CN111040427A - Preparation method of plant extract modified PU (polyurethane) pipe - Google Patents
Preparation method of plant extract modified PU (polyurethane) pipe Download PDFInfo
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Abstract
The invention provides a preparation method of a plant extract modified PU pipe, wherein the content of the plant extract in the PU pipe is 0.1-5%, the preparation method comprises the steps of preparation of plant fat-soluble extract, preparation of a diatomite composite porous material, blending, plastication, mixing and extrusion molding, and the PU pipe comprises the following raw materials in parts by weight: 55-70 parts of thermoplastic polyurethane, 20-25 parts of linear low-density polyethylene, 0.5-3 parts of plant fat-soluble extract, 6-8 parts of diatomite composite porous material, 2 parts of castor oil, 3-5 parts of lauric acid diethanol amine and 4-6 parts of promoter 2, 2-bis (4-hydroxyphenyl) propane.
Description
Technical Field
The invention belongs to the technical field of plastic modification, and particularly relates to a preparation method of a plant extract modified PU pipe.
Background
With the development of industry, the living standard of people is gradually improved, the district heating is gradually popularized throughout the country, and a heating pipeline is a necessary condition for ensuring effective heating. Due to the limitation of special application conditions, the limitation of some pipe materials can cause that the pipe materials can not meet the requirement of heat supply, for example, the inner wall of a steel pipe is difficult to polish, has high rust prevention difficulty and is easy to corrode, and leakage and damage are generated; pure plastic pipes often fail to meet the requirements in terms of high temperature and compressive strength and impact resistance. Polyurethane (PU) has been widely used in the coating, adhesive, leather, textile and construction industries due to its unique excellent characteristics, and has excellent wear resistance, chemical corrosion resistance, high temperature resistance, etc., thus having wide development prospects.
The invention patent CN102838867B discloses a polyurethane and polyethylene nano modified material, which comprises 100 parts of polyurethane, 30-60 parts of polyethylene, and substances such as functional modifier, nano material and plasticizer, wherein the elongation at break of the prepared polyurethane modified material is 520-595%, but the tensile strength is only 7.9-8.2MPa, and the material has good toughness but insufficient strength, and has limited pressure resistance when being used as a heating pipeline.
In addition, the polyurethane pipeline product is easy to be catalyzed and hydrolyzed by fungi and aged under certain temperature and humidity conditions, and the phenomena of discoloration and odor, material fracture, yellowing of light-colored products and the like are generated, and the addition of the common inorganic nano silver ion antibacterial agent and the common organic vanillin antibacterial agent can cause high-temperature carbonization in the plastic product molding process, influence the toughness of the material and reduce the impact resistance of the material.
Disclosure of Invention
In order to solve the problems in the prior art and further optimize the prior art, the invention provides a preparation method of a plant extract modified PU pipe, which aims to realize the following purposes:
1. improving the tensile strength of the material
2. Improve the shock resistance of the material
3. Increase the pressure resistance
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a plant extract modified PU pipe is characterized in that the content of plant extract in the PU pipe is 0.1-5%;
the plant extract is one or more of folium Artemisiae Argyi extract, herba Pileae Scriptae extract, lavender extract, rhizoma et radix Valerianae extract, and Sargassum extract, or one or more of salicylic acid, emodin, menthol, menthone, hyperoside, linalool, caffeic acid, and calcium alginate;
the plant extracts are not limited to the above-listed kinds of plant extracts;
the preparation method of the plant extract modified PU pipe is characterized by comprising the steps of preparing a plant fat-soluble extract, preparing a diatomite composite porous material, batching, plasticating, mixing and extruding for molding;
the plant extracts are not limited to the above-listed kinds of plant extracts;
the preparation of the plant fat-soluble extract comprises extraction, column chromatography separation and recrystallization;
