JP6405349B2 - 熱処理ポリマー粉末 - Google Patents
熱処理ポリマー粉末 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/02—Conditioning or physical treatment of the material to be shaped by heating
- B29B13/021—Heat treatment of powders
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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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
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- 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
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C39/04—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles using movable moulds not applied
- B29C39/08—Introducing the material into the mould by centrifugal force
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- 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
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/141—Processes of additive manufacturing using only solid materials
- B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/02—Condensation polymers of aldehydes or ketones with phenols only of ketones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2071/00—Use of polyethers, e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof, as moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0037—Other properties
- B29K2995/004—Semi-crystalline
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing oxygen in addition to the ether group
- C08G2650/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing oxygen in addition to the ether group containing ketone groups, e.g. polyarylethylketones, PEEK or PEK
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Optics & Photonics (AREA)
- Thermal Sciences (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Moulding By Coating Moulds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
ポリマー組成物に最も有用なポリマーは、多形半結晶性ポリマー及び/又はポリマーのガラス転移温度を超える温度に付すと半結晶性になることができるポリマーである。本明細書で用いる「半結晶性又は結晶性多形ポリマー」とは、ポリマーが、1つ以上の結晶形で存在することができること、また、ポリマーが、結晶性である、及び/又は熱処理すると、1つ以上の結晶性領域を形成することができることを意味する。こうしたポリマーの例として、限定するものではないが、ポリアリールエーテルケトン(PAEK)若しくは交互ポリケトン又はこれらの混合物を含む。ポリアリールエーテルケトン(PAEK)は、非常に高い融点を有し、多くの場合、様々な形状に結晶化する。これらの両特性により、本発明の熱処理は、粉末化材料が長期間にわたって高温にさらされる用途に用いる場合、特にPAEKポリマーに有用となる。
−A−C(=O)−B−C(=O)− I
−A−C(=O)−D−C(=O)− II
(式中、Aは、p,p’−Ph−O−Ph−基であり、Phは、フェニレン基であり、Bはp−フェニレンであり、Dは、m−フェニレンである)。ポリエーテルケトンケトンにおける式I:式II異性体の比(一般に、T:I比と呼ばれる)を選択することにより、ポリマーの総結晶度を変える。T/I比は、一般に、50:50から90:10まで変動し、いくつかの実施形態では、60/40〜80/20である。高いT:I比(例えば、80:20)ほど、低いT:I比(例えば、60:40)と比べて、高い結晶化度をもたらす。
本発明に従い、結晶の融点を高めることにより、高温での粉体流動性が求められる用途において、より優れた粉体処理及び耐久性をもたらすような方法で、様々な構造を有する多形半結晶性又は結晶形成ポリマーを熱処理する。
T:I比が、60:40のように比較的低い場合、結晶化の速度は、非常に遅いため、ポリマーをそのガラス転移温度より高い温度で一定時間維持することにより、材料を熱処理するか、又はアニールしない限り、一般に、溶融処理ポリマー中に結晶は形成されない。従って、これらのポリマーは、本来半結晶性であっても、非晶質ポリマーと呼ばれることが多い。本発明の目的のための非晶質ポリマーは、X線回析によって結晶相を示さないポリマーを意味する。PEKKの市販のOXPEKK(商標)−SPポリマーグレードは、初め非晶質であるが、ガラス転移温度より高い温度で熱処理すると、部分的に結晶性になる組成物の一例である。
