JP5889058B2 - Cement-based cured body and cement mortar or concrete curing method - Google Patents
Cement-based cured body and cement mortar or concrete curing method Download PDFInfo
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- JP5889058B2 JP5889058B2 JP2012059065A JP2012059065A JP5889058B2 JP 5889058 B2 JP5889058 B2 JP 5889058B2 JP 2012059065 A JP2012059065 A JP 2012059065A JP 2012059065 A JP2012059065 A JP 2012059065A JP 5889058 B2 JP5889058 B2 JP 5889058B2
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- 238000001723 curing Methods 0.000 title claims description 78
- 239000004567 concrete Substances 0.000 title claims description 60
- 239000004568 cement Substances 0.000 title claims description 38
- 239000011083 cement mortar Substances 0.000 title claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 68
- 239000003795 chemical substances by application Substances 0.000 claims description 49
- -1 fatty acid ester Chemical class 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 31
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- 238000000034 method Methods 0.000 claims description 20
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- 125000005471 saturated fatty acid group Chemical group 0.000 claims 4
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- 125000004429 atom Chemical group 0.000 claims 2
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- 125000005313 fatty acid group Chemical group 0.000 description 29
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- 238000011160 research Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- UWHZIFQPPBDJPM-BQYQJAHWSA-N trans-vaccenic acid Chemical compound CCCCCC\C=C\CCCCCCCCCC(O)=O UWHZIFQPPBDJPM-BQYQJAHWSA-N 0.000 description 1
- UCSBCWBHZLSFGC-UHFFFAOYSA-N tributoxysilane Chemical compound CCCCO[SiH](OCCCC)OCCCC UCSBCWBHZLSFGC-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- BJDLPDPRMYAOCM-UHFFFAOYSA-N triethoxy(propan-2-yl)silane Chemical compound CCO[Si](OCC)(OCC)C(C)C BJDLPDPRMYAOCM-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- LGROXJWYRXANBB-UHFFFAOYSA-N trimethoxy(propan-2-yl)silane Chemical compound CO[Si](OC)(OC)C(C)C LGROXJWYRXANBB-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 239000013053 water resistant agent Substances 0.000 description 1
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- Aftertreatments Of Artificial And Natural Stones (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Polyethers (AREA)
Description
本発明は、脂肪酸エステル混合物及びアルコキシシラン誘導体を含有するコンクリート用養生剤を使用したセメント系硬化体並びに該養生剤を用いたセメントモルタル又はコンクリートの養生方法に関し、詳細には、セメント系硬化体の打設後、表面からの水分の浸入および逸散を防止し、乾燥収縮の低減と耐久性の改善を図り、さらに長期にわたって劣化の防止を目指したセメント系硬化体並びにセメントモルタル又はコンクリートの養生方法に関する。 The present invention relates to a cement-based cured body using a curing agent for concrete containing a fatty acid ester mixture and an alkoxysilane derivative, and a method for curing cement mortar or concrete using the curing agent. Cement-based hardened body and cement mortar or concrete curing method aimed at preventing moisture from entering and escaping from the surface after casting, reducing drying shrinkage and improving durability, and preventing deterioration over a long period of time About.
セメント系硬化体が所要の強度および耐久性を発揮できる緻密な構造を持つためには、水和進行過程の初期段階で十分な養生を実施し、収縮低減を図ることが必要である。このため、日本建築学会の「JASS 5」では養生期間、方法および乾燥収縮量が規定され
ており、セメント系硬化体の打設後の急激な乾燥を防ぐために湿潤養生が必要不可欠である。
養生方法には、コンクリートに水分を供給する方法(水中養生、湛水養生、散水養生、湿布養生など)と、水分の逸散を防止する方法(被膜養生、シート養生など)がある。水中養生や湛水養生は最も有効な湿潤養生であるが、実際の構造物で行うのは困難な場合が多い。一方、被膜養生は、コンクリート表面に被膜養生剤を散布または塗布して表面に膜を作り、水分の外部への蒸発を防止して水和を進める方法である。
In order for the cement-based hardened body to have a dense structure capable of exhibiting the required strength and durability, it is necessary to carry out sufficient curing at the initial stage of the hydration progress process to reduce shrinkage. For this reason, “JASS 5” of the Architectural Institute of Japan defines the curing period, method, and amount of drying shrinkage, and wet curing is indispensable in order to prevent rapid drying after placing the cement-based cured body.
