CN111647177B - Pollution-resistant isatis root modified PP master batch and preparation method thereof - Google Patents
Pollution-resistant isatis root modified PP master batch and preparation method thereof Download PDFInfo
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Abstract
The invention provides a pollution-resistant isatis root modified PP master batch and a preparation method thereof, wherein the preparation method comprises the following steps of: comprises selecting radix Isatidis extract, high temperature treating, and microwave treating; the high temperature treatment comprises the following steps: the treatment temperature is 180-190 ℃ and the treatment time is 15-20s; the microwave treatment comprises the following steps: the microwave frequency is 20-24GH. The method also comprises the step of modifying the isatis root extract: adding the pretreated radix Isatidis extract into deionized water, stirring at 1800-2000rpm for 15-20min, and completely dissolving at bath ratio of 1:15-20. Sequentially adding mangosteen polyphenol and fructus Hippophae flavone into radix Isatidis extract solution, heating the solution to 90-95deg.C, and performing ultrasonic-assisted dispersion.
Description
Technical Field
The invention belongs to the technical field of fiber manufacturing, and particularly relates to a pollution-resistant isatis root modified PP master batch and a preparation method thereof.
Background
With the continuous improvement of the living standard of people, the functional demands of people on daily fabrics are also improved. Antibacterial properties are one of the properties of great concern. Antibacterial modification technology of PP masterbatch is also an important aspect of research of technicians in recent years. The traditional antibacterial means is to add inorganic antibacterial agent, organic antibacterial agent and natural antibacterial agent. Among them, natural antibacterial agents are the most popular antibacterial means for people to pursue and love due to their green, plant source, harmless properties and the like. However, the natural antibacterial agent is not as mature in industrial application as the application process of inorganic antibacterial agent and organic antibacterial agent. The existing natural antibacterial agent has the technical problems of poor antibacterial effect, instability, easy failure and the like. Radix Isatidis is a natural antibacterial substance and is a hot spot for related researches in the field. Meanwhile, in order to pursue comfort, it is necessary to improve the water absorption of the PP master batch, but the water absorption of the PP master batch in the prior art is very poor, and generally about 0.01%.
Patent CN201710646998.6 provides a preparation method of a biomass antibacterial PP master batch, a product and application thereof, wherein the biomass antibacterial PP master batch comprises a matrix resin, a biomass antibacterial agent, 1-5 wt% of a lubricant and 0.05-0.2 wt% of a blending component of a composite antioxidant: the main components of the biomass antibacterial agent are dried fruits, leaves and roots of Mahonia, and the biomass antibacterial agent is prepared from the following fruits: leaf: mixing the root=1:2-5:3-7, mineralizing the biomass material with the antibacterial effect by using amorphous minerals, wherein the mass ratio of the biomass material to the master batch is 10-30wt%; firstly, placing matrix resin, a lubricant and a biomass antioxidant in a high-speed mixer to be stirred uniformly; and adding a biomass antibacterial agent, mixing again until the mixture is uniform, and preparing the antibacterial agent by adopting a double-screw extruder. The antibacterial master batch prepared by the method has higher antibacterial rate, is used for antibacterial modification of polypropylene, and solves the problem that a biomass antibacterial agent cannot be processed at high temperature.
In the prior art, for the technology of modifying PP master batch by adopting isatis root, the following technical defects exist: (1) The modified PP master batch has unsatisfactory antibacterial effect and poor storage stability; (2) easy elution and no water washing resistance; (3) the water absorption effect is not ideal; (4) poor contamination resistance.
Disclosure of Invention
In order to solve the problems in the prior art, the prior art is further optimized, and the pollution-resistant isatis root modified PP master batch and the preparation method thereof are provided for realizing the following purposes:
the antibacterial stability and the washing resistance of the isatis root modified PP master batch are improved; improving the water absorption performance and the pollution resistance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of pollution-resistant isatis root modified PP master batch comprises the following steps:
step 1, pretreatment of radix isatidis extract
(1) Selecting radix Isatidis extract
Selected isatis root extract: 100% of the total bacterial count is sieved by a 800-mesh sieve, the content of active ingredients is 97.8-98.2%, the moisture is 5-6%, the total bacterial count is less than 100cfu/g, no salmonella and escherichia coli are detected, and the quality guarantee period is 24 months.
