CN115679464A - Pearl and protein mixed slurry and preparation method and application of fibers thereof - Google Patents
Pearl and protein mixed slurry and preparation method and application of fibers thereof Download PDFInfo
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- CN115679464A CN115679464A CN202111018725.XA CN202111018725A CN115679464A CN 115679464 A CN115679464 A CN 115679464A CN 202111018725 A CN202111018725 A CN 202111018725A CN 115679464 A CN115679464 A CN 115679464A
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- proteins
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- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 102
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 102
- 239000000835 fiber Substances 0.000 title claims abstract description 81
- 239000011268 mixed slurry Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000011049 pearl Substances 0.000 claims abstract description 137
- 239000000843 powder Substances 0.000 claims abstract description 81
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 239000012460 protein solution Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 235000018102 proteins Nutrition 0.000 claims description 96
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000009987 spinning Methods 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 20
- 239000004408 titanium dioxide Substances 0.000 claims description 20
- 229920000297 Rayon Polymers 0.000 claims description 17
- 230000001804 emulsifying effect Effects 0.000 claims description 16
- 239000011550 stock solution Substances 0.000 claims description 16
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 13
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 13
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- 238000000227 grinding Methods 0.000 claims description 9
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- 238000010298 pulverizing process Methods 0.000 claims description 9
- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229960004670 didecyldimethylammonium chloride Drugs 0.000 claims description 8
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 7
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical group CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
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- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 claims description 3
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- 108010082495 Dietary Plant Proteins Proteins 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
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- 241000233866 Fungi Species 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
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- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- 244000098338 Triticum aestivum Species 0.000 description 1
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Landscapes
- Artificial Filaments (AREA)
Abstract
The invention relates to a pearl and protein mixed slurry and a preparation method and application of fibers thereof. The mixed slurry comprises 15-20wt% of pearl powder, 8-12wt% of protein solution, 3-8wt% of antibacterial agent, 5-10wt% of dispersing agent, 3-8wt% of anti-settling agent, 8-15wt% of protective solution and the balance of water. The fibers prepared by adding the mixed slurry of the pearls and the protein improve the health care function, and have better fiber glossiness and hand feeling. The unique structure of protein is utilized to contribute to the dispersibility of pearl powder. The dispersing agent and the anti-settling agent make the pearl powder not easy to settle and agglomerate, do not block a machine used for preparing the fiber, and make the pearl powder and the protein uniformly dispersed in the fiber. The MOFs material can avoid the crystal complex compound which reacts with acid to form acid salt to block the spinneret orifice, and simultaneously protect and improve the antibacterial effect. By adhering and wrapping the PVP polymer, the pearl powder and the protein, the loss of effective components in the production and preparation process of the fiber is avoided.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to pearl and protein mixed slurry and a preparation method and application of fibers thereof.
Background
The pearl has the effects of detoxifying, promoting granulation, maintaining beauty, keeping young, tranquilizing, whitening, lightening spots and the like, and has wide application prospect in the fields of food, medicine, health-care products and the like. With the increase of the demand of people on functional fibers, fiber products with the functions of health care, antibiosis and whitening can better meet the demand of consumers. The pearl is added into the fiber by people to prepare close-fitting articles such as clothes, socks, bedding and the like containing the pearl, the cool feeling and the body feeling are comfortable, meanwhile, the pearl contains various amino acids and trace elements, the unique health care function of the pearl can be utilized, and the fiber containing the pearl is deeply loved by consumers.
The pearl viscose fiber and the production method thereof of CN100360726C add pearl powder particle liquid slurry before the wet spinning process, adopt the viscose line production, improve the content of pearl powder in the fiber, the textile made can exert the health care function of pearl, and is comfortable to contact with human skin. However, the pearl particles in the prepared pearl powder liquid slurry are easy to settle, and the spinning process is influenced.