Curing methods include a method of supplying moisture to concrete (such as underwater curing, submerged curing, watering curing, and compressing curing) and a method of preventing moisture dissipation (such as film curing and sheet curing). Underwater curing and submerged curing are the most effective wet curing, but are often difficult to perform with actual structures. On the other hand, film curing is a method in which a film curing agent is sprayed or applied on a concrete surface to form a film on the surface, thereby preventing evaporation of moisture to the outside and promoting hydration.
上記被膜養生剤としては、ポリマーやワックスを有機溶剤に溶かした溶剤タイプと、水中に乳化させた水性タイプがあり、種々の養生剤が提案されている(特許文献1乃至3)。
養生剤の代表的なものとしてパラフィン系の養生剤(特許文献2等)があり、パラフィン系養生剤は、コンクリートやモルタルの水分の蒸発を防ぐ養生効果に優れ、安全性が高い。また、ブリーディングが無く、粘性が高い高強度コンクリートの仕上げ作業を容易にし、プラスチックひび割れを抑制する効果がある。
As the film curing agent, there are a solvent type in which a polymer or a wax is dissolved in an organic solvent, and an aqueous type in which the polymer or wax is emulsified in water, and various curing agents have been proposed (
As a typical curing agent, there is a paraffin-based curing agent (
またセメント系硬化体は、打設直後だけでなく、長期間経過時の乾燥防止も重要である。これは、硬化体が長期にわたり乾燥を受けると、収縮によって部材のひずみが生じ、やがては部材面でのひび割れ発生、漏水等によるコンクリート構造物の劣化を促進し、ひいては構造的欠陥に繋がるおそれがあるためである。また乾燥による劣化以外にも、例えばアルカリ骨材反応、塩害といったセメント系硬化体の劣化現象が挙げられるが、これらの劣化現象は硬化体内部への水分浸入により促進されるものである。 In addition, it is important for the cement-based cured body not only to be dried immediately after being cast, but also to prevent drying after a long period of time. This is because if the cured body is dried over a long period of time, the member will be distorted due to shrinkage, eventually causing cracks on the member surface, promoting deterioration of the concrete structure due to water leakage, etc., which may lead to structural defects. Because there is. In addition to deterioration due to drying, for example, deterioration phenomena of cement-based hardened bodies such as alkali-aggregate reaction and salt damage can be mentioned, but these deterioration phenomena are promoted by moisture intrusion into the hardened body.
上記劣化現象の防止策として、例えば特許文献4には、脂肪酸エステルを用いた撥水剤組成物が提案されている。特許文献5には、飽和脂肪酸エステルのエマルジョンが乾燥抑制剤として適用されている。また、シラン系化合物からなる耐久性向上剤も種々提案されている。例えば、特許文献6には撥水性を有するアルキルポリシロキサンを内添した成形体が提案されており、更に特許文献7にはアルキルアルコキシシランをコンクリート表面に含浸させて撥水性を付与する方法が提案されている。また、乾燥収縮の低減と水分の浸入を防止する表面含浸剤として、特許文献8にオルガノアルコキシシランとグリコールエーテル系界面活性剤の混合物が提案されている。また、特許文献9には、長期に渡って防水性を維持し、乾燥収縮の低減する剤としてテトラアルコキシシランのポリアルキレンオキサイド誘導体が提案されている。 As a measure for preventing the deterioration phenomenon, for example, Patent Document 4 proposes a water repellent composition using a fatty acid ester. In Patent Document 5, an emulsion of a saturated fatty acid ester is applied as a drying inhibitor. Various durability improvers made of silane compounds have also been proposed. For example, Patent Document 6 proposes a molded article in which an alkylpolysiloxane having water repellency is internally added, and Patent Document 7 proposes a method of impregnating a concrete surface with alkylalkoxysilane to impart water repellency. Has been. Further, as a surface impregnating agent for reducing drying shrinkage and preventing moisture from entering, Patent Document 8 proposes a mixture of an organoalkoxysilane and a glycol ether surfactant. Patent Document 9 proposes a polyalkylene oxide derivative of tetraalkoxysilane as an agent that maintains waterproofness for a long period of time and reduces drying shrinkage.
