CN110272563A - A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing - Google Patents
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing Download PDFInfo
- Publication number
- CN110272563A CN110272563A CN201910566431.7A CN201910566431A CN110272563A CN 110272563 A CN110272563 A CN 110272563A CN 201910566431 A CN201910566431 A CN 201910566431A CN 110272563 A CN110272563 A CN 110272563A
- Authority
- CN
- China
- Prior art keywords
- antioxidant
- composite antioxidant
- powder
- composite
- auxiliary
- 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.)
- Pending
Links
Classifications
-
- 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
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- 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
- 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
- C08K5/0041—Optical brightening agents, organic pigments
-
- 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
- C08K5/0091—Complexes with metal-heteroatom-bonds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of with the more preferable composite antioxidant preparation method for improving Polymer Processing and long-term ageing and turning yellow, the composite antioxidant uses primary antioxidant, auxiliary antioxidant, dispersing agent, organic pigment, inorganic pigment for main material preparation, first by primary antioxidant, auxiliary antioxidant mixed melting at melt, then addition dispersant is uniform, the ultrasonication under ultrasonic wave again, organic pigment powder, inorganic pigment powder is added, it is uniformly dispersed, most obtains composite antioxidant particle through double screw extruder extruding pelletization afterwards.The present invention is carried out by the melt of main and auxiliary aid anti-oxidants with pigment compound, dispersing agent function and ultrasonic technology are combined, keep pigment powder more uniform in the melt dispersion of antioxidant, keep the pigment content in single composite antioxidant particle uniform, by compound in the composite antioxidant and polymer, the complementary color effect that pigment colours polymer color is improved, Polymer Processing is effectively improved and long-term ageing turns yellow.
Description
Technical field
The present invention relates to a kind of with the more preferable composite antioxidant preparation side for improving Polymer Processing and long-term ageing and turning yellow
Method belongs to antioxidant complex technique field.
Background technique
Polymer, such as acrylic resin, polyvinyl resin, EVA, polycarbonate resin, in synthesis since technique is made
The problems such as at fault of construction, the residual of metal ion, or in hot-working to the destruction of molecular structure, and stored for a long time
Aging occurs in journey can all generate some chromophores, these chromophores will cause polymer color coloring, numerous in polymer
Also red or green chromophore can be mixed while being largely displaing yellow in chromophore.Antioxidant is protection Polymer Processing
And the functional aid of long-term ageing, polymer aging can be delayed and the chromophore that is formed, to avoid the xanthochromia of polymer.
But antioxidant can not carry out the destruction in structure to the chromophore formed and change color, for chromophore in raw material
The problem of causing polymer color to colour can carry out complementary color using pigment, if antioxidant, pigment are separately added into polymer
Middle carry out compound, can to polymer color colour complementary color, but pigment in the polymer be unevenly distributed so that complementary color imitate
Fruit is poor.Therefore, be badly in need of one kind can antioxidant and pigment is compound, preferably improve Polymer Processing and long-term ageing xanthochromia
Method.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of with more preferable improvement Polymer Processing and long-term
Dispersing agent function and ultrasonic technology are combined, can be improved main and auxiliary antioxidant by the composite antioxidant preparation method of aging yellowing
With the compound uniformity of pigment, simple process.
To achieve the goals above, the present invention adopts the following technical scheme: it is a kind of have it is more preferable improve Polymer Processing and
Long-term ageing turn yellow composite antioxidant preparation method, the composite antioxidant using primary antioxidant, auxiliary antioxidant, dispersing agent,
Organic pigment, inorganic pigment are main material preparation, it is specific the preparation method is as follows:
(1) first organic pigment, inorganic pigment are ground respectively, and is filtered with 800~900 mesh filter screens, obtain organic pigment
Powder, inorganic pigment powder, it is spare；
(2) primary antioxidant, auxiliary antioxidant are mixed, heating stirring gradually rises temperature to 250 DEG C, then keeps 30
~60min, then temperature is reduced to 230 DEG C, 40~50min is stirred, mixing speed is 1000~1500r/min, is obtained compound anti-
Oxygen agent mixed liquor I；
(3) dispersing agent then is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), is stirred at 230 DEG C of temperature
30~40min is mixed, is uniformly mixed, temperature is reduced to 200 DEG C, stirs 40~50min, obtain composite antioxidant mixed liquor II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, above-mentioned step is added
Suddenly the organic pigment powder in (1), ultrasonic time are added the inorganic pigment powder in above-mentioned steps (1), continue after being 2~3min
Ultrasonic treatment, is uniformly dispersed, and ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Preferably, the primary antioxidant be phenolic antioxidant or amine antioxidants, phenolic antioxidant include antioxidant 1010,
Antioxidant 1076, antioxidant 1098, amine antioxidants include antioxidant 5057, antioxidant 405；Auxiliary antioxidant is phosphorous acid
Esters antioxidant or sulphur ester antioxidant；Auxiliary antioxidant is phosphite ester antioxidant or sulphur ester antioxidant, phosphorous acid
Esters antioxidant irgasfos 168, antioxidant 626, antioxidant 618, antioxidant 9228, sulphur ester antioxidant include antioxidant
DLTDP, antioxidant DSTDP, antioxidant 412S；The dispersing agent is calcium stearate or zinc stearate；The organic pigment is phthalein
One or more kinds of arbitrary proportion mixing of ultramarine, transparent violet B, vat brilliant violet RR, transparent green 5B；The inorganic pigment is
Ultramarine.
Preferably, the primary antioxidant is 1010 antioxidant；Auxiliary antioxidant is 168 antioxidant；The dispersing agent is
Calcium stearate or zinc stearate；The organic pigment is the mixture of phthalocyanine blue and transparent violet B；The inorganic pigment is ultramarine.
