CN111690237A - Flame-retardant radix isatidis PET master batch and preparation method thereof - Google Patents
Flame-retardant radix isatidis PET master batch and preparation method thereof Download PDFInfo
- Publication number
- CN111690237A CN111690237A CN202010612236.6A CN202010612236A CN111690237A CN 111690237 A CN111690237 A CN 111690237A CN 202010612236 A CN202010612236 A CN 202010612236A CN 111690237 A CN111690237 A CN 111690237A
- Authority
- CN
- China
- Prior art keywords
- radix isatidis
- preparation
- steps
- flame
- retardant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0058—Biocides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a preparation method of flame-retardant radix isatidis PET master batches, which comprises the steps of preparing radix isatidis extract, preparing modified radix isatidis extract, loading modified substances and preparing radix isatidis PET master batches; the modified substance is loaded: comprises the steps of preparing a loading agent, mixing with a modified substance, carrying out heat treatment and carrying out reduced pressure distillation; the preparation of the load carrier comprises the following steps: the adopted raw materials comprise diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate. The flame-retardant radix isatidis PET master batch prepared by the invention has the advantages of good loading effect of the radix isatidis extract, good antibacterial effect, flame retardance and washing resistance.
Description
Technical Field
The invention belongs to the technical field of fiber manufacturing, and particularly relates to a flame-retardant radix isatidis PET master batch and a preparation method thereof.
Background
PET is synthetic fiber, which is fiber made by using Pure Terephthalic Acid (PTA) or dimethyl terephthalate (DMT) and Ethylene Glycol (EG) as raw materials and through esterification or ester exchange and polycondensation reaction to prepare fiber-forming high polymer, namely polyethylene terephthalate (PET), and spinning and post-treatment. PET is widely applied to various aspects such as clothes, decoration, household textiles, industrial textiles, national defense, industrial engineering and the like. The polyester fiber can be spun and woven purely, can be blended and interwoven with natural fibers such as cotton, wool, silk, hemp and the like and other chemical fibers, and can be used for processing wool-like, cotton-like, silk-like and hemp-like fabrics with various colors, easy washing and drying, no-iron and other ideal performances.
In recent years, researches on antibacterial property of PET master batch are gradually increasing at home and abroad.
Isatis root, commonly known as indigo root, isatis root, is the dried root of Isatis tinctoria of Brassicaceae, usually harvested in autumn and processed before use as medicine. Produced in all parts of China. The radix Isatidis is divided into north radix Isatidis and south radix Isatidis, the north radix Isatidis is derived from root of Isatis tinctoria L of Brassicaceae, and the south radix Isatidis is rhizome and root of Baphicacanthus cusia (Nees) Brem of Acanthaceae. It is cold in nature, slightly sweet in taste and bitter in flavor, and has effects of clearing away heat and toxic materials, preventing common cold, and relieving sore throat. Is mainly used for treating diseases such as warm toxicity and macula, crimson and dark tongue, throat ulcer and erysipelas.
Patent CN201310361459.X discloses a PET flame-retardant film master batch, a preparation method thereof and a PET flame-retardant film product, wherein the PET flame-retardant film master batch comprises decabromodiphenylethane, antimony trioxide, bisphenol A bis, 1010 antioxidant, 168 antioxidant, diffusion oil, zinc borate and PBT; also discloses a preparation method of the PET flame-retardant film master batch and a PET flame-retardant film product. The PET flame-retardant film product prepared by the PET flame-retardant film master batch has the advantages of good toughness, high tensile strength, good flame-retardant effect, low cost, simple preparation process, easiness in implementation and contribution to wide popularization and application. Although the technology has a good flame retardant effect, the adopted flame retardant components affect the loading of the effective substances of the radix isatidis, and the technology cannot be used in the process of modifying the radix isatidis by using the PET master batch.
For the technology of modifying the PET master batch by adopting the isatis root, the research of technicians in the field is less, and a plurality of technical problems exist at present; the PET master batch in the prior art has the problems of poor functionality, poor antibacterial effect, poor flame retardant property, easy elution of modified effective substances and the like.