Disclosure of Invention
In view of the above, the invention aims to provide a pearl-protein mixed slurry and a preparation method and application of fibers thereof, which can solve the problem that pearl powder is easy to agglomerate or settle to influence the fiber preparation process by spinning, improve the content of protein in the fibers and further enhance the health care effect of the fibers.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a pearl and protein mixed slurry, which comprises 15-20wt% of pearl powder, 8-12wt% of protein solution, 3-8wt% of antibacterial agent, 5-10wt% of dispersing agent, 3-8wt% of anti-settling agent, 8-15wt% of protective solution and the balance of water.
Further, the mass concentration of the protein in the protein solution is 40-50wt%.
Further, the protein is selected from at least one of animal protein, plant protein and artificial synthetic protein.
Furthermore, the pearl powder is crushed to D90 less than 2 μm.
Further, the plant protein is protein extracted from plant fruit or leaf stem containing protein, and the plant fruit is selected from one or more of soybean, rapeseed, cottonseed, peanut, sunflower seed, sesame, kidney bean, broad bean, pea, black bean, corn, wheat, barley, rice or millet.
Furthermore, the animal protein is protein extracted from animal dander hair and animal bone powder.
Further, the antibacterial powder is metal-organic framework Materials (MOFs), and the metal is selected from at least one of Cu, zn, MOF and MOF.
Further, the antibacterial powder consists of the following components: 1-2 parts of metal oxide, 0.5-0.8 part of gallium sesquioxide, 1-2 parts of titanium dioxide, 2-4 parts of didecyl dimethyl ammonium chloride, 1-1.5 parts of polyacrylic acid and deionized water.
Further, the dispersing agent is at least one of polyethylene glycol and polypropylene glycol.
Further, the protective solution is PVP polymer.
Further, the anti-settling agent is at least one selected from nano hydrophilic silica and alginate.
Further, the alginate is sodium alginate or calcium alginate.
Furthermore, the pearl powder can be coated by microcapsules or high molecular polymers.
The second aspect of the invention provides a preparation method of mixed slurry of pearls and protein, which comprises the following steps:
s1, weighing each component in a formula amount;
s2, pulverizing pearl powder to below 5 microns, stirring with a protein solution and a dispersing agent, adding water, grinding until the particle size of the pearl powder reaches D90 less than 2 microns, and feeding the pearl powder into an emulsifying machine for emulsification to obtain a stock solution;
s3, adding an anti-settling agent into the stock solution prepared in the step S2, stirring, and adding an antibacterial agent and a protective agent to obtain the mixed slurry of the pearls and the proteins.
The third aspect of the invention provides a pearl and protein mixed pulp and application of the preparation method thereof in spinning preparation of fibers containing pearls and proteins, wherein the fibers are regenerated cellulose fibers selected from any one of modal fibers, viscose fibers, tencel fibers, lyocell and cuprammonium fibers.
Furthermore, the fiber containing the pearls and the protein consists of mixed slurry of the pearls and the protein and cellulose, and the mass of the mixed slurry is 3-8% of the total mass of the regenerated cellulose fiber spinning solution.
The fourth aspect of the invention provides a preparation method of fibers containing pearls and protein, which comprises the following steps: the cellulose A is sequentially alkalized, yellowed, dissolved, filtered for the first time, matured, defoamed and filtered for the second time to obtain spinning viscose, then the mixed slurry of the pearl and the protein prepared by the invention is added, and the steps of wet spinning, solidification, plasticizing and drafting, cutting, post-treatment, drying and packaging are carried out to obtain the viscose fiber containing the pearl and the protein. Or the following steps are adopted: sequentially carrying out dipping, squeezing, etiolation, dissolution, primary filtration, aging, secondary filtration, ripening and deaeration and tertiary filtration on alpha cellulose, then adding the mixed slurry of the pearl and the protein prepared by the invention, and carrying out wet spinning, post-treatment and tube forming to obtain the viscose fiber containing the pearl and the protein.
