CN115678212A - Pearl protein modified polyester master batch and fiber preparation method thereof - Google Patents
Pearl protein modified polyester master batch and fiber preparation method thereof Download PDFInfo
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Abstract
The invention provides a pearl protein modified polyester master batch and a preparation method of polyester fiber thereof, comprising the following steps: preparing protein into protein polypeptide solution, wherein the mass ratio of protein polypeptide to water is 1:0.5 to 2; pulverizing Margarita powder to below 5 μm, mixing Margarita powder 1.5-5 mass parts and protein polypeptide solution 2-6 mass parts, and controlling solid content to 55% -70%; adding hydrophilic nano silicon dioxide with the total mass ratio of 0.1-1% into the mixed slurry, and stirring; and (3) preparing the pearl protein modified polyester master batch by adding equal mass parts of slurry 45-65, equal mass parts of polyester master batch 55-75 and equal mass parts of antibacterial agent 1-5. The pearl protein modified polyester master batch and the common polyester master batch are mixed according to the proportion of 1:5-20 proportion for producing the polyester fiber.
Description
Technical Field
The invention relates to the technical field of fiber preparation, in particular to a pearl protein modified polyester fiber and a production process thereof.
Background
The polyethylene terephthalate (PET) fiber has the advantages of high strength, good elasticity, good processing performance, excellent textile performance, excellent wearability and the like, is a synthetic fiber variety with the largest world yield and the widest application, and can be used for clothing, bedding, various decorative fabrics, national defense and military special fabrics, other industrial fiber products and the like. Along with the improvement of living standard of people, higher requirements are put forward on the comfort of clothes. The research shows that the polyester fiber has good hygroscopicity because of the existence of a large amount of hydrophilic groups such as amino, hydroxyl, carboxyl and the like in the protein molecules when the protein is added into the polyester fiber.
In addition, the pearl is a natural and rare traditional Chinese medicine. The traditional Chinese medicine considers that: the pearl has cold nature, sweet and salty taste, enters heart and liver channels, has the functions of beautifying and beautifying skin, moistening skin and promoting tissue regeneration, removing freckles and wrinkles and delaying senility; and the pearl grows in water, is cold in nature and has the effects of clearing away fire and removing toxicity. When pearl is added into polyester fiber, cool fiber fabric can be prepared, and the fabric can be used for summer clothing and the like. For example, chinese patent publication No. CN101487149a in the prior art discloses a method for manufacturing pearl protein cellulose fiber, which has the excellent performance of pearls and contains relatively more plant protein, so that the total amount of protein in the fiber is greatly increased; however, as the pearl is used as a powdery inorganic material, the nano-scale pearl powder is difficult to obtain and mostly exists in a micron scale, and the micron-scale pearl powder has an unsatisfactory dispersing performance and is easy to agglomerate; meanwhile, when the pearl powder and the amino acid are spun after being simply and mechanically mixed with the protein liquid, the pearl powder, the amino acid and other components are easy to run off, the water washing resistance is poor, the efficacy of the product is greatly reduced after the product is used for a period of time, and the user experience is influenced.
The patent with publication number CN112176441A in the prior art discloses a preparation method of pearl protein fiber, and the pearl protein fiber comprises the following components in percentage by weight: 3.0 to 5.5 percent of pearl powder, 0.5 to 2 percent of amino acid and 0.1 to 0.5 percent of dispersant, and the pearl slurry and the plant protein liquid are heated and mixed and then added into the fiber spinning slurry according to the amount to carry out wet spinning. In the prior art, the pearl and the protein are introduced into the fiber at the same time, so that the fiber has protein hygroscopicity and pearl cool feeling, although the dispersibility of the pearl powder in water is improved by introducing the dispersing agent, the pearl slurry is easy to agglomerate and sink the pearl powder particles when being mixed with the vegetable protein, and particularly for the pearl powder particles with the particle size of micron order, the agglomeration and sink of the pearl powder particles are easy to occur, so that the production of the subsequent modified polyester fiber is influenced. And when the aqueous dispersing agent such as PEG is added into the formula, the production risk is high, the molten polyester liquid is unstable after melting, and the spinning stage is difficult to control.