Disclosure of Invention
In order to solve the problems in the prior art and further optimize the prior art, the invention provides the flame-retardant radix isatidis PET master batch and the preparation method thereof, so as to realize the following purposes:
the antibacterial performance, the water washing resistance and the storage resistance of the isatis root modified PET master batch are improved; improve the flame retardant property of the master batch.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of flame-retardant radix isatidis PET master batches comprises the following steps:
(1) preparation of extract of radix Isatidis
Extracting with dried root of Isatis tinctoria to obtain radix Isatidis extract;
100 percent of the isatis root extract is sieved by a 800-mesh sieve, the content of active ingredients is 97.8 to 98.2 percent, the water content is 5 to 6 percent, the total number of bacterial colonies is less than 100cfu/g, salmonella and escherichia coli can not be detected, and the quality guarantee period is 24 months.
(2) Preparation of modified radix Isatidis extract
Mixing radix Isatidis extract with mangosteen polyphenol and xylitol at a mass ratio of 75:2-3:1-1.8 to obtain mixed modified substance, and dissolving the mixed modified substance with deionized water at a bath ratio of 1: 25-28; then, heating the solution to 64-65 deg.C for 15-18 min. Distilling the heated mixed solution under reduced pressure for 1-1.5h to obtain modified radix Isatidis extract.
(3) Modified substance loading
Mixing diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate to obtain the load carrier. Mixing the carrier agent and the modified isatis root extract according to the mass ratio of 8-9: 1-2; then dissolving the mixture in deionized water, heating to 80-85 ℃, and stirring at 1800-2000rad/min for 35-40 min; then heating to 98-100 ℃, and stirring for 35-40min at the speed of 2500-; then cooling to normal temperature; distilling under reduced pressure to remove water to obtain the modifier.
The mixing mass ratio of the diatomite, the superfine bamboo charcoal powder, the zinc stearate and the di-sec-octyl maleate sodium sulfonate is 4-4.5: 25-28: 0.3-0.5: 0.3-0.5.
(4) Preparation of isatis root PET master batch
Mixing PET slices, aspartic acid, polyoxyethylene ether and acrylic resin, uniformly stirring, sequentially adding a modifier and a flame retardant, and drying for 24 hours at the temperature of 120-; then adding the mixture into a double-screw extruder, controlling the melting temperature at 275 ℃ and 280 ℃, and carrying out melt blending for 30-40 min; the rotating speed of the screw is 260-270 r/min, high-speed mixing and extrusion granulation are carried out, and functional master batches are obtained; namely the radix isatidis PET master batch.
The mass ratio of the PET slices to the aspartic acid to the polyoxyethylene ether to the acrylic resin is 100:5-6:3-7: 11-12;
the addition amount of the modifier is 5.8-6.5% of the mass of the PET slice;
the addition amount of the flame retardant is 4.5-5.1% of the mass of the PET slice;
the flame retardant consists of magnesium aluminum silicate, silicon dioxide, zinc borate and pentaerythritol ester in a mass ratio of 18-20:11-12.5:3-5: 0.8-1.3.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the flame-retardant radix isatidis PET master batch prepared by the invention has a good antibacterial effect; the bacteriostatic rate to typhoid bacillus and staphylococcus aureus is above 94%; the bacteriostasis rate to colibacillus and candida albicans is over 98 percent.
2. The flame-retardant radix isatidis PET master batch prepared by the invention has high radix isatidis extract solid carrying degree and good washing resistance effect; after washing for 150 times, the bacteriostasis rate still reaches over 90 percent. The prepared flame-retardant radix isatidis PET master batch has a good storage-resistant effect; after the food is stored for 3 years, the bacteriostatic rate of the food on typhoid bacillus, staphylococcus aureus, escherichia coli and candida albicans can still reach more than 91%.
3. The flame-retardant radix isatidis PET master batch prepared by the invention has a good flame-retardant effect, and can reach V0 level.
Detailed Description
The invention is further illustrated below with reference to specific examples.