(2) High temperature treatment
Mixing radix Isatidis extract, and treating at 180-190 deg.C for 15-20s; the isatis root extract is led out after instantaneous high-temperature treatment and cooled to normal temperature for standby.
(3) Microwave treatment
Placing the heat-treated radix Isatidis extract in a microwave device, and treating for 100-150s under the condition of microwave frequency of 20-24 GH; guiding out after microwave treatment, and cooling radix Isatidis extract to 0-2deg.C at a speed of 4-5deg.C/min; then keeping for 1-2h, and then naturally heating to 25-28 ℃ for standby.
Step 2, modification of the isatis root extract
(1) Dissolving
Adding the pretreated radix Isatidis extract into deionized water, stirring at 1800-2000rpm for 15-20min, and completely dissolving at bath ratio of 1:15-20; obtaining the isatis root extract solution.
(2) Adding modifying substances
Sequentially adding mangosteen polyphenol and seabuckthorn flavone into the radix isatidis extract solution; stirring at 1800-2000rpm for 30-40min; then heating the solution to 90-95 ℃ and performing ultrasonic-assisted dispersion, wherein the ultrasonic frequency is 30-38KHz, and the dispersion time is 90-100s; after dispersion, the dissolution liquid is cooled to 25-35 ℃ to obtain the modified isatis root extract solution.
The adding amount of the mangosteen polyphenol is 2.8-3.1% of the isatis root extract solution;
the addition amount of the seabuckthorn flavone is 1.9-2.5% of the isatis root extract solution.
Step 3, preparing a functional modifier
Mixing the loading agent and the modified isatis root extract solution according to the mass ratio of 1:8-10; heating the mixed solution to 90-100deg.C, and stirring at 4000-4500rad/min for 50-60min; then cooling to 60-64 ℃, stirring for 20-30min at 2800-3000 rad/min; then cooling to 25-35 ℃; distilling under reduced pressure for 40-50min to obtain the functional modifier.
The loading agent comprises the following raw material components in parts by weight: 4-5 parts of nano bentonite, 0.5-1 part of magnesium stearate and 7-10 parts of nano activated carbon; the loading agent comprises: 100% is sieved by a 8000 mesh sieve.
Step 4, preparing functional master batch
Mixing PP slice, functional modifier, antioxidant 1076, tert-butyl p-hydroxy anisole and polyoxyethylene ether, and oven drying at 120-125deg.C for 24 hr; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 220-250 ℃, carrying out melt blending for 40-50min, and carrying out high-speed mixing, extrusion granulation at the screw rotating speed of 320-350 r/min to obtain the functional master batch.
The mass ratio of the PP slice to the functional modifier to the antioxidant 1076 to the tert-butyl p-hydroxy anisole to the polyoxyethylene ether is 100:6-6.8:1.5-2.5:1.1-1.3:0.5-0.6.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the isatis root modified PP master batch prepared by the invention has good antibacterial effect; the antibacterial rate of the master batch on staphylococcus aureus, escherichia coli and candida albicans is over 96 percent; in particular to the inhibition rate of typhoid bacillus reaching more than 98 percent.
2. The prepared isatis root modified PP master batch has good pollution resistance; the antifouling grade is greater than 4, and the soil release grade is greater than 4.
3. The water absorption performance of the isatis root modified PP master batch prepared by the invention reaches 0.5-0.8%.