しかしながら、前述した従来のパラフィン系養生剤は、養生剤塗布後に仕上げ材を施工する場合、付着強度が低下し、仕上げ材の剥がれ・ひび割れ・浮き等の発生が懸念される。したがって、パラフィン系養生剤塗布後に仕上げ材を施工する場合には、サンダー掛けによる下地研磨や高圧洗浄などで養生剤の除去を行うことが必要とされている。
またこれまで提案されてきた脂肪酸エステル化合物やアルコキシシラン類を用いたコンクリートの耐久性向上剤は、上述の文献に示されているように、硬化体の乾燥抑制による圧縮強度の増進や撥水性の付与等を主目的とするものであった。しかしながら、これらの技術は打設後短期間での劣化防止能には優れているものの、防水効果が経時で低下するなど、材齢28日以上の長期の耐久性確保においては未だ改善の余地があった。また、近年の土木建築構造物の長寿命化に加え、コンクリートのひび割れ防止の一手段としての収縮低減の需要も多い。
また、硬化体表面に塗布する塗料型の養生剤における高機能化という点において、従来は塗膜の表面の改質のみが着目され、コンクリートの表層から内部に渡って含浸させ、硬化体そのものを物理的性状を改質する技術については、未だ改善の余地があった。
本発明は、養生効果によるセメント系硬化体の強度を充分に発現し、吸水防止性および収縮低減性に優れ、表面のひび割れ発生に対する抵抗性も備え、さらには炭酸ガスや塩化物イオンの侵入を抑制してこれらによるコンクリート劣化を低減できる、セメント系硬化体並びにセメントモルタル及びコンクリートの養生方法を提供することを目的とする。
However, when the above-mentioned conventional paraffin-based curing agent is applied with a finishing material after the curing agent is applied, the adhesion strength is reduced, and there is a concern that the finishing material may be peeled, cracked, floated, or the like. Therefore, when the finishing material is applied after the application of the paraffinic curing agent, it is necessary to remove the curing agent by ground polishing by sanding or high-pressure cleaning.
In addition, the concrete durability improvers using fatty acid ester compounds and alkoxysilanes that have been proposed so far are, as shown in the above-mentioned literature, an increase in compressive strength and water repellency by suppressing drying of the cured product. The main purpose was granting. However, although these technologies are excellent in the ability to prevent deterioration in a short period of time after placement, there is still room for improvement in securing long-term durability over 28 days of age, such as a decrease in waterproofing effect over time. there were. In addition to the long life of civil engineering structures in recent years, there is also a great demand for shrinkage reduction as a means of preventing cracks in concrete.
In addition, in terms of enhancing the functionality of the paint-type curing agent applied to the surface of the cured body, conventionally, only the surface modification of the coating film has been focused, and the cured body itself is impregnated from the surface layer of the concrete. There is still room for improvement in the technology for modifying physical properties.
The present invention sufficiently exhibits the strength of the cement-based cured body due to the curing effect, is excellent in water absorption prevention and shrinkage reduction, has resistance to the occurrence of cracks on the surface, and further invades carbon dioxide and chloride ions. An object of the present invention is to provide a cement-based cured body, a cement mortar, and a curing method for concrete, which can be suppressed and concrete deterioration due to these can be reduced.