Example 1 preparation method of flame-retardant radix isatidis PET master batch
The method comprises the following steps:
(1) preparation of extract of radix Isatidis
Extracting with dried root of Isatis tinctoria to obtain radix Isatidis extract;
100 percent of the isatis root extract is sieved by a 800-mesh sieve, the content of active ingredients is 97.8 to 98.2 percent, the water content is 5 to 6 percent, the total number of bacterial colonies is less than 100cfu/g, salmonella and escherichia coli can not be detected, and the quality guarantee period is 24 months.
(2) Preparation of modified radix Isatidis extract
Mixing the isatis root extract, mangosteen polyphenol and xylitol according to the mass ratio of 75: 3:1 to obtain a mixed modified substance, and dissolving the mixed modified substance by using deionized water at the bath ratio of 1: 25; then, the solution was heated to 65 ℃ for 18 min. And distilling the heated mixed solution under reduced pressure for 1.5h to obtain the modified isatis root extract.
(3) Modified substance loading
Mixing diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate to obtain the load carrier. Mixing the carrier agent and the modified isatis root extract according to the mass ratio of 9: 2; then dissolving the mixture in deionized water, heating to 80 ℃, and stirring at 1800rad/min for 35 min; then heating to 98 ℃, and stirring for 35min at the speed of 2500 rad/min; then cooling to normal temperature; distilling under reduced pressure to remove water to obtain the modifier.
The mixing mass ratio of the diatomite, the superfine bamboo charcoal powder, the zinc stearate and the di-sec-octyl maleate sodium sulfonate is 4: 25: 0.3: 0.3.
(4) preparation of isatis root PET master batch
Mixing PET slices, aspartic acid, polyoxyethylene ether and acrylic resin, uniformly stirring, then sequentially adding a modifier and a flame retardant, and drying for 24 hours at 124 ℃; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 275 ℃, and carrying out melt blending for 30 min; the rotating speed of the screw is 260 r/min, high-speed mixing, extruding and granulating are carried out, and functional master batches are obtained; namely the radix isatidis PET master batch.
The mass ratio of the PET slices to the aspartic acid to the polyoxyethylene ether to the acrylic resin is 100:5:3: 11;
the addition amount of the modifier is 5.8 percent of the mass of the PET slice;
the addition amount of the flame retardant is 4.5 percent of the mass of the PET slices;
the flame retardant consists of magnesium aluminum silicate, silicon dioxide, zinc borate and pentaerythritol ester in a mass ratio of 18:11:3: 0.8.
The flame-retardant isatis root PET master batch prepared by the embodiment has the bacteriostasis rate of 95.08% on typhoid bacillus and 96.52% on staphylococcus aureus; the bacteriostasis rate to colibacillus is 98.5 percent, and the bacteriostasis rate to candida albicans is 98.9 percent. After the prepared flame-retardant isatis root PET master batch is washed for 150 times, the bacteriostasis rate to typhoid bacillus is 90.2 percent, and the bacteriostasis rate to staphylococcus aureus is 91.05 percent; the bacteriostasis rate to colibacillus is 90.88 percent, and the bacteriostasis rate to candida albicans is 92.01 percent. The prepared flame-retardant radix isatidis PET master batch is stored for 3 years, the bacteriostasis rate to typhoid bacillus is 92.53%, and the bacteriostasis rate to staphylococcus aureus is 93.45%; the bacteriostasis rate to escherichia coli is 92.46%, and the bacteriostasis rate to candida albicans is 93.5%. The prepared flame-retardant radix isatidis PET master batch is V0 grade.
Embodiment 2 preparation method of flame-retardant radix isatidis PET master batch
The method comprises the following steps:
(1) preparation of extract of radix Isatidis
Extracting with dried root of Isatis tinctoria to obtain radix Isatidis extract;
100 percent of the isatis root extract is sieved by a 800-mesh sieve, the content of active ingredients is 97.8 to 98.2 percent, the water content is 5 to 6 percent, the total number of bacterial colonies is less than 100cfu/g, salmonella and escherichia coli can not be detected, and the quality guarantee period is 24 months.