4. The prepared isatis root modified PP master batch has good storage-resistant and washing-resistant effects; after 5 years of storage, the antibacterial performance can still reach more than 94%; after 150 times of water washing, the bacteriostasis rate still reaches more than 93 percent.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1 preparation method of pollution-resistant Isatis root modified PP masterbatch
Step 1, pretreatment of radix isatidis extract
(1) Selecting radix Isatidis extract
Selected isatis root extract: 100% of the total bacterial count is sieved by a 800-mesh sieve, the content of active ingredients is 97.8-98.2%, the moisture is 5-6%, the total bacterial count is less than 100cfu/g, no salmonella and escherichia coli are detected, and the quality guarantee period is 24 months.
(2) High temperature treatment
Mixing radix Isatidis extract, and treating at 180deg.C for 15s; the isatis root extract is led out after instantaneous high-temperature treatment and cooled to normal temperature for standby.
(3) Microwave treatment
Placing the heat-treated radix Isatidis extract in a microwave device, and treating for 100s under the condition of microwave frequency of 20 GH; guiding out after microwave treatment, and cooling the radix Isatidis extract to 1deg.C at a speed of 4deg.C/min; then keeping for 1h, and then naturally heating to 25 ℃ for standby.
Step 2, modification of the isatis root extract
(1) Dissolving
Adding the pretreated radix Isatidis extract into deionized water, stirring at 1800rpm for 15min, and completely dissolving with bath ratio of 1:15; obtaining the isatis root extract solution.
(2) Adding modifying substances
Sequentially adding mangosteen polyphenol and seabuckthorn flavone into the radix isatidis extract solution; stirring at 1800rpm for 30min; then heating the dissolution liquid to 90 ℃ and performing ultrasonic-assisted dispersion, wherein the ultrasonic frequency is 30KHz, and the dispersion time is 90s; after dispersion, the dissolution liquid is cooled to 25 ℃ to obtain the modified isatis root extract solution.
The adding amount of the mangosteen polyphenol is 2.8% of the isatis root extract solution;
the addition amount of the seabuckthorn flavone is 1.9% of the isatis root extract solution.
Step 3, preparing a functional modifier
Mixing a loading agent and a modified isatis root extract solution according to a mass ratio of 1:8; then heating the mixture to 90 ℃ and stirring at a speed of 4000rad/min for 50min; then cooling to 60 ℃, and stirring for 20min at the speed of 2800 rad/min; then cooling to 35 ℃; and (5) distilling under reduced pressure for 50min to obtain the functional modifier.
The loading agent comprises the following raw material components in parts by weight: 4 parts of nano bentonite, 0.5 part of magnesium stearate and 10 parts of nano activated carbon; the loading agent comprises: 100% is sieved by a 8000 mesh sieve.
Step 4, preparing functional master batch
Mixing PP slice, functional modifier, antioxidant 1076, tert-butyl p-hydroxy anisole and polyoxyethylene ether, and oven drying at 120deg.C for 24 hr; then adding the mixture into a double-screw extruder, controlling the melting temperature to 220 ℃, carrying out melt blending for 40min, mixing at a high speed, extruding and granulating at a screw speed of 320 revolutions per minute, and obtaining the functional master batch.
The mass ratio of the PP slice to the functional modifier to the antioxidant 1076 to the tert-butyl p-hydroxy anisole to the polyoxyethylene ether is 100:6:1.5:1.3:0.6.
the antibacterial rate of the isatis root modified PP master batch prepared in the embodiment to staphylococcus aureus is 97.8%, the antibacterial rate to escherichia coli is 98.2%, and the antibacterial rate to candida albicans is 98.9%; in particular to the inhibition rate of typhoid bacillus reaching 98.5 percent. The prepared isatis root modified PP master batch has the antifouling grade of 4 and the easy decontamination grade of 4. The prepared isatis root modified PP master batch has water absorption performance reaching 0.5 percent. The prepared isatis root modified PP master batch is stored for 5 years, the antibacterial rate of the isatis root modified PP master batch for staphylococcus aureus is 93.5%, the antibacterial rate for escherichia coli is 94.4%, the antibacterial rate for candida albicans is 94.25%, and the antibacterial rate for typhoid bacillus is 93.15%. The prepared isatis root modified PP master batch has the bacteriostasis rate of 94.25% on staphylococcus aureus, 95.15% on escherichia coli, 95.08% on candida albicans and 94.5% on typhoid bacillus after being washed for 150 times.