Disclosure of Invention
In view of the above, the invention aims to provide a pearl protein modified polyester fiber and a production process thereof, so as to solve the problems that in the prior art, pearl protein slurry is easy to agglomerate and sink and cannot be stably stored in the production process of the pearl protein modified polyester fiber.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of pearl protein modified polyester master batch comprises the following steps: (1) Preparing protein into protein polypeptide solution, wherein the mass ratio of protein polypeptide to water is 1:1 to 5;
(2) Pulverizing Margarita powder to below 5 μm, mixing Margarita powder 1.5-5 mass parts and active protein polypeptide solution 2-6 mass parts, and controlling solid content to 60-70%;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 0.1-1% into the mixed slurry obtained in the step (2), and stirring;
(4) And (4) preparing the pearl protein modified polyester master batch by equal mass of 45-65 parts of the slurry obtained in the step (3), equal mass of 55-75 parts of the polyester master batch treated by the catalyst and equal mass of 1-5 parts of the antibacterial agent.
Further, the antibacterial agent is a metal oxide, or a metal oxide of an organic skeleton.
Furthermore, the polyester master batch contains 30-40% of powder mass ratio including protein polypeptide, pearl powder and nano silicon dioxide, and the balance is polyester.
Further, in the step (4): and (3) fully evaporating the water at the high temperature of 125-135 ℃ in equal parts by mass of the slurry obtained in the step (3) and the polyester master batch 65, and adding an antibacterial agent during stirring evaporation to prepare the pearl protein modified polyester master batch.
Further, the preparation of the protein into protein polypeptide solution comprises the following steps;
a) Adding protein into 1mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the sodium hydroxide aqueous solution to the protein is 3:1, and gradually heating to 60 ℃ to obtain protein polypeptide solution;
b) Slowly cooling the dissolved protein polypeptide solution to 40 ℃, adding citric acid to adjust the pH value to about 8, adding trimethylolpropane triglycidyl ether into the protein polypeptide solution, wherein the mass ratio of the trimethylolpropane triglycidyl ether to the protein polypeptide solution is 1.
Furthermore, the pearl powder can be wrapped by a microcapsule or a high-molecular polymer film and then added into the protein polypeptide solution.
Further, the polyester is one of PBT, PET, PTT, PC, nylon 6, nylon 66, polypropylene nitrile, polyvinyl alcohol, polypropylene alcohol and polylactic acid.
Further, in the step (4): adding functional powder in the process of mixing the mixed slurry and the polyester master batch, wherein the functional powder is at least one of carbon-based powder, silicon-based powder, alginate, mineral powder and metal oxide powder.
The invention also provides a preparation method of the pearl protein modified polyester fiber, which comprises the following steps of mixing the pearl protein modified polyester master batch and the common polyester master batch according to the ratio of 1:5-20 proportion for producing the polyester fiber.
Compared with the prior art, the preparation method of the pearl protein modified polyester master batch has the following advantages:
(1) Can eliminate electrostatic of terylene, and has effects of pearl anion, protein-rich skin-moistening, antibacterial, and antivirus. The honeycomb structure of the pearl powder and the silicon dioxide have good heat conductivity coefficient, so that the fabric has good far infrared ray reflection effect, ultraviolet prevention effect and instant cool feeling of contact. The raw material proportion and the process of the invention are also suitable for the production and the process of polyamide fiber or fiber master batches of acrylic fiber, aramid fiber, polylactic acid and the like.
(2) The protein polypeptide solution is activated by adopting the activating agent, and the polyester master batch is subjected to surface oxidation treatment by using the catalyst, so that the combination strength of the pearl powder and the polyester master batch can be increased, and meanwhile, the protein polypeptide is grafted to the polyester master batch, and the content of protein in the modified polyester fiber is increased.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments thereof are described in detail below.