The fifth aspect of the invention provides a preparation method of antibacterial powder MOFs material, namely metal nano powder of organic framework. The antibacterial powder MOFs material comprises the following components: metal1-2 parts of oxide, 0.5-0.8 part of gallium sesquioxide, 1-2 parts of titanium dioxide, 2-4 parts of didecyl dimethyl ammonium chloride, 1-1.5 parts of polyacrylic acid and deionized water. The preparation method comprises the following steps: adding metal oxide and gallium sesquioxide into didecyl dimethyl ammonium chloride, uniformly mixing, heating to 150-200 ℃ in a vacuum degree environment of 0.1MPa, preserving heat for 15-20h, and naturally cooling to obtain an MOF material; weighing titanium dioxide, polyacrylic acid and the prepared MOF material, adding the titanium dioxide, the polyacrylic acid and the prepared MOF material into deionized water, magnetically stirring for 1-3h, transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal treatment at 150-180 ℃ for 12-15h, centrifugally washing and drying the obtained solution to obtain MOF/TiO 2 An antibacterial powder.
Compared with the prior art, the preparation method and the application of the mixed slurry of pearls and proteins and the fibers thereof have the following advantages:
(1) The pearl and protein mixed slurry contains protein, and the unique structure of the protein is utilized, so that the pearl powder dispersibility is facilitated, the pearl powder dispersibility is better by the dispersing agent, and the pearl and protein mixed slurry has good stability and is not easy to settle.
(2) The mixed slurry of the pearls and the proteins forms fully emulsified uniform suspension by using the anti-settling agent, so that powder precipitation or aggregation in the storage and later production processes is avoided. The pearl powder is not easy to settle and agglomerate, so that the pearl powder is favorable for being added into the spinning solution to prepare the fiber, the machine for preparing the fiber is not blocked, the pearl powder and the protein are uniformly dispersed into the fiber, and the strength of the fiber is not influenced.
(3) According to the fiber containing the pearls and the protein, as the pearls and the protein are added, the prepared fiber not only has pearls but also contains the protein, so that the health-care function is improved, and the softness and the hand feeling of the fiber are better; the polyethylene glycol remained in the fiber can also improve the softness of the fiber; the nanometer silicon dioxide can improve the ultraviolet resistance of the fiber and improve the cool feeling of the contact.
(4) The pearl and protein-containing fiber provided by the invention is coated by the PVP polymer and the pearl powder and protein in the mixed slurry in an adhesion manner, so that the loss of effective components caused by multiple acid-base water washing in the production and preparation processes of the fiber is avoided, and the utilization rate of the mixed slurry is greatly improved.
(5) The fiber containing the pearls and the proteins, disclosed by the invention, has an excellent antibacterial effect by taking the MOF material as an antibacterial component, and avoids loss of the antibacterial component due to reaction with strong acid in the fiber preparation process.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be noted that the data in the following experimental examples and examples are obtained by the inventors through a number of experiments, are not limited to space, only a part of which is shown in the specification, and those skilled in the art can understand and implement the present invention based on the data. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Furthermore, it should be understood that various changes or modifications to the invention may be made by those skilled in the art after reading the disclosure of the present invention, and these changes or modifications also fall within the scope of the protection of the present application.
EXAMPLES 1-4 preparation of Metal nanopowder of organic skeleton
Experimental example 1
Weighing 10g of zinc oxide and 5g of gallium sesquioxide, adding the zinc oxide and the gallium sesquioxide into 20g of didecyl dimethyl ammonium chloride, uniformly mixing, heating to 150 ℃ in a vacuum degree environment of 0.1MPa, preserving heat for 15h, and naturally cooling to obtain a Zn-MOF material; weighing 10g of titanium dioxide, 10g of polyacrylic acid and the prepared Zn-MOF material, adding the titanium dioxide, the 10g of polyacrylic acid and the prepared Zn-MOF material into 945g of deionized water, magnetically stirring for 1h, transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal treatment at 150 ℃ for 12h, carrying out centrifugal washing on the obtained solution, and drying to obtain Zn-MOF/TiO 2 An antibacterial powder.
Experimental example 2
Weighing 20g of copper oxide and 8g of gallium trioxide, adding the copper oxide and the gallium trioxide into 30g of didecyl dimethyl ammonium chloride, uniformly mixing, heating to 200 ℃ in a vacuum degree environment of 0.1MPa, preserving heat for 20h, and naturally cooling to obtain a Cu-MOF material; weighing 20g of titanium dioxide and 15g of titanium dioxideAdding the polyacrylic acid and the prepared Cu-MOF material into 907g of deionized water, magnetically stirring for 3 hours, transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 15 hours, carrying out centrifugal washing and drying on the obtained solution, and obtaining the Cu-MOF/TiO 2 An antibacterial powder.