本発明者等は上記課題について検討し、研究を進めた結果、特定の構成を有する脂肪酸エステル混合物とアルコキシシラン誘導体を含有する養生剤をセメント系硬化体に適用することにより、硬化後のコンクリート収縮を抑制し、コンクリート硬化体の強度発現を増進し、硬化後の経時的な使用を経て発生する乾燥収縮の低減や吸水防止性を長期に渡って維持できることを見出した。 As a result of studying the above-mentioned problems and conducting research, the present inventors applied a curing agent containing a fatty acid ester mixture having a specific configuration and an alkoxysilane derivative to a cement-based hardened body, thereby causing concrete shrinkage after hardening. It was found that the strength development of the hardened concrete is suppressed, and the reduction of drying shrinkage and water absorption prevention that occur after use over time can be maintained over a long period of time.
すなわち、本発明は、下記一般式(1)で表される脂肪酸エステル混合物(A)と、アルコキシシラン、その加水分解物又はその重縮合物と、下記一般式(2)で表されるポリオキシアルキレン化合物を反応させることによって得られるアルコキシシラン誘導体(B)を含有するコンクリート用養生剤が表面から表層に含浸されてなるセメント系硬化体に関する。
R1CO−O−R2 (1)
(式中、R1COは炭素原子数12〜24の脂肪酸残基を表し、その全脂肪酸残基中、炭
素原子数16〜24の長鎖飽和脂肪酸残基の割合が3〜40質量%、炭素原子数16〜24の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、炭素原子数16〜24の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であり、そして炭素原子数16〜24の長鎖トリ不飽和脂肪酸残基の割合が0〜10質量%の割合であり、R2は炭素原子数1〜8
のアルキル基を表す。)
R3O−(AO)n−H (2)
(式中、R3は炭素原子数が1〜18の炭化水素基を表し、AOは炭素原子数2〜4のオ
キシアルキレン基を表し、nは1〜20の整数を表す。)
That is, the present invention includes a fatty acid ester mixture (A) represented by the following general formula (1), an alkoxysilane, a hydrolyzate thereof or a polycondensate thereof, and a polyoxy represented by the following general formula (2). The present invention relates to a hardened cementitious material obtained by impregnating a surface layer with a curing agent for concrete containing an alkoxysilane derivative (B) obtained by reacting an alkylene compound.
R 1 CO—O—R 2 (1)
(In the formula, R 1 CO represents a fatty acid residue having 12 to 24 carbon atoms, and the proportion of long-chain saturated fatty acid residues having 16 to 24 carbon atoms in the total fatty acid residues is 3 to 40% by mass, The proportion of long-chain monounsaturated fatty acid residues having 16 to 24 carbon atoms is 30 to 50% by mass, the proportion of long-chain diunsaturated fatty acid residues having 16 to 24 carbon atoms is 20 to 40% by mass, and a percentage ratio of 0 mass% of long chain tri-unsaturated fatty acid residues of carbon atoms 16 to 24, R 2 is 1 to 8 carbon atoms
Represents an alkyl group. )
R 3 O— (AO) n —H (2)
(In the formula, R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, AO represents an oxyalkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 to 20).
また本発明は、下記一般式(1)で表される脂肪酸エステル混合物(A)と、アルコキシシラン、その加水分解物又はその重縮合物と、下記一般式(2)で表されるポリオキシアルキレン化合物を反応させることによって得られるアルコキシシラン誘導体(B)を含有するコンクリート用養生剤をセメント系硬化体表面に施工することを特徴とする、セメントモルタル又はコンクリートの養生方法に関する。
R1CO−O−R2 (1)
(式中、R1COは炭素原子数12〜24の脂肪酸残基を表し、その全脂肪酸残基中、炭
素原子数16〜24の長鎖飽和脂肪酸残基の割合が3〜40質量%、炭素原子数16〜24の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、炭素原子数16〜24の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であり、そして炭素原子数16〜24の長鎖トリ不飽和脂肪酸残基の割合が0〜10質量%の割合であり、R2は炭素原子数1〜8
のアルキル基を表す。)
R3O−(AO)n−H (2)
(式中、R3は炭素原子数が1〜18の炭化水素基を表し、AOは炭素原子数2〜4のオ
キシアルキレン基を表し、nは1〜20の整数を表す。)
The present invention also includes a fatty acid ester mixture (A) represented by the following general formula (1), an alkoxysilane, a hydrolyzate thereof or a polycondensate thereof, and a polyoxyalkylene represented by the following general formula (2). The present invention relates to a method for curing cement mortar or concrete, characterized in that a concrete curing agent containing an alkoxysilane derivative (B) obtained by reacting a compound is applied to the surface of a cement-based cured body.