Preferably, the gross mass of primary antioxidant and auxiliary antioxidant accounts for primary antioxidant, auxiliary antioxidant, divides in the raw material
The 75%~90% of the main material gross mass of powder, organic pigment, inorganic pigment composition, the primary antioxidant, auxiliary antioxidant
Mass ratio be 1:4~1:0.5.
Preferably, the quality of dispersing agent accounts for primary antioxidant, auxiliary antioxidant, dispersing agent, organic pigment, nothing in the raw material
The 8%~20% of the main material gross mass of machine pigment composition, remaining is organic pigment powder and inorganic pigment powder.
Preferably, organic pigment powder in the raw material, inorganic pigment powder mass ratio be 17:1~30:1.
Preferably, the ultrasonication in above-mentioned steps (4), ultrasonic power be 1000~1200W, frequency 20KHz,
Temperature is 190~200 DEG C.
Preferably, the primary antioxidant be phenolic antioxidant or amine antioxidants,
Beneficial effects of the present invention:
The present invention is compound by the melt of main and auxiliary aid anti-oxidants and pigment progress, by dispersing agent function and ultrasonic technology
In conjunction with, make pigment powder antioxidant melt dispersion it is more uniform, be effectively prevented the sedimentation and cohesion of pigment powder, make list
Pigment content in a composite antioxidant particle is uniform, by compound in the composite antioxidant and polymer, improves pigment to poly-
The complementary color effect for closing object color dyes, effectively improves Polymer Processing and long-term ageing turns yellow.
Dispersing agent is added in the melt of main and auxiliary aid anti-oxidants in the present invention, and the viscosity of the melt of antioxidant is effectively reduced, mentions
The motility of high pigment particles, it is ensured that composite antioxidant colours the relatively high colouring quantity of complementary color to polymer color, while improving multiple
The stability for closing antioxidant, enhances the tinting strength, tinting power of composite antioxidant, and color saturation is high.
Using organic pigment as main color-compensation dye in composite antioxidant of the invention, to the complementary color of polymer color coloring
Effect is preferable；Meanwhile inorganic pigment, as auxiliary color-compensation dye, inorganic pigment uses ultramarine, one side ultramarine and organic dyestuff
Synergy, another aspect inorganic pigment ultramarine have special crystal lattice because containing sodium polysulfide, inside, have and eliminate yellow color
The efficiency of light substantially increases the complementary color effect to polymer color coloring, while by main and auxiliary aid anti-oxidants and complementary color dye
The screening of material, obtained compounded combination act synergistically so that composite antioxidant has optimal thermal oxidation stability in process
Property, and best improvement is reached to the aging yellowing of acrylic resin.
Solvent-free use in complex technique of the invention avoids the waste of solvent, reduces production cost, environmentally protective；It should
Complex technique uses ultrasonic technology, is effectively shortened the production time, improves production efficiency, and energy saving improves economical
Benefit.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not the limitation to invention.
Blank example
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(2) 20g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), at 230 DEG C of temperature
30~40min of lower stirring is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, obtain composite antioxidant mixed liquor
Ⅱ；
(3) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle, detecting its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument is -1.2.
One, the screening embodiment of pigment and main and auxiliary aid anti-oxidants compounding process:
Screen embodiment 1
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) it first by phthalocyanine blue, ultramarine to grind respectively, and is filtered with 800~900 mesh filter screens, obtains phthalocyanine blue powder, group
Green powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3), temperature is kept for 200 DEG C, is added above-mentioned steps (1)
In 3.60g phthalocyanine blue powder, stir 60~90min after be added above-mentioned steps (1) in 0.15g ultramarine powder, continue to stir,
It is uniformly dispersed, stirs 90~100min, obtain composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Screen embodiment 2
All steps (1), (2), (3), (5) in this screening embodiment and all steps (1) in screening embodiment 1,
(2), (3), (5) are identical, and difference is, (4) of this screening embodiment mix the composite antioxidant in above-mentioned steps (3)
The ultrasonication under ultrasonic wave of liquid II, ultrasonic power are 1000~1200W, and frequency 20KHz, temperature is 190~200
DEG C, the 3.60g phthalocyanine blue powder in above-mentioned steps (1) is added, ultrasonic time is added in above-mentioned steps (1) after being 2~3min
0.15g ultramarine powder, continues to be ultrasonically treated, be uniformly dispersed, and ultrasonic time is 3~4min, obtains composite antioxidant lotion.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 1 below:
| Yellow colour index | |
| Blank example | -1.2 |
| Screen embodiment 1 | -5.4 |
| Screen embodiment 2 | -7.3 |
Through being uniformly dispersed, being obtained in master, irgasfos 168 melt using ultrasonic technology processing pigment described in upper table 1
Composite antioxidant is best to the aging yellowing improvement of acrylic resin.
Two, the gross mass of primary antioxidant and auxiliary antioxidant, dispersing agent quality account for the ratio screening of main material gross mass in fact
Apply example:
Screen embodiment 3
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) it first by phthalocyanine blue, ultramarine to grind respectively, and is filtered with 800~900 mesh filter screens, obtains phthalocyanine blue powder, group
Green powder, it is spare；
(2) 22.5g antioxidant 1010, the mixing of 45g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C,
Then 30~60min is kept, then reduces temperature to 230 DEG C, stirs 40~50min, mixing speed is 1000~1500r/min,
Obtain composite antioxidant mixed liquor I；
(3) 4.5g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature 230
30~40min is stirred at DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, obtain composite antioxidant mixed liquor
Ⅱ；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 2.88g phthalocyanine blue powder in above-mentioned steps (1) is added
End, ultrasonic time are added the 0.12g ultramarine powder in above-mentioned steps (1), continue to be ultrasonically treated, be uniformly dispersed after being 2~3min,
Ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Screen embodiment 4
All steps in this screening embodiment are identical as all steps in screening embodiment 3, and difference is, this screening
6g calcium stearate is weighed in the step of embodiment (3), weighs 1.44g phthalocyanine blue powder, 0.06g ultramarine powder in step (4) respectively
End.
