the composite slurry, the content of the flame retardant is 18.0wt%, the content of the rare earth lanthanum chloride microcapsule is 2.0wt%, and the content of the dispersant peregal is 2.0 wt%.
In order to prevent the lanthanum chloride from losing, the lanthanum chloride is prepared into a microcapsule with a melamine formaldehyde resin as a capsule wall, and the content of the lanthanum chloride in the capsule is 70 wt%.
2. Preparation of a Coolant slurry
Adding deionized water into a preparation tank, adding a dispersant silane coupling agent, uniformly stirring, adding graphene aerogel with the particle size D90 of 1.758 mu m, stirring for 1.0 hour, adding mica powder and anti-ultraviolet agent argil, and rotating the stirrer at the speed of 1800 r/min. Grinding for 3 hours by a grinding machine, wherein the rotation speed of the grinding machine is 4000r/min, then carrying out ultrasonic treatment for 30min, the power of the ultrasonic machine is 960w, and the detected particle size D90 is 1.802 mu m. The cooling agent slurry is kept in a stirring state before the spinning solution is added, and the rotating speed of the stirrer is 1400 r/min.
Wherein the slurry contains 12.0wt% of mica powder, 17.0wt% of graphene aerogel, 7.0wt% of argil and 1.5wt% of silane coupling agent.
3. Preparing a blended spinning solution: cellulose pulp is used as a raw material, and viscose is prepared by the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving, mixing, filtering, defoaming and the like, wherein the index of the spinning glue is as follows: microfiber content 9.46%, alkali content 5.48%, viscosity 43.2s (falling ball method), and degree of ripening 14.2ml (10% ammonium chloride value).
By utilizing a pre-spinning injection system, adding composite flame retardant slurry with the content of 18.0wt% of alpha cellulose calculated according to the effective components of the composite flame retardant into spinning glue, adding cooling agent slurry with the content of 4.0wt% of alpha cellulose calculated according to the effective components of the cooling agent into the spinning glue, and uniformly mixing the mixture by using a dynamic mixer to obtain the blended spinning solution.
4. Spinning and post-treatment: and (3) feeding the blended spinning solution into a coagulating bath for spinning, wherein 120.62g/L of sulfuric acid, 310.36g/L of sodium sulfate and 13.55g/L of zinc sulfate are contained in the coagulating bath. And (4) performing multistage drafting on the tows to obtain the formed tows. The obtained tows are subjected to post-treatment processes of cutting, desulfurization, washing, oiling, drying and the like to obtain the cellulose fiber with the flame-retardant and cool functions.
The detection fiber indexes are as follows: the dry breaking strength of the fiber is 2.01 cN/dtex, the wet breaking strength is 1.04 cN/dtex, the limiting oxygen index is 29.4 percent, the bacteriostasis rate to staphylococcus aureus is 99.6 percent, the bacteriostasis rate to escherichia coli is 99.2 percent, the UPF value is 43, and the UVA value is 4.08 percent.
Comparative example
The following comparative tests were carried out in the same manner as in example 1, with the following parameters being varied on the basis of example 1:
the above table shows that the pyrophosphate, the magnesium hydroxide microcapsule and the rare earth lanthanum chloride play a synergistic role, and the flame retardant property of the fiber is improved together.
On the basis of example 1, the following comparative tests were carried out with the following process parameters being varied and the remaining processes being unchanged:
the table shows that both mica and graphene aerogel in the cooling agent can improve the flame retardant performance of the fiber, and if the mica or the graphene aerogel is not added, the limiting oxygen index of the fiber is obviously reduced.
Unless otherwise specified, the proportions used in the present invention are mass proportions, and the percentages used are mass percentages.
Claims (10)
1. A preparation method of flame-retardant cool cellulose fiber for summer curtains is characterized by comprising the following steps: the preparation method comprises the steps of preparing composite flame retardant slurry, preparing ice coolant slurry, preparing blended spinning solution and spinning.
2. The method for preparing the flame retardant cool cellulose fiber for summer window curtains according to claim 1, wherein the method comprises the following steps: the composite flame retardant slurry comprises 15.0-25.0 wt% of a flame retardant, 1.0-3.0 wt% of a rare earth lanthanum chloride microcapsule and 0.5-2.0 wt% of a dispersing agent.
3. The method for preparing the flame retardant cool cellulose fiber for summer window curtains as claimed in claim 2, wherein the method comprises the following steps: the flame retardant is a mixture of one or more of a phosphorus flame retardant, a silicon nitrogen flame retardant and a melamine resin flame retardant and magnesium hydroxide microcapsules, and the mass ratio of the phosphorus flame retardant to the silicon nitrogen flame retardant to the melamine resin flame retardant is 15: 1-2.
4. The method for preparing the flame retardant cool cellulose fiber for summer window curtains as claimed in claim 2, wherein the method comprises the following steps: the particle size D90 of the composite flame retardant slurry is less than or equal to 2.0 mu m.
5. The method of claim 3, wherein the method comprises the steps of: the wall material of the magnesium hydroxide microcapsule is melamine formaldehyde resin, and the content of magnesium hydroxide in the capsule is 60-80 wt%; the capsule wall material of the rare earth lanthanum chloride microcapsule is melamine formaldehyde resin, and the content of the rare earth lanthanum chloride in the capsule is 60-80 wt%.
6. The method for preparing the flame retardant cool cellulose fiber for summer window curtains according to claim 1, wherein the method comprises the following steps: the cooling agent slurry comprises 10.0-15.0 wt% of mica powder, 15.0-20.0 wt% of graphene aerogel, 6.0-8.0 wt% of an ultraviolet-proof agent and 0.5-2.0 wt% of a dispersing agent.
7. The method for preparing the flame retardant cool cellulose fiber for summer window curtains according to claim 6, wherein the method comprises the following steps: the particle size D90 of the mica powder is not more than 0.9 mu m, the particle size D90 of the graphene aerogel is 1-2 mu m, and the particle size D90 of the ultraviolet-proof agent is not more than 1 mu m.
8. The method for preparing the flame retardant cool cellulose fiber for summer window curtains according to claim 6, wherein the method comprises the following steps: the ultraviolet-proof agent is one or more of titanium dioxide, talcum powder and argil;
the dispersing agent is one or more of sodium dodecyl benzene sulfonate, sodium hexametaphosphate and silane coupling agent.
9. The method for preparing the flame retardant cool cellulose fiber for summer window curtains according to claim 1, wherein the method comprises the following steps: preparing the blended spinning solution, namely adding the composite flame retardant slurry and the cooling agent slurry into spinning glue, and uniformly mixing to obtain the blended spinning solution; the mass sum of the flame retardant and the rare earth lanthanum chloride microcapsule in the composite flame retardant slurry accounts for 15-20 wt% of the alpha cellulose; the mass sum of the mica powder, the graphene aerogel and the ultraviolet-proof agent in the cooling agent slurry accounts for 3-5 wt% of the alpha cellulose.
10. The method of claim 9, wherein the method comprises the steps of: the indexes of the spinning glue are as follows: 9.2-9.6% of alpha-cellulose, 5.2-6.0% of alkali, 40-50 s of viscosity and 12-18 ml of ripening degree under the 10% ammonium chloride value; the spinning adopts a coagulating bath which comprises the following components: 110-130 g/L sulfuric acid, 10-15 g/L zinc sulfate and 300-320 g/L sodium sulfate.
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