extracting, wherein the extracting solution is ethanol water with volume fraction of 75-78%; the mass ratio of the polyglutamic acid to the polyethylene glycol is 2-6: 1; the total dosage of polyglutamic acid and polyethylene glycol is 2.6-5wt% of ethanol water solution, wherein the molecular weight of the polyglutamic acid is 20000-50000 Da; polyethylene glycol with the molecular weight of 1350-;
performing column chromatography separation, wherein the volume ratio of the ethyl acetate to the methanol is 4-6: 1;
the recrystallization comprises the steps of dissolving the raw materials by absolute ethyl alcohol, heating the raw materials to 60 ℃, putting the raw materials into a refrigerator at the temperature of minus 20 ℃ for recrystallization, and standing for 20 to 24 hours;
the preparation method of the diatomite composite porous material is characterized by comprising the steps of dilatation treatment, ball milling, aging and sintering;
the capacity expansion treatment is to add concentrated sulfuric acid solution into the diatomite and stir the diatomite for 2 to 3 hours in a water bath kettle at the temperature of between 90 and 95 ℃;
and in the ball milling, the mass ratio of the alumina to the sodium metaaluminate to the diatomite is 2-5: 4-5: 16-20;
the aging is carried out, wherein the adding amount of the binder PEG-200 accounts for 1.8-4.5% of the total amount of the mixture, the aging time is 8-9h, the environmental temperature is 40 ℃, and the humidity is 82-85%;
sintering at 1050 ℃ for 2-3 h;
the ingredients comprise the following components in parts by weight: 55-70 parts of thermoplastic polyurethane, 20-25 parts of linear low-density polyethylene, 0.5-3 parts of plant fat-soluble extract, 6-8 parts of diatomite composite porous material, 2-4 parts of castor oil, 3-5 parts of lauric acid diethanol amine and 4-6 parts of accelerator 2, 2-bis (4-hydroxyphenyl) propane;
the thermoplastic polyurethane is a linear block copolymer composed of 2-4' -diphenylmethane diisocyanate and polyether glycol, the melting point is 100-105 ℃, and the Shore hardness is 60-90D;
the linear low-density polyethylene has a melt index of 2-4g/10min and a density of 0.91-0.92g/cm3;
The diatomite composite porous material has the average granularity of 40-70 meshes;
plasticating, wherein the temperature during plasticating is 160-170 ℃, the time is 150-180S, and the pressure is 0.60 MPa;
the mixing is carried out at the temperature of 150-;
the extrusion molding and the processing technology temperature of each area of the double-screw extruder are respectively as follows: the first zone is 125-140 ℃, the second zone is 140-150 ℃, the third zone is 150-160 ℃, the fourth zone is 160-170 ℃, the fifth zone is 165-160 ℃, the pressure is 15MPa, and the rotation speed of the twin screw is 28-30 rpm.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the plant extract modified PU pipe is prepared by the methodThe PU pipe has high mechanical strength, the tensile strength is 48-55MPa, the tensile elastic modulus is 1900-1950MPa, the bending elastic modulus is 2.2-2.4GPa, and the notch impact strength is 38.6-40.2KJ/m2;
2. The PU pipe prepared by the preparation method of the plant extract modified PU pipe has better toughness,
according to the detection standard of GB/T15560-1995, the phenomena of cracking, expansion and the like do not occur at 40 ℃ under 8.4MPa and under the pressure of 8 hours, the pressure-bearing capacity is good, and the water pressure resistance is good;
3. the PU pipe prepared by the preparation method of the plant extract modified PU pipe has a certain antibacterial effect, can reduce the attachment of bacteria, and has an antibacterial rate of 85-87% on the bacteria such as staphylococcus aureus, escherichia coli, candida albicans and the like which are susceptible to human body;
4. by adopting the preparation method of the plant extract modified PU pipe, the heat preservation effect of the PU pipe is good, and according to the test standard of GB/T3399, the heat conductivity coefficient of the PU pipe is 0.020-0.025W/M.K, so that the loss of energy is reduced;
5. by adopting the preparation method of the plant extract modified PU pipe, according to the detection standard of GBT11546.1, under the stress of 50MPa, the creep rate of the material after 120h is 0.30-0.42%, and the mechanical recovery performance is excellent;
the specific implementation mode is as follows:
the invention is further illustrated below with reference to specific examples.