A preparation method of pearl protein modified polyester master batch comprises the following steps: (1) Preparing protein into protein polypeptide solution, wherein the mass ratio of protein polypeptide to water is 1:1 to 5;
(2) Pulverizing Margarita powder to below 5 μm, mixing Margarita powder 1.5-5 mass parts and active protein polypeptide solution 2-4 mass parts, and controlling solid content to 55% -70%;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 0.1-1% into the mixed slurry obtained in the step (2), and stirring;
(4) And (4) preparing the pearl protein modified polyester master batch by using 45-65 mass parts of the slurry obtained in the step (3), 55-75 mass parts of the activated polyester master batch and 1-5 mass parts of the antibacterial agent.
Further, the antibacterial agent is a metal oxide, or a metal oxide of an organic skeleton. For example, the antibacterial agent may be a metal oxide or a metal oxide of an organic skeleton.
Furthermore, when the antibacterial agent is a zinc oxide organic framework, the preparation method of the antibacterial agent comprises the following steps: dissolving 0.5-2 parts by weight of zinc oxide powder with the particle size of 40nm in 1mol/L hydrochloric acid solution, mixing with 1-5 parts by weight of trimesic acid, and reacting for 1.5 hours in a closed reaction kettle with pressure and added nitrogen at 60 ℃ to obtain a material A;
the material A is mixed and stirred with 1 to 5 weight parts of 2,4,4 '-trichloro-2' -hydroxydiphenyl ether, and then is subjected to heat treatment at 180 to 250 ℃ in a water vapor atmosphere to obtain the zinc oxide-loaded organic framework antibacterial agent.
Furthermore, the pearl protein modified polyester master batch contains 30 to 40 mass percent of powder containing protein polypeptide, pearl powder and nano silicon dioxide, and the balance is polyester.
Further, in the step (4): and (3) uniformly mixing 45-65 mass parts of the slurry obtained in the step (3) and 65 mass parts of the activated polyester master batch, fully evaporating water at the high temperature of 125-135 ℃, and adding an antibacterial agent in the stirring evaporation process to prepare the pearl protein modified polyester master batch.
Furthermore, the specific preparation process of the activated polyester master batch comprises the following steps: dissolving hydroquinone oxidase and 2,2,6,6-tetramethylpiperidine-nitrogen-oxide in deionized water, adjusting the pH value of the solution to 4-5 to ensure that the solubility of the hydroquinone oxidase is 5U/mL, the concentration of 2,2,6,6-tetramethylpiperidine-nitrogen-oxide is 2g/L, adding polyester master batch into the mixed solution, wherein the mass ratio of the polyester master batch to the deionized water is 1:10, keeping the temperature at about 30 ℃, soaking for 3 hours, and washing and drying the activated polyester master batch after the treatment is finished.
Further, the step (1) of preparing the protein into protein polypeptide solution comprises the following steps;
a) Adding protein into 1mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the sodium hydroxide aqueous solution to the protein is 3:1, and gradually heating to 60 ℃ to obtain protein polypeptide solution;
b) Slowly cooling the dissolved protein polypeptide solution to 40 ℃, adding citric acid to adjust the pH value to about 8, adding trimethylolpropane triglycidyl ether into the protein polypeptide solution, wherein the mass ratio of the trimethylolpropane triglycidyl ether to the protein polypeptide solution is 1.
Furthermore, the pearl powder can be wrapped by a microcapsule or a high-molecular polymer film and then added into the protein polypeptide solution.
Further, the polyester is any one or combination of polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate (PTT), polycarbonate (PC), nylon 6, nylon 66, polyacrylonitrile, polyvinyl alcohol, polypropylene alcohol and polylactic acid.
Further, in the step (4): at least one of carbon-based powder, silicon-based powder, alginate, ore powder, metal oxide powder and other functional powder can be added in the process of mixing the mixed slurry and the activated polyester master batch to modify the polyester master batch, so as to prepare the modified polyester fiber with composite function. Preferably, mineral powder can be added in the step (4) to improve the heating and antibacterial functions of the fiber.
