CN108659254A - The preparation method of polyetherimide expanded moldings - Google Patents
The preparation method of polyetherimide expanded moldings Download PDFInfo
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- CN108659254A CN108659254A CN201710197119.6A CN201710197119A CN108659254A CN 108659254 A CN108659254 A CN 108659254A CN 201710197119 A CN201710197119 A CN 201710197119A CN 108659254 A CN108659254 A CN 108659254A
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- Prior art keywords
- polyetherimide
- preparation
- expanded
- particle
- adhesive
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/224—Surface treatment
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
- C08J9/236—Forming foamed products using binding agents
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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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to thermoplastic material technical fields, and in particular to a kind of preparation method of polyetherimide expanded moldings.The preparation method includes the following steps：Obtain polyetherimide expanded particle；By the surface adhesive coating of the polyetherimide expanded particle；Hot-press solidifying processing will be carried out in the polyetherimide expanded particle injection mold for being coated with adhesive, obtains polyetherimide expanded moldings.The preparation method of polyetherimide expanded moldings provided by the invention, adhesive is directly evenly applied to polyetherimide expanded particle surface, it is injected into mold again, it is compressed, be heating and curing to obtain, therefore this method is simple and practicable, it is easy to industrialized production, the thermoplastic polyimide expanded moldings material being prepared has many advantages, such as that density is low, size shape is controllable, do not have shed powder using process, has a good application prospect.
Description
Technical field
The invention belongs to thermoplastic material technical fields, and in particular to a kind of preparation side of polyetherimide expanded moldings
Method.
Background technology
Polyetherimide (Polyetherimide, abbreviation PEI) is the Super Engineering manufactured by amorphous polyetherimide
Plastics, polyethyerimide foam have excellent high and low temperature resistance, from spies such as flame retardant property, low smoke and non-toxic, radiation resistances
Point, thus it is widely used in the high-tech areas such as Aeronautics and Astronautics, naval vessels, rail traffic.The main preparation of polyethyerimide foam
Route is small molecule dianhydride and diamine monomer is aggregated obtains polyetherimide amino acid, and polyetherimide amino acid is in subsequent imidization
It is crosslinked in foaming in journey, to be prepared into polyethyerimide foam.Since there are technology path length, low production efficiency, imines
Change not exclusively, the problems such as high-temperature solvent is not easy to remove, product is scaling-off serious, the price of polyetherimide foam materials it is high and
Product quality is irregular.
The preparation method of existing polyetherimide expanded material, main includes paste foaming, powder foam method and microballoon
Foaming.Paste foaming carries out heating foaming using high solids content polyimide precursor paste, by controlling paste
Solid content can adjust the density of polyimides expanded material, and the density of the polyimides expanded material prepared by this method can be with
Down to 2kg/m3.Powder foam method is prepared by the way that a certain proportion of fragrant tetracid, aromatic multi-amine, two silica ether of diamines is blended first
Then polyimide precursor powder heats polyimide precursor powder to 300~500 DEG C of preparation apparent densities and is less than 70kg/m3
Polyimides expanded material.Microballoon method first has to prepare polyimide precursor powder, then makes polyimides by heating
The microballoon of part imidizate is finally heated preparation by powder prefoam at higher temperatures at the microballoon of part imidizate
At polyimides expanded material.
Polyetherimide is amorphous polymer, and the heat distortion temperature of polyetherimide expanded particle is high, need to reach 250 DEG C
~350 DEG C, therefore it is molding of the heat medium realization to polyetherimide expanded particle to be difficult to adopt vapor.In addition, experiment
It was found that outer surface softening will not occur when heated for polyetherimide expanded particle, but rapid desufflation occurs, this is also unfavorable for
The formation bonded between expanded particle.
Invention content
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, a kind of polyetherimide expanded moldings are provided
Preparation method, it is intended to solve that existing polyetherimide expanded moldings performance is unstable, polyetherimide expanded moldings make
With a large amount of shed powders are easy tod produce in the process, the technical issues of influencing to construct.