Screen embodiment 5
All steps in this screening embodiment are identical as all steps in screening embodiment 3, and difference is, this screening
20g antioxidant 1010,40g irgasfos 168 are weighed in the step of embodiment (2), step weighs 6g calcium stearate, step in (3)
(4) 8.64g phthalocyanine blue powder, 0.36g ultramarine powder are weighed in respectively.
Screen embodiment 6
All steps in this screening embodiment are identical as all steps in screening embodiment 3, and difference is, this screening
20g antioxidant 1010,40g irgasfos 168 are weighed in the step of embodiment (2), step weighs 11.25g calcium stearate in (3),
3.65g phthalocyanine blue powder, 0.15g ultramarine powder are weighed in step (4) respectively.
Screen embodiment 7
All steps in this screening embodiment are identical as all steps in screening embodiment 8, and difference is, this screening
18.75g antioxidant 1010,37.5g irgasfos 168 are weighed in the step of embodiment (2), step weighs 15g stearic acid in (3)
Calcium weighs 3.60g phthalocyanine blue powder, 0.15g ultramarine powder in step (4) respectively.
Screen embodiment 8
All steps in this screening embodiment are identical as all steps in screening embodiment 3, and difference is, this screening
18.75g antioxidant 1010,37.5g irgasfos 168 are weighed in the step of embodiment (2), step weighs 16.5g stearic acid in (3)
Calcium weighs 2.16g phthalocyanine blue powder, 0.09g ultramarine powder in step (4) respectively.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 2 below:
Through described in upper table 2, the gross mass of antioxidant 1010 and irgasfos 168 account for primary antioxidant in above-mentioned steps (2) and
It is total that the gross mass of auxiliary antioxidant accounts for primary antioxidant 1010, irgasfos 168, calcium stearate, phthalocyanine blue, the main material of ultramarine composition
The 75~90% of quality, calcium stearate quality account for primary antioxidant 1010, irgasfos 168, calcium stearate, phthalocyanine blue, ultramarine composition
Main material gross mass 8~20% when, pigment is uniformly dispersed and stablizes, and obtained composite antioxidant is to the old of acrylic resin
Change flavescence effect and color uniformity more preferably, while observing the color saturation with higher of improved acrylic resin particle
Degree.
Three, the mass ratio screening embodiment of primary antioxidant, auxiliary antioxidant:
Screen embodiment 9
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) it first by phthalocyanine blue, ultramarine to grind respectively, and is filtered with 800~900 mesh filter screens, obtains phthalocyanine blue powder, group
Green powder, it is spare；
(2) 10.91g antioxidant 1010, the mixing of 49.09g irgasfos 168 are weighed, heating stirring gradually rises temperature extremely
250 DEG C, 30~60min then being kept, then reduce temperature to 230 DEG C, stirs 40~50min, mixing speed is 1000~
1500r/min obtains composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 3.60g phthalocyanine blue powder in above-mentioned steps (1) is added
End, ultrasonic time are added the 0.15g ultramarine powder in above-mentioned steps (1), continue to be ultrasonically treated, be uniformly dispersed after being 2~3min,
Ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Screen embodiment 10
All steps in this screening embodiment are identical as all steps in screening embodiment 9, and difference is, this screening
12g antioxidant 1010, the mixing of 48g irgasfos 168 are weighed in the step of embodiment (2).
Screen embodiment 11
All steps in this screening embodiment are identical as screening all steps of embodiment 9, and difference is, this screening is real
20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed in the step of applying (2).
Screen embodiment 12
All steps in this screening embodiment are identical as all steps in screening embodiment 9, and difference is, this screening
40g antioxidant 1010, the mixing of 20g irgasfos 168 are weighed in the step of embodiment (2).
Screen embodiment 13
All steps in this screening embodiment are identical as all steps in screening embodiment 9, and difference is, this screening
41.38g antioxidant 1010, the mixing of 18.62g irgasfos 168 are weighed in the step of embodiment (2).
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 3 below:
| Yellow colour index | |
| Blank example | -1.2 |
| Screen embodiment 9 | -5.6 |
| Screen embodiment 10 | -7.2 |
| Screen embodiment 11 | -7.3 |
| Screen embodiment 12 | -7.2 |
| Screen embodiment 13 | -5.8 |
Through described in upper table 3, mass ratio when being 1:4~1:0.5 of the antioxidant 1010, auxiliary anti-oxidant, what is obtained is compound
Antioxidant to the aging yellowing improvement of acrylic resin more preferably.
Four, the mass ratio of organic pigment and inorganic pigment screens embodiment:
Screen embodiment 14
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) it first by phthalocyanine blue, ultramarine to grind respectively, and is filtered with 800~900 mesh filter screens, obtains phthalocyanine blue powder, group
Green powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 3.53g phthalocyanine blue powder in above-mentioned steps (1) is added
End, ultrasonic time are added the 0.22g ultramarine powder in above-mentioned steps (1), continue to be ultrasonically treated, be uniformly dispersed after being 2~3min,
Ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Screen embodiment 15
All steps in this screening embodiment are identical as all steps in screening embodiment 14, and difference is, this sieve
0.19g phthalocyanine blue powder, 3.56g ultramarine powder are weighed in the step of selecting embodiment (4) respectively.
