CN108587083A - A kind of resistant to hydrolysis antibacterial PET Masterbatch and preparation method thereof - Google Patents
A kind of resistant to hydrolysis antibacterial PET Masterbatch and preparation method thereof Download PDFInfo
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- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K7/22—Expanded, porous or hollow particles
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- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Abstract
The invention discloses a kind of resistant to hydrolysis antibacterial PET Masterbatch, are made of the raw material of following weight parts：PET 40 60, inorganic pigment 20 30, fiber 10 15, anti-hydrolysis agent 35, dispersant 24, polyethers E1000 23, nucleating agent 12；PET color master batch provided by the invention contains bamboo charcoal fiber, and antibiotic rate is up to 90% or more, and ultraviolet ray transmissivity is low, and anti-aging property is strong；The coconut palm Carbon fibe contained, far infrared release rate are up to 90% or more, can promote blood circulation and improve human body environment.When the coloring applied to PET products, have many advantages, such as that antibiotic property is good, hydrolytic resistance is good, uniform coloring, colour stability are high, concentration is high, dosage is few and on plasthetics mechanical performance without influencing.
Description
Technical field
The invention belongs to technical field of polymer materials more particularly to a kind of resistant to hydrolysis antibacterial PET Masterbatch and its preparations
Method.
Background technology
PET, that is, polyethylene terephthalate is a kind of crystalline polymer, because it is with excellent mechanical property, resistance to
Heat and chemical-resistant stability, are mainly used for the fields such as polyester fiber.Decoration method is to carry out colouring common method to polyester fiber,
However since polyester fiber fibre belongs to hydrophobic fibre, therefore water-soluble dye is extremely low to its dye-uptake, and easily in dyeing course
Middle appearance dyeing it is uneven and loosely phenomena such as, not only increase dyeing cost, but also increase the discharge of waste water from dyestuff.As people give birth to
Running water flat raising and environmental requirement prepare Masterbatch as carrier using PET and carry out dyeing to polyester fiber melt as a kind of nothing
Pollution, low-carbon environment-friendly color method, while after Masterbatch colours terylene, the tinctorial yield higher of terylene, color fastness be stronger,
Coloring is more uniform.
It is that the pigment of super quantity is uniformly attached to tree as colorant, carrier, dispersant three parts that Masterbatch, which is mainly organized,
Prepared by fat polymer compound, selected by resin to colorant have good wetting and peptizaiton, and
There is good compatibility with by coloured material.
Country's Masterbatch product structure is single at present, kind is not complete, and universal product accounts for very big proportion, and plastics need to colour
When coloured using monochromatic Masterbatch, need to add Anti-static electricity color master batch when antistatic property, addition resistance when needing flame retardant property
Fire Masterbatch.The method for adding single master batch to need to add when having high requirement to vector resin comprehensive performance
Thus the Masterbatch of a variety of different roles to consume a large amount of vector resin, and brings antioxidant in process to consume
The shortcomings of amount is high, downstream processing and forming component is more, complex process, following Masterbatch will be towards multifunction, high color content
It is continued to develop with the direction of high technology content.
PET has ester bond, can decompose under strong acid, highly basic and water vapor acting, and crystalline rate is slow, processing and forming
It is difficult, molding temperature is high, the production cycle is long, impact property is poor.Simultaneously with the continuous improvement of people's living standards, people more
Pursuit itself living environment it is clean comfortable, and often appear in people at one's side, be in direct contact the plastic products of human body,
The anti-microbial property of itself is more efficient, can more reduce disease incident, improve people's living environment, protection health, for this purpose,
The present invention essential Masterbatch from plastic formula is set about, and a kind of PET having both hydrolytic Resistance and anti-microbial property is provided
Masterbatch and preparation method thereof.