For achieving the above object, the technical solution adopted by the present invention is as follows：
The present invention provides a kind of preparation method of polyetherimide expanded moldings, which includes the following steps：
Obtain polyetherimide expanded particle；
By the surface adhesive coating of the polyetherimide expanded particle；
Hot-press solidifying processing will be carried out in the polyetherimide expanded particle injection mold for being coated with adhesive, obtains polyethers
Acid imide expanded moldings.
The preparation method of polyetherimide expanded moldings provided by the invention, is directly evenly applied to polyethers by adhesive
Acid imide expanded particle surface, then be injected into mold, it is compressed, be heating and curing to obtain, on the one hand because having good mechanical property
The lightweight polyetherimide expanded particle of energy makes polyetherimide expanded moldings performance stablize, another aspect polyetherimide hair
Steep size, the controlled shape of formed body.Therefore, preparation method is simple for polyetherimide expanded moldings of the invention,
It is easy to industrialized production, the thermoplastic polyimide expanded moldings material being prepared is low with density, size shape is controllable,
There is no the advantages that shed powder using process, has a good application prospect.
Specific implementation mode
In order to make technical problems, technical solutions and advantageous effects to be solved by the present invention be more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
On the one hand, an embodiment of the present invention provides a kind of preparation method of polyetherimide expanded moldings, the preparation sides
Method includes the following steps：
S01：Obtain polyetherimide expanded particle；
S02：By the surface adhesive coating of above-mentioned polyetherimide expanded particle；
S03：Hot-press solidifying processing will be carried out in the above-mentioned polyetherimide expanded particle injection mold for being coated with adhesive, obtained
Polyetherimide expanded moldings.
Adhesive is directly evenly applied to polyetherimide expanded particle surface by the preparation method, then is injected into mould
Tool, it is compressed, be heating and curing to obtain, on the one hand because having the lightweight polyetherimide expanded particle of excellent mechanical performances to make polyethers
Acid imide expanded moldings performance is stablized, the size of another aspect polyetherimide expanded moldings, controlled shape.Therefore, originally
Preparation method is simple for the polyetherimide expanded moldings of invention, is easy to industrialized production, the thermoplasticity being prepared
Polyimides expanded moldings material has many advantages, such as that density is low, size shape is controllable, does not have shed powder using process, has
Good application prospect.
Specifically, in above-mentioned steps S01, the preparation process of polyetherimide expanded particle is：Using extrusion by melting
Polyetherimide raw material is extruded into thermoplastic polyetherimide particle；And thermoplastic polyetherimide particle is injected by overcritical
The high-pressure mixing fluid of fluid carbon dioxide and organic solvent composition, obtains polyetherimide expanded particle.
It is theoretical according to polymer fretting map, to realize the highly expanded foaming of polyetherimide resin, it is necessary to provide high hair
Infusion concentration.But carbon dioxide shows low solubility in thermoplastic polyetherimide matrix, in addition, polyetherimide
Polyimide resin has high matrix modulus and high glass transition temperature, these factors micro- to low density heat plasticity polyetherimide
The preparation of expanded material brings technical barrier.When pressure is 5MPa, dissolving of the carbon dioxide in thermoplastic polyetherimide
Degree is 3~5wt%；But at normal temperatures and pressures, solubility of the tetrahydrofuran in thermoplastic polyetherimide be 18wt%,
Solubility of the pyridine in thermoplastic polyetherimide is 23wt%.And in the embodiment of the present invention, creatively with shooting flow
Body carbon dioxide is that physical blowing agent carries out physical blowing to thermoplastic polyetherimide, while being added to organic solvent, and normal
Rule method is compared, and solubility of the polyetherimide to the physical blowing agent is remarkably improved, and obtains low density heat plasticity polyethers acyl
Imines expanded particle material；Meanwhile the present invention can significantly improve solubility of the polyetherimide to physical blowing agent, and drop
Low ratio foamed temperature, to allow polyetherimide to be realized under lower blowing temperature, high magnification expands, and obtains degrees of expansion
The polyetherimide expanded particle that height, any surface finish, soft texture, foam structure are uniform, cell density is big, tensile property is excellent
Material, and then provide solid foundation for the performance of the polyetherimide expanded moldings subsequently prepared stabilization.