Screen embodiment 16
All steps in this screening embodiment are identical as all steps in screening embodiment 14, and difference is, this sieve
3.56g phthalocyanine blue powder, 0.19g ultramarine powder are weighed in the step of selecting embodiment (4) respectively.
Screen embodiment 17
All steps in this screening embodiment are identical as all steps in screening embodiment 14, and difference is, this sieve
3.60g phthalocyanine blue powder, 0.15g ultramarine powder are weighed in the step of selecting embodiment (4) respectively.
Screen embodiment 18
All steps in this screening embodiment are identical as all steps in screening embodiment 13, and difference is, this sieve
3.63g phthalocyanine blue powder, 0.12g ultramarine powder are weighed in the step of selecting embodiment (4) respectively.
Screen embodiment 19
All steps in this screening embodiment are identical as all steps in screening embodiment 13, and difference is, this sieve
3.75g phthalocyanine blue powder is weighed in the step of selecting embodiment (4) respectively.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 4 below:
| Yellow colour index | |
| Blank example | -1.2 |
| Screen embodiment 14 | -7.2 |
| Screen embodiment 15 | -7.1 |
| Screen embodiment 16 | -7.2 |
| Screen embodiment 17 | -7.3 |
| Screen embodiment 18 | -6.1 |
| Screen embodiment 19 | -6.1 |
Through described in upper table 4, mass ratio when being 0~30:1 of organic pigment powder, inorganic pigment powder, what is obtained is compound anti-
Oxygen agent is preferable to the aging yellowing effect of acrylic resin, but the mass ratio of organic pigment powder, inorganic pigment powder be 0~
When 16:1, so that the color of polyacrylic polymer is variant, therefore the mass ratio of organic pigment powder, inorganic pigment powder is
Composite antioxidant is preferable to the aging yellowing effect and color uniformity of acrylic resin when 17:1~30:1.
Five, the component screening embodiment of primary antioxidant, auxiliary antioxidant, pigment:
Screen embodiment 21
All steps in this screening embodiment are identical as all steps in screening embodiment 2, and difference is, selects not
Same primary antioxidant is compounded with irgasfos 168, calcium stearate, phthalocyanine blue, ultramarine:
21.1 primary antioxidants select antioxidant 1076,20g antioxidant 1076 and 40g irgasfos 168,11.25g stearic acid
Calcium, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
21.2 primary antioxidants select antioxidant 1098,20g antioxidant 1098 and 40g irgasfos 168,11.25g stearic acid
Calcium, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
21.3 primary antioxidants select antioxidant 5057,20g antioxidant 5057 and 40g irgasfos 168,11.25g stearic acid
Calcium, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
21.4 primary antioxidants select antioxidant 405,20g antioxidant 405 and 40g irgasfos 168,11.25g calcium stearate,
3.60g phthalocyanine blue, 0.15g ultramarine are compounded.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 5 below:
Screen embodiment 22
All steps in this screening embodiment are identical as all steps in screening embodiment 2, and difference is, selects not
Same auxiliary antioxidant is compounded with primary antioxidant 1010, calcium stearate, phthalocyanine blue, ultramarine:
22.1 primary antioxidants select antioxidant 626,40g antioxidant 626 and 20g antioxidant 1010,11.25g calcium stearate,
3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.2 primary antioxidants select antioxidant 618,40g antioxidant 618 and 20g antioxidant 1010,11.25g calcium stearate,
3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.3 primary antioxidants select antioxidant 626,40g antioxidant 626 and 20g antioxidant 1010,11.25g calcium stearate,
3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.4 primary antioxidants select antioxidant 9228,40g antioxidant 9228 and 20g antioxidant 1010,11.25g stearic acid
Calcium, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.5 primary antioxidants select antioxidant DLTDP, and 40g antioxidant DLTDP and 20g antioxidant 1010,11.25g are stearic
Sour calcium, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.6 primary antioxidants select antioxidant DSTDP, 40g antioxidant antioxidant DSTDP and 20g antioxidant 1010,
11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
22.7 primary antioxidants select antioxidant antioxidant 412S, 40g antioxidant antioxidant 412S and 20g antioxidant 1010,
11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 6 below:
Screen embodiment 23
All steps in this screening embodiment are identical as all steps in screening embodiment 2, and difference is, selects not
Auxiliary antioxidant together, primary antioxidant are compounded with calcium stearate, phthalocyanine blue, ultramarine:
23.1 primary antioxidants select antioxidant 1076, auxiliary antioxidant to select antioxidant 618,20g antioxidant 1076 and 40g
Antioxidant 618,11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
23.2 primary antioxidants select antioxidant 1098, auxiliary antioxidant to select antioxidant 626,20g antioxidant 1098 and 40g
Antioxidant 626,11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
21.3 primary antioxidants select antioxidant 5057, auxiliary antioxidant select antioxidant DSTDP, 20g antioxidant 5057 with
40g antioxidant DSTDP, 11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded；
21.4 primary antioxidants select antioxidant 405, auxiliary antioxidant to select antioxidant DLTDP, 20g antioxidant 405 and 40g
Antioxidant DLTDP, 11.25g calcium stearate, 3.60g phthalocyanine blue, 0.15g ultramarine are compounded.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 7 below:
Screen embodiment 24
All steps in this screening embodiment are identical as all steps in screening embodiment 2, and difference is, selects not
Same organic pigment is compounded with antioxidant 1010 with irgasfos 168, calcium stearate ultramarine:
24.1 organic pigments select transparent violet B, 3.60g transparent violet B and 20g antioxidant 1010,40g irgasfos 168,
11.25g calcium stearate, 0.15g ultramarine are compounded；
24.2 organic pigments select vat brilliant violet RR, 3.60g vat brilliant violet RR and 20g antioxidant 1010,40g antioxidant
168,11.25g calcium stearate, 0.15g ultramarine are compounded；
24.3 organic pigments select transparent green 5B, 3.60g transparent green 5B and 20g antioxidant 1010,40g irgasfos 168,
11.25g calcium stearate, 0.15g ultramarine are compounded；
24.4 organic pigments select phthalocyanine blue, transparent violet B, 3g phthalocyanine blue and 0.6g transparent violet B and 20g antioxidant 1010,
40g irgasfos 168,11.25g calcium stearate, 0.15g ultramarine are compounded；
24.5 organic pigments select phthalocyanine blue, transparent green 5B, 3g phthalocyanine blue and 0.6g transparent green 5B and 20g antioxidant
1010,40g irgasfos 168,11.25g calcium stearate, 0.15g ultramarine are compounded.