Example 1 preparation method of plant extract modified PU pipe
A preparation method of a wormwood extract modified PU pipe comprises the following steps:
1. preparing a wormwood fat-soluble extract:
1) extraction:
air drying folium Artemisiae Argyi, pulverizing to 50 mesh, weighing quantitative folium Artemisiae Argyi powder, adding 20 times of 78% ethanol water solution, dissolving, simultaneously adding polyglutamic acid and polyethylene glycol, extracting in Soxhlet extractor for 100min each time, repeating the extraction for three times, mixing the three extractive solutions, evaporating to remove ethanol, and concentrating to obtain folium Artemisiae Argyi crude extract;
the mass ratio of the polyglutamic acid to the polyethylene glycol is 2: 1; the total amount of the polyglutamic acid is 2.6wt% of ethanol aqueous solution, wherein the molecular weight of the polyglutamic acid is 25000 Da; polyethylene glycol with molecular weight of 1350 and hydroxyl value of 60 mgKOH/g;
2) separating by column chromatography
Separating and refining folium Artemisiae Argyi crude extract with silica gel column, eluting with mixed solution of ethyl acetate and methanol, collecting eluate, and rotary evaporating to obtain crude crystal;
the mixing volume ratio of the ethyl acetate to the methanol is 4: 1;
3) recrystallization
Dissolving the crude crystal with anhydrous ethanol, heating to 60 deg.C under stirring, placing into-20 deg.C refrigerator for recrystallization after dissolving completely, vacuum filtering for 20 hr to obtain refined folium Artemisiae Argyi extract, and drying to obtain the final product;
the folium Artemisiae Argyi extract contains quercetin 0.5-2.0% and salicylic acid 11-12.5%;
2. preparing a diatomite composite porous material:
1) capacity expansion process
Adding concentrated sulfuric acid solution into diatomite, stirring in a water bath kettle at 95 ℃ for 2h, then performing suction filtration, and washing with water until the pH of the filtrate is close to neutral;
2) ball mill
Mixing and batching alumina, sodium metaaluminate and diatomite according to a proportion, adding the mixture into a ball mill, mixing and grinding at the rotating speed of 800r/min for 1.5 hours;
the mass ratio of the alumina to the sodium metaaluminate to the diatomite is 2: 4: 16;
3) aging of the mixture
Adding a binder PEG-200, mixing, and performing extrusion molding to prepare solid particles; aging the solid particles in a damp and hot environment for 8h, wherein the environment temperature is 40 ℃ and the humidity is 82%;
the adding amount of the PEG-200 accounts for 1.8 percent of the total amount of the mixture;
4) and (3) sintering:
sintering the solid particles in a box-type electric furnace at 1050 ℃ for 2h, cooling with the furnace to obtain the diatomite composite porous material,
the diatomite composite porous material has the average granularity of 40 meshes;
3. ingredients
The plant functional PU plastic product is prepared from the following raw materials in parts by weight:
55 parts of thermoplastic polyurethane, 20 parts of linear low-density polyethylene, 0.5 part of wormwood fat-soluble extract, 6 parts of diatomite composite porous material, 2 parts of castor oil, 3 parts of lauric acid diethanol amine, 4 parts of accelerant 2, 2-bis (4-hydroxyphenyl) propane,
the thermoplastic polyurethane is a linear block copolymer consisting of 2-4' -diphenylmethane diisocyanate and polyether glycol, the melting point is 100 ℃, and the Shore hardness is 60D;
the linear low-density polyethylene has a melt index of 2g/10min and a density of 0.91g/cm3;
4. Plastication
Firstly, feeding thermoplastic polyurethane and polyethylene into a drying room for drying glue, drying until the water content is less than 2%, and then plasticating the thermoplastic polyurethane and the polyethylene at the temperature of 160 ℃, the time of 180S and the pressure of 0.60 MPa;
5. mixing the raw materials
After plastication, adding the rest of wormwood fat-soluble extract, diatomite composite porous material, castor oil, lauric acid diethanol amine and accelerator 2, 2-bis (4-hydroxyphenyl) propane, and feeding into an internal mixer for further mixing at 160 ℃, for 10min, with the top plug pressure of 0.6MPa and the rotor rotation speed of 50 r/min;
6. extrusion molding
After mixing by an internal mixer, the plastic can be introduced into a double-screw extruder, and is subjected to melt shearing, mixing, homogenization and extrusion molding to prepare the plant functional PU plastic product, wherein the processing process temperature of each area of the double-screw extruder is respectively as follows: the first zone is 125-140 ℃, the second zone is 140-150 ℃, the third zone is 150-160 ℃, the fourth zone is 160-170 ℃, the fifth zone is 165-160 ℃, the pressure is 15MPa, and the rotation speed of the twin screw is 28 rpm.