R 1 CO—O—R 2 (1)
(In the formula, R 1 CO represents a fatty acid residue having 12 to 24 carbon atoms, and the proportion of long-chain saturated fatty acid residues having 16 to 24 carbon atoms in the total fatty acid residues is 3 to 40% by mass, The proportion of long-chain monounsaturated fatty acid residues having 16 to 24 carbon atoms is 30 to 50% by mass, the proportion of long-chain diunsaturated fatty acid residues having 16 to 24 carbon atoms is 20 to 40% by mass, and a percentage ratio of 0 mass% of long chain tri-unsaturated fatty acid residues of carbon atoms 16 to 24, R 2 is 1 to 8 carbon atoms
Represents an alkyl group. )
R 3 O— (AO) n —H (2)
(In the formula, R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, AO represents an oxyalkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 to 20).
前記セメント系硬化体並びに前記セメントモルタル又はコンクリートの養生方法において、一般式(1)で表される脂肪酸エステル混合物(A)において、R1COは、その全
脂肪酸残基中、炭素原子数18の長鎖飽和脂肪酸残基の割合が10質量%未満、炭素原子数18の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、そして炭素原子数18の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であることがより好ましい。
In the curing method of the cement-based cured body and the cement mortar or concrete, in the fatty acid ester mixture (A) represented by the general formula (1), R 1 CO is a C 18 carbon atom in the total fatty acid residue. The proportion of long-chain saturated fatty acid residues is less than 10% by mass, the proportion of long-chain monounsaturated fatty acid residues having 18 carbon atoms is 30-50% by mass, and the long-chain diunsaturated fatty acid residues having 18 carbon atoms Is more preferably 20 to 40% by mass.
本発明によれば、高い圧縮強度を有し、乾燥収縮が低減され、また長期にわたって乾燥の防止と防水性が維持されたセメント系硬化体を提供することができる。しかも本発明によれば、表面からの炭酸ガスや塩化物イオンの侵入をも抑制した硬化体となるため、これらの侵入によるコンクリート劣化防止に寄与できる硬化体を提供できる。
また本発明のセメントモルタル又はコンクリートの養生方法を適用することにより、適用初期には硬化体の乾燥を防止し強度発現を促進するとともに収縮をも低減し、長期にわたって硬化体の乾燥を防止しつつ防水性を維持することができる。
ADVANTAGE OF THE INVENTION According to this invention, it can provide the cement-type hardened | cured material which has high compressive strength, drying shrinkage was reduced, and also the prevention of drying and waterproofing were maintained over a long period of time. And according to this invention, since it becomes a hardening body which also suppressed the penetration | invasion of the carbon dioxide gas and chloride ion from the surface, the hardening body which can contribute to the concrete deterioration prevention by these penetration | invasion can be provided.
In addition, by applying the cement mortar or concrete curing method of the present invention, at the initial stage of application, the cured body is prevented from drying, strength development is promoted, shrinkage is reduced, and the cured body is prevented from drying over a long period of time. Waterproofness can be maintained.
