JP2017537241A - 表面変性ポリオレフィン繊維 - Google Patents
表面変性ポリオレフィン繊維 Download PDFInfo
- Publication number
- JP2017537241A JP2017537241A JP2017528567A JP2017528567A JP2017537241A JP 2017537241 A JP2017537241 A JP 2017537241A JP 2017528567 A JP2017528567 A JP 2017528567A JP 2017528567 A JP2017528567 A JP 2017528567A JP 2017537241 A JP2017537241 A JP 2017537241A
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- JP
- Japan
- Prior art keywords
- fiber
- polyolefin fiber
- modified polyolefin
- fibers
- binder composition
- 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.)
- Granted
Links
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
- C04B16/06—Macromolecular compounds fibrous
- C04B16/0616—Macromolecular compounds fibrous from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B16/0625—Polyalkenes, e.g. polyethylene
- C04B16/0633—Polypropylene
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
- C04B16/06—Macromolecular compounds fibrous
- C04B16/0616—Macromolecular compounds fibrous from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B16/0625—Polyalkenes, e.g. polyethylene
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/0048—Fibrous materials
- C04B20/0068—Composite fibres, e.g. fibres with a core and sheath of different material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
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- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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Abstract
Description
本発明は、以下の実施形態を有する表面変性ポリオレフィン繊維を提供する:
1.以下:
a)プラズマ反応器内での電気的に励起可能なガスを用いたプラズマ処理によりポリオレフィン繊維を前処理して、前記繊維の表面上に極性基を有するポリオレフィン繊維を得るステップと、
b)前記ポリオレフィン繊維を、プラズマ反応器内でガス状のシロキサンまたはシラザン化合物の存在下で電気的に励起可能なガスを用いてプラズマ処理するステップと、
を含む方法により得ることができる(または得られた)、表面変性ポリオレフィン繊維。
a)実施形態1から43までのいずれかに記載の表面変性ポリオレフィン繊維を無機結合材組成物に組み込むステップと、b)前記無機結合材組成物を硬化させるステップと、を含む、前記方法。
a)プラズマ反応器内でポリオレフィン繊維を電気的に励起可能なガスと接触させることによって前記ポリオレフィン繊維を前処理して、前記繊維の表面上に極性基を有するポリオレフィン繊維を得るステップと、
b)前記ポリオレフィン繊維をプラズマ反応器内でガス状のシロキサンまたはシラザン化合物の存在下で電気的に励起可能なガスを用いてプラズマ処理するステップと、
を含む、前記方法。
本発明のポリオレフィン繊維は、例えばポリエチレンやポリプロピレンといったポリオレフィン、それらのコポリマーおよびこうした繊維のブレンドから構成される。本発明のポリオレフィン繊維が、例えばフィラー、ガラス繊維、相容化剤、変性剤等の一般的な添加剤を含みうることは、当業者にとって自明である。
本発明の表面変性ポリオレフィン繊維は、実施形態1記載の方法によって得られる。一実施形態において、ステップa)は、電気的に励起可能なガスを用いたプラズマ処理のみを含み、機械的処理を含まない。好ましい一実施形態において、ステップa)は、機械的処理と、電気的に励起可能なガスの存在下でのプラズマ処理と、の双方を含む。前処理のこれら2つの選択可能な処理の順序は可変である。しかし、プラズマ処理前に機械的処理を行うことが好ましい。
ポリオレフィン繊維の機械的成形は任意であり、好ましくはステップa)の前に行う。機械的成形にはポリオレフィンフィラメントを使用し、この機械的成形のプロセス後にこのポリオレフィンフィラメントを所望の長さに切断する。機械的成形には、好ましくはエンボス加工、捲縮および/または延伸といった技術が含まれ、その際、延伸が好ましい。こうした技術を組み合わせて適用することもできる。特に、繊維を最初に延伸させ、次いでエンボス加工を施しかつ/または捲縮させることができる。エンボス加工、捲縮または延伸の方法は従来のものであり、例えば米国特許第3956450号明細書(US 3956450)、国際公開第2007/036058号(WO 2007/036058 A1)または独国特許出願公開第2927238号明細書(DE 2927238 A1)に開示されている。