Example 2 preparation method of pollution-resistant Isatis root modified PP masterbatch
Step 1, pretreatment of radix isatidis extract
(1) Selecting radix Isatidis extract
Selected isatis root extract: 100% of the total bacterial count is sieved by a 800-mesh sieve, the content of active ingredients is 97.8-98.2%, the moisture is 5-6%, the total bacterial count is less than 100cfu/g, no salmonella and escherichia coli are detected, and the quality guarantee period is 24 months.
(2) High temperature treatment
Mixing radix Isatidis extract, and treating at 185 deg.C for 17s; the isatis root extract is led out after instantaneous high-temperature treatment and cooled to normal temperature for standby.
(3) Microwave treatment
Placing the heat-treated radix Isatidis extract in a microwave device, and treating under the condition of microwave frequency of 22GH for 130s; guiding out after microwave treatment, and cooling the radix Isatidis extract to 2deg.C at a speed of 4.5deg.C/min; then keeping for 1.5h, and then naturally heating to 26 ℃ for standby.
Step 2, modification of the isatis root extract
(1) Dissolving
Adding the pretreated radix Isatidis extract into deionized water, stirring at 1900rpm for 18min, and completely dissolving with bath ratio of 1:18; obtaining the isatis root extract solution.
(2) Adding modifying substances
Sequentially adding mangosteen polyphenol and seabuckthorn flavone into the radix isatidis extract solution; stirring at 1900rpm for 35min; then heating the dissolution liquid to 93 ℃ and performing ultrasonic-assisted dispersion, wherein the ultrasonic frequency is 35KHz, and the dispersion time is 95s; after dispersion, the dissolution liquid is cooled to 30 ℃ to obtain the modified isatis root extract solution.
The adding amount of the mangosteen polyphenol is 2.9% of the isatis root extract solution;
the addition amount of the seabuckthorn flavone is 2.2% of the isatis root extract solution.
Step 3, preparing a functional modifier
Mixing a loading agent and modified isatis root extract solution according to a mass ratio of 1:9; then heating the mixture to 95 ℃ and stirring at 4300rad/min for 54min; then cooling to 62 ℃, and stirring for 25min at a speed of 2900 rad/min; then cooling to 30 ℃; distilling under reduced pressure for 45min to obtain the functional modifier.
The loading agent comprises the following raw material components in parts by weight: 4.5 parts of nano bentonite, 0.8 part of magnesium stearate and 9 parts of nano activated carbon; the loading agent comprises: 100% is sieved by a 8000 mesh sieve.
Step 4, preparing functional master batch
Mixing PP slice, functional modifier, antioxidant 1076, tert-butyl p-hydroxy anisole and polyoxyethylene ether, and oven drying at 122 deg.C for 24 hr; then adding the mixture into a double-screw extruder, controlling the melting temperature to 240 ℃, carrying out melt blending for 45min, mixing at a high speed with the screw rotating speed of 340 rpm, and carrying out extrusion granulation to obtain the functional master batch.
The mass ratio of the PP slice to the functional modifier to the antioxidant 1076 to the tert-butyl p-hydroxy anisole to the polyoxyethylene ether is 100:6.5:2:1.2:0.5.
the antibacterial rate of the isatis root modified PP master batch prepared in the embodiment to staphylococcus aureus is 98.23%, the antibacterial rate to escherichia coli is 99.25%, and the antibacterial rate to candida albicans is 99.2%; in particular to the inhibition rate of typhoid bacillus reaching 99.5 percent. The prepared isatis root modified PP master batch has the antifouling grade of 4 and the easy decontamination grade of 4. The prepared isatis root modified PP master batch has water absorption performance reaching 0.8 percent. The prepared isatis root modified PP master batch is stored for 5 years, the antibacterial rate of the isatis root modified PP master batch on staphylococcus aureus is 94.6%, the antibacterial rate on escherichia coli is 95.2%, the antibacterial rate on candida albicans is 94.7%, and the antibacterial rate on typhoid bacillus is 94.32%. The prepared isatis root modified PP master batch has the bacteriostasis rate of 94.89% on staphylococcus aureus, 95.85% on escherichia coli, 96.5% on candida albicans and 95.05% on typhoid bacillus after being washed for 150 times.
