CN106566235A - High-temperature-resistant nylon/attapulgite composite material and preparation method thereof - Google Patents
High-temperature-resistant nylon/attapulgite composite material and preparation method thereof Download PDFInfo
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- CN106566235A CN106566235A CN201510657792.4A CN201510657792A CN106566235A CN 106566235 A CN106566235 A CN 106566235A CN 201510657792 A CN201510657792 A CN 201510657792A CN 106566235 A CN106566235 A CN 106566235A
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- attapulgite
- resistant nylon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- 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
Abstract
The invention discloses a high-temperature-resistant nylon/attapulgite composite material. The high-temperature-resistant nylon/attapulgite composite material is prepared from the following components in parts by weight: 75-89.5 parts of high-temperature-resistant nylon, 0.5-15 parts of modified attapulgite, 3-8 parts of a lubricating agent and 2-7 parts of an antioxidant. The invention further discloses a preparation method of the high-temperature-resistant nylon/attapulgite composite material. The preparation method comprises the following steps: evenly mixing 75-89.5 parts by weight of the dried high-temperature-resistant nylon, 0.5-15 parts by weight of the dried modified attapulgite, 2-7 parts by weight of the antioxidant and 3-8 parts by weight of the lubricating agent, and then pouring the mixture into a hopper of an extruder; and starting the extruder and a vacuum pump, and extruding the mixture via a double-screw extruder, and pelleting and drying the mixture to obtain the high-temperature-resistant nylon/attapulgite composite material. According to the prepared high-temperature-resistant nylon/attapulgite composite material, a processing technology is simple and stable, the attapulgite is uniformly dispersed in high-temperature-resistant nylon resin, the compatibility of the attapulgite and the high-temperature-resistant nylon resin is perfect, and therefore, the high-temperature-resistant nylon/attapulgite composite material has perfect mechanical properties and excellent heat resistance. The material can be widely used for the fields of high temperature, high heat and the like.
Description
Technical field
The invention belongs to composite high-molecular material technical field, more particularly to a kind of high temperature resistant nylon/attapulgite composite material and its
Preparation method.
Background technology
Nylon (polyamide) is a kind of widest thermoplastic engineering plastic of current domestic and international application, and it has tough wear-resisting, resistance to
The excellent specific property such as impact, endurance, corrosion-resistant, oil resistant, is widely used in the row such as auto-parts, electronic apparatus, machinery
Industry, over 60 years, the steady-state growth in the keen competition of engineering plastics, its demand occupy five large-engineering plastics so far always
It is the first.
Attapulgite (attapulgite, abbreviation ATP) is a kind of natural hydration magnesium alumino metasilicate with bar-shaped, needle-shaped crystal structure
Salt, with unique microcosmic crystal structure, exterior appearance, has a wide range of applications as the filler of macromolecular material.
But abundant silicone hydroxyl is contained on its surface, polarity is big, the poor compatibility with non-polar polymer, have impact on ATP nonpolar poly-
Dispersion effect in compound.
Literature searches of the Jing to prior art finds that Chinese patent CN103614804 A disclose a kind of nylon66 fiber/attapulgite
The preparation method of nano-composite fiber, although improve attapulgite and the matrix resin compatibility and scattering problem to a certain extent,
But its application mainly facilitates the production of fiber, with certain limitation.
The content of the invention
For the deficiencies in the prior art, to overcome the attapulgite defect that application is present in the polymer, the purpose of the present invention is to carry
For a kind of high temperature resistant nylon/attapulgite composite material and preparation method thereof.
For achieving the above object, the present invention is employed the following technical solutions：
The invention provides a kind of high temperature resistant nylon/attapulgite composite material, is made up of the component comprising following weight portion：
The high temperature resistant nylon be selected from PA610T, PA66T, PA6T/6I, PA10T, PA9T or PA12T, preferred PA610T,
PA66T、PA6T/6I。
It is described it is attapulgite modified be to be prepared by following methods：By attapulgite, under the conditions of 100～115 DEG C, drying 4～6 is little
When, to remove wherein moisture；The KH550 for weighing dry attapulgite and attapulgite quality 3% is dissolved in 200～350ml ice
In acetic acid, by above-mentioned solution in 40～45 DEG C of ultrasonic disperses 40 minutes；Then there-necked flask is placed in water-bath, stirring heats up,
40～45 DEG C of bath temperature of control, response time are 3 hours；Finally by reacted mixture vacuum filtration, produce after sucking filtration
Thing is washed with dehydrated alcohol, deionized water for several times successively, obtains attapulgite modified after dry, crushing.