Embodiment 2 preparation method of plant extract modified PU (polyurethane) pipe
A preparation method of a sarcandra glabra extract modified PU pipe comprises the following steps:
1. preparing the sarcandra glabra fat-soluble extract:
1) extraction:
air drying herba Pileae Scriptae, pulverizing to 60 mesh, weighing quantitative herba Pileae Scriptae powder, adding 25 times of 78% ethanol water solution, dissolving, adding polyglutamic acid and polyethylene glycol, extracting in a Soxhlet extractor for 60min each time, repeating the extraction for three times, mixing the extractive solutions, evaporating to remove ethanol, and concentrating to obtain herba Pileae Scriptae crude extract;
the mass ratio of the polyglutamic acid to the polyethylene glycol is 5: 1; the total amount is 5wt% of ethanol water solution, wherein the molecular weight of polyglutamic acid is 38000 Da; polyethylene glycol with molecular weight of 1550 and hydroxyl value of 73 mgKOH/g;
2) separating by column chromatography
Separating and refining the coarse sarcandra glabra extract by using a silica gel column, eluting with a mixed solution of ethyl acetate and methanol, collecting eluent, and evaporating to dryness to obtain a coarse crystal;
the mixing volume ratio of the ethyl acetate to the methanol is 5: 1;
3) recrystallization
Dissolving the coarse crystal with anhydrous ethanol, heating to 60 deg.C under stirring, recrystallizing in-20 deg.C refrigerator after dissolving completely, filtering under reduced pressure for 20 hr to obtain refined herba Pileae Scriptae extract, and drying to obtain the final product;
the sarcandra glabra extract contains 5-9% of fiber and 0.5-2.0% of hyperoside;
2. preparing a diatomite composite porous material:
1) capacity expansion process
Adding concentrated sulfuric acid solution into diatomite, stirring in a water bath kettle at 95 ℃ for 2h, then performing suction filtration, and washing with water until the pH of the filtrate is close to neutral;
2) ball mill
Mixing and batching alumina, sodium metaaluminate and diatomite according to a proportion, adding the mixture into a ball mill, mixing and grinding at the rotating speed of 800r/min for 1.5 hours;
the mass ratio of the alumina to the sodium metaaluminate to the diatomite is 4: 5: 16;
3) aging of the mixture
Adding a binder PEG-200, mixing, and performing extrusion molding to prepare solid particles; aging the solid particles in a damp and hot environment for 9h, wherein the environment temperature is 40 ℃ and the humidity is 82%;
the adding amount of the PEG-200 accounts for 3.0 percent of the total amount of the mixture;
4) and (3) sintering:
sintering the solid particles in a box-type electric furnace at 1050 ℃ for 3h, and cooling along with the furnace to obtain the diatomite composite porous material;
the diatomite composite porous material has the average granularity of 50 meshes;
3. ingredients
The plant functional PU plastic product is prepared from the following raw materials in parts by weight:
60 parts of thermoplastic polyurethane, 25 parts of linear low-density polyethylene, 2 parts of sarcandra glabra fat-soluble extract, 6 parts of diatomite composite porous material, 3 parts of castor oil, 4 parts of lauric acid diethanol amine, 4 parts of accelerator 2, 2-bis (4-hydroxyphenyl) propane,
the thermoplastic polyurethane is a linear block copolymer consisting of 2-4' -diphenylmethane diisocyanate and polyether glycol, the melting point is 105 ℃, and the Shore hardness is 80D;
the linear low-density polyethylene has a melt index of 3.3g/10min and a density of 0.91g/cm3;
4. Plastication
Firstly, feeding thermoplastic polyurethane and polyethylene into a drying room for drying glue, drying until the water content is less than 2%, and then plasticating the thermoplastic polyurethane and the polyethylene at the temperature of 170 ℃, the time of 16S and the pressure of 0.60 MPa;
5. mixing the raw materials
After plastication is finished, adding the rest sarcandra glabra fat-soluble extract, the diatomite composite porous material, the castor oil, the lauric acid diethanol amine and the accelerator 2, 2-bis (4-hydroxyphenyl) propane, and feeding the mixture into an internal mixer for further mixing, wherein the mixing temperature is 150 ℃, the mixing time is 15min, the top plug pressure is 0.65MPa, and the rotor rotation speed is 60 r/min;
6. extrusion molding
After mixing by an internal mixer, the plastic can be introduced into a double-screw extruder, and is subjected to melt shearing, mixing, homogenization and extrusion molding to prepare the plant functional PU plastic product, wherein the processing process temperature of each area of the double-screw extruder is respectively as follows: the first zone is 125-140 ℃, the second zone is 140-150 ℃, the third zone is 150-160 ℃, the fourth zone is 160-170 ℃, the fifth zone is 165-160 ℃, the pressure is 15MPa, and the rotation speed of the twin screw is 28-30 rpm.