Invention content
The present invention overcomes prior art deficiencies, provide a kind of resistant to hydrolysis antibacterial PET Masterbatch and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of resistant to hydrolysis antibacterial PET Masterbatch, is made of the raw material of following weight parts：
PET 40-60, inorganic pigment 20-30, fiber 10-15, anti-hydrolysis agent 3-5, dispersant 2-4, polyethers E1000 2-
3, nucleating agent 1-2.
The inorganic pigment be titanium dioxide, carbon black, cadmium yellow, lead chromate yellow, cadmium red, iron oxide red, iron oxide yellow, barba hispanica,
It is one or more in cobalt blue, iron oxide brown, chrome oxide green, cobalt green.
It is 3 in mass ratio that the fiber, which is by bamboo charcoal fiber, coconut palm Carbon fibe, glass fibre,：1：2 ratio composition.
The anti-hydrolysis agent be by carbodiimides, 3- glycidyl ether oxypropyltriethoxysilanes in mass ratio
2：1 ratio composition.
The dispersant is by dispersant YY -5023, maleic anhydride grafted polyethylene wax, nano silicon dioxide by quality
Than for 1-2：1：1 ratio composition.
The nucleating agent is talcum powder, macromolecular carboxylic acid's salt is 2 in mass ratio：1 ratio composition.
A kind of resistant to hydrolysis antibacterial PET Masterbatch preparation method, includes the following steps：
(1) it is filtered after impregnating inorganic pigment 1-2 days with 2-3 times of deionized water, obtained filter residue 3-5 wash with distilled water
Secondary removal water-solubility impurity, microwave drying 2-3 minutes in the case where power is 400-500W, obtained pigment and aluminate coupling agent,
Triethylenediamine, polybutadiene epoxy resin 20-25 in mass ratio:4:1:2 ratio is sent into micronizer, batch mixing 1-
1.5 hours, obtain the modified pigment that grain size is 0.5-10 μm；
(2) PET is mixed by weight proportion with fiber, anti-hydrolysis agent, dispersant, polyethers E1000, nucleating agent, in 1000-
It is stirred 30-50 minutes under the mixing speed of 1200r/min, is sent into pulverizer and crushes after cooling, obtaining particle size is
100-300 μm of mixture；
(3) above-mentioned modified pigment is sent into autoclave, carbon dioxide is added, adjust the pressure in autoclave
For 50-60MPa, temperature is 100-140 DEG C, and carbon dioxide is made to become supercritical fluid；
(4) it being stirred using magnetic stirring apparatus, post-modification pigment is completely dissolved in supercritical fluid within 3-5 hours, then
Above-mentioned mixture is added, continues stirring 20-30 hours, maintains temperature-resistant reduction pressure to 1-5MPa, it is small to continue stirring 10-15
When, it is deflated by gas bleeder valve, thick color masterbatch is taken out after cooling；
(5) above-mentioned thick color masterbatch is subjected to melting extrusion, screw speed 200-300r/min, spiral shell with double screw extruder
Bar temperature：One 120-130 DEG C of area's temperature, two 130-140 DEG C of area's temperature, three 140-150 DEG C of area's temperature, four area temperature 145-155
DEG C, five 135-145 DEG C of area's temperature, obtain extruded stock；
(6) above-mentioned extruded stock is put into the flowing water that temperature is 30-40 DEG C and is cooled down, water velocity 20-30L/
Min, then microwave drying 3-5 minutes in the case where power is 400-500W, carry out pelletizing, it is 1- to obtain particle size using pelleter
The PET color master batch of 10mm.
Compared with prior art, it is an advantage of the invention that：
The present invention effectively enhances the compatibility with carrier, pigment is made to be uniformly dispersed, more preferably by the way that inorganic pigment to be modified
Coloring, and modified pigment does not allow fugitive color, it is more aesthetically pleasing, substantially prolong its service life.
The bamboo charcoal fiber of honeycomb microporous structure is mixed with carrier, auxiliary agent, elliptical shaped apertures have been covered in mixture.It will
Inorganic pigment is dissolved in supercritical carbon dioxide fluid, is penetrated into mixture after numerous hole after it, by decompression expansion,
Micron-sized inorganic pigment can be gradually deposited in mixture, carbon dioxide recoverable.