ポリオレフィン繊維と電気的に励起可能なガスとの接触(ステップa)と、ガス状のシロキサンまたはシラザン化合物の存在下での該ポリオレフィン繊維のプラズマ処理とを、プラズマ反応に適した従来の装置内で、例えばプラズマ反応器内で行う。
本発明はさらに、特に水硬性の無機結合材組成物における補強材としての表面変性ポリオレフィン繊維の使用に関し、これによって、極めて強度が高いにもかかわらず軽量である材料が提供される。本発明により、例えばポリプロピレンのような高分子繊維質材料を使用した場合に認められる結合性の制限が克服される。結合特性が向上した結果、本発明の表面変性ポリオレフィン繊維を含む結合材組成物によって、総じて、同等の未処理のポリオレフィン繊維を用いて製造された組成物よりも30%〜40%高い残留引張強度が生じる。
以下の例で使用するポリオレフィン繊維の製造を、溶融押出、配向、機械的成形および切断によって行った。Isplen PP 020 G3Eなる名称のポリプロピレンホモポリマー(Repsol社製)を、240℃の温度に設定した単軸押出機内で溶融させ、次いで矩形のダイを通じて押し出した。この押出物を冷却し、15℃の一定温度に保持した水浴中に浸漬させて固化させ、次いで異なる速度で回転するロールを用いて延伸させて所望の延伸比とすることで、最終的な引張強度を高めた。この延伸プロセスを、2つの異なる延伸段階により行った。第1の延伸段階では、150℃の温度に設定した電気オーブンを通過させたフィラメントを、延伸比9で延伸させた。第2の延伸段階では、230℃の温度に設定した電気オーブンを通過させたフィラメントを、延伸比1.7で延伸させた。したがって、これら2つの延伸プロセスの全延伸比は15.3であった。これらの延伸段階の後に、このフィラメントを2つの回転ロールを備えたエンボス加工機に案内し、このエンボス加工機においてこのフィラメントの表面を室温で成形した。これらの2つのロールは、以下のパラメータにより規定されるものであった:外径(図7B−R1)は66.6mmであり、凸部の高さ(図7B−h)は0.2mmであり、2つの山部の間の角距離(図7B−α)は3°であり、山部の長さ(図7B−g)は0.90mmであり、これらのロールの回転軸の間の間隔(図7B−D)は133.7mmであり、位相のずれ(図7B−φ)は0.5°であり、軸パターンは回転軸に対して45°の角度(図7C−β)だけ傾斜していた。これらのロールによって、図6A、図6Bおよび図6Cに示したようなエンボスパターンを生成した。このエンボス加工後にこのフィラメントを切断機に案内し、この切断機においてこのフィラメントを切断して長さ52mmの繊維とした。得られた繊維は、EN 14889−2規格により測定した場合に約500MPaの引張強度を有していた。この繊維の幾何学的形状を規定するパラメータの値を、EN 14889−2規格により光学顕微鏡で測定した。繊維の幅(図6A−Dmax)は1.22mmであり、繊維の厚さ(図6B−Dmin)は0.55mmであり、エンボスの高さ(図6B−he)は0.90mmであり、エンボス単位の長さ(図6B−h)は1.74mmであり、エンボスの深さ(図6C−pe)は0.04mmであり、ずれ(図6B−se)は0.30mmであり、角度(図6A−α)は45°であり、角度(図6A−β)は90°であった。エンボス比(ER)の値は0.52であった。
上記のようにして得られたポリプロピレン繊維を、室温で超音波浴中のイソプロピルアルコール中で15分間洗浄した。その後、この繊維を室温で窒素気流中で60分間乾燥させた。この洗浄して乾燥させたポリプロピレン繊維(50g)をプラズマ反応器(Thin Films srl社製バレルコーター)に充填し、このプラズマ反応器を真空引きして5×10−3ミリバールの圧力とした。第1のステップで、このポリプロピレン繊維を以下の条件下で酸素流で処理した:
酸素流量:20sccm
RF電力:50W
処理時間:30分間
回転速度:20rpm
周波数:13.56MHz。
処理時間:30分間
回転速度:20rpm
周波数:13.56MHz。
上記の通りに得られたポリプロピレン繊維を、例1に記載した通りに洗浄し、乾燥させた。この洗浄して乾燥させたポリプロピレン繊維(50g)を、例1で使用したプラズマ反応器に充填し、次いで真空引きして5×10−3ミリバールの圧力とした。このポリプロピレン繊維を以下の条件下で酸素流で処理した:
酸素流量:20sccm
RF電力:50W
処理時間:30分間
回転速度:20rpm
周波数:13.56MHz。
上記のようにして得られたポリプロピレン繊維を、例1に記載した通りに洗浄し、乾燥させた。この洗浄して乾燥させたポリプロピレン繊維(50g)を、例1で使用したプラズマ反応器に充填し、そして真空引きして5×10−3ミリバールの圧力とした。このポリプロピレン繊維を以下の条件下で処理した:
酸素流量:35sccm
ヘキサメチルジシロキサン流量:3.5sccm
RF電力:50W
処理時間:30分間
回転速度:20rpm
周波数:13.56MHz。
例1〜3の3つのプラズマ処理済みポリプロピレン繊維と、未処理のポリプロピレン繊維とを、単繊維引抜き試験で試験した。この目的のために、以下の成分を各当量で含むモルタル組成物を混合により調製した:
CEM I 52.5 R Cementerie Monselice 1.0当量
CEN− Normsand DIN 196 3.0当量
Cremaschi石灰石フィラー 0.2当量
Master Glenium(登録商標)SKY 623 (セメント質量に対して)1.2%
MasterMATRIX(登録商標)150 (セメント質量に対して)0.9%
水 0.5当量。
例1〜3の表面変性ポリプロピレン繊維または未処理のポリプロピレン繊維のうちの1つを含む異なるコンクリート組成物の残留引張強度を比較した。この測定に用いたコンクリート組成物のベースは、表1に記載のモルタル混合物であった:
表1:モルタル混合物1および2
− fR1は、CMOD 0.5mmでの荷重であり、
− fR2は、CMOD 1.5mmでの荷重であり、
− fR3は、CMOD 2.5mmでの荷重であり、
− fR4は、CMOD 3.5mmでの荷重である。
Claims (15)
- 以下:
a)プラズマ反応器内での電気的に励起可能なガスを用いたプラズマ処理によりポリオレフィン繊維を前処理して、表面上に極性基を有するポリオレフィン繊維を得るステップと、
b)前記ポリオレフィン繊維を、プラズマ反応器内でガス状のシロキサンまたはシラザン化合物の存在下で電気的に励起可能なガスを用いてプラズマ処理するステップと、
を含む方法により得ることができる、表面変性ポリオレフィン繊維。 - 前記ポリオレフィン繊維が、ポリエチレン繊維、ポリプロピレン繊維、もしくはそれらのコポリマーからの繊維、またはそれらのブレンドから選択される、請求項1記載の表面変性ポリオレフィン繊維。
- ガス状のシロキサンまたはシラザン化合物と電気的に励起可能なガスとの比が、1/1〜1/20(シロキサンまたはシラザン化合物/電気的に励起可能なガス)である、請求項1または2記載の表面変性ポリオレフィン繊維。
- 前記電気的に励起可能なガスが、アルゴン、酸素、窒素、空気、アンモニア、二酸化炭素、水またはそれらの2つ以上の混合物から選択される、請求項1から3までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 前記ポリオレフィン繊維の表面上の極性基が、カルボニル基、カルボキシル基、ヒドロキシル基、アミド基、イミド基および/またはニトリル基から選択される、請求項1から4までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 前記ガス状のシロキサンまたはシラザン化合物が、直鎖状もしくは環状のモノアルキル化もしくはポリアルキル化シロキサン、もしくは直鎖状もしくは環状のモノアルキル化もしくはポリアルキル化シラザン、またはそれらの混合物から選択される、請求項1から5までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 前記ガス状のシロキサンまたはシラザン化合物が、ヘキサメチルジシロキサン、ヘキサメチルジシラザン、デカメチルシクロペンタシロキサンまたはそれらの混合物から選択される、請求項6記載の表面変性ポリオレフィン繊維。
- ガス状のシロキサンまたはシラザン化合物の存在下での前記ポリオレフィン繊維のプラズマ処理が、前記ポリオレフィンの表面上にシリカを堆積させるのに適したエネルギーレベルで行われる、請求項1から7までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 前記プラズマ処理におけるイオンおよびラジカルが、0.1eV〜100eVのエネルギーレベルを有する、請求項8記載の表面変性ポリオレフィン繊維。
- ステップ(a)による前処理の前に、前記ポリオレフィン繊維が機械的に成形される、請求項1から9までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 前記機械的成形が、エンボス加工、捲縮、撚糸および/または延伸を含む、請求項10記載の表面変性ポリオレフィン繊維。
- 10mm〜60mmの長さ、0.5mm〜3mmの幅および0.2mm〜1mmの厚さを有する、請求項1から11までのいずれか1項記載の表面変性ポリオレフィン繊維。
- 無機結合材組成物における、請求項1から12までのいずれか1項記載の表面変性ポリオレフィン繊維の使用。
- 請求項1から12までのいずれか1項記載の表面変性ポリオレフィン繊維を含む、無機結合材組成物。
- 無機結合材組成物の補強方法であって、
a)請求項1から12までのいずれか1項記載の表面変性ポリオレフィン繊維を無機結合材組成物に組み込むステップと、
b)前記無機結合材組成物を硬化させるステップと、
を含む、前記方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP14195064.2 | 2014-11-27 | ||
EP14195064 | 2014-11-27 | ||
PCT/EP2015/068357 WO2016082949A1 (en) | 2014-11-27 | 2015-08-10 | Surface-modified polyolefin fibers |
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JP2022505856A (ja) * | 2018-10-31 | 2022-01-14 | アドフィル エヌ.フェー. | コンクリート補強用繊維 |
KR102513582B1 (ko) * | 2021-10-19 | 2023-03-24 | 주식회사 효산화이버 | 콘크리트 보강용 복합 수지 파이버 제조 방법 및 그 복합 수지 파이버 |
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LT3517515T (lt) | 2017-12-15 | 2022-03-25 | Omnicor - Manufacturas Internacionais de Cordoarias, Lda | Cementinei matricai sustiprinti skirtas pluošto ryšulys, jo naudojimas ir gavimo būdas |
CN109967019A (zh) * | 2019-04-19 | 2019-07-05 | 华东理工大学 | 一种颗粒干法连续表面改性反应器 |
CN114702282B (zh) * | 2021-06-03 | 2023-01-10 | 广州珠江装修工程有限公司 | 一种吸声降噪混凝土 |
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US20180327309A1 (en) | 2018-11-15 |
CN107532375B (zh) | 2022-05-13 |
BR112017011062A2 (pt) | 2018-05-08 |
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BR112017011062B1 (pt) | 2021-11-16 |
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