Example 3 preparation method of pollution-resistant Isatis root modified PP masterbatch
Step 1, pretreatment of radix isatidis extract
(1) Selecting radix Isatidis extract
Selected isatis root extract: 100% of the total bacterial count is sieved by a 800-mesh sieve, the content of active ingredients is 97.8-98.2%, the moisture is 5-6%, the total bacterial count is less than 100cfu/g, no salmonella and escherichia coli are detected, and the quality guarantee period is 24 months.
(2) High temperature treatment
Mixing radix Isatidis extract, and treating at 190 deg.C for 20s; the isatis root extract is led out after instantaneous high-temperature treatment and cooled to normal temperature for standby.
(3) Microwave treatment
Placing the heat-treated radix Isatidis extract in a microwave device, and treating for 150s under the condition of microwave frequency of 24 GH; guiding out after microwave treatment, and cooling the radix isatidis extract to 2 ℃ at a speed of 5 ℃/min; then keeping for 2 hours, and then naturally heating to 28 ℃ for standby.
Step 2, modification of the isatis root extract
(1) Dissolving
Adding the pretreated radix Isatidis extract into deionized water, stirring at 2000rpm for 20min, and dissolving completely with bath ratio of 1:20; obtaining the isatis root extract solution.
(2) Adding modifying substances
Sequentially adding mangosteen polyphenol and seabuckthorn flavone into the radix isatidis extract solution; stirring at 2000rpm for 40min; then heating the dissolution liquid to 90 ℃ and performing ultrasonic-assisted dispersion, wherein the ultrasonic frequency is 30KHz, and the dispersion time is 100s; after dispersion, the dissolution liquid is cooled to 35 ℃ to obtain the modified isatis root extract solution.
The adding amount of the mangosteen polyphenol is 3.1% of the isatis root extract solution;
the addition amount of the seabuckthorn flavone is 2.5% of the isatis root extract solution.
Step 3, preparing a functional modifier
Mixing the loading agent and the modified isatis root extract solution according to the mass ratio of 1:10; then heating the mixture to 100deg.C, stirring at 4500rad/min for 60min; then cooling to 64 ℃, and stirring for 30min at a speed of 3000 rad/min; then cooling to 35 ℃; and (5) distilling under reduced pressure for 50min to obtain the functional modifier.
The loading agent comprises the following raw material components in parts by weight: 5 parts of nanometer bentonite, 1 part of magnesium stearate and 10 parts of nanometer activated carbon; the loading agent comprises: 100% is sieved by a 8000 mesh sieve.
Step 4, preparing functional master batch
Mixing PP slice, functional modifier, antioxidant 1076, tert-butyl p-hydroxy anisole and polyoxyethylene ether, and oven drying at 125deg.C for 24 hr; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 250 ℃, carrying out melt blending for 50min, mixing at a high speed, extruding and granulating at a screw speed of 350 rpm, and obtaining the functional master batch.
The mass ratio of the PP slice to the functional modifier to the antioxidant 1076 to the tert-butyl p-hydroxy anisole to the polyoxyethylene ether is 100:6.8:2.5:1.3:0.6.