Supercritical carbon dioxide fluid viscosity is low, diffusion property coefficient is big, diffusion boundary layer is small, the inorganic face of unimolecule of dissolving
Material can be rapidly soaked into gap in mixture, and coloration efficiency is far above traditional handicraft, substantially reduce the production cycle, and
Color is uniform, aberration is smaller, colour stability greatly improves.
It, can using dispersant YY -5023, the dispersant of maleic anhydride grafted polyethylene wax, nano silicon dioxide composition
The melt flow rate (MFR) of Masterbatch is improved, increases counter balance torque, the time reached needed for peak torque is shortened, in the shortest time
It is interior to obtain ideal dispersion effect, and dispersant dosage is reduced, reduce cost.
The hydrolysis-stable of epoxide acts on compared with carbodiimides, not only by the end carboxylic with hydrolyzation catalysis effect
Based compound is converted into the non-catalytic product with pendant hydroxyl group, and is reacted with terminal hydroxy group, and chain rupture is made to reconnect.Using carbonization
Diimine, 3- glycidyl ether oxypropyltriethoxysilanes form anti-hydrolysis agent, can significantly improve the resistant to hydrolysis of Masterbatch
Performance, and dosage is less, reduces production cost.
Addition polyethers is conducive to the crystallization of PET, but cannot significantly improve crystalline rate, and the addition of nucleating agent can be significantly
PET crystalline rates, the high temperature nucleation capability of talcum powder and the low temperature nucleation capability collective effect of macromolecular carboxylic acid's salt are improved, significantly
Improve the crystallizing power of PET.
PET color master batch provided by the invention contains bamboo charcoal fiber, and antibiotic rate is up to 90% or more, and ultraviolet ray transmissivity is low,
Anti-aging property is strong；The coconut palm Carbon fibe contained, far infrared release rate are up to 90% or more, can promote blood circulation and change
Kind human body environment.When the coloring applied to PET products, with antibiotic property is good, hydrolytic resistance is good, uniform coloring, colour stable
Property it is high, concentration is high, dosage is few and on plasthetics mechanical performance without influencing the advantages that.
Specific implementation mode
With reference to embodiment, present invention is further described in detail：
Embodiment：
A kind of resistant to hydrolysis antibacterial PET Masterbatch, is made of the raw material of following weight parts：
40 parts of PET, 20 parts of inorganic pigment, 10 parts of fiber, 3 parts of anti-hydrolysis agent, 2 parts of dispersant, 2 parts of polyethers E1000, at
1 part of core agent.
The inorganic pigment is cobalt blue.
It is 3 in mass ratio that the fiber, which is by bamboo charcoal fiber, coconut palm Carbon fibe, glass fibre,：1：2 ratio composition.
The anti-hydrolysis agent be by carbodiimides, 3- glycidyl ether oxypropyltriethoxysilanes in mass ratio
2：1 ratio composition.
The dispersant is by dispersant YY -5023, maleic anhydride grafted polyethylene wax, nano silicon dioxide by quality
Than being 1：1：1 ratio composition.
The nucleating agent is talcum powder, macromolecular carboxylic acid's salt is 2 in mass ratio：1 ratio composition.