(2) Preparation of modified radix Isatidis extract
Mixing radix Isatidis extract with mangosteen polyphenol and xylitol at a mass ratio of 75:2.5:1.5 to obtain a mixed modified substance, and dissolving the mixed modified substance with deionized water at a bath ratio of 1: 27; then, the solution was heated to 64.5 ℃ for 16 min. And distilling the heated mixed solution under reduced pressure for 1.2h to obtain the modified isatis root extract.
(3) Modified substance loading
Mixing diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate to obtain the load carrier. Mixing the carrier agent and the modified isatis root extract according to the mass ratio of 8.5: 1.4; then dissolving the mixture in deionized water, heating to 83 ℃, and stirring at the speed of 1900rad/min for 35-40 min; then the temperature is increased to 99 ℃, and the mixture is stirred for 38min at the speed of 2800 rad/min; then cooling to normal temperature; distilling under reduced pressure to remove water to obtain the modifier.
The mixing mass ratio of the diatomite, the superfine bamboo charcoal powder, the zinc stearate and the di-sec-octyl maleate sodium sulfonate is 4.3: 25: 0.4: 0.4.
(4) preparation of isatis root PET master batch
Mixing PET slices, aspartic acid, polyoxyethylene ether and acrylic resin, uniformly stirring, then sequentially adding a modifier and a flame retardant, and drying for 24 hours at 120 ℃; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 278 ℃, and carrying out melt blending for 35 min; the rotating speed of the screw is 265 r/min, high-speed mixing, extruding and granulating are carried out, and functional master batches are obtained; namely the radix isatidis PET master batch.
The mass ratio of the PET slices to the aspartic acid to the polyoxyethylene ether to the acrylic resin is 100:5.5:5: 11.5;
the addition amount of the modifier is 6.1 percent of the mass of the PET slice;
the addition amount of the flame retardant is 4.8 percent of the mass of the PET slices;
the flame retardant consists of magnesium aluminum silicate, silicon dioxide, zinc borate and pentaerythritol ester in a mass ratio of 19:12:3: 0.8.
The flame-retardant isatis root PET master batch prepared by the embodiment has the bacteriostasis rate of 97.25% on typhoid bacillus and 97.04% on staphylococcus aureus; the bacteriostasis rate to colibacillus is 99.02 percent, and the bacteriostasis rate to candida albicans is 99.8 percent. After the prepared flame-retardant isatis root PET master batch is washed for 150 times, the bacteriostasis rate to typhoid bacillus is 91.23%, and the bacteriostasis rate to staphylococcus aureus is 92.21%; the bacteriostasis rate to colibacillus is 90.9 percent, and the bacteriostasis rate to candida albicans is 92.7 percent. The prepared flame-retardant radix isatidis PET master batch is stored for 3 years, the bacteriostasis rate to typhoid bacillus is 93.25%, and the bacteriostasis rate to staphylococcus aureus is 94.55%; the bacteriostasis rate to colibacillus is 93.25 percent, and the bacteriostasis rate to candida albicans is 94.4 percent.
The prepared flame-retardant radix isatidis PET master batch is V0 grade.
Embodiment 3 preparation method of flame-retardant radix isatidis PET master batch
The method comprises the following steps:
(1) preparation of extract of radix Isatidis
Extracting with dried root of Isatis tinctoria to obtain radix Isatidis extract;
100 percent of the isatis root extract is sieved by a 800-mesh sieve, the content of active ingredients is 97.8 to 98.2 percent, the water content is 5 to 6 percent, the total number of bacterial colonies is less than 100cfu/g, salmonella and escherichia coli can not be detected, and the quality guarantee period is 24 months.
(2) Preparation of modified radix Isatidis extract
Mixing radix Isatidis extract with mangosteen polyphenol and xylitol at a mass ratio of 75:2:1 to obtain a mixed modified substance, and dissolving the mixed modified substance with deionized water at a bath ratio of 1: 25; then, the solution was heated to 64 ℃ for 15 min. And distilling the heated mixed solution under reduced pressure for 1h to obtain the modified isatis root extract.