As part of the embodiment of the present invention, the functional powder in step (4) may be combined with the polyester masterbatch to prepare the functional polyester masterbatch, and then perform the catalytic treatment on the polyester masterbatch. Specifically, taking PET or PBT polyester and alginate as examples, the preparation of the functional polyester master batch specifically comprises the following steps:
weighing the following components in parts by weight: 80-100 parts of polyester slice, 5-10 parts of diatomite, 10-20 parts of sodium alginate, 0.1-0.5 part of trihydroxy stearin and 2-5 parts of zinc oxide organic framework antibacterial agent;
adding sodium alginate and diatomite into a sodium hydroxide solution, and then adding silicon dioxide and an ethanol solution to form a colloidal material A;
step three, stirring and mixing the polyester slices and trihydroxy stearin uniformly at a high speed under a heating condition, and heating to a molten state to obtain a material B;
and step four, uniformly mixing and stirring the material A, the material B and the zinc oxide organic framework antibacterial agent, and then carrying out extrusion granulation by a double-screw extruder to prepare the functional polyester master batch.
The sodium alginate and the diatomite are attached to the polyester to form inside and on the surface of the polyester master batch, so that the hydrophilicity of the polyester can be improved, the finally obtained fiber has high hygroscopicity, and the trihydroxystearin serving as the dispersing agent can improve the dispersibility of the antibacterial agent, the diatomite and the sodium alginate in the molten polyester. When the master batch prepared by the method is used as a raw material to spin fiber, the spinnability is good, the spinning of filament is facilitated, and the moisture absorption of the spun polyester fiber is obviously better than that of the common polyester fiber.
Furthermore, the nano calcium carbonate can be used for replacing pearl powder, so that the cost is reduced.
The embodiment of the invention also provides a preparation method of the pearl protein modified polyester fiber, which comprises the following steps of mixing the pearl protein modified polyester master batch and the common unmodified polyester master batch according to the ratio of 1:5-20 proportion for fiber production.
Furthermore, the process can be applied to the production of PBT, PET, PTT, PC, nylon 6, nylon 66, polyacrylonitrile fiber, polyvinyl alcohol fiber, polypropylene alcohol fiber or polylactic acid fiber.
Furthermore, the pearl powder in the invention can be replaced by nano calcium carbonate, thus reducing the cost.
Furthermore, the pearl powder or other powder can be wrapped by a microcapsule or a high-molecular polymer film, so that high-temperature damage or loss in the production process can be avoided.
Example 1
(1) Preparing protein into protein polypeptide solution, which comprises the following steps:
a) Adding protein into 1mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the sodium hydroxide aqueous solution to the protein is 1:1, and gradually heating to 60 ℃ to obtain protein polypeptide solution;
b) Slowly cooling the dissolved protein polypeptide solution to 40 ℃, adding citric acid to adjust the pH value to about 8, adding trimethylolpropane triglycidyl ether into the protein polypeptide solution, wherein the mass ratio of the trimethylolpropane triglycidyl ether to the protein polypeptide solution is 1.
(2) Pulverizing Margarita powder to below 5 μm, mixing Margarita powder 2 mass parts and active protein polypeptide liquid 2 mass parts, and controlling solid content to 60-70%;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 0.1% into the mixed slurry obtained in the step (2), and stirring;
(4) The method comprises the following steps of (1) treating original polyester master batch by using a catalyst, wherein the specific treatment process comprises the following steps: dissolving hydroquinone oxidase and 2,2,6,6-tetramethylpiperidine-nitrogen-oxide in deionized water, adjusting the pH value of the solution to 4-5 to ensure that the solubility of the hydroquinone oxidase is 5U/mL, the concentration of 2,2,6,6-tetramethylpiperidine-nitrogen-oxide is 2g/L, adding polyester master batch into the mixed solution, wherein the mass ratio of the polyester master batch to the deionized water is 1:10, keeping the temperature at about 30 ℃, soaking for 3 hours, and washing and drying the activated polyester master batch after the treatment is finished.