It is further preferred that the volume ratio range of above-mentioned supercritical fluid carbon dioxide and organic solvent is (2:1)-(4:
1), preferably 2:1.Under the conditions of the volume ratio of supercritical fluid carbon dioxide provided in an embodiment of the present invention and organic solvent, gather
Etherimide significantly improves the solubility of carbon dioxide, and significantly reduces blowing temperature, therefore, polyetherimide foaming grain
Son expansion and cell density reach optimum state.
It is further preferred that above-mentioned organic solvent includes at least one of ethyl alcohol, pyridine and tetrahydrofuran.The present invention is real
The organic solvent for applying example offer is that there are commonly solvents in prepared by organic solvent foamed thermoplastic polyetherimide.
Preferably, in above-mentioned steps S02, adhesive is pressure-sensitive adhesive or acrylic pressure-sensitive adhesive.Adhesive is can be with
Thermoplastic polyetherimide expanded particle forms chemical bond and sprayable adhesive.Pressure-sensitive adhesive one kind is mainly by organic
The composition of silicon-based polymer composition, preferably includes the solution of dimethyl silicone polymer and polysiloxane resin rubbers.Acrylic acid
It is adhesive, including iso-octyl acrylate or 2-ethylhexyl acrylate and acrylamide or acrylic acid, butyl acrylate
With the blend of butyl isocrotonate.Adhesive provided in an embodiment of the present invention can not only imitate and improve polyetherimide foaming
The caking property of formed body, and the interior shed powder of polyetherimide expanded moldings can be further prevented, further carry
The convenience of high polyetherimide expanded moldings.
Preferably, in above-mentioned steps S02, the surface of polyetherimide expanded particle uses spraying method coated with adhesive.
Spraying method not only convenient raising working efficiency, but also coating effect can be improved, so that adhesive is more preferably applied to polyetherimide
The surface of expanded particle.
Preferably, in above-mentioned steps S03, the temperature range of hot-press solidifying is 210 DEG C -250 DEG C.It is carried in the embodiment of the present invention
Hot-press solidifying is carried out within the temperature range of, can preferably play the glueability of adhesive, makes polyetherimide foaming grain
Son is preferably bonded together.
Specifically, in above-mentioned steps S03, mold is arbitrary in rectangular mould, truncated cone-shaped mold and hemispherical
It is a kind of.The selection of mold can be various solids (packet depending on the concrete application situation of polyetherimide expanded moldings
Abnormity is included, bi-curved die cavity is such as carried).In embodiments of the present invention, it is 500mm × 500mm × 100mm's preferably to select size
The truncated cone-shaped of the hemispherical or a diameter of 300mm, a height of 100mm of rectangular mould or a diameter of 300mm.
The present invention successively carried out test of many times, and it is further detailed to invention progress as reference now to lift A partial experiment result
Thin description, is described in detail with reference to specific embodiment.
Embodiment 1
A kind of preparation method of polyetherimide expanded moldings, the preparation method include the following steps：
S11：Obtain polyetherimide expanded particle.
Detailed process：Polyetherimide raw material is put into extruder, using extrusion by melting, by polyetherimide original
Material is extruded into thermoplastic polyetherimide particle；Then thermoplastic polyetherimide particle is put into autoclave, pressure is
12MPa injects the high-pressure mixing fluid of supercritical fluid carbon dioxide and ethyl alcohol composition, obtains polyetherimide expanded particle；Its
In, high-pressure mixing fluid is that the volume ratio of supercritical fluid carbon dioxide and ethyl alcohol is 3:The saturation state high pressure mixing of 1 composition
Fluid.