Experimental example 3
Weighing 15g of ferric oxide and 6g of gallium sesquioxide, adding the ferric oxide and the gallium sesquioxide into 40g of didecyl dimethyl ammonium chloride, uniformly mixing, heating to 180 ℃ in a vacuum degree environment of 0.1MPa, preserving heat for 18h, and naturally cooling to obtain a Fe-MOF material; weighing 15g of titanium dioxide, 12g of polyacrylic acid and a prepared Fe-MOF material, adding the titanium dioxide, the polyacrylic acid and the prepared Fe-MOF material into 912g of deionized water, magnetically stirring for 2 hours, transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 14 hours, carrying out centrifugal washing on the obtained solution, and drying to obtain Fe-MOF/TiO 2 An antibacterial powder.
Experimental example 4
Weighing 20g of silver oxide and 7g of gallium sesquioxide, adding the silver oxide and the gallium sesquioxide into 25g of didecyl dimethyl ammonium chloride, uniformly mixing, heating to 170 ℃ in a vacuum degree environment of 0.1MPa, preserving heat for 15 hours, and naturally cooling to obtain an Ag-MOF material; weighing 15g of titanium dioxide, 13g of polyacrylic acid and the prepared Ag-MOF material, adding the titanium dioxide, the 13g of polyacrylic acid and the prepared Ag-MOF material into 920g of deionized water, magnetically stirring for 2 hours, transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal treatment at 150 ℃ for 12 hours, carrying out centrifugal washing on the obtained solution, and drying to obtain Ag-MOF/TiO 2 An antibacterial powder.
Examples 1-6 preparation of blended slurry of pearls and proteins
Example 1
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 15 parts of Margarita powder to below 5 μm, stirring with 8 parts of casein solution and 5 parts of polyethylene glycol with molecular weight of 400, adding 65 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 1 hr to obtain stock solution; wherein the casein in the casein solution is artificially synthesized, and the mass concentration is 40wt%;
adding 3 parts of nano hydrophilic silicon dioxide into the stock solution, fully stirring for 1h, and adding 4 parts of nano metal zinc powder to obtain mixed slurry of pearls and proteins.
Example 2
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 15 parts of Margarita powder to below 5 μm, stirring with 8 parts of casein solution and 5 parts of polyethylene glycol with molecular weight of 400, adding 65 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 1 hr to obtain stock solution; wherein the casein in the casein solution is artificially synthesized, and the mass concentration is 40wt%;
adding 3 parts of nano hydrophilic silicon dioxide into the stock solution, fully stirring for 1h, and adding 4 parts of Zn-MOF/TiO prepared in experimental example 1 2 Antibacterial powder to obtain mixed slurry of Margarita and protein.
Example 3
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 15 parts of Margarita powder to below 5 μm, stirring with 8 parts of casein solution and 5 parts of polyethylene glycol with molecular weight of 400, adding 57 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 1 hr to obtain stock solution; wherein the casein in the casein solution is artificially synthesized, and the mass concentration is 40wt%;
adding 3 parts of nano hydrophilic silicon dioxide into the stock solution, fully stirring for 1h, and adding 4 parts of Zn-MOF/TiO prepared in experimental example 1 2 Antibacterial powder and 8 parts of PVP polymer to obtain mixed slurry of pearl and protein.
Example 4
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 20 parts of Margarita powder to below 5 μm, stirring with 10 parts of animal protein solution and 10 parts of polyethylene glycol with molecular weight of 200, adding 37 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 1.5 hr to obtain stock solution; wherein the animal protein in the animal protein solution is animal protein extracted from pig bones, and the mass concentration is 50wt%;
in the stock solution8 parts of nano hydrophilic silicon dioxide is added, fully stirred for 2 hours and then 5 parts of Cu-MOF/TiO prepared in experimental example 2 are added 2 Antibacterial powder and 10 parts of PVP polymer to obtain mixed slurry of pearl and protein.