(3) Modified substance loading
Mixing diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate to obtain the load carrier. Mixing the carrier agent and the modified isatis root extract according to the mass ratio of 8: 1; then dissolving the mixture in deionized water, heating to 80 ℃, and stirring at 1800rad/min for 35 min; then heating to 98 ℃, and stirring for 35min at the speed of 2500 rad/min; then cooling to normal temperature; distilling under reduced pressure to remove water to obtain the modifier.
The mixing mass ratio of the diatomite, the superfine bamboo charcoal powder, the zinc stearate and the di-sec-octyl maleate sodium sulfonate is 4: 28: 0.3: 0.3.
(4) preparation of isatis root PET master batch
Mixing PET slices, aspartic acid, polyoxyethylene ether and acrylic resin, uniformly stirring, then sequentially adding a modifier and a flame retardant, and drying for 24 hours at 125 ℃; then adding the mixture into a double-screw extruder, controlling the melting temperature to be 280 ℃, and carrying out melt blending for 40 min; the rotating speed of the screw is 270 r/min, high-speed mixing and extrusion granulation are carried out, and functional master batches are obtained; namely the radix isatidis PET master batch.
The mass ratio of the PET slices to the aspartic acid to the polyoxyethylene ether to the acrylic resin is 100: 6: 7: 12;
the addition amount of the modifier is 6.5 percent of the mass of the PET slice;
the addition amount of the flame retardant is 5.1 percent of the mass of the PET slices;
the flame retardant consists of magnesium aluminum silicate, silicon dioxide, zinc borate and pentaerythritol ester in a mass ratio of 20: 12.5: 5: 1.3.
The flame-retardant isatis root PET master batch prepared by the embodiment has the bacteriostasis rate of 96.95% on typhoid bacillus and 96.5% on staphylococcus aureus; the bacteriostasis rate to colibacillus is 99.0 percent, and the bacteriostasis rate to candida albicans is 98.9 percent. After the prepared flame-retardant isatis root PET master batch is washed for 150 times, the bacteriostasis rate to typhoid bacillus is 91.05%, and the bacteriostasis rate to staphylococcus aureus is 91.92%; the bacteriostasis rate to colibacillus is 90.46 percent, and the bacteriostasis rate to candida albicans is 92.05 percent. The prepared flame-retardant radix isatidis PET master batch is stored for 3 years, the bacteriostasis rate to typhoid bacillus is 92.75 percent, and the bacteriostasis rate to staphylococcus aureus is 93.02 percent; the bacteriostasis rate to colibacillus is 92.84 percent, and the bacteriostasis rate to candida albicans is 93.5 percent.
The prepared flame-retardant radix isatidis PET master batch is V0 grade.
Except for special description, the percentages are mass percentages, and the proportions are mass ratios.
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. A preparation method of flame-retardant radix isatidis PET master batches is characterized by comprising the following steps: comprises the steps of preparing an isatis root extract, preparing a modified isatis root extract, loading a modified substance and preparing isatis root PET master batches; the modified substance is loaded: comprises the steps of preparing a loading agent, mixing with a modified substance, carrying out heat treatment and carrying out reduced pressure distillation; the preparation of the load carrier comprises the following steps: the adopted raw materials comprise diatomite, superfine bamboo charcoal powder, zinc stearate and sodium di-sec-octyl maleate sulfonate.
2. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 1, characterized by comprising the following steps: the mixing mass ratio of the diatomite, the superfine bamboo charcoal powder, the zinc stearate and the di-sec-octyl maleate sodium sulfonate is 4-4.5: 25-28: 0.3-0.5: 0.3-0.5.
3. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 1, characterized by comprising the following steps: mixing with a modifying substance: the mass ratio of the carrier agent to the modified isatis root extract is 8-9: 1-2.
4. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 1, characterized by comprising the following steps: the heat treatment comprises the following steps: dissolving the mixture in deionized water, heating to 80-85 deg.C, and stirring at 1800 & 2000rad/min for 35-40 min; then the temperature is raised to 98-100 ℃, and the mixture is stirred for 35-40min at the speed of 2500-.
5. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 1, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: mixing PET slices, aspartic acid, polyoxyethylene ether and acrylic resin, uniformly stirring, sequentially adding a modifier and a flame retardant, and drying for 24 hours at the temperature of 120-; then adding the mixture into a double-screw extruder, wherein the melting temperature is 275 ℃ and 280 ℃, and the melt blending time is 30-40 min.
6. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 5, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: the screw rotating speed is 260-270 rpm.
7. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 5, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: the mass ratio of the PET slices to the aspartic acid to the polyoxyethylene ether to the acrylic resin is 100:5-6:3-7: 11-12.
8. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 5, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: the flame retardant consists of magnesium aluminum silicate, silicon dioxide, zinc borate and pentaerythritol ester in a mass ratio of 18-20:11-12.5:3-5: 0.8-1.3.
9. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 5, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: the addition amount of the modifier is 5.8-6.5% of the mass of the PET slice.
10. The preparation method of the flame-retardant radix isatidis PET master batch according to claim 5, characterized by comprising the following steps: the preparation of the radix isatidis PET master batch comprises the following steps: the addition amount of the flame retardant is 4.5-5.1% of the mass of the PET slice.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010612236.6A CN111690237B (en) | 2020-06-30 | 2020-06-30 | Flame-retardant radix isatidis PET master batch and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010612236.6A CN111690237B (en) | 2020-06-30 | 2020-06-30 | Flame-retardant radix isatidis PET master batch and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111690237A true CN111690237A (en) | 2020-09-22 |
| CN111690237B CN111690237B (en) | 2023-03-28 |
Family
ID=72484569
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010612236.6A Active CN111690237B (en) | 2020-06-30 | 2020-06-30 | Flame-retardant radix isatidis PET master batch and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111690237B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101400734A (en) * | 2006-02-21 | 2009-04-01 | 沙伯基础创新塑料知识产权有限公司 | Flame retardant resin composition |
| CN104441899A (en) * | 2014-12-03 | 2015-03-25 | 华侨大学 | Preparation method of efficient and antibacterial composite film with water-meeting sensitivity |
| CN105086938A (en) * | 2015-08-03 | 2015-11-25 | 来安县隆华摩擦材料有限公司 | Flame-retardant automobile clutch friction material and preparing method thereof |
| CN110054787A (en) * | 2019-05-06 | 2019-07-26 | 湖南工程学院 | Functional master batch, antibacterial ultraviolet-resistannanofiber line fiber and cloth and preparation method thereof |
| CN110229473A (en) * | 2018-03-06 | 2019-09-13 | 中国科学院化学研究所 | A kind of PET nanocomposite and preparation method thereof |
| CN111171531A (en) * | 2020-03-18 | 2020-05-19 | 百事基材料（青岛）股份有限公司 | Seaweed polyester master batch and preparation process thereof |
| CN111253675A (en) * | 2018-11-30 | 2020-06-09 | 中科纺织研究院（青岛）有限公司 | Plant source PP master batch and preparation method and application thereof |
| CN111534007A (en) * | 2020-06-24 | 2020-08-14 | 广州市中诚新型材料科技有限公司 | Compound antiviral antibacterial health-care multifunctional fiber master batch and preparation and application thereof |
| CN111607111A (en) * | 2020-06-08 | 2020-09-01 | 百草边大生物科技(青岛)有限公司 | Anti-aging tea polyphenol, naringin or emodin modified polyamide master batch and preparation process thereof |
-
2020
- 2020-06-30 CN CN202010612236.6A patent/CN111690237B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101400734A (en) * | 2006-02-21 | 2009-04-01 | 沙伯基础创新塑料知识产权有限公司 | Flame retardant resin composition |