And (3) mixing the activated polyester master batch 55 parts by mass with the slurry 45 parts by mass obtained in the step (3), fully evaporating water at the high temperature of 125-135 ℃, adding 1 part by mass of the antibacterial agent zinc oxide with the particle size of 40nm in the stirring evaporation process, and preparing the pearl protein modified polyester master batch.
Example 2
Step (1) is the same as in example 1.
(2) Pulverizing Margarita powder to below 5 μm, and controlling solid content at 60-70% with 1 mass equal part of Margarita powder and 2 mass equal parts of active protein polypeptide liquid;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 0.5% into the mixed slurry in the step (2), and stirring;
(4) The method comprises the following steps of (1) treating original polyester master batch by using a catalyst, wherein the specific treatment process comprises the following steps: dissolving hydroquinone oxidase and 2,2,6,6-tetramethylpiperidine-nitrogen-oxide in deionized water, adjusting the pH value of the solution to 4-5 to ensure that the solubility of the hydroquinone oxidase is 5U/mL, the concentration of 2,2,6,6-tetramethylpiperidine-nitrogen-oxide is 2g/L, adding polyester master batch into the mixed solution, wherein the mass ratio of the polyester master batch to the deionized water is 1:10, maintaining the temperature at about 30 ℃, soaking for 3 hours, and washing and drying the activated polyester master batch after the treatment is finished.
And (3) fully evaporating water at the high temperature of 125-135 ℃ by equal mass of the slurry obtained in the step (3) and equal mass of the activated polyester master batch 65, adding 3 equal mass of the antibacterial agent zinc oxide during stirring and evaporation, wherein the particle size of the zinc oxide is 40nm, and preparing the pearl protein modified polyester master batch.
Example 3
Step (1) is the same as in example 1.
(2) Pulverizing Margarita powder to below 5 μm, mixing Margarita powder 1 mass part and active protein polypeptide liquid 3 mass part, and controlling solid content to 60-70%;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 1% into the mixed slurry obtained in the step (2), and stirring;
(4) The method comprises the following steps of (1) treating original polyester master batch by using a catalyst, wherein the specific treatment process comprises the following steps: dissolving hydroquinone oxidase and 2,2,6,6-tetramethylpiperidine-nitrogen-oxide in deionized water, adjusting the pH value of the solution to 4-5 to ensure that the solubility of the hydroquinone oxidase is 5U/mL, the concentration of 2,2,6,6-tetramethylpiperidine-nitrogen-oxide is 2g/L, adding polyester master batch into the mixed solution, wherein the mass ratio of the polyester master batch to the deionized water is 1:10, keeping the temperature at about 30 ℃, soaking for 3 hours, and washing and drying the polyester master batch after the treatment is finished.
And (3) fully evaporating water at the high temperature of 125-135 ℃ by equal mass of the slurry obtained in the step (3) and equal mass of the activated polyester master batch, adding 5 equal mass of the antibacterial agent zinc oxide during stirring and evaporation, wherein the particle size of the zinc oxide is 40nm, and preparing the pearl protein modified polyester master batch.
Example 4
The steps (1) to (3) are the same as in example 2.
(4) And (3) preparing the pearl protein modified polyester master batch by equal mass of the slurry obtained in the step (3), equal mass of the activated polyester master batch 65 and equal mass of the antibacterial agent 3.
The antimicrobial agents in this example were: the zinc oxide organic framework, the specific antibacterial agent preparation process is: dissolving 4 parts by weight of zinc oxide powder with the particle size of 40nm by using 1mol/L hydrochloric acid solution to form solution, mixing the solution with 4 parts by weight of trimesic acid, and reacting for 1.5 hours in a closed reaction kettle with pressure and nitrogen addition at 60 ℃ to obtain a material A;
and mixing and stirring the material A and 4 parts by weight of 2,4,4 '-trichloro-2' -hydroxydiphenyl ether, and performing heat treatment at 180-250 ℃ in a water vapor atmosphere to obtain the zinc oxide organic framework antibacterial agent.
Example 5
The steps (1) to (3) are the same as in example 2.