A kind of resistant to hydrolysis antibacterial PET Masterbatch preparation method, includes the following steps：
(1) it is filtered after impregnating inorganic pigment 1 day with 3 times of deionized waters, 3 removals wash with distilled water of obtained filter residue
Water-solubility impurity, the microwave drying 3 minutes in the case where power is 400W, obtained pigment and aluminate coupling agent, triethylenediamine,
Polybutadiene epoxy resin in mass ratio 20:4:1:2 ratio is sent into micronizer, and batch mixing 1.5 hours, obtaining grain size is
0.5 μm of modified pigment；
(2) PET is mixed by weight proportion with fiber, anti-hydrolysis agent, dispersant, polyethers E1000, nucleating agent,
It is stirred 50 minutes under the mixing speed of 1000r/min, is sent into pulverizer and crushes after cooling, it is 100 μ to obtain particle size
The mixture of m；
(3) above-mentioned modified pigment is sent into autoclave, carbon dioxide is added, adjust the pressure in autoclave
For 60MPa, temperature is 140 DEG C, and carbon dioxide is made to become supercritical fluid；
(4) it is stirred using magnetic stirring apparatus, post-modification pigment is completely dissolved in supercritical fluid within 3 hours, then is added
Enter above-mentioned mixture, continue stirring 20 hours, maintains temperature-resistant reduction pressure to 3MPa, continue stirring 10 hours, by letting out
Air valve is deflated, and thick color masterbatch is taken out after cooling；
(5) above-mentioned thick color masterbatch is subjected to melting extrusion, screw speed 300r/min, screw rod temperature with double screw extruder
Degree：One 120 DEG C of area's temperature, 130 DEG C of two area's temperature, 140 DEG C of three area's temperature, 145 DEG C of four area's temperature, 135 DEG C of five area's temperature, obtain
Extruded stock；
(6) above-mentioned extruded stock is put into the flowing water that temperature is 30 DEG C and is cooled down, water velocity 30L/min, then
Power is microwave drying 3 minutes under 500W, and pelletizing is carried out using pelleter, obtains the PET color master batch that particle size is 2mm.
Comparative example：
Weigh the raw material of following weight parts：40 parts of PET, 20 parts of cobalt blue, 3 parts of carbodiimides, maleic anhydride are grafted poly- second
2 parts of alkene wax, 2 parts of polyethers E1000,1 part of talcum powder are uniformly mixed, are heated to 50 DEG C, small using magnetic stirring apparatus high-speed stirred 3
When, then with double screw extruder melting, squeeze out, be granulated, obtain particle size be 2mm Masterbatch.
Embodiment and Masterbatch made from comparative example are tested for the property, as shown in the table：
As can be seen from the above table, the Masterbatch aberration of production technology according to the invention production is small, strong coloring force, and melt is viscous
Degree is preferable, has excellent color fastness.And after adding fiber, the Masterbatch of preparation is to the bacteriostasis rate of Escherichia coli 99%
More than, anti-microbial property is high；Anti-hydrolysis agent is by carbodiimides, 3- glycidyl ether oxypropyltriethoxysilane mixing groups
At after Masterbatch 120 DEG C of the temperature steam treatment 80 hours of preparation, Masterbatch stretching strength retentivity is higher, hydrolysis rate
Relatively low, hydrolytic Resistance is stronger.
The above embodiment is merely an example for clearly illustrating the present invention, and is not the embodiment party to the present invention
The restriction of formula.For those skilled in the art, other differences can be made on the basis of the above description
The variation or variation of form.There is no necessity and possibility to exhaust all the enbodiments.And these belong to the essence of the present invention
The obvious changes or variations that god extends out are among protection scope of the present invention and the open scope.
Claims (7)
1. a kind of resistant to hydrolysis antibacterial PET Masterbatch, it is characterised in that be made of the raw material of following weight parts：
PET 40-60, inorganic pigment 20-30, fiber 10-15, anti-hydrolysis agent 3-5, dispersant 2-4, polyethers E1000 2-3, at
Core agent 1-2.
2. a kind of resistant to hydrolysis antibacterial PET Masterbatch as described in claim 1, which is characterized in that the inorganic pigment is titanium
White powder, carbon black, cadmium yellow, lead chromate yellow, cadmium red, iron oxide red, iron oxide yellow, barba hispanica, cobalt blue, iron oxide brown, chrome oxide green, cobalt green
In it is one or more.