Through above-mentioned experiment, the composite antioxidant particle 2g for taking each screening embodiment to prepare is respectively added to the poly- of 1000ml
In allyl resin lotion, it is uniformly mixed, injection molding goes out machine extruding pelletization, improved polypropylene tree at 180~210 DEG C
Rouge particle detects its yellow colour index through HunterLab LabScan XE chromascope-yellow colour index instrument, as a result as shown in table 8 below:
Through described in upper table 5, table 6, table 7, table 8, antioxidant 1010 and irgasfos 168, calcium stearate, phthalocyanine blue, ultramarine are multiple
There is preferable improvement to acrylic resin aging yellowing with composite antioxidant obtained, and select phthalocyanine blue and transparent violet
B compound organic pigment compounds composite antioxidant obtained with antioxidant 1010 with irgasfos 168, calcium stearate, ultramarine to poly- third
Olefine resin aging yellowing has better improvement.
Embodiment 1
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) first by organic pigment be phthalocyanine blue be grind respectively, and with 800~900 mesh filter screens filter, obtain organic pigment
Powder, inorganic pigment powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 3.75g phthalocyanine blue powder in above-mentioned steps (1) is added
End, ultrasonic time are 2~3min, are uniformly dispersed, obtain composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Embodiment 2
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) by organic pigment be first phthalocyanine blue, transparent violet B is to grind respectively, and filtered with 800~900 mesh filter screens, obtain
Organic pigment powder, inorganic pigment powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, be added 1.9g phthalocyanine blue powder in above-mentioned steps (1),
1.85g transparent violet B, ultrasonic time are 2~3min, are uniformly dispersed, obtain composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Embodiment 3
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) by organic pigment be first phthalocyanine blue, ultramarine is to grind respectively, and filtered with 800~900 mesh filter screens, had
Machine pigment powder, inorganic pigment powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 3.60g phthalocyanine blue powder in above-mentioned steps (1) is added
End, ultrasonic time are added the 0.15g ultramarine powder in above-mentioned steps (1), continue to be ultrasonically treated, be uniformly dispersed after being 2~3min,
Ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Embodiment 4
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) by organic pigment be first phthalocyanine blue, transparent violet B, ultramarine are to grind respectively, and with 800~900 mesh filter screen mistakes
Filter, obtains organic pigment powder, inorganic pigment powder, spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 will be weighed, heating stirring gradually rises temperature to 250 DEG C,
Then 30~60min is kept, then reduces temperature to 230 DEG C, stirs 40~50min, mixing speed is 1000~1500r/min,
Obtain composite antioxidant mixed liquor I；
(3) 11.25g calcium stearate is weighed, is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), in temperature
30~40min is stirred at 230 DEG C, is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, it is mixed to obtain composite antioxidant
Close liquid II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, be added 1.8g phthalocyanine blue powder in above-mentioned steps (1),
1.8g transparent violet B powder, ultrasonic time are added the 0.15g ultramarine powder in above-mentioned steps (1), continue ultrasound after being 2~3min
Processing, is uniformly dispersed, and ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (4)
180~200 DEG C, obtain composite antioxidant particle.
Embodiment 5
A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, specific method
It is as follows:
(1) by organic pigment be first phthalocyanine blue, ultramarine is to grind respectively, and filtered with 800~900 mesh filter screens, had
Machine pigment powder, inorganic pigment powder, it is spare；
(2) 20g antioxidant 1010, the mixing of 40g irgasfos 168 are weighed, heating stirring gradually rises temperature to 250 DEG C, so
30~60min is kept afterwards, then reduces temperature to 230 DEG C, stirs 40~50min, and mixing speed is 1000~1500r/min, is obtained
To composite antioxidant mixed liquor I；
(3) by the composite antioxidant mixed liquor I in above-mentioned steps (2) under ultrasonic wave ultrasonication, ultrasonic power
For 1000~1200W, frequency 20KHz, temperature is 190~200 DEG C, and the 3.6g phthalocyanine blue powder in above-mentioned steps (1) is added,
The 0.15g ultramarine powder in above-mentioned steps (1) is added in ultrasonic time after being 2~3min, continue to be ultrasonically treated, be uniformly dispersed, and surpasses
The sound time is 3~4min, obtains composite antioxidant lotion；
(4) through double screw extruder extruding pelletization, extruding pelletization temperature is the composite antioxidant lotion in above-mentioned steps (3)
180~200 DEG C, obtain composite antioxidant particle.
Through above-mentioned experiment, the composite antioxidant particle 2g of each embodiment 1-4 preparation, embodiment 5 is taken to prepare compound anti-
Oxygen agent particle 1.71g, is respectively added in the acrylic resin lotion of 1000ml, is uniformly mixed, is molded at 180~210 DEG C
Mold machine extruding pelletization, improved acrylic resin particle.