S12：By the surface spraying adhesive of above-mentioned polyetherimide expanded particle.
S13：The above-mentioned polyetherimide expanded particle for being coated with adhesive is injected into 500mm × 500mm × 100mm cuboids
In mold, hot-press solidifying processing is carried out under conditions of temperature is 210 DEG C, obtains polyetherimide expanded moldings.
Embodiment 2
A kind of preparation method of polyetherimide expanded moldings, the preparation method include the following steps：
S21：Obtain polyetherimide expanded particle.
Detailed process：Polyetherimide raw material is put into extruder, using extrusion by melting, by polyetherimide original
Material is extruded into thermoplastic polyetherimide particle；Then thermoplastic polyetherimide particle is put into autoclave, pressure is
16MPa injects the high-pressure mixing fluid of supercritical fluid carbon dioxide and tetrahydrofuran composition, obtains polyetherimide foaming grain
Son；Wherein, it is 4 that high-pressure mixing fluid, which is the volume ratio of supercritical fluid carbon dioxide and tetrahydrofuran,:The saturation state of 1 composition
High-pressure mixing fluid.
S22：By the surface spraying adhesive of above-mentioned polyetherimide expanded particle.
S23：The above-mentioned polyetherimide expanded particle for being coated with adhesive is injected into 500mm × 500mm × 100mm cuboids
In mold, hot-press solidifying processing is carried out under conditions of temperature is 230 DEG C, obtains polyetherimide expanded moldings.
Embodiment 3
A kind of preparation method of polyetherimide expanded moldings, the preparation method include the following steps：
S31：Obtain polyetherimide expanded particle.
Detailed process：Polyetherimide raw material is put into extruder, using extrusion by melting, by polyetherimide original
Material is extruded into thermoplastic polyetherimide particle；Then thermoplastic polyetherimide particle is put into autoclave, pressure is
12MPa injects the high-pressure mixing fluid of supercritical fluid carbon dioxide and tetrahydrofuran composition, obtains polyetherimide foaming grain
Son；Wherein, it is 2 that high-pressure mixing fluid, which is the volume ratio of supercritical fluid carbon dioxide and tetrahydrofuran,:The saturation state of 1 composition
High-pressure mixing fluid.
S32：By the surface spraying adhesive of above-mentioned polyetherimide expanded particle.
S33：The above-mentioned polyetherimide expanded particle for being coated with adhesive is injected to the hemispherical of a diameter of 300mm
In, hot-press solidifying processing is carried out under conditions of temperature is 250 DEG C, obtains polyetherimide expanded moldings.
Embodiment 4
A kind of preparation method of polyetherimide expanded moldings, the preparation method include the following steps：
S41：Obtain polyetherimide expanded particle.
Detailed process：Upper polyetherimide raw material is put into extruder, using extrusion by melting, by the polyetherimide
Raw material is extruded into thermoplastic polyetherimide particle；Then thermoplastic polyetherimide particle is put into autoclave, pressure is
17MPa injects the high-pressure mixing fluid of supercritical fluid carbon dioxide and pyridine composition, obtains polyetherimide expanded particle；Its
In, high-pressure mixing fluid is that the volume ratio of supercritical fluid carbon dioxide and pyridine is 3:The saturation state high pressure mixing of 1 composition
Fluid.
S42：By the surface spraying adhesive of above-mentioned polyetherimide expanded particle.
S33：The above-mentioned polyetherimide expanded particle for being coated with adhesive is injected to the circle of a diameter of 300mm, a height of 100mm
Platform shape mold carries out hot-press solidifying processing under conditions of temperature is 240 DEG C, obtains polyetherimide expanded moldings.