Example 5
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 18 parts of pearl powder to below 5 μm, stirring with 9 parts of vegetable protein solution and 9 parts of polypropylene alcohol, adding 35 parts of water, grinding until the particle diameter of the pearl powder reaches D90 less than 1 μm, and emulsifying in an emulsifying machine for 2 hr to obtain stock solution; wherein the vegetable protein in the vegetable protein solution is vegetable protein extracted from soybean, and the mass concentration is 50wt%;
adding 8 parts of sodium alginate into the stock solution, fully stirring for 2h, and adding 8 parts of Fe-MOF/TiO prepared in experimental example 3 2 Antibacterial powder and 13 parts of PVP polymer to obtain the mixed slurry of pearl and protein.
Example 6
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 16 parts of Margarita powder to below 5 μm, mixing with 12 parts of animal protein solution and 8 parts of polyethylene glycol with molecular weight of 600, stirring, adding 39 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 2 hr to obtain stock solution; wherein the animal protein in the animal protein solution is extracted from wool, and has a mass concentration of 50wt%;
the particle diameter is 0.2 mu m, the pore diameter of the micropore is 2nm, and the specific surface area is 1000m 2 Per g, pore volume of 0.50cm 3 The pearl powder and the protein are encapsulated in the honeycomb micropores of the honeycomb silica to prepare the microcapsule. Then 7 parts of calcium alginate are added, the mixture is fully stirred for 2 hours, and then 3 parts of Ag-MOF/TiO prepared in experimental example 4 are added 2 Antibacterial powder and 15 parts of PVP polymer to obtain the mixed slurry of pearl and protein.
Examples 7-12 preparation of pearl protein-containing fiber by spinning of mixed pearl protein slurry
Example 7
Sequentially carrying out alkalization, etiolation, dissolution, primary filtration, ripening, deaeration and secondary filtration on alpha cellulose, then adding the mixed slurry of the pearls and the protein prepared in the embodiment 1, wherein the mass of the mixed slurry is 3% of the total mass of the spinning viscose, and carrying out wet spinning, solidification, plasticizing and drafting, cutting, post-treatment, drying and packaging to obtain the viscose containing the pearls and the protein.
Wherein the key process parameters of each main step are as follows: in the alkalization step, the adding amount of (280 +/-0.5) g/L alkali liquor is 925L, in the yellowing step, the adding amount of CS2 is 110L, the yellowing time is 45min, the initial temperature is 26 ℃, and the finishing temperature is 21 ℃; in the dissolving step, the dissolved water is 1800L, and the viscosity of the spinning glue after ripening and defoaming is 50 seconds; in the wet spinning step, the spinning nozzle has 0.06mm × 20000 holes, the spinning speed is 55m/min, and the coagulation bath comprises the following components: 140g/L of sulfuric acid, 9g/L of zinc sulfate and 250g/L of sodium sulfate, and the temperature is 50 ℃.
Example 8
The method for spinning and preparing the fiber in the example 8 is the same as the example 7, except that the mixed slurry of the pearl and the protein prepared in the example 2 is added after the secondary filtration, and the mass of the mixed slurry is 3% of the total mass of the spinning viscose.
Example 9
The method for spinning the fiber in example 9 is the same as that in example 7, except that after the secondary filtration, the mixed slurry of the pearl and the protein prepared in example 3 is added, and the mass of the mixed slurry is 3% of the total mass of the spinning viscose.
Example 10
The method for spinning and preparing the fiber in the example 10 is the same as the example 7, except that the mixed slurry of the pearl and the protein prepared in the example 4 is added after the secondary filtration, and the mass of the mixed slurry is 7% of the total mass of the spinning viscose.
Example 11
The method for spinning and preparing the fiber in the example 11 is the same as the example 7, except that the mixed slurry of the pearl and the protein prepared in the example 5 is added after the secondary filtration, and the mass of the mixed slurry is 8% of the total mass of the spinning viscose.