Comparative example 1
The specific method is as follows:
(1) 0.53g antioxidant 1010,1.07g irgasfos 168,0.3g calcium stearate, 0.1g phthalocyanine blue powder are first weighed respectively
End.
(2) above-mentioned weighed antioxidant 1010, irgasfos 168, calcium stearate are first respectively added to poly- the third of 1000ml
It in olefine resin lotion, is uniformly mixed, adds above-mentioned weighed phthalocyanine blue powder, be uniformly mixed.
(3) injection molding goes out machine extruding pelletization, improved acrylic resin particle at 180~210 DEG C.
Comparative example 2
The specific method is as follows:
(1) 0.53g antioxidant 1010,1.07g irgasfos 168,0.3g calcium stearate, 0.05g phthalocyanine blue are first weighed respectively
Powder, 0.05 transparent violet B powder.
(2) above-mentioned weighed antioxidant 1010, irgasfos 168, calcium stearate are first respectively added to poly- the third of 1000ml
It in olefine resin lotion, is uniformly mixed, adds above-mentioned weighed phthalocyanine blue powder, transparent violet B powder, be uniformly mixed.
(3) injection molding goes out machine extruding pelletization, improved acrylic resin particle at 180~210 DEG C.
Comparative example 3
The specific method is as follows:
(1) 0.53g antioxidant 1010,1.07g irgasfos 168,0.3g calcium stearate, 0.096g phthalocyanine blue are first weighed respectively
Powder, 0.004g ultramarine powder.
(2) above-mentioned weighed antioxidant 1010, irgasfos 168, calcium stearate are first respectively added to poly- the third of 1000ml
It in olefine resin lotion, is uniformly mixed, adds above-mentioned weighed phthalocyanine blue powder, be uniformly mixed, add above-mentioned weighed group
Green powder is uniformly mixed.
(3) injection molding goes out machine extruding pelletization, improved acrylic resin particle at 180~210 DEG C.
Comparative example 4
The specific method is as follows:
(1) it is green that 0.53g antioxidant 1010,1.07g irgasfos 168,0.48g calcium stearate, 0.048g phthalein are first weighed respectively
Blue powder end, 0.048g transparent violet B powder, 0.004g ultramarine powder.
(2) above-mentioned weighed antioxidant 1010, irgasfos 168, calcium stearate are first respectively added to poly- the third of 1000ml
It in olefine resin lotion, is uniformly mixed, adds above-mentioned weighed phthalocyanine blue powder, transparent violet B powder, be uniformly mixed, add
Above-mentioned weighed ultramarine powder is uniformly mixed.
(3) injection molding goes out machine extruding pelletization, improved acrylic resin particle at 180~210 DEG C.
Comparative example 5
The specific method is as follows:
(1) 0.53g antioxidant 1010,1.07g irgasfos 168,0.096g phthalocyanine blue powder, 0.004 group are first weighed respectively
Green powder.
(2) above-mentioned weighed antioxidant 1010, irgasfos 168 are first respectively added to the acrylic resin lotion of 1000ml
In, it is uniformly mixed, adds above-mentioned weighed phthalocyanine blue powder, be uniformly mixed, add above-mentioned weighed ultramarine powder, mix
Uniformly.
(3) injection molding goes out machine extruding pelletization, improved acrylic resin particle at 180~210 DEG C.
It, will the compound antioxygen made from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 through above-mentioned experiment
Agent carrys out the acrylic resin particle of compound acrylic resin resulting improvement, comparative example 1, comparative example 2, comparative example 3, comparative example 4,
The acrylic resin particle of 5 resulting improvement of comparative example is detected through HunterLab LabScan XE chromascope-yellow colour index instrument
Its yellow colour index, as a result as shown in table 9 below:
| Yellow colour index | |
| Blank example | -1.2 |
| Embodiment 1 | -6.1 |
| Embodiment 2 | -7.2 |
| Embodiment 3 | -7.3 |
| Embodiment 4 | -8.2 |
| Embodiment 5 | -2.8 |
| Comparative example 1 | -3.3 |
| Comparative example 2 | -2.9 |
| Comparative example 3 | -3.3 |
| Comparative example 4 | -3.8 |
| Comparative example 5 | -0.8 |
Through described in upper table 9, organic pigment has complementary color effect, organic pigment and inorganic pigment to the flavescence to acrylic resin
The complementary color effect that synergistic effect improves flavescence to polymer is preferable, addition dispersing agent calcium stearate make pigment be uniformly dispersed and
Stablize, the aging yellowing of polymer is further improved, aging of the composite antioxidant that the present invention obtains to acrylic resin
Flavescence effect and color uniformity more preferably, the color of acrylic resin particle saturation degree with higher.
Finally it should be noted that the above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although reference
Above-described embodiment describes the invention in detail, it will be appreciated by those skilled in the art that can still carry out to the present invention
Modification or equivalent replacement should all cover without departing from the spirit or scope of the invention, or any substitutions
In scope of the presently claimed invention.