本発明は特定の構成を有する脂肪酸エステル混合物とアルコキシシラン誘導体を含有するコンクリート用養生剤をセメント系硬化体に適用することを特徴とする。
以下、本発明について更に詳しく説明する。
The present invention is characterized in that a concrete curing agent containing a fatty acid ester mixture having a specific configuration and an alkoxysilane derivative is applied to a cement-based cured body.
Hereinafter, the present invention will be described in more detail.
[コンクリート用養生剤]
<(A)一般式(1)で表される脂肪酸エステル混合物>
本発明において、コンクリート用養生剤に用いられる(A)脂肪酸エステルは下記一般
式(1)で表される脂肪酸エステルである。
R1CO−O−R2 (1)
(式中、R1COは炭素原子数12〜24の脂肪酸残基を表し、その全脂肪酸残基中、炭
素原子数16〜24の長鎖飽和脂肪酸残基の割合が3〜40質量%、炭素原子数16〜24の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、炭素原子数16〜24の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であり、そして炭素原子数16〜24の長鎖トリ不飽和脂肪酸残基の割合が0〜10質量%の割合であり、R2は炭素原子数1〜8
のアルキル基を表す。)
[Curing agent for concrete]
<(A) Fatty acid ester mixture represented by the general formula (1)>
In the present invention, the (A) fatty acid ester used in the concrete curing agent is a fatty acid ester represented by the following general formula (1).
R 1 CO—O—R 2 (1)
(In the formula, R 1 CO represents a fatty acid residue having 12 to 24 carbon atoms, and the proportion of long-chain saturated fatty acid residues having 16 to 24 carbon atoms in the total fatty acid residues is 3 to 40% by mass, The proportion of long-chain monounsaturated fatty acid residues having 16 to 24 carbon atoms is 30 to 50% by mass, the proportion of long-chain diunsaturated fatty acid residues having 16 to 24 carbon atoms is 20 to 40% by mass, and a percentage ratio of 0 mass% of long chain tri-unsaturated fatty acid residues of carbon atoms 16 to 24, R 2 is 1 to 8 carbon atoms
Represents an alkyl group. )
上記R1COにおいて、炭素原子数12〜24の脂肪酸残基としては炭素原子数12〜
24の長鎖飽和脂肪酸残基、炭素原子数12〜24の長鎖モノ、長鎖ジ、又は長鎖トリ不飽和脂肪酸残基などが挙げられる。なお吸水防止性及び収縮低減性の観点より、上記R1
COは、より好ましくは、その全脂肪酸残基中、炭素原子数16〜24の長鎖飽和脂肪酸残基及び炭素原子数16〜24の長鎖モノ、長鎖ジ、又は長鎖トリ不飽和脂肪酸残基を多く含むことが好ましい。
炭素原子数12〜24の長鎖飽和脂肪酸残基としては、ラウリン酸、ミリスチン酸、ペンタシル酸、パルミチン酸、マルガリン酸、オクタデカン酸、ノナデカン酸、アラキジン酸、ベヘン酸及びリグノセリン酸等由来の脂肪酸残基が挙げられる。
炭素原子数12〜24の長鎖モノ不飽和脂肪酸残基としては、ミリストレイン酸、パルミトレイン酸、オレイン酸、エライジン酸、バクセン酸、ガドレイン酸、エイコセン酸、エルカ酸、ネルボン酸等由来の脂肪酸残基が挙げられる。
炭素原子数12〜24の長鎖ジ不飽和脂肪酸残基としては、リノール酸、エイコサジエン酸、ドコサジエン酸、等由来の脂肪酸残基が挙げられる。炭素原子数12〜24の長鎖トリ不飽和脂肪酸残基としては、リノレン酸、ピノレン酸、エレオステアリン酸、ミード酸、ジホモ−γ−リノレン酸、エイコサトリエン酸等由来の脂肪酸残基が挙げられる。
In the above R 1 CO, the fatty acid residue having 12 to 24 carbon atoms has 12 to 12 carbon atoms.