3. a kind of resistant to hydrolysis antibacterial PET Masterbatch as described in claim 1, which is characterized in that the fiber is by bamboo charcoal
Fiber, coconut palm Carbon fibe, glass fibre are 3 in mass ratio：1：2 ratio composition.
4. a kind of resistant to hydrolysis antibacterial PET Masterbatch as described in claim 1, which is characterized in that the anti-hydrolysis agent be by
Carbodiimides, 3- glycidyl ether oxypropyltriethoxysilanes in mass ratio 2：1 ratio composition.
5. a kind of resistant to hydrolysis antibacterial PET Masterbatch as described in claim 1, which is characterized in that the dispersant is by dividing
Powder YY -5023, maleic anhydride grafted polyethylene wax, nano silicon dioxide are 1-2 in mass ratio：1：1 ratio composition.
6. a kind of resistant to hydrolysis antibacterial PET Masterbatch as described in claim 1, which is characterized in that the nucleating agent is talcum
Powder, macromolecular carboxylic acid's salt are 2 in mass ratio：1 ratio composition.
7. a kind of resistant to hydrolysis antibacterial PET Masterbatch preparation method, which is characterized in that include the following steps：
(1) it is filtered after impregnating inorganic pigment 1-2 days with 2-3 times of deionized water, obtained filter residue is gone for 3-5 times wash with distilled water
Except water-solubility impurity, microwave drying 2-3 minutes, obtained pigment and aluminate coupling agent, Sanya in the case where power is 400-500W
Ethyldiamine, polybutadiene epoxy resin 20-25 in mass ratio:4:1:2 ratio is sent into micronizer, batch mixing 1-1.5
Hour, obtain the modified pigment that grain size is 0.5-10 μm；
(2) PET is mixed by weight proportion with fiber, anti-hydrolysis agent, dispersant, polyethers E1000, nucleating agent, in 1000-
It is stirred 30-50 minutes under the mixing speed of 1200r/min, is sent into pulverizer and crushes after cooling, obtaining particle size is
100-300 μm of mixture；
(3) above-mentioned modified pigment is sent into autoclave, carbon dioxide is added, the pressure adjusted in autoclave is
50-60MPa, temperature are 100-140 DEG C, and carbon dioxide is made to become supercritical fluid；
(4) it is stirred using magnetic stirring apparatus, post-modification pigment is completely dissolved in supercritical fluid within 3-5 hours, is added
Above-mentioned mixture continues stirring 20-30 hours, maintains temperature-resistant reduction pressure to 1-5MPa, continues stirring 10-15 hours,
It is deflated by gas bleeder valve, thick color masterbatch is taken out after cooling；
(5) above-mentioned thick color masterbatch is subjected to melting extrusion, screw speed 200-300r/min, screw rod temperature with double screw extruder
Degree：One 120-130 DEG C of area's temperature, two 130-140 DEG C of area's temperature, three 140-150 DEG C of area's temperature, four 145-155 DEG C of area's temperature, five
135-145 DEG C of area's temperature, obtains extruded stock；
(6) above-mentioned extruded stock is put into the flowing water that temperature is 30-40 DEG C and is cooled down, water velocity 20-30L/min, then
In the case where power is 400-500W, microwave drying 3-5 minutes, pelletizing is carried out using pelleter, and it is 1-10mm's to obtain particle size
PET color master batch.
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| CN113337087A (en) * | 2021-06-17 | 2021-09-03 | 贵州省材料产业技术研究院 | High-performance polyester alloy material and preparation method thereof |
| CN114775098A (en) * | 2022-06-07 | 2022-07-22 | 浙江伟星实业发展股份有限公司 | PET monofilament, preparation method thereof, nylon zipper with high-temperature and high-humidity resistant teeth and chemical protective clothing |
| EP4034501A4 (en) * | 2019-09-27 | 2024-01-24 | Nature Coatings Inc | Plant char carbon pigments and liquid dispersions thereof |
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Application publication date: 20180928 |