Adhesive, is directly evenly applied to by the preparation method for the polyetherimide expanded moldings that above-described embodiment provides
Polyetherimide expanded particle surface, then be injected into mold, compressed, be heating and curing to obtain, therefore, the preparation method is simple
It is easy, it is easy to industrialized production, the thermoplastic polyimide expanded moldings material being prepared low, size shape with density
Controllably, there is no the advantages that shed powder using process, have a good application prospect.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (8)
1. a kind of preparation method of polyetherimide expanded moldings, which is characterized in that include the following steps：
Obtain polyetherimide expanded particle；
By the surface adhesive coating of the polyetherimide expanded particle；
Hot-press solidifying processing will be carried out in the polyetherimide expanded particle injection mold for being coated with adhesive, obtains polyetherimide
Amine expanded moldings.
2. preparation method as described in claim 1, which is characterized in that the preparation process of the polyetherimide expanded particle
For：Polyetherimide raw material is extruded by thermoplastic polyetherimide particle using extrusion by melting；And by the thermoplastic polyether
Acid imide particle injects the high-pressure mixing fluid being made of supercritical fluid carbon dioxide and organic solvent, obtains polyetherimide hair
Steep particle.
3. preparation method as claimed in claim 2, which is characterized in that the supercritical fluid carbon dioxide and described organic molten
The volume ratio range of agent is (2:1)-(4:1).
4. preparation method as claimed in claim 2, which is characterized in that the organic solvent includes ethyl alcohol, pyridine and tetrahydrochysene furan
At least one of mutter.
5. preparation method as described in claim 1, which is characterized in that the adhesive is pressure-sensitive adhesive or acrylic acid series
Adhesive.
6. preparation method as described in claim 1, which is characterized in that the surface of the polyetherimide expanded particle is using spray
Painting mode coats the adhesive.
7. preparation method as described in claim 1, which is characterized in that the temperature range of the hot-press solidifying is 210 DEG C -250
℃。
8. preparation method as described in claim 1, which is characterized in that the mold be rectangular mould, truncated cone-shaped mold and
Any one in hemispherical.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710197119.6A CN108659254A (en) | 2017-03-29 | 2017-03-29 | The preparation method of polyetherimide expanded moldings |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710197119.6A CN108659254A (en) | 2017-03-29 | 2017-03-29 | The preparation method of polyetherimide expanded moldings |
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| CN108659254A true CN108659254A (en) | 2018-10-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022117331A1 (en) * | 2020-12-02 | 2022-06-09 | Evonik Operations Gmbh | Adhesion of blowing agent-containing particles based on polyimides or polyacrylates |
| CN115534446A (en) * | 2022-09-23 | 2022-12-30 | 中国舰船研究设计中心 | Low-toxicity flame-retardant bulkhead composite material for ship and preparation method thereof |
| WO2023011410A1 (en) * | 2021-07-31 | 2023-02-09 | 华为技术有限公司 | Foamed material, and preparation method therefor and use thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702562A (en) * | 2012-05-24 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method for thermoplastic polyimide foaming particle and formed body thereof |
| CN102702561A (en) * | 2012-05-25 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of low-density thermoplastic polyimide micro-foamed material |
-
2017
- 2017-03-29 CN CN201710197119.6A patent/CN108659254A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702562A (en) * | 2012-05-24 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method for thermoplastic polyimide foaming particle and formed body thereof |
| CN102702561A (en) * | 2012-05-25 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of low-density thermoplastic polyimide micro-foamed material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022117331A1 (en) * | 2020-12-02 | 2022-06-09 | Evonik Operations Gmbh | Adhesion of blowing agent-containing particles based on polyimides or polyacrylates |
| WO2023011410A1 (en) * | 2021-07-31 | 2023-02-09 | 华为技术有限公司 | Foamed material, and preparation method therefor and use thereof |
| CN115534446A (en) * | 2022-09-23 | 2022-12-30 | 中国舰船研究设计中心 | Low-toxicity flame-retardant bulkhead composite material for ship and preparation method thereof |
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