Claims (7)
1. a kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing, feature exist
In, which uses primary antioxidant, auxiliary antioxidant, dispersing agent, organic pigment, inorganic pigment for main material preparation,
It is specific the preparation method is as follows:
(1) first organic pigment, inorganic pigment are ground respectively, and with 800~900 mesh filter screens filter, obtain organic pigment powder,
Inorganic pigment powder, it is spare；
(2) primary antioxidant, auxiliary antioxidant being mixed, heating stirring gradually rises temperature to 250 DEG C, then keep 30~
60min, then temperature is reduced to 230 DEG C, 40~50min is stirred, mixing speed is 1000~1500r/min, obtains compound antioxygen
Agent mixed liquor I；
(3) dispersing agent then is added in the composite antioxidant mixed liquor I in above-mentioned steps (2), stirs 30 at 230 DEG C of temperature
~40min is uniformly mixed, and is reduced temperature to 200 DEG C, is stirred 40~50min, obtain composite antioxidant mixed liquor II；
(4) by the composite antioxidant mixed liquor II in above-mentioned steps (3) under ultrasonic wave ultrasonication, be added above-mentioned steps
(1) organic pigment powder in, ultrasonic time are added the inorganic pigment powder in above-mentioned steps (1), continue to surpass after being 2~3min
Sonication is uniformly dispersed, and ultrasonic time is 3~4min, obtains composite antioxidant lotion；
(5) for the composite antioxidant lotion in above-mentioned steps (4) through double screw extruder extruding pelletization, extruding pelletization temperature is 180
~200 DEG C, obtain composite antioxidant particle.
2. according to claim 1 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that the primary antioxidant is phenolic antioxidant or amine antioxidants；Auxiliary antioxidant is phosphorous acid
Esters antioxidant or sulphur ester antioxidant；The dispersing agent is calcium stearate or zinc stearate；The organic pigment be phthalocyanine blue,
One or more kinds of arbitrary proportion mixing of transparent violet B, vat brilliant violet RR, transparent green 5B；The inorganic pigment is ultramarine.
3. according to claim 2 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that the primary antioxidant is 1010 antioxidant；Auxiliary antioxidant is 168 antioxidant；The dispersion
Agent is calcium stearate or zinc stearate；The organic pigment is the mixture of phthalocyanine blue and transparent violet B；The inorganic pigment is group
It is green.
4. according to claim 3 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that the gross mass of primary antioxidant and auxiliary antioxidant accounts for primary antioxidant, auxiliary antioxygen in the raw material
The 75%~90% of the main material gross mass that agent, dispersing agent, organic pigment, inorganic pigment form, the primary antioxidant, auxiliary are anti-
The mass ratio of oxygen agent is 1:4~1:0.5.
5. according to claim 4 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that the quality of dispersing agent accounts for primary antioxidant, auxiliary antioxidant, dispersing agent, You Jiyan in the raw material
The 8%~20% of the main material gross mass of material, inorganic pigment composition, remaining is organic pigment powder and inorganic pigment powder.
6. according to claim 5 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that organic pigment powder in the raw material, inorganic pigment powder mass ratio be 17:1~30:1.
7. according to claim 6 a kind of with the more preferable composite antioxidant for improving Polymer Processing and long-term ageing and turning yellow
Preparation method, which is characterized in that the ultrasonication in above-mentioned steps (4), ultrasonic power are 1000~1200W, and frequency is
20KHz, temperature are 190~200 DEG C.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910566431.7A CN110272563A (en) | 2019-06-27 | 2019-06-27 | A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing |
| PCT/CN2019/128319 WO2020258792A1 (en) | 2019-06-27 | 2019-12-25 | Method for preparing composite antioxidant for better improving yellowing of polymer caused by processing and long-term aging |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910566431.7A CN110272563A (en) | 2019-06-27 | 2019-06-27 | A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110272563A true CN110272563A (en) | 2019-09-24 |
Family
ID=67963509
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910566431.7A Pending CN110272563A (en) | 2019-06-27 | 2019-06-27 | A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN110272563A (en) |
| WO (1) | WO2020258792A1 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560138A (en) * | 2020-06-04 | 2020-08-21 | 呈和科技股份有限公司 | Anti-yellowing agent for polyolefin, polyolefin modified premix and polyolefin product |
| WO2020258792A1 (en) * | 2019-06-27 | 2020-12-30 | 江苏极易新材料有限公司 | Method for preparing composite antioxidant for better improving yellowing of polymer caused by processing and long-term aging |
| CN113667182A (en) * | 2021-08-24 | 2021-11-19 | 长春工业大学 | Method for continuously producing aqueous antioxidant emulsion |
| CN114350022A (en) * | 2021-12-03 | 2022-04-15 | 国家能源集团宁夏煤业有限责任公司 | Anti-yellowing antioxidant and application thereof, anti-yellowing polyolefin composition and application thereof, anti-yellowing polyolefin and preparation method and application thereof |
| WO2022169129A1 (en) * | 2021-02-05 | 2022-08-11 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and method for producing same |
| KR20220113599A (en) * | 2021-02-05 | 2022-08-16 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
| KR20220113598A (en) * | 2021-02-05 | 2022-08-16 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070062412A1 (en) * | 2005-03-23 | 2007-03-22 | Basf Corporation | Pigment dispersant, method of making coating compositions, and coating compositions |
| CN103709668A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Color master batch for polyester and preparation method thereof |
| WO2017066974A1 (en) * | 2015-10-23 | 2017-04-27 | 揭东巴黎万株纱华纺织有限公司 | Process for preparing colour masterbatch |