The attapulgite is selected from Anhui Ming Mei mineral Chemical Co., Ltd., and particular technique index is as follows, outward appearance：Light gray-white surpasses
Fine powder, viscosity >=2500cps, bulk density≤0.44g/ml, fineness is 325 mesh, dry screen is remaining≤and 1%, moisture≤15%,
PH value is 8.0～9.5.
The lubricant is ethylene acrylic acid co polymer (A-C540A).
The antioxidant is antioxidant 1010, antioxidant 107, antioxidant 1790, antioxidant 1098, irgasfos 168 or antioxygen
One or two kinds of compounding in agent S9228, preferred antioxidant 1098 and irgasfos 168 compounding or antioxidant 1790 and antioxygen
Agent S9228 is compounded, and the two compound proportion is 1:1.
Present invention also offers a kind of preparation method of above-mentioned high temperature resistant nylon/attapulgite composite material, comprises the following steps：
By 75～89.5 parts of high temperature resistant nylon after drying, it is dried 0.5～15 part of post-modification attapulgite, 2～7 parts of antioxidant and lubrication
Extruder hopper is poured into after 3～8 parts of mix homogeneously of agent；Startup extruder, unlatching vacuum pump, Jing double screw extruder extruding pelletizations,
It is dried, obtains high temperature resistant nylon/attapulgite composite material.
After the drying, high temperature resistant nylon is dried 6～10 hours under the conditions of temperature is for 100～120 DEG C.
The post-modification attapulgite that is dried is dried 4～6 hours under the conditions of temperature is for 100～115 DEG C.
It is described it is attapulgite modified be to be prepared by following methods：Weigh dry attapulgite and attapulgite quality 3%
KH550 is dissolved in 200～350ml glacial acetic acids, by above-mentioned solution in 40～45 DEG C of ultrasonic disperses 40 minutes；Then by there-necked flask
It is placed in water-bath, stirring heats up, controls 40～45 DEG C of bath temperature, the response time is 3 hours；Finally by reacted mixing
Thing vacuum filtration, takes out filtered product and is washed with dehydrated alcohol, deionized water successively for several times, is changed after dry, crushing
Property attapulgite.
The screw slenderness ratio of the double screw extruder is (30～50):1, extrusion temperature is 300～340 DEG C from 1st area to head scope,
Rotating speed is 200～350r/min.
The Jing double screw extruders extruding pelletization, drying are dried 2～6 hours under the conditions of temperature is for 90～110 DEG C.
The present invention compared with the existing technology, with advantages below：
The materials hot deformation temperature that the present invention is provided is high, fine heat-resisting performance；Preparation technology is relatively simple, is easy to commercial introduction；
Expressing technique is stable, and material property is superior；Attapulgite is good with the resin matrix compatibility and is uniformly dispersed.
High temperature resistant nylon/the attapulgite composite material prepared by the present invention, processing technique simple and stable, attapulgite exist
It is uniformly dispersed in high temperature resistant nylon resin, the two compatibility is ideal, therefore with preferable mechanical property and excellent heat-resisting
Performance；The material can be widely applied to the fields such as high temperature hyperpyrexia.
Specific embodiment
With reference to embodiment, the present invention is further detailed explanation.
Attapulgite employed in following examples is selected from Anhui Ming Mei mineral Chemical Co., Ltd., and particular technique index is as follows,
Outward appearance：Light gray-white superfines, viscosity >=2500cps, bulk density≤0.44g/ml, fineness is 325 mesh, dry screen is remaining≤
1%, moisture≤15%, pH value are 8.0～9.5.
Below in an example, using following detection method：
Tensile property presses ASTM D638-10 tests, rate of extension 5mm/min.
Simply supported beam notch impact strength presses ASTM D6110-10 tests.
Bending strength presses ASTM D790-10 tests, pushes speed 1.25mm/min.
Heat distortion temperature presses ASTM D1525-09 tests.
Embodiment 1
A kind of preparation method of high temperature resistant nylon/attapulgite composite material, is made up of by weight following components：High temperature resistant nylon
Resin PA66T：It is 89.5 parts, attapulgite modified：0.5 part, lubricant (ethylene acrylic acid co polymer A-C540A)：3 parts,
Antioxidant (antioxidant 1098：Irgasfos 168 compounding=1：1)：7 parts, nylon resin PA66T is done under the conditions of 100 DEG C
Dry 10 hours with fully removing wherein moisture；
6 hours are dried under the conditions of 100 DEG C fully to remove wherein moisture by attapulgite modified；
High temperature resistant nylon resin PA66T, attapulgite modified, antioxidant, lubricant are sufficiently mixed in homogenizer
It is even to pour extruder hopper into；Start extruder, and open vacuum pump, Jing double screw extruder extruding pelletizations are dried, obtain resistance to
High-temperature nylon/attapulgite composite material.
It is described it is attapulgite modified be to be prepared by following methods：Attapulgite is dried 6 hours under the conditions of 100 DEG C, with
Remove wherein moisture；Weigh the attapulgite and 6gKH550 (the 3% of attapulgite quality) and 200ml ice second of 200g dryings
Acid in there-necked flask, by above-mentioned solution in 40-45 DEG C or so ultrasonic disperse 40 minutes；Then there-necked flask is placed in water-bath,
Stirring heats up, control bath temperature (40-45 DEG C), and the response time is 3 hours；Finally reacted mixture is taken out with vacuum
Filter, takes out filtered product and is washed with dehydrated alcohol, deionized water successively for several times, obtains modified attapulgite after dry, crushing
Soil is with standby；
The screw slenderness ratio of the double screw extruder is 30:1, extrusion temperature from 1st area to head be respectively 305 DEG C, 310 DEG C,
315 DEG C, 320 DEG C, 330 DEG C, 335 DEG C, 340 DEG C, rotating speed is 200r/min；
The Jing double screw extruders extruding pelletization, drying are dried 6 hours under the conditions of temperature is for 90 DEG C.
The injection mo(u)lding on injection machine by high temperature resistant nylon/attapulgite composite material, injection temperature it is interval for 330 DEG C, 335 DEG C,
325 DEG C, the batten for correlated performance test is obtained, detailed performance is shown in Table 1.
Embodiment 2
A kind of preparation method of high temperature resistant nylon/attapulgite composite material, is made up of by weight following components：High temperature resistant nylon
Resin PA6T/6I：It is 82.5 parts, attapulgite modified：7.5 parts, lubricant (ethylene acrylic acid co polymer A-C540A)：5
Part, antioxidant (antioxidant 1098：Irgasfos 168 compounding=1：1)：5 parts, by high temperature resistant nylon resin PA6T/6I in 105 DEG C
Under the conditions of be dried 8 hours fully to remove wherein moisture；
5 hours are dried under the conditions of 105 DEG C fully to remove wherein moisture by attapulgite modified；
High temperature resistant nylon resin PA6T/6I, attapulgite modified, antioxidant, lubricant are sufficiently mixed in homogenizer
Extruder hopper is poured into uniformly；Start extruder, and open vacuum pump, Jing double screw extruder extruding pelletizations are dried, obtain
High temperature resistant nylon/attapulgite composite material；
It is described it is attapulgite modified be to be prepared by following methods：Attapulgite is dried 5 hours under the conditions of 105 DEG C, with
Remove wherein moisture；Weigh the KH550 (the 3% of attapulgite quality) and 300ml of the attapulgite and 7.5g of 250g dryings
Glacial acetic acid in there-necked flask, by above-mentioned solution in 40-45 DEG C or so ultrasonic disperse 40 minutes；Then there-necked flask is placed in into water
In bath, stirring heats up, control bath temperature (40-45 DEG C), and the response time is 3 hours；Finally reacted mixture is used
Vacuum filtration, takes out filtered product and is washed with dehydrated alcohol, deionized water successively for several times, obtains modified after dry, crushing
Attapulgite is with standby；
The screw slenderness ratio of the double screw extruder is 40:1, extrusion temperature from 1st area to head be respectively 300 DEG C, 305 DEG C,
310 DEG C, 315 DEG C, 320 DEG C, 330 DEG C, 335 DEG C, rotating speed is 260r/min；
The Jing double screw extruders extruding pelletization, drying are dried 4 hours under the conditions of temperature is for 100 DEG C.
The injection mo(u)lding on injection machine by high temperature resistant nylon/attapulgite composite material, injection temperature it is interval for 325 DEG C, 330 DEG C,
320 DEG C, the batten for correlated performance test is obtained, detailed performance is shown in Table 1.
Embodiment 3
A kind of preparation method of high temperature resistant nylon/attapulgite composite material, is made up of by weight following components：High temperature resistant nylon
Resin PA610T：It is 75 parts, attapulgite modified：15 parts, lubricant (ethylene acrylic acid co polymer A-C540A)：8 parts,
Antioxidant (antioxidant 1098：Irgasfos 168 compounding=1：1)：2 parts；By high temperature resistant nylon resin PA610T in 120 DEG C of bars
It is dried 6 hours fully to remove wherein moisture under part；
4 hours are dried under the conditions of 115 DEG C fully to remove wherein moisture by attapulgite modified；
High temperature resistant nylon resin PA610T, attapulgite modified, antioxidant, lubricant are sufficiently mixed in homogenizer
It is even to pour extruder hopper into；Start extruder, and open vacuum pump, Jing double screw extruder extruding pelletizations are dried, obtain resistance to
High-temperature nylon/attapulgite composite material.
It is described it is attapulgite modified be to be prepared by following methods：Attapulgite is dried 4 hours under the conditions of 115 DEG C, with
Remove wherein moisture；Weigh the attapulgite and 9gKH550 (the 3% of attapulgite quality) and 350ml ice second of 300g dryings
Acid in there-necked flask, by above-mentioned solution in 40-45 DEG C or so ultrasonic disperse 40 minutes；Then there-necked flask is placed in water-bath,
Stirring heats up, control bath temperature (40-45 DEG C), and the response time is 3 hours；Finally reacted mixture is taken out with vacuum
Filter, takes out filtered product and is washed with dehydrated alcohol, deionized water successively for several times, obtains modified attapulgite after dry, crushing
Soil is with standby.
The screw slenderness ratio of the double screw extruder is 50:1, extrusion temperature from 1st area to head be respectively 300 DEG C, 305 DEG C,
310 DEG C, 315 DEG C, 320 DEG C, 330 DEG C, 335 DEG C, rotating speed is 350r/min；
The Jing double screw extruders extruding pelletization, drying are dried 2 hours under the conditions of temperature is for 110 DEG C.
The injection mo(u)lding on injection machine by high temperature resistant nylon/attapulgite composite material, injection temperature it is interval for 325 DEG C, 330 DEG C,
320 DEG C, the batten for correlated performance test is obtained, detailed performance is shown in Table 1.
Comparative example 1
Nylon66 fiber T is dried into 8 hours fully to remove wherein moisture under the conditions of 100 DEG C, high temperature resistant nylon resin is weighed
PA66T：89.5 parts, unmodified attapulgite：0.5 part, lubricant (ethylene acrylic acid co polymer A-C540A)：3 parts,
Antioxidant (antioxidant 1098：Irgasfos 168 compounding=1：1)：7 parts, uniform rear extruding pelletization is sufficiently mixed, finally in note
Molding machine injection mo(u)lding, it is 325,330,320 that injection temperature is interval, obtains the batten for correlated performance test, and with enforcement
Example 1 is contrasted, and detailed performance is shown in Table 1.
Comparative example 2
Nylon 6T6I is dried into 8 hours fully to remove wherein moisture under the conditions of 100 DEG C, high temperature resistant nylon resin is weighed
PA6T6I：90 parts, lubricant (ethylene acrylic acid co polymer A-C540A)：5 parts, antioxidant (antioxidant 1098：Antioxygen
Agent 168 compounds=1：1)：5 parts, be sufficiently mixed it is uniform, finally in injection machine injection mo(u)lding, injection temperature it is interval for 320,325,
315, the batten for correlated performance test is obtained, and is contrasted with embodiment 2, detailed performance is shown in Table 1.
Table 1
Comparative example 1 is compared with the properties of product of comparative example 1 as can be seen that relative to unmodified attapulgite, being modified concavo-convex
The addition of rod soil, the tensile strength of material property, impact strength, bending strength, heat distortion temperature etc. are improved significantly.
Illustrate that silane coupler serves fine modified effect to attapulgite, while also demonstrating resin and attapulgite to a certain extent
The compatibility it is preferable.Compare from the properties of product of comparative example 2 and embodiment 2 as can be seen that attapulgite modified addition can be big
Width improves nylon resin materials performance, so as to widen its range of application.
By the implementation process and testing result of each embodiment, it is known that by preparation method of the present invention 0.5～15 part of modified attapulgite
The composite that soil is obtained in being added to fire resistant resin, on the premise of the smooth processing and forming of system is guaranteed, can make material have reason
The mechanical property thought and heat resistance, with preferable market using value.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply the present invention.It is familiar with
The personnel of art technology obviously easily can make various modifications to these embodiments, and should General Principle described herein
Use in other embodiment without through performing creative labour.Therefore, the invention is not restricted to embodiment here, this area skill
Art personnel announcement of the invention, the improvement made without departing from scope and modification all should be in the protection models of the present invention
Within enclosing.
Claims (10)
1. a kind of high temperature resistant nylon/attapulgite composite material, it is characterised in that：It is made up of the component comprising following weight portion：
2. high temperature resistant nylon/attapulgite composite material according to claim 1, it is characterised in that：The high temperature resistant Buddhist nun
Dragon is selected from PA610T, PA66T, PA6T/6I, PA10T, PA9T or PA12T, preferred PA610T, PA66T, PA6T/6I.
3. high temperature resistant nylon/attapulgite composite material according to claim 1, it is characterised in that：It is described modified concavo-convex
Rod soil is prepared by following methods：Attapulgite is dried 4～6 hours under the conditions of 100～115 DEG C；Weigh dry recessed
The KH550 of convex rod soil and attapulgite quality 3% is dissolved in 200～350ml glacial acetic acids, and above-mentioned solution is ultrasonic at 40～45 DEG C
Dispersion 40 minutes；Then there-necked flask is placed in water-bath, stirring heats up, controls 40～45 DEG C of bath temperature, the response time is
3 hours；Finally by reacted mixture vacuum filtration, take out filtered product and washed with dehydrated alcohol, deionized water successively
Wash for several times, after dry, crushing, obtain attapulgite modified.
4. high temperature resistant nylon/attapulgite composite material according to claim 3, it is characterised in that：The attapulgite
Viscosity >=2500cps, bulk density≤0.44g/ml, fineness is 325 mesh, and dry screen is remaining≤1%, moisture≤15%, and pH value is
8.0～9.5.
5. high temperature resistant nylon/attapulgite composite material according to claim 1, it is characterised in that：The lubricant is
Ethylene acrylic acid co polymer.
6. high temperature resistant nylon/attapulgite composite material according to claim 1, it is characterised in that：The antioxidant is
One kind in antioxidant 1010, antioxidant 107, antioxidant 1790, antioxidant 1098, irgasfos 168 or antioxidant S9228
Or two kinds of compoundings, preferred antioxidant 1098 and irgasfos 168 compounding or antioxidant 1790 and antioxidant S9228 compoundings, two
Person's compound proportion is 1:1.
7. the preparation method of the arbitrary described high temperature resistant nylon/attapulgite composite material of a kind of claim 1 to 6, its feature
It is：Comprise the following steps：
By 75～89.5 parts of high temperature resistant nylon after drying, it is dried 0.5～15 part of post-modification attapulgite, 2～7 parts of antioxidant and lubrication
Extruder hopper is poured into after 3～8 parts of mix homogeneously of agent；Startup extruder, unlatching vacuum pump, Jing double screw extruder extruding pelletizations,
It is dried, obtains high temperature resistant nylon/attapulgite composite material.
8. the preparation method of high temperature resistant nylon/attapulgite composite material according to claim 7, it is characterised in that：Institute
Stating high temperature resistant nylon after being dried is dried 6～10 hours under the conditions of temperature is for 100～120 DEG C；
Or the post-modification attapulgite that is dried is dried 4～6 hours under the conditions of temperature is for 100～115 DEG C.
9. the preparation method of high temperature resistant nylon/attapulgite composite material according to claim 7, it is characterised in that：Institute
Stating attapulgite modified is prepared by following methods：Weigh the KH550 of dry attapulgite and attapulgite quality 3%
It is dissolved in 200～350ml glacial acetic acids, by above-mentioned solution in 40～45 DEG C of ultrasonic disperses 40 minutes；Then there-necked flask is placed in into water
In bath, stirring heats up, and controls 40～45 DEG C of bath temperature, and the response time is 3 hours；Finally by reacted mixture with very
Empty sucking filtration, takes out filtered product and is washed with dehydrated alcohol, deionized water successively for several times, obtains modified concavo-convex after dry, crushing
Rod soil.
10. the preparation method of high temperature resistant nylon/attapulgite composite material according to claim 7, it is characterised in that：Institute
The screw slenderness ratio for stating double screw extruder is (30～50):1, extrusion temperature is 300～340 DEG C from 1st area to head scope, is turned
Speed is 200～350r/min；
Or the Jing double screw extruders extruding pelletization, drying are dried 2～6 hours under the conditions of temperature is for 90～110 DEG C.
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