高温で良好な粉体流動性から利益を得られる用途の例として、回転成形、選択的レーザー焼結及び粉末コーティングがあるが、本発明の熱処理方法で製造された粉末の使用はこれらの用途に限定されるわけではない。熱処理を受ける粉末は、粉末の良好な流動性、はっきりとした融点及び耐久性が要求されるあらゆる用途で有用である。驚くことに、これらの熱処理粉末は、最終製品の優れた特性及び優れた外観を提供するだけではなく、この粉末から形成される最終製品の物理的性質を改善することもできることが見出された。
管電流=40mA、管電圧=40kV、Cu K−α線
発散スリット=1mm、平行スリットアナライザー(0.011°)
2θ範囲=5°〜80°、滞留時間=5秒、増分=0.02°
発散Hスリット=10mm、平行ビーム光学系、ソーラースリット=5°
散乱スリット=受光スリット=開
Claims (10)
- 少なくとも2つの異なる融点を有する少なくとも2種の半結晶性の又は結晶形成可能なポリエーテルケトンケトン多形体を含み、選択的レーザー焼結、回転成形又は粉末コーティングに適した被熱処理ポリマー粉末組成物を製造する方法であって、
(a)最も高い融解結晶性多形体の融点より20℃未満低く、かつ、その他の結晶性多形体の融点以上の温度を選択することによって熱処理条件を決定し、
(b)前記の最も高い融解結晶性多形体の融点より20℃未満低く、かつ、前記のその他の結晶性多形体の融点以上の温度で、ポリマー組成物において最も高い融解結晶性多形体の含量をその他の結晶性多形体に対して増加させる時間にわたり、ポリマー組成物を熱処理するステップを少なくとも含み、
前記ポリエーテルケトンケトンが式I又はII:
−A−C(=O)−B−C(=O)− I(異性体T)
−A−C(=O)−D−C(=O)− II(異性体I)
(式中、Aは、p,p’−Ph−O−Ph−基であり、Phは、フェニレン基であり、Bはp−フェニレンであり、Dは、m−フェニレンである)によって表される反復単位を含み、T:I異性体比が、60/40〜80/20の範囲である、前記方法。 - 熱処理したポリマー組成物を粉末に粉砕するステップであって、結晶度を低下させないステップをさらに含む、請求項1に記載の方法。
- 前記半結晶性の又は結晶形成可能な多形体が、熱処理前及び/又は熱処理後に、15〜150μmの重量平均粒度を有する粒子の形態である、請求項1に記載の方法。
- 熱処理の温度が、最も高い融解結晶性多形体の融点より15℃未満低い、請求項1に記載の方法。
- 熱処理の温度が、最も高い融解結晶性多形体の融点より10℃未満低い、請求項1に記載の方法。
- 熱処理の温度が、最も高い融解結晶性多形体の融点より5℃未満低い、請求項1に記載の方法。
- 前記ポリマー組成物が、非多形ポリマー、充填剤、及び繊維からなる群から選択される1つ以上の他の成分をさらに含む、請求項1に記載の方法。
- 前記熱処理温度が、230℃〜300℃の範囲である、請求項1に記載の方法。
- 前記熱処理温度が、270℃〜375℃の範囲である、請求項1に記載の方法。
- 得られた被熱処理ポリマー組成物が、ポリエーテルケトンケトン中のI型及びII型の総量に基づき、90%以上のI型ポリエーテルケトンケトンを含む、請求項1に記載の方法。
Applications Claiming Priority (2)
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US38674110P | 2010-09-27 | 2010-09-27 | |
US61/386,741 | 2010-09-27 |
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JP2013530411A Division JP6041806B2 (ja) | 2010-09-27 | 2011-09-27 | 熱処理ポリマー粉末 |
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JP2016216744A JP2016216744A (ja) | 2016-12-22 |
JP6405349B2 true JP6405349B2 (ja) | 2018-10-17 |
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JP2016176899A Active JP6405349B2 (ja) | 2010-09-27 | 2016-09-09 | 熱処理ポリマー粉末 |
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US (4) | US9587107B2 (ja) |
EP (2) | EP2627687B1 (ja) |
JP (2) | JP6041806B2 (ja) |
CN (1) | CN103140527B (ja) |
CA (1) | CA2812758C (ja) |
ES (1) | ES2899663T3 (ja) |
WO (1) | WO2012047613A1 (ja) |
Families Citing this family (33)
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ES2899663T3 (es) | 2022-03-14 |
US10519309B2 (en) | 2019-12-31 |
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US20130323416A1 (en) | 2013-12-05 |
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US20210292544A1 (en) | 2021-09-23 |
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US20200109279A1 (en) | 2020-04-09 |
US9587107B2 (en) | 2017-03-07 |
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US11046847B2 (en) | 2021-06-29 |
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