Example 12
The alpha cellulose is sequentially subjected to dipping, squeezing, yellowing, dissolving, primary filtering, ageing, secondary filtering, ripening, defoaming and tertiary filtering, then the pearl and protein mixed slurry prepared in example 6 is added, the mass of the mixed slurry is 3.1% of the total mass of the spinning viscose, and wet spinning, post-treatment and tube forming are carried out, so that the viscose fiber containing the pearls and the protein is obtained.
Wherein the key process parameters of each main step are as follows: the spinning viscosity after aging and deaeration was 40 seconds, and the composition of the coagulation bath in the wet spinning step was: 140g/L of sulfuric acid, 9g/L of zinc sulfate and 250g/L of sodium sulfate, and the temperature is 50 ℃.
Comparative example 1
The preparation method of the mixed slurry of the pearls and the proteins comprises the following steps:
pulverizing 15 parts of Margarita powder to below 5 μm, stirring with 8 parts of casein solution and 5 parts of polyethylene glycol with molecular weight of 400, adding 60 parts of water, grinding until the particle diameter of Margarita powder reaches D90 less than 1 μm, and emulsifying in emulsifying machine for 1 hr to obtain stock solution; wherein the casein in the casein solution is artificially synthesized, and the mass concentration is 40wt%;
4 parts of Zn-MOF/TiO prepared in Experimental example 1 were added to the stock solution 2 Antibacterial powder and 8 parts of PVP polymer to obtain the mixed slurry of pearl and protein.
The method for preparing the fiber by spinning is the same as that of the embodiment 7, and the difference is that after the secondary filtration, the mixed slurry of the pearl and the protein prepared by the steps is added, and the mass of the mixed slurry is 3 percent of the total mass of the spinning viscose.
Comparative example 2
The pearl powder particle liquid slurry and the cotton pearl viscose fiber prepared by the method of example 1 in CN100360726C are adopted.
Comparative example 3
The pearl slurry prepared by the method of example 1 in CN101487149A is mixed with protein cellulose fiber.
Performance testing
The dispersion stability of the mixed slurry of pearls and proteins prepared in examples 1 to 6, the mixed slurry of pearl powder particles in comparative example 1, the mixed slurry of pearl powder particles in comparative example 2 and the slurry of pearl powder particles in comparative example 3 were tested by a high and low temperature cycle test under the conditions of 24 hours at a high temperature of 60 ℃ and 24 hours at a low temperature of-20 ℃, which is called a cycle, and the cycle is repeated for three cycles, which is 6 days in total, wherein the particle size is measured by a particle sizer, and the specific test results are shown in table 1.
TABLE 1
As can be seen from Table 1, the mixed slurry of pearls and proteins of examples 1 to 6 was excellent in dispersibility and free from aggregation. Before and after high and low temperature circulation, the particle size of the mixed slurry is not changed greatly, the appearance is always kept dispersed uniformly, and no agglomeration phenomenon occurs. The mixed slurry of the pearls and the protein not only improves the dispersibility of the pearl powder in water by adding the water-soluble dispersant polyethylene glycol or polypropylene glycol, but also contains the protein, the inside of the spherical protein in the protein contains hydrophobic bonds, the outside is hydrophilic and has cracks, the mixed slurry is helpful for being mixed with the hydrophilic pearls, and the spherical protein and the cracks can disperse the pearl powder to reduce the agglomeration of the pearl powder. In addition, the mixed slurry of the invention is added with nano-scale hydrophilic silicon dioxide or alginate, which is also beneficial to the dispersion stability of the pearl powder. The nanometer level hydrophilic silica makes the pearl powder form homogeneous emulsion with reversible hydrogen bond network structure to avoid precipitation and aggregation of the powder during storage and production. Meanwhile, the silicon dioxide can improve the ultraviolet resistance of the fiber and improve the cool feeling in contact. The alginate can also play a role in preventing powder from settling or aggregating and clustering, and the alginate can also have a cross-linking reaction with calcium carbonate overflowing from the pearl powder, thereby being beneficial to the combination and inlaying of the pearl powder in the spinning solution. The fibers prepared by the methods of examples 8-12 of the present application had no fuzz or yarn breakage during the production process. The mixed slurry of the pearls and the protein prepared by the invention has good stability and is not easy to agglomerate, so that a machine used for spinning cannot be blocked due to agglomeration when the fibers are prepared by spinning, and the mixed slurry can be uniformly dispersed in the fibers, so that the contents of the pearls and the protein are uniformly distributed, pearls ultra-washing particles are uniformly distributed in the fibers and on the surfaces of the fibers, and the fibers have smooth and cool hand feeling and bright appearance. And does not affect the strength of the fiber.