Examples include 24 long-chain saturated fatty acid residues, long-chain mono-, long-chain di-, or long-chain tri-unsaturated fatty acid residues having 12 to 24 carbon atoms. From the viewpoint of water absorption prevention and shrinkage reduction, the above R 1
More preferably, CO is a long-chain saturated fatty acid residue having 16 to 24 carbon atoms and a long-chain mono-, long-chain di-, or long-chain triunsaturated fatty acid having 16 to 24 carbon atoms in the total fatty acid residues. It is preferable to contain many residues.
Examples of long-chain saturated fatty acid residues having 12 to 24 carbon atoms include fatty acid residues derived from lauric acid, myristic acid, pentasilic acid, palmitic acid, margaric acid, octadecanoic acid, nonadecanoic acid, arachidic acid, behenic acid and lignoceric acid Groups.
Examples of long-chain monounsaturated fatty acid residues having 12 to 24 carbon atoms include fatty acid residues derived from myristoleic acid, palmitoleic acid, oleic acid, elaidic acid, vaccenic acid, gadoleic acid, eicosenoic acid, erucic acid, nervonic acid, etc. Groups.
Examples of the long-chain diunsaturated fatty acid residue having 12 to 24 carbon atoms include fatty acid residues derived from linoleic acid, eicosadienoic acid, docosadienoic acid, and the like. Examples of the long-chain triunsaturated fatty acid residue having 12 to 24 carbon atoms include fatty acid residues derived from linolenic acid, pinolenic acid, eleostearic acid, mead acid, dihomo-γ-linolenic acid, eicosatrienoic acid, and the like. Can be mentioned.
特に上記R1COはその全脂肪酸残基中、より好ましくは、炭素原子数18の長鎖飽和
脂肪酸残基の割合が10質量%未満、炭素原子数18の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、そして炭素原子数18の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であることが好ましい。
In particular, the R 1 CO is more preferably the proportion of long-chain monounsaturated fatty acid residues having less than 10% by mass of long-chain saturated fatty acid residues having 18 carbon atoms and 18 carbon atoms in the total fatty acid residues. The proportion is preferably 30 to 50% by mass, and the proportion of long-chain diunsaturated fatty acid residues having 18 carbon atoms is preferably 20 to 40% by mass.
上記R2において、炭素原子数1〜8のアルキル基としては、メチル基、エチル基、n
−プロピル基、n−ブチル基、n−ペンチル基、n−ヘキシル基、n−ノニル基又はn−オクチル基である直鎖アルキル基;イソプロピル基、イソブチル基、sec−ブチル基、tert−ブチル基、ネオペンチル基、1−エチルプロピル基、2−エチルヘキシル基等の分岐鎖アルキル基等が挙げられる。
中でもメチル基、n−ブチル基、イソプロピル基、イソブチル基、sec−ブチル基、tert−ブチル基、n−オクチル基、2−エチルヘキシル基が好ましく、イソブチル基、sec−ブチル基およびtert−ブチル基が最も好ましい。
In the above R 2 , the alkyl group having 1 to 8 carbon atoms includes a methyl group, an ethyl group, n
A linear alkyl group which is a -propyl group, n-butyl group, n-pentyl group, n-hexyl group, n-nonyl group or n-octyl group; isopropyl group, isobutyl group, sec-butyl group, tert-butyl group , Branched chain alkyl groups such as neopentyl group, 1-ethylpropyl group and 2-ethylhexyl group.
Among them, methyl group, n-butyl group, isopropyl group, isobutyl group, sec-butyl group, tert-butyl group, n-octyl group and 2-ethylhexyl group are preferable, and isobutyl group, sec-butyl group and tert-butyl group are preferable. Most preferred.