The original polyester master batch in step (4) of example 2 was replaced with a functional polyester master batch, and the other cartridges were the same as in example 2. The preparation method of the functional polyester master batch comprises the following steps:
weighing the following components in parts by weight: 80-100 parts of polyester slice, 5-10 parts of diatomite, 10-20 parts of sodium alginate, 0.1-0.5 part of trihydroxy stearin and 2-5 parts of zinc oxide organic framework antibacterial agent;
adding sodium alginate and diatomite into a sodium hydroxide solution, and then adding silicon dioxide and an ethanol solution to form a colloidal material A;
step three, stirring and mixing the polyester slices and trihydroxy stearin uniformly at a high speed under a heating condition, and heating to a molten state to obtain a material B;
and step four, uniformly mixing and stirring the material A, the material B and the zinc oxide organic framework antibacterial agent, and then carrying out extrusion granulation by a double-screw extruder to prepare the functional polyester master batch.
Comparative example 1
The steps (1), (2) and (4) are the same as the embodiment 2, and the step of adding the hydrophilic nano silicon dioxide in the step (3) is omitted;
comparative example 2
(1) The method for preparing the protein polypeptide solution from the protein comprises the following steps:
a) Adding protein into 1mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the sodium hydroxide aqueous solution to the protein is 3:1, and gradually heating to 60 ℃ to obtain protein polypeptide solution;
steps (2) to (4) were the same as in example 2,
comparative example 3
The steps (1) to (3) are the same as in example 2,
(4) And (3) preparing the pearl protein modified polyester master batch by equal mass of 65 parts of the polyester master batch which is not treated by the catalyst, equal mass of 55 parts of the slurry obtained in the step (3) and equal mass of 3 parts of the antibacterial agent zinc oxide, wherein the particle size of the zinc oxide is 40 nm.
Experimental example 1
The suspensions obtained by adding the hydrophilic nano-silica in the above examples 1 to 3 and comparative example 1 were respectively collected and allowed to standDevice for placingThe amount of precipitates in each slurry was observed and recorded, and the fibers prepared in the above examples and comparative examples were spun by dry spinning, and the fibers prepared in the above examples were tested for water absorption according to the test method of GB/T21655.2-2019, and the overall results are shown in Table 1 below:
TABLE 1
The comparison of the above examples shows that, because the protein polypeptide liquid is used as the dispersing agent of the pearl powder, the pearl powder can be well dispersed in the protein polypeptide liquid without adding the polyethylene glycol dispersing agent in the mixed slurry of the pearl protein.
When the hydrophilic silicon dioxide is not added into the pearl protein slurry, although the dispersibility of the pearl powder in the protein solution is good in a short time, a large amount of precipitates can be generated along with the extension of time, and even a clear layering phenomenon can be generated inside the slurry, namely although the pearl powder can be temporarily dispersed in the protein solution by the protein polypeptide liquid, a polymerization cohesion or precipitation phenomenon can be generated among pearl powder particles along with the extension of time, and the modification of the polyester master batch is influenced. After the hydrophilic silicon dioxide is added, the silicon dioxide in the slurry forms a reversible hydrogen bond network structure in the slurry, so that the agglomeration and sinking of the pearl powder can be prevented to a certain extent, the mixed slurry is kept in a stable dispersion state, and meanwhile, when the mixed slurry is mixed with the polyester master batch, the silicon dioxide nano particles are used as a solid dispersing agent in the material mixing process along with the evaporation of water, so that the agglomeration of the pearl powder in the material mixing process is avoided.
When the original polyester master batch is replaced by the functional polyester master batch, the moisture absorption of the polyester fiber is greatly improved due to the addition of the diatomite and the sodium alginate.