Embodiment 3 preparation method of plant extract modified PU pipe
The preparation method of the mint extract modified PU pipe comprises the following steps:
1. preparation of a mint fat-soluble extract:
1) extraction:
air drying herba Menthae, pulverizing to 60 mesh, weighing a certain amount of herba Menthae powder, adding 30 times of 75% ethanol water solution, dissolving, simultaneously adding polyglutamic acid and polyethylene glycol, extracting in Soxhlet extractor for 60min each time, repeating the extraction for three times, mixing the three extractive solutions, evaporating to remove ethanol, and concentrating to obtain herba Menthae crude extract;
the mass ratio of the polyglutamic acid to the polyethylene glycol is 6: 1; the total amount of the polyglutamic acid is 5wt% of ethanol aqueous solution, wherein the molecular weight of the polyglutamic acid is 50000 Da; polyethylene glycol with molecular weight of 1650 and hydroxyl value of 83 mgKOH/g;
2) separating by column chromatography
Separating and refining the crude extract of herba Menthae with silica gel column by chromatography, eluting with mixed solution of ethyl acetate and methanol, collecting eluate, and rotary evaporating to obtain crude crystal;
the mixing volume ratio of the ethyl acetate to the methanol is 6: 1;
3) recrystallization
Dissolving the crude crystal with anhydrous ethanol, heating to 60 deg.C under stirring, recrystallizing in-20 deg.C refrigerator after dissolving completely, filtering under reduced pressure for 20 hr to obtain refined herba Menthae extract, and drying to obtain the final product;
the content of emodin in the mint extract is 4.5-5.0%, and the content of menthol is 22-25%;
2. preparing a diatomite composite porous material:
1) capacity expansion process
Adding concentrated sulfuric acid solution into diatomite, stirring in a water bath kettle at 90 ℃ for 3h, then performing suction filtration, and washing with water until the pH of the filtrate is close to neutral;
2) ball mill
Mixing and batching alumina, sodium metaaluminate and diatomite according to a proportion, adding the mixture into a ball mill, mixing and grinding at the rotating speed of 800r/min for 2 hours;
the mass ratio of the alumina to the sodium metaaluminate to the diatomite is 5: 5: 20;
3) aging of the mixture
Adding a binder PEG-200, mixing, and performing extrusion molding to prepare solid particles; aging the solid particles in a damp and hot environment for 9h, wherein the environment temperature is 40 ℃ and the humidity is 85%;
the adding amount of the PEG-200 accounts for 4.5 percent of the total amount of the mixture;
4) and (3) sintering:
sintering the solid particles in a box-type electric furnace at 1050 ℃ for 3h, and cooling along with the furnace to obtain the diatomite composite porous material;
the diatomite composite porous material has the average granularity of 70 meshes;
3. ingredients
The plant functional PU plastic product is prepared from the following raw materials in parts by weight:
70 parts of thermoplastic polyurethane, 25 parts of linear low-density polyethylene, 3 parts of mint fat-soluble extract, 8 parts of diatomite composite porous material, 4 parts of castor oil, 5 parts of lauric acid diethanol amine, 6 parts of accelerator 2, 2-bis (4-hydroxyphenyl) propane,
the thermoplastic polyurethane is a linear block copolymer consisting of 2-4' -diphenylmethane diisocyanate and polyether glycol, the melting point is 105 ℃, and the Shore hardness is 90D;
the linear low-density polyethylene has a melt index of 4g/10min and a density of 0.92g/cm3;
4. Plastication
Firstly, feeding thermoplastic polyurethane and polyethylene into a drying room for drying glue, drying until the water content is less than 2%, and then plasticating the thermoplastic polyurethane and the polyethylene at the temperature of 170 ℃, the time of 150S and the pressure of 0.60 MPa;
5. mixing the raw materials
After plastication, adding the rest of mint fat-soluble extract, diatomite composite porous material, castor oil, lauric acid diethanol amine and an accelerant 2, 2-bis (4-hydroxyphenyl) propane, and sending into an internal mixer for further mixing, wherein the mixing temperature is 150 ℃, the mixing time is 10min, the top plug pressure is 0.55MPa, and the rotor rotation speed is 60 r/min;
6. extrusion molding
After mixing by an internal mixer, the plastic can be introduced into a double-screw extruder, and is subjected to melt shearing, mixing, homogenization and extrusion molding to prepare the plant functional PU plastic product, wherein the processing process temperature of each area of the double-screw extruder is respectively as follows: the first zone is 125-140 ℃, the second zone is 140-150 ℃, the third zone is 150-160 ℃, the fourth zone is 160-170 ℃, the fifth zone is 165-160 ℃, the pressure is 15MPa, and the rotation speed of the twin screw is 28-30 rpm.