The mixed slurry of comparative example 1 does not include the anti-settling agent of the present application, and the pearl slurry slightly agglomerates after high and low temperature circulation, and the particle size of the pearl powder is increased more. The pearl powder particle liquid slurry of the comparative example 2 only contains water-soluble dispersant and does not contain protein and anti-settling agent, after high-temperature and low-temperature circulation, the pearl slurry is agglomerated and layered, and the particle size of the pearl powder is increased more. The pearl slurry and protein slurry of comparative example 3 also slightly increased in particle size after high and low temperature cycles, and slight agglomeration occurred, indicating that the improvement ability of the dispersibility of pearl powder by adding only protein was limited.
The fibers prepared in the above examples and comparative examples were tested for antibacterial properties according to the AATCC-100 textile antibacterial property test method, and the test strains were staphylococcus aureus and escherichia coli, with specific results shown in table 2.
TABLE 2
In the process of preparing the fiber by spinning, the metal powder is added as the antibacterial agent in the example 7 to improve the antibacterial performance of the fiber, but the metal powder is directly corroded by strong acid and strong base used in the spinning process, and the crystal substances which can generate sulfate can block the spinneret orifice, and the antibacterial effect is not as good as that of the examples 8-12. In examples 8 to 12 and comparative example 1, the phenomenon of clogging the spinneret orifice during the spinning process was not caused, and the metal antibacterial oxide (metal oxide such as zinc oxide, copper oxide, iron oxide, silver oxide, etc.) was used in the MOF organic chemistryThe frame is used as a carrier to prepare an organic framework material for bearing the sterilization material, so that the condition that components with sterilization function overflow and strong acid and strong base in the fiber preparation process are subjected to chemical reaction to generate sulfate crystals is avoided, the loss of the antibacterial agent is small, and the antibacterial effect is favorably exerted. The bacteriostatic rates of examples 8-12 and comparative example 1 were high, and showed good antibacterial properties, regardless of staphylococcus aureus or escherichia coli. Titanium dioxide (TiO) 2 ) Is a very common photocatalytic sterilization material, especially can be excited under ultraviolet light to have sterilization effect, but has weak absorption capacity to visible light, and other materials such as Cu, fe, ag and Zn can be used for improving TiO 2 The absorption capacity to visible light generates a large number of active oxygen and electron hole pairs under the excitation of light, and the active oxygen and the electron hole pairs have super-strong redox performance and can destroy the structures of bacteria or fungi to cause the bacteria or the fungi to die. With Zn carried in the MOF material 2+ 、Cu 2+ 、Ag + Etc. also have certain bactericidal performance. Gallium sesquioxide is introduced in the preparation process of the organic framework material, so that the thermal stability of the organic framework material can be improved, the organic framework material is beneficial to being added into spinning solution to prepare fibers, and the influence of the spinning process on metal nano powder of the organic framework is reduced. The bacteriostatic rates of examples 8-12 on staphylococcus aureus and escherichia coli are higher than those of the fibers of example 7 and comparative examples 2-3, and the bactericidal effect can be better exerted.
The fibers prepared in the above examples and comparative examples are tested for ultraviolet resistance according to the test method of GB/T18830-2009; the cool feeling performance is detected according to the detection method of GB/T35263-2017 detection and evaluation of cool feeling performance at the moment of textile contact, and the specific result is shown in Table 3.
TABLE 3
Note: when UPF > 40 and T (UVA) AV/% < 5%, it can be called UV-protection product.
In the samples of examples 7 to 10, since silica is added, the ultraviolet resistance of the fiber product is facilitated, the cool feeling upon contact is improved, and the performance of the fiber product is improved.