Experimental example 2
Mixing the pearl protein modified polyester master batch obtained in each embodiment with common polyester master batch according to the weight ratio of 1:5-20, and simultaneously carrying out a durability test (10 washing tests and 200 rubbing tests) on the prepared fiber, and measuring the content of amino acid in every 100g of the fiber and the content of calcium element in every 1g of the fiber before and after the durability test, wherein the specific contents are shown in the following table 2:
TABLE 2
The comparison shows that the calcium element and the amino acid in the example 2 have the highest contents and are far higher than those in the comparative examples 1-3, wherein the comparative example 3 is lower than that in the comparative example 1, and the comparative example 1 is lower than that in the comparative example 2, which shows that when the pearl powder content in the pearl protein suspension is higher, the calcium element content in the prepared fiber is higher, and the hydrophilic silicon dioxide obviously improves the dispersibility of the pearl powder in the polypeptide solution, so that the pearl powder content in the modified polyester fiber is improved.
In the comparative example 1, because the hydrophilic nano silicon dioxide is not added, a large amount of agglomeration and precipitation phenomena occur in the pearl powder in the mixing process, so that the content of the pearl powder grafted to the polyester fiber is low.
Compared with the data in the comparative examples 2 to 3, the amino acid content in the comparative example 2 is lower than that in the comparative example 3, and the amino acid content in the comparative example 3 is obviously lower than that in the example 2, it can be seen that the protein polypeptide solution is activated, so that the surface of the protein polypeptide contains a large amount of epoxy groups, the polyester master batch is subjected to surface oxidation treatment, the content of carboxyl groups on the surface of the polyester master batch is increased, and when the polyester master batch is modified, the epoxy groups on the surface of the protein polypeptide react with the carboxyl groups on the surface of the polyester master batch, so that a large amount of protein polypeptide is grafted onto the polyester master batch, and further the content of protein in the modified polyester fiber is increased. Meanwhile, after the surface oxidation treatment is carried out on the polyester master batch, the polyester master batch is very easy to combine with pearl powder, and the content of calcium element on the modified polyester fiber can be increased.
After washing, it can be found that the content of protein and calcium in examples 1 to 3 is reduced a little, the content of calcium in comparative example 3 is reduced a lot, and the content of protein in comparative example 2 is reduced a lot, so that it can be found that after the protein polypeptide solution is activated and the surface oxidation treatment is performed on the polyester master batch, the protein polypeptide can be grafted to the surface of the polyester fiber, and the surface oxidation treatment is performed on the polyester master batch, so that the binding fastness of the pearl powder and the polyester master batch can be increased.
Experimental example 3
Mixing the pearl protein modified polyester master batch obtained in each embodiment with common polyester master batch according to the weight ratio of 1:5-20, performing dry spinning to prepare fibers, testing the ultraviolet resistance of the examples and the comparative examples by using a testing method of GB/T18830-2009, and testing the cooling performance of the examples and the comparative examples by using a testing method of GB/T35263-2017, namely detection and evaluation of the cooling performance of textiles at the moment of contact, wherein the results are shown in the following table 3.
TABLE 3
Note: when UPF is more than 40 and T (UVA) AV/% < 5%, the product can be called ultraviolet-proof product
Comparative example 1, when hydrophilic silica was not added, resulted in a lower pearl content, which in turn resulted in poor cool touch and uv protection of the fibers.
The antibacterial rate of the polyester fibers obtained in each example is tested by using a detection mode of GB/T20944.3-2008, and the results are shown in Table 4.