The performance indexes of the plant extract modified PU pipe prepared by the technical schemes of the above examples 1-3 are shown in the following table:
the above examples are only preferred examples and are not limited to the above listed kinds of plant extracts.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the plant extract modified PU pipe is characterized in that the content of the plant extract in the PU pipe is 0.1-5%.
2. The method according to claim 1, wherein the plant extract is one or more of an artemisia argyi extract, an sarcandra glabra extract, a lavender extract, a valerian extract and a seaweed extract, or one or more of salicylic acid, emodin, menthol, menthone, hyperoside, linalool, caffeic acid and calcium alginate.
3. The preparation method of the plant extract modified PU pipe material according to claim 1, wherein the preparation method comprises the steps of preparation of plant fat-soluble extract, preparation of diatomite composite porous material, blending, plastication, mixing and extrusion molding;
the ingredients comprise the following components in parts by weight: 55-70 parts of thermoplastic polyurethane, 20-25 parts of linear low-density polyethylene, 0.5-3 parts of plant fat-soluble extract, 6-8 parts of diatomite composite porous material, 2-4 parts of castor oil, 3-5 parts of lauric acid diethanol amine and 4-6 parts of accelerator 2, 2-bis (4-hydroxyphenyl) propane.
4. The preparation method according to claim 3, wherein the formulation is characterized in that the thermoplastic polyurethane is a linear block copolymer composed of 2-4' -diphenylmethane diisocyanate and polyether glycol, the melting point is 100-105 ℃, and the Shore hardness is 60-90D; the diatomite composite porous material has the average granularity of 40-70 meshes.
5. The preparation method according to claim 3, wherein the preparation of the diatomite composite porous material comprises expansion treatment, ball milling, aging and sintering; the capacity expansion treatment is to add concentrated sulfuric acid solution into the diatomite and stir the diatomite for 2 to 3 hours in a water bath kettle at the temperature of between 90 and 95 ℃.
6. The preparation method of claim 5, wherein the ball mill is prepared from alumina, sodium metaaluminate and diatomite in a mass ratio of 2-5: 4-5: 16-20; the aging is carried out, wherein the adding amount of the binder PEG-200 accounts for 1.8-4.5% of the total amount of the mixture, the aging time is 8-9h, the environmental temperature is 40 ℃, and the humidity is 82-85%; and sintering at 1050 ℃ for 2-3 h.
7. The preparation method of claim 3, wherein the preparation of the plant liposoluble extract comprises extraction, column chromatography separation and recrystallization; extracting, wherein the extracting solution is ethanol water with volume fraction of 75-78%; the mass ratio of the polyglutamic acid to the polyethylene glycol is 2-6: 1; the total dosage of polyglutamic acid and polyethylene glycol is 2.6-5wt% of ethanol water solution, wherein the molecular weight of the polyglutamic acid is 20000-50000 Da; polyethylene glycol with molecular weight of 1350-1650 and hydroxyl value of 60-83 mgKOH/g.
8. The preparation method of claim 7, wherein the column chromatography separation is carried out, and the mixing volume ratio of ethyl acetate to methanol is 4-6: 1; and (3) dissolving the crystals by using absolute ethyl alcohol, heating the crystals to 60 ℃, putting the crystals into a refrigerator at the temperature of-20 ℃ for recrystallization, and standing the crystals for 20-24 hours.
9. The preparation method as claimed in claim 3, wherein the plastication and plastication are carried out at a temperature of 160-170 ℃, a time of 150-180S and a pressure of 0.60 MPa.
10. The preparation method according to claim 3, wherein the mixing temperature is 150-.
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CN113563714A (en) * | 2021-07-24 | 2021-10-29 | 浙江天源网业有限公司 | Nano silver carbon antibacterial anti-mite honeycomb net material and preparation method thereof |
CN115449284A (en) * | 2022-10-10 | 2022-12-09 | 四川大学 | Preparation method of antibacterial and mildewproof leather finishing agent containing plant source-based functional factors |
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