The prepared fiber samples were tested for calcium content and total amino acid content, and the specific results are shown in table 4.
TABLE 4
As can be seen from table 4, the fibers of examples 7 and 8 have low contents of calcium element and amino acid. Due to the fact that active ingredients such as pearls and proteins in the pulp are destroyed or lost during the fiber preparation process. After the mixed slurry of pearls and proteins is added with the protective solution of PVP polymer, for example, in examples 9-12 or comparative example 1, the PVP polymer is adhered and wrapped with pearl powder and proteins in the mixed slurry, so that the loss of effective components caused by multiple acid-base water washing in the production and preparation process of fibers is avoided, and the utilization rate of the mixed slurry is greatly improved. The total amount of calcium element and amino acid in the fibers of examples 9-12 and comparative example 1 is higher than that in examples 7-8, so that pearls and protein can be retained and protected to a greater extent, and the functionality of the fibers can be improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (14)
1. The mixed slurry of the pearl and the protein is characterized by comprising 15-20wt% of pearl powder, 8-12wt% of protein solution, 3-8wt% of antibacterial agent, 5-10wt% of dispersing agent, 3-8wt% of anti-settling agent, 8-15wt% of protective solution and the balance of water.
2. The mixed slurry of pearls and proteins as claimed in claim 1, wherein the mass concentration of proteins in the protein solution is 40-50wt%.
3. The mixed slurry of pearls and proteins as claimed in claim 2, wherein said proteins are selected from at least one of animal proteins, plant proteins, and synthetic proteins.
4. A mixed slurry of pearl and protein according to claim 1, wherein the pearl powder is pulverized to D90 < 2 μm in particle size.
5. The mixed slurry of pearls and proteins as claimed in claim 1, wherein the antibacterial powder is a metal-organic framework material, and the metal is at least one selected from Cu, zn, MOF and MOF.
6. The mixed slurry of pearls and proteins as claimed in claim 5, wherein the antibacterial powder consists of the following components: 1-2 parts of metal oxide, 0.5-0.8 part of gallium sesquioxide, 1-2 parts of titanium dioxide, 2-4 parts of didecyl dimethyl ammonium chloride, 1-1.5 parts of polyacrylic acid and deionized water.
7. The pearl protein mixed slurry according to claim 1, wherein said dispersing agent is at least one of polyethylene glycol and polypropylene glycol.
8. The pearl and protein mixed slurry according to claim 1, wherein said protective solution is PVP polymer.
9. The pearl protein mixed slurry according to claim 1, wherein the anti-settling agent is at least one selected from nano hydrophilic silica and alginate.
10. The mixed slurry of pearls and proteins as claimed in claim 9, wherein said alginate is sodium alginate or calcium alginate.
11. The mixed slurry of pearls and proteins as claimed in claim 1, wherein said pearls powder can be encapsulated by microcapsules or high molecular polymer.
12. A method for preparing a mixed slurry of pearls and proteins according to any one of claims 1 to 11, characterized in that it comprises the following steps:
s1, weighing each component in a formula amount;
s2, pulverizing pearl powder to below 5 microns, stirring with a protein solution and a dispersing agent, adding water, grinding until the particle size of the pearl powder reaches D90 less than 2 microns, and feeding the pearl powder into an emulsifying machine for emulsification to obtain a stock solution;
s3, adding an anti-settling agent into the stock solution prepared in the step S2, stirring, and adding an antibacterial agent and a protective agent to obtain the mixed slurry of the pearls and the proteins.
13. Use of the pearl and protein mixed pulp according to any one of claims 1 to 12 and the preparation method thereof for spinning to prepare pearl and protein-containing fibers, wherein the fibers are regenerated cellulose fibers selected from any one of modal fibers, viscose fibers, lyocell fibers and cuprammonium fibers.
14. The use according to claim 13, wherein the pearl and protein containing fiber consists of a mixed slurry of pearl and protein and cellulose, and the mass of the mixed slurry is 3-8% of the total mass of the regenerated cellulose fiber spinning solution.
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