TABLE 4
| Staphylococcus aureus (/%) | Escherichia coli (/%) | Candida albicans (/%) | |
| Example 1 | 96.7 | 96.4 | 95.9 |
| Example 2 | 97.2 | 96.9 | 96.3 |
| Example 3 | 96.3 | 97.1 | 97.4 |
| Example 4 | 98.3 | 99.1 | 99 |
| Example 5 | 97.9 | 98.3 | 96.8 |
In examples 1 to 3, zinc oxide is added as an antibacterial agent to prepare the polyester fiber, although the polyester fiber has better antibacterial performance, compared with example 4, the antibacterial performance of example 4 is the best, and it can be seen that when a zinc oxide organic framework is used as an antibacterial material, the antibacterial capability of the obtained pearl protein modified polyester fiber can be effectively improved, mainly because the organic framework can form a specific structure through self-assembly, and has the characteristics of high porosity, large specific surface area, safety and no toxicity, zinc ions are attached to the organic framework and fully contact with various types of bacterial viruses, so that the antibacterial and bactericidal effects are improved, and the organic framework plays a role in fixing the zinc ions and prevents the zinc ions from falling off. However, when the zinc oxide organic framework antibacterial agent is added to the functional polyester master batch, the antibacterial performance of the zinc oxide organic framework antibacterial agent can be improved to a certain extent due to the small addition amount of the antibacterial agent, but the improvement of the antibacterial performance is limited.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The preparation method of the pearl protein modified polyester master batch is characterized by comprising the following steps:
(1) Preparing protein into protein polypeptide solution, wherein the mass ratio of protein polypeptide to water is 1:1 to 5;
(2) Pulverizing Margarita powder to below 5 μm, mixing Margarita powder 1.5-5 mass parts and active protein polypeptide solution 2-6 mass parts, and controlling solid content to 55% -70%;
(3) Adding hydrophilic nano silicon dioxide with the total mass ratio of 0.1-1% into the mixed slurry obtained in the step (2), and stirring;
(4) And (4) preparing the pearl protein modified polyester master batch by using 45-65 mass parts of the slurry obtained in the step (3), 55-75 mass parts of the activated polyester master batch and 1-5 mass parts of the antibacterial agent.
2. The method for preparing the pearl protein modified polyester masterbatch according to claim 1, wherein the antibacterial agent is a metal oxide or a metal oxide with an organic skeleton.
3. The method for preparing the pearl protein modified polyester master batch according to claim 1, wherein the mass ratio of the powder containing the protein polypeptide, the pearl powder and the nano silicon dioxide in the pearl protein modified polyester master batch is 30-40%, and the balance is polyester.
4. The method for preparing the pearl protein modified polyester master batch according to claim 1, wherein in the step (4): and (4) uniformly mixing 45-65 mass parts of the slurry obtained in the step (3) and 65 mass parts of the activated polyester master batch, fully evaporating water at the high temperature of 125-135 ℃, and adding an antibacterial agent in the stirring evaporation process to prepare the pearl protein modified polyester master batch.
5. The method for preparing the pearl protein modified polyester master batch according to claim 1, wherein the step of preparing protein polypeptide solution from protein comprises the following steps;
a) Adding protein into 1mol/L sodium hydroxide aqueous solution, wherein the mass ratio of the sodium hydroxide aqueous solution to the protein is 3:1, and gradually heating to 60 ℃ to obtain protein polypeptide solution;
b) Slowly cooling the dissolved protein polypeptide solution to 40 ℃, adding citric acid to adjust the pH value to about 8, adding trimethylolpropane triglycidyl ether into the protein polypeptide solution, wherein the mass ratio of the trimethylolpropane triglycidyl ether to the protein polypeptide solution is 1.
6. The method for preparing the pearl protein modified polyester master batch according to claim 1, wherein the pearl powder can be wrapped by a microcapsule or a high molecular polymer film and then added into a protein polypeptide solution.
7. The method for preparing the pearl protein modified polyester master batch according to any one of claims 1 to 6, wherein the polyester is at least one of PBT, PET, PTT, PC, nylon 6, nylon 66, polyacrylonitrile, polyvinyl alcohol, polypropylene alcohol and polylactic acid.
8. The method for preparing the pearl protein modified polyester master batch according to claim 1, wherein in the step (4): adding functional powder in the process of mixing the mixed slurry and the activated polyester master batch, wherein the functional powder is at least one of carbon-based powder, silicon-based powder, alginate, mineral powder and metal oxide powder.
9. A preparation method of pearl protein modified polyester fiber is characterized in that the pearl protein modified polyester master batch of any one of claims 1 to 8 and common polyester master batch are mixed according to the proportion of 1:5-20 proportion for fiber production.
10. The method of claim 9, wherein the fiber comprises at least one of PBT, PET, PTT, PC, nylon 6, nylon 66, polyacrylonitrile fiber, polyvinyl alcohol fiber, polypropylene alcohol fiber, or polylactic acid fiber.
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