the antibacterial rate of the isatis root modified PP master batch prepared in the embodiment to staphylococcus aureus is 99.1%, the antibacterial rate to escherichia coli is 98.9%, and the antibacterial rate to candida albicans is 98.95%; in particular to the inhibition rate of typhoid bacillus reaching 99.3 percent. The prepared isatis root modified PP master batch has the antifouling grade of 4 and the easy decontamination grade of 4. The prepared isatis root modified PP master batch has water absorption performance reaching 0.7 percent. The prepared isatis root modified PP master batch is stored for 5 years, the antibacterial rate of the isatis root modified PP master batch on staphylococcus aureus is 94.2%, the antibacterial rate on escherichia coli is 94.9%, the antibacterial rate on candida albicans is 94.25%, and the antibacterial rate on typhoid bacillus is 93.8%. The prepared isatis root modified PP master batch has the bacteriostasis rate of 93.95 percent on staphylococcus aureus, 94.52 percent on escherichia coli, 95.9 percent on candida albicans and 94.8 percent on typhoid bacillus after being washed for 150 times.
The proportions described in the invention are mass proportions, and the percentages are mass percentages unless otherwise specified.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A preparation method of pollution-resistant isatis root modified PP master batch is characterized by comprising the following steps:
step 1, pretreatment of radix isatidis extract
(1) Selecting radix Isatidis extract
Selected isatis root extract: 100% of the total bacterial count is sieved by a 800-mesh sieve, the content of active ingredients is 97.8-98.2%, the moisture is 5-6%, the total bacterial count is less than 100cfu/g, no salmonella and escherichia coli are detected, and the quality guarantee period is 24 months;
(2) High temperature treatment
Mixing radix Isatidis extract, and treating at 180-190 deg.C for 15-20s; the isatis root extract is led out after instantaneous high-temperature treatment and cooled to normal temperature for standby;
(3) Microwave treatment
Placing the heat-treated radix Isatidis extract in a microwave device, and treating for 100-150s under the condition of microwave frequency of 20-24 GH; guiding out after microwave treatment, and cooling radix Isatidis extract to 0-2deg.C at a speed of 4-5deg.C/min; then keeping for 1-2h, and then naturally heating to 25-28 ℃ for standby;
step 2, modification of the isatis root extract
(1) Dissolving
Adding the pretreated radix Isatidis extract into deionized water, stirring at 1800-2000rpm for 15-20min, and completely dissolving at bath ratio of 1:15-20; obtaining a isatis root extract solution;
(2) Adding modifying substances
Sequentially adding mangosteen polyphenol and seabuckthorn flavone into the radix isatidis extract solution; stirring at 1800-2000rpm for 30-40min; then heating the solution to 90-95 ℃ and performing ultrasonic-assisted dispersion, wherein the ultrasonic frequency is 30-38KHz, and the dispersion time is 90-100s; cooling the solution to 25-35deg.C to obtain modified radix Isatidis extract solution;
the adding amount of the mangosteen polyphenol is 2.8-3.1% of the isatis root extract solution;
the addition amount of the seabuckthorn flavone is 1.9-2.5% of the isatis root extract solution;
step 3, preparing a functional modifier
Mixing the loading agent and the modified isatis root extract solution according to the mass ratio of 1:8-10; heating the mixed solution to 90-100deg.C, and stirring at 4000-4500rad/min for 50-60min; then cooling to 60-64 ℃, stirring for 20-30min at 2800-3000 rad/min; then cooling to 25-35 ℃; distilling under reduced pressure for 40-50min to obtain functional modifier;
the loading agent comprises the following raw material components in parts by weight: 4-5 parts of nano bentonite, 0.5-1 part of magnesium stearate and 7-10 parts of nano activated carbon; the loading agent comprises: 100% is sieved by a 8000 mesh sieve;
step 4, preparing functional master batch
Mixing PP slice, functional modifier, antioxidant 1076, tert-butyl p-hydroxy anisole and polyoxyethylene ether, and oven drying at 120-125deg.C for 24 hr; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 220-250 ℃, carrying out melt blending for 40-50min, mixing at a high speed with the screw rotating speed of 320-350 r/min, and carrying out extrusion granulation to obtain functional master batch;
the mass ratio of the PP slice to the functional modifier to the antioxidant 1076 to the tert-butyl p-hydroxy anisole to the polyoxyethylene ether is 100:6-6.8:1.5-2.5:1.1-1.3:0.5-0.6.
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