| CN104441899A (en) * | 2014-12-03 | 2015-03-25 | 华侨大学 | Preparation method of efficient and antibacterial composite film with water-meeting sensitivity |
| CN105086938A (en) * | 2015-08-03 | 2015-11-25 | 来安县隆华摩擦材料有限公司 | Flame-retardant automobile clutch friction material and preparing method thereof |
| CN110229473A (en) * | 2018-03-06 | 2019-09-13 | 中国科学院化学研究所 | A kind of PET nanocomposite and preparation method thereof |
| CN111253675A (en) * | 2018-11-30 | 2020-06-09 | 中科纺织研究院（青岛）有限公司 | Plant source PP master batch and preparation method and application thereof |
| CN110054787A (en) * | 2019-05-06 | 2019-07-26 | 湖南工程学院 | Functional master batch, antibacterial ultraviolet-resistannanofiber line fiber and cloth and preparation method thereof |
| CN111171531A (en) * | 2020-03-18 | 2020-05-19 | 百事基材料（青岛）股份有限公司 | Seaweed polyester master batch and preparation process thereof |
| CN111607111A (en) * | 2020-06-08 | 2020-09-01 | 百草边大生物科技(青岛)有限公司 | Anti-aging tea polyphenol, naringin or emodin modified polyamide master batch and preparation process thereof |
| CN111534007A (en) * | 2020-06-24 | 2020-08-14 | 广州市中诚新型材料科技有限公司 | Compound antiviral antibacterial health-care multifunctional fiber master batch and preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蒋侬辉，等: "中草药包装对肉制品保质效能的研究", 《包装工程》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111690237B (en) | 2023-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108385203B (en) | Preparation method of discoloration-resistant antibacterial polyamide fiber | |
| CN111440339B (en) | Tea polyphenol, naringin or emodin modified PET master batch and preparation process thereof | |
| CN105200550B (en) | A kind of low melting point antibacterial special polyester monofilament and its processing method | |
| CN113046859A (en) | Dacron macrobiological fiber containing coffee active component and preparation method thereof | |
| WO2021174720A1 (en) | Seaweed polyester long fiber and preparation method therefor | |
| CN111171532A (en) | Chitin polyester masterbatch and preparation process thereof | |
| CN113122957A (en) | Preparation method of antibacterial and antiviral polyester filament containing PHBV material | |
| CN111270335B (en) | Antibacterial polyester fiber and preparation method thereof | |
| CN111548607A (en) | Preparation method of antibacterial color master batch and stock solution colored PET antibacterial functional fiber | |
| CN111647216A (en) | Antibacterial and heat-storage radix isatidis modified PE master batch and preparation method thereof | |
| US20220162774A1 (en) | Chitin-containing polyester filament and preparation method thereof | |
| CN106987944A (en) | Sun-proof anti-bacterial fibre mixed yarn | |
| CN112281245A (en) | Olive-containing polyester fiber and preparation method thereof | |
| CN101240464A (en) | Polylactic acid hydrolysis-resisting fibre and preparation method thereof | |
| CN115028968A (en) | Antibacterial functional master batch, preparation method thereof, antibacterial polyester fiber and fabric | |
| CN111690237B (en) | Flame-retardant radix isatidis PET master batch and preparation method thereof | |
| CN101158061A (en) | Antibacterial terephthalic acid trimethylene glycol ester staple fiber and production method thereof | |
| CN112981610A (en) | Environment-friendly hydrophilic low-melting-point PET composite short fiber and preparation method thereof | |
| CN111253719B (en) | Organic zinc antibacterial PET granules and preparation method thereof | |
| CN110144650B (en) | Multifunctional pearl polylactic acid blended yarn and preparation method thereof | |
| CN115433440B (en) | Natural herbal antibacterial master batch for polymeric fibers, preparation method and fabric containing natural grass and wood antibacterial components | |
| CN1468983A (en) | Polypropylene fiber with mosquito repelling function | |
| CN111253718B (en) | Organic zinc antibacterial master batch for spinning and preparation method thereof | |
| JPH03113011A (en) | Synthetic yarn and production thereof | |
| CN113308750A (en) | Preparation method of polyester macrobio-fiber containing yucca active ingredient |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |