CN114196195B - Preparation method of PA6 wave-absorbing master batch and product thereof - Google Patents
Preparation method of PA6 wave-absorbing master batch and product thereof Download PDFInfo
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- CN114196195B CN114196195B CN202111589331.XA CN202111589331A CN114196195B CN 114196195 B CN114196195 B CN 114196195B CN 202111589331 A CN202111589331 A CN 202111589331A CN 114196195 B CN114196195 B CN 114196195B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses a preparation method of PA6 wave-absorbing master batch and a product thereof, comprising the steps of preparing dry PA6 powder; preparing wave-absorbing microcapsule particles: dissolving a PA6 slice in dimethylformamide to prepare a PA6 dimethylamide solution, adding carbonyl iron powder into the PA6 dimethylamide solution, performing ultrasonic oscillation, ethanol cleaning, suction filtration and drying to obtain wave-absorbing microcapsule particles; preparing master batches: uniformly mixing the wave-absorbing microcapsule particles and the dried PA6 powder to obtain a mixture, adding the mixture into an extruder, and extruding and granulating after melt mixing to obtain the PA6 wave-absorbing master batch. The invention provides a preparation method of a PA6 wave-absorbing master batch, which can reduce pollution to the wave-absorbing master batch in the preparation process and improve the wave-absorbing performance of the wave-absorbing master batch.
Description
Technical Field
The invention belongs to the field of master batch material preparation, and particularly relates to a preparation method of PA6 wave-absorbing master batch and a product thereof.
Background
PA6 engineering plastic name: polyamide 6, nylon 6, traits: translucent or opaque milky white crystalline polymer, characteristics: the thermoplastic, light, toughness, chemical resistance and durability are good, and can be applied to the fields of clothing, construction, chemical industry and the like.
In recent years, with the development of functional master batch technology, wave-absorbing master batch is rapidly developed. However, the prior wave-absorbing master batch has a plurality of defects, so that the use is limited.
At present, in the existing wave-absorbing master batch production process, a stirrer is generally adopted for crushing and mixing, an extruder is used for extrusion, shearing force is applied in the stirring, crushing and extrusion processes, and wave-absorbing metal particles have the characteristics of larger hardness and high melting point, so that the wave-absorbing metal particles rub against the inner wall of a machine in the stirring, mixing and melting mixing processes, impurities are easy to appear, the wave-absorbing master batch is polluted in the preparation process, the performance of the wave-absorbing master batch is further reduced, the higher the content of the wave-absorbing metal particles is, the friction probability between the wave-absorbing metal particles and the inner wall of the machine is increased, and the serious pollution to the wave-absorbing master batch is caused.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of PA6 wave-absorbing master batch.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of PA6 wave-absorbing master batch comprises,
preparing dry PA6 powder;
preparing wave-absorbing microcapsule particles: dissolving a PA6 slice in dimethylformamide to prepare a PA6 dimethylamide solution, adding carbonyl iron powder into the PA6 dimethylamide solution, performing ultrasonic oscillation, ethanol cleaning, suction filtration and drying to obtain wave-absorbing microcapsule particles;
preparing master batches: uniformly mixing the wave-absorbing microcapsule particles and the dried PA6 powder to obtain a mixture, adding the mixture into an extruder, and extruding and granulating after melt mixing to obtain the PA6 wave-absorbing master batch.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the particle size of the PA6 powder is 0.8-1.5 mm, and the water content of the PA6 powder is less than or equal to 800ppm.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the preparation method of the dry PA6 powder comprises the following steps of,
after the PA6 slice is crushed and ground, PA6 particles pass through a plurality of layers of sieve plates which are sequentially arranged layer by layer, flowing hot air is introduced between the sieve plates, the pore diameter of the sieve plates is reduced layer by layer, PA6 particles with small particle size fall to a lower layer sieve plate through the sieve holes, the PA6 particles are dried by hot air in the falling process, and the PA6 particles with large particle size are recovered and continuously ground to finally obtain dry PA6 powder.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the microwave absorbing microcapsule particles are prepared, wherein the mass-volume ratio of the PA6 slice to the dimethylamide is 1:5 in g/mL.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the microwave absorbing microcapsule particles are prepared, wherein the mass volume ratio of carbonyl iron powder to a dimethylamide solution of PA6 is as follows: the mL is 1:10-1:20.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the ultrasonic vibration is carried out, wherein the power is 600W, the time is 15min, and the temperature is 65 ℃.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: and drying to obtain the wave-absorbing microcapsule particles, wherein the drying temperature is 80 ℃ and the drying time is 4 hours.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: and uniformly mixing the wave-absorbing microcapsule particles and the dried PA6 powder, wherein the mass ratio of the wave-absorbing microcapsule particles to the dried PA6 powder is 1:2-4.
As a preferable scheme of the preparation method of the PA6 wave-absorbing master batch, the invention comprises the following steps: the extruder is a lining type charging barrel extruder, a lining of a carbonyl iron powder layer is arranged in a charging barrel of the lining type charging barrel extruder, and the rotating speed of a screw rod of the lining type charging barrel extruder is 80-150 r/min; and extruding and granulating after melting and mixing, wherein the double-screw extrusion temperature is 275 ℃.
The invention aims to overcome the defects in the prior art and provide the PA6 wave-absorbing master batch prepared by the preparation method of the PA6 wave-absorbing master batch.
The invention has the beneficial effects that:
the invention provides a preparation method of PA6 wave-absorbing master batch, which is characterized in that PA6 capsule materials are wrapped outside carbonyl iron powder to form wave-absorbing microcapsule particles, so that abrasion of the carbonyl iron powder to a machine in the production process is reduced, pollution to the wave-absorbing master batch is reduced, and the PA6 capsule materials are the same as the base material PA6 powder materials of the wave-absorbing master batch, so that the PA6 wave-absorbing master batch with higher uniformity can be prepared;
according to the invention, the replaceable carbonyl iron bushing is assembled in the charging barrel of the bushing type charging barrel extruder, and when the PA6 capsule material outside the wave-absorbing microcapsule particles is melted in the melting and mixing process, the carbonyl iron powder rubs with the inner wall of the carbonyl iron bushing, and the generated substances are carbonyl iron powder, so that the pollution of wave-absorbing master batches is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
fig. 1 is a diagram of PA6 wave-absorbing master batch prepared in the example of the present invention.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
PA6 sections of the invention: guangdong New Conmeida Chinlon stock Co., ltd; carbonyl iron powder: the Jiangsu Tian superfine metal powder Co., ltd are all common commercial products.
Example 1
Preparation of PA6 powder: after the PA6 slices are crushed and ground, PA6 particles pass through a plurality of layers of sieve plates which are sequentially arranged, flowing hot air is introduced between the sieve plates, the pore diameters of the sieve plates are reduced layer by layer, PA6 particles with small particle diameters fall to a lower layer sieve plate through the sieve holes, the PA6 particles are dried by the hot air in the falling process, and the PA6 particles with large particle diameters are recovered and continuously ground to finally obtain PA6 powder with the particle diameters smaller than 0.8mm and dried;
and (3) preparing wave-absorbing microcapsule particles: weighing 20gPA slices, dissolving in a beaker containing 100mL of dimethylformamide, stirring at normal temperature until the slices are dissolved, adding 10g of carbonyl iron powder, carrying out ultrasonic vibration, ethanol cleaning and filtering, and drying in a forced air drying oven at 80 ℃ until the weight is constant to obtain the wave-absorbing microcapsule particles.
Preparing master batches: mixing the microwave absorbing microcapsule particles and PA6 powder according to a mass ratio of 1:3, wherein the speed of the mixing is 50r/min, the temperature of the mixing is kept at 25 ℃, a mixture is obtained after uniform mixing, the mixture is added into a bushing type barrel extruder with the screw speed of 80r/min, a bushing of a carbonyl iron powder layer is arranged in a barrel of the bushing type barrel extruder, and the mixture is extruded and granulated after melt mixing at 220 ℃ to obtain the PA6 microwave absorbing master batch.
Example 2:
preparation of PA6 powder: after the PA6 slices are crushed and ground, PA6 particles pass through a plurality of layers of sieve plates which are sequentially arranged layer by layer, flowing hot air is introduced between the sieve plates, the pore diameter of the sieve plates is reduced layer by layer, PA6 particles with small particle size fall to a lower layer sieve plate through the sieve holes, the PA6 particles are dried by the hot air in the falling process, and the PA6 particles with large particle size are recovered and continuously ground to finally obtain PA6 powder with the particle size of about 1mm and dried;
and (3) preparing wave-absorbing microcapsule particles: weighing 20gPA slices, dissolving in a beaker containing 100mL of dimethylformamide, stirring at normal temperature until the slices are dissolved, adding 8g of carbonyl iron powder, carrying out ultrasonic vibration, ethanol cleaning and filtering, and drying in a forced air drying oven at 70 ℃ until the weight is constant, thus obtaining the wave-absorbing microcapsule particles.
Preparing master batches: mixing the microwave absorbing microcapsule particles and PA6 powder according to a mass ratio of 1:3, wherein the speed of the mixing is 80r/min, the temperature of the mixing is kept at 25 ℃, a mixture is obtained after uniform mixing, the mixture is added into a bushing type barrel extruder with the screw speed of 100r/min, a bushing of a carbonyl iron powder layer is arranged in a barrel of the bushing type barrel extruder, and the mixture is extruded and granulated after melt mixing at 220 ℃ to obtain the PA6 microwave absorbing master batch.
Example 3:
preparation of PA6 powder: after the PA6 slices are crushed and ground, PA6 particles pass through a plurality of layers of sieve plates which are sequentially arranged, flowing hot air is introduced between the sieve plates, the pore diameters of the sieve plates are reduced layer by layer, PA6 particles with small particle diameters fall to a lower layer sieve plate through the sieve holes, the PA6 particles are dried by the hot air in the falling process, and the PA6 particles with large particle diameters are recovered and continuously ground to finally obtain PA6 powder with the particle diameters of about 1.5mm and dried;
and (3) preparing wave-absorbing microcapsule particles: weighing 20gPA slices, dissolving in a beaker containing 100mL of dimethylformamide, stirring at normal temperature until the slices are dissolved, adding 5g of carbonyl iron powder, carrying out ultrasonic vibration, ethanol cleaning and filtering, and drying in a forced air drying oven at 70 ℃ until the weight is constant, thus obtaining the wave-absorbing microcapsule particles.
Preparing master batches: mixing the microwave absorbing microcapsule particles and PA6 powder according to a mass ratio of 1:3, wherein the speed of the mixing is 90r/min, the temperature of the mixing is kept at 25 ℃, a mixture is obtained after uniform mixing, the mixture is added into a bushing type barrel extruder with the screw speed of 150r/min, a bushing of a carbonyl iron powder layer is arranged in a barrel of the bushing type barrel extruder, and the mixture is extruded and granulated after melt mixing at 220 ℃ to obtain the PA6 microwave absorbing master batch.
Comparative example 1:
preparing master batches: mixing carbonyl iron powder and PA6 slices according to a mass ratio of 1:3, stirring and mixing at a speed of 200r/min, uniformly mixing to obtain a mixture, adding the mixture into a bushing type barrel extruder with a screw speed of 300r/min, and extruding and granulating after melt mixing at a temperature of 180 ℃ to obtain PA6 wave-absorbing master batch.
The PA6 absorbing master batches prepared in examples 1 to 3 were subjected to the absorbing test and compared with comparative example 1, specifically as shown in table 1 below.
TABLE 1 test of wave absorbing Properties of the PA6 wave absorbing masterbatch of the invention
Wherein the reflectivity is the reflectivity in the frequency range of 1-18GHZ under the condition that the master batch is pressed into a flat plate with the thickness of 180mm multiplied by 5 mm; measurement of reflectivity reference standard "method for testing reflectivity of Radar absorbing Material GJB2038A-2011
As can be seen from the data in Table 1, the preparation method of the invention can obviously improve the performance of the PA6 wave-absorbing master batch, particularly the wave-absorbing performance is improved substantially, and a plurality of tests prove that the method can reduce the pollution to the wave-absorbing master batch in the preparation process, improve the wave-absorbing performance of the wave-absorbing master batch, and under the condition of emitting equal amount of electromagnetic waves, the reflectivity of the PA wave-absorbing master batch prepared by the invention is lower, more absorbed electromagnetic waves are represented, and the wave-absorbing performance is better.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (10)
1. A preparation method of PA6 wave-absorbing master batch is characterized in that: comprising the steps of (a) a step of,
preparing dry PA6 powder;
preparing wave-absorbing microcapsule particles: dissolving a PA6 slice in dimethylformamide to prepare a PA6 dimethylamide solution, adding carbonyl iron powder into the PA6 dimethylamide solution, performing ultrasonic oscillation, ethanol cleaning, suction filtration and drying to obtain wave-absorbing microcapsule particles;
preparing master batches: uniformly mixing the wave-absorbing microcapsule particles and the dried PA6 powder to obtain a mixture, adding the mixture into an extruder, and extruding and granulating after melt mixing to obtain the PA6 wave-absorbing master batch.
2. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: the particle size of the PA6 powder is 0.8-1.5 mm, and the water content of the PA6 powder is less than or equal to 800ppm.
3. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: the preparation method of the dry PA6 powder comprises the following steps of,
after the PA6 slice is crushed and ground, PA6 particles pass through a plurality of layers of sieve plates which are sequentially arranged layer by layer, flowing hot air is introduced between the sieve plates, the pore diameter of the sieve plates is reduced layer by layer, PA6 particles with small particle size fall to a lower layer sieve plate through the sieve holes, the PA6 particles are dried by hot air in the falling process, and the PA6 particles with large particle size are recovered and continuously ground to finally obtain dry PA6 powder.
4. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: the microwave absorbing microcapsule particles are prepared, wherein the mass-volume ratio of the PA6 slice to the dimethylamide is 1:5 in g/mL.
5. The method for preparing the PA6 wave-absorbing master batch according to claim 1 or 4, wherein: the microwave absorbing microcapsule particles are prepared, wherein the mass volume ratio of carbonyl iron powder to a dimethylamide solution of PA6 is as follows: the mL is 1:10-1:20.
6. The method for preparing the PA6 wave-absorbing master batch according to any one of claims 1 to 4, characterized in that: the ultrasonic vibration is carried out, wherein the power is 600W, the time is 15min, and the temperature is 65 ℃.
7. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: and drying to obtain the wave-absorbing microcapsule particles, wherein the drying temperature is 80 ℃ and the drying time is 4 hours.
8. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: and uniformly mixing the wave-absorbing microcapsule particles and the dried PA6 powder, wherein the mass ratio of the wave-absorbing microcapsule particles to the dried PA6 powder is 1:2-4.
9. The method for preparing the PA6 wave-absorbing master batch according to claim 1, wherein: the extruder is a lining type charging barrel extruder, a lining of a carbonyl iron powder layer is arranged in a charging barrel of the lining type charging barrel extruder, and the rotating speed of a screw rod of the lining type charging barrel extruder is 80-150 r/min; and extruding and granulating after melting and mixing, wherein the double-screw extrusion temperature is 275 ℃.
10. The PA6 wave-absorbing master batch produced by the production method of the PA6 wave-absorbing master batch according to any one of claims 1 to 9.
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| CN103483792A (en) * | 2012-06-14 | 2014-01-01 | 潘智军 | Wave absorption and radiation protection plastic and preparation method thereof |
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| CN113352706A (en) * | 2021-06-15 | 2021-09-07 | 武汉中科先进技术研究院有限公司 | Basalt fiber structural wave-absorbing composite material and preparation method thereof |
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- 2021-12-23 CN CN202111589331.XA patent/CN114196195B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20050018422A (en) * | 2003-08-13 | 2005-02-23 | 주식회사 이엠에프 세이프티 | Electromagenetic wave absorptive material composed of ferrite composite material and its manufacturing method |
| WO2012089081A1 (en) * | 2010-12-28 | 2012-07-05 | 上海杰事杰新材料(集团)股份有限公司 | Nano particle/polyamide composite material, preparation method therefor, and use thereof |
| CN103483792A (en) * | 2012-06-14 | 2014-01-01 | 潘智军 | Wave absorption and radiation protection plastic and preparation method thereof |
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| CN113352706A (en) * | 2021-06-15 | 2021-09-07 | 武汉中科先进技术研究院有限公司 | Basalt fiber structural wave-absorbing composite material and preparation method thereof |
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