| CN107828169A (en) * | 2017-11-20 | 2018-03-23 | 安徽华美新材料科技有限公司 | A kind of formula and its production technology of the general plastic cement color masterbatch of high power capacity |
| CN108285640A (en) * | 2017-12-26 | 2018-07-17 | 浙江普利特新材料有限公司 | A kind of resisting high-temperature yellowing nylon material and preparation method thereof |
| CN109306138A (en) * | 2018-09-25 | 2019-02-05 | 蚌埠创特新材料科技有限公司 | A kind of polyvinyl chloride resin of high color stability |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709652A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Color master batch for polyethylene glycol terephthalate, and preparation method thereof |
| CN110272563A (en) * | 2019-06-27 | 2019-09-24 | 江苏极易新材料有限公司 | A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing |
-
2019
- 2019-06-27 CN CN201910566431.7A patent/CN110272563A/en active Pending
- 2019-12-25 WO PCT/CN2019/128319 patent/WO2020258792A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070062412A1 (en) * | 2005-03-23 | 2007-03-22 | Basf Corporation | Pigment dispersant, method of making coating compositions, and coating compositions |
| CN103709668A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Color master batch for polyester and preparation method thereof |
| WO2017066974A1 (en) * | 2015-10-23 | 2017-04-27 | 揭东巴黎万株纱华纺织有限公司 | Process for preparing colour masterbatch |
| CN107828169A (en) * | 2017-11-20 | 2018-03-23 | 安徽华美新材料科技有限公司 | A kind of formula and its production technology of the general plastic cement color masterbatch of high power capacity |
| CN108285640A (en) * | 2017-12-26 | 2018-07-17 | 浙江普利特新材料有限公司 | A kind of resisting high-temperature yellowing nylon material and preparation method thereof |
| CN109306138A (en) * | 2018-09-25 | 2019-02-05 | 蚌埠创特新材料科技有限公司 | A kind of polyvinyl chloride resin of high color stability |
Non-Patent Citations (1)
| Title |
|---|
| 论坛 交流: "色母粒专题", 《中国塑料》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020258792A1 (en) * | 2019-06-27 | 2020-12-30 | 江苏极易新材料有限公司 | Method for preparing composite antioxidant for better improving yellowing of polymer caused by processing and long-term aging |
| CN111560138A (en) * | 2020-06-04 | 2020-08-21 | 呈和科技股份有限公司 | Anti-yellowing agent for polyolefin, polyolefin modified premix and polyolefin product |
| WO2022169129A1 (en) * | 2021-02-05 | 2022-08-11 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and method for producing same |
| KR20220113599A (en) * | 2021-02-05 | 2022-08-16 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
| KR20220113598A (en) * | 2021-02-05 | 2022-08-16 | 에스케이씨 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
| KR102514285B1 (en) | 2021-02-05 | 2023-03-28 | 에스케이마이크로웍스 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
| KR102514280B1 (en) | 2021-02-05 | 2023-03-28 | 에스케이마이크로웍스 주식회사 | Polyester resin pellet, polyester film, and preperation method thereof |
| CN113667182A (en) * | 2021-08-24 | 2021-11-19 | 长春工业大学 | Method for continuously producing aqueous antioxidant emulsion |
| CN114350022A (en) * | 2021-12-03 | 2022-04-15 | 国家能源集团宁夏煤业有限责任公司 | Anti-yellowing antioxidant and application thereof, anti-yellowing polyolefin composition and application thereof, anti-yellowing polyolefin and preparation method and application thereof |
| CN114350022B (en) * | 2021-12-03 | 2023-12-22 | 国家能源集团宁夏煤业有限责任公司 | Anti-yellowing antioxidant and application thereof, anti-yellowing polyolefin composition and application thereof, anti-yellowing polyolefin and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2020258792A1 (en) | 2020-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110272563A (en) | A kind of composite antioxidant preparation method to turn yellow with more preferable improvement Polymer Processing and long-term ageing | |
| CN102020871B (en) | Pigment synergist | |
| CN101392077B (en) | Polypropylene color master-batch with pearlescent interference effect and preparation method thereof | |
| DE3708904A1 (en) | PIGMENT PREPARATIONS | |
| DE4325247A1 (en) | Pigment preparations with perylene derivatives as dispersants | |
| CN106751931B (en) | A kind of tertiary colour cake and preparation method thereof | |
| TWI713998B (en) | Preparation of a titanium dioxide-containing slurry and its application to recycled polyester fiber | |
| CN107083705B (en) | A kind of high coloring rate heat sublimation ink and preparation method thereof based on disperse red 60 dyestuff | |
| CN112143184B (en) | Biodegradable color master batch and preparation method thereof | |
| DE102009008740A1 (en) | Easily dispersible solid pigment preparations | |
| CN106117940A (en) | Composite that a kind of aging resistance can infrared penetrate and preparation method thereof | |
| CN108192235A (en) | A kind of PVC hose special color master batch and preparation method thereof | |
| CN114249935A (en) | Weather-resistant color master batch and preparation method thereof | |
| CN1643082A (en) | Black pigment compositions | |
| CN105924926A (en) | Anti-aging infrared-penetrable novel composite material and preparation method thereof | |
| CN108073039A (en) | Blue color blocking, color membrane substrates, liquid crystal display and application | |
| EP1163294B1 (en) | Crimson-colored pigment composition and the utilization thereof | |
| ES2461868T3 (en) | Additive with low powder content and pigment blends with improved color | |
| KR102280464B1 (en) | Color masterbatch composition used for dark-colored textiles or engineering plastics and products thereof | |
| DE2642639A1 (en) | PIGMENT-LIKE 2,9-DICHLORCHINACRIDONE AND THIS PREPARATION | |
| CN107400409A (en) | It is a kind of without glimmering inner-printing ink shown and preparation method thereof | |
| CN114316814B (en) | Packaging adhesive film with color gradual change effect and preparation method thereof | |
| CN116120738B (en) | High-dispersibility, migration-resistant and aging-resistant yellow tool material and preparation method thereof | |
| CN116926703A (en) | Color paste for ultra-high molecular weight polyethylene fiber and dyeing method thereof | |
| CN116554593A (en) | Lighting process LED lamp bead cap weather-resistant pigment and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190924 |
|
| RJ01 | Rejection of invention patent application after publication |