<(B)アルコキシシラン誘導体>
本発明において、コンクリート用養生剤に用いられる(B)アルコキシシラン誘導体は、アルコキシシラン、その加水分解物又はその重縮合物と、下記一般式(2)で表されるポリオキシアルキレン化合物を反応させることによって得られるものである。
R3O−(AO)n−H (2)
(式中、R3は炭素原子数が1〜18の炭化水素基を表し、AOは炭素原子数2〜4のオ
キシアルキレン基を表し、nは1〜20の整数を表す。)
<(B) Alkoxysilane Derivative>
In the present invention, the (B) alkoxysilane derivative used in the curing agent for concrete reacts an alkoxysilane, a hydrolyzate thereof or a polycondensate thereof with a polyoxyalkylene compound represented by the following general formula (2). Can be obtained.
R 3 O— (AO) n —H (2)
(In the formula, R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, AO represents an oxyalkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 to 20).
上記アルコキシシランとしては、例えばテトラメトキシシラン、テトラエトキシシラン、テトラプロポキシシラン、テトライソプロポキシシラン、テトラブトキシシラン等のテ
トラアルコキシシラン類;メチルトリメトキシシラン、メチルトリエトキシシラン、メチルトリプロポキシシラン、メチルトリブトキシシラン、エチルトリメトキシシラン、エチルトリエトキシシラン、n−プロピルトリメトキシシラン、n−プロピルトリエトキシシラン、イソプロピルトリメトキシシラン、イソプロピルトリエトキシシラン等のトリアルコキシシラン類;ジメチルジメトキシシラン、ジメチルジエトキシシラン、ジエチルジメトキシシラン、ジエチルジエトキシシラン等のジアルコキシシラン類等を用いることができる。これらのうち、本発明においては入手容易性、取扱性等の観点からテトラメトキシシラン及びテトラエトキシシランの使用が特に好ましい。
Examples of the alkoxysilane include tetraalkoxysilanes such as tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, and tetrabutoxysilane; methyltrimethoxysilane, methyltriethoxysilane, methyltripropoxysilane, methyl Trialkoxysilanes such as tributoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, isopropyltrimethoxysilane, isopropyltriethoxysilane; dimethyldimethoxysilane, dimethyldi Dialkoxysilanes such as ethoxysilane, diethyldimethoxysilane, and diethyldiethoxysilane can be used. Of these, the use of tetramethoxysilane and tetraethoxysilane is particularly preferred in the present invention from the viewpoints of availability, handling, and the like.
アルコキシシランの加水分解物/重縮合物は、例えば、アルコキシシランの所定量を水、メタノール、エタノール、酢酸エチル等の水もしくは有機溶媒に溶解し、そのまま加熱あるいは所定量の酸もしくは塩基を添加して部分的に加水分解させることにより調製することができる。通常、重合度は2〜10が好ましい。 The alkoxysilane hydrolyzate / polycondensate is prepared, for example, by dissolving a predetermined amount of alkoxysilane in water, water such as methanol, ethanol, ethyl acetate or an organic solvent, and heating or adding a predetermined amount of acid or base. And can be prepared by partial hydrolysis. Usually, the degree of polymerization is preferably 2 to 10.
前記一般式(2)で表されるポリオキシアルキレン化合物において、R3は炭素原子数
が1〜18の炭化水素基を表し、該炭化水素基としては炭素原子数1〜30のアルキル基;フェニル基、アルキルフェニル基、アルキルフェニル基で置換されたフェニル基、及びナフチル基等のベンゼン環を有する炭素原子数6〜18の芳香族基;並びにオレイル基、リノレイル基等の炭素原子数2乃至18のアルケニル基が挙げられ、中でも炭素原子数1〜30のアルキル基であることが好ましい。
炭素原子数1〜30のアルキル基としては、具体的にはメチル基、エチル基、n−プロピル基、n−ブチル基、n−ペンチル基、n−ヘキシル基、n−オクチル基、n−デシル基、n−ドデシル基、n−テトラデシル基、n−ヘキサデシル基、n−オクタデシル基等の直鎖アルキル基;イソプロピル基、sec−ブチル基、tert−ブチル基、ネオペンチル基、1−エチルプロピル基、1−ヘプチルデシル基、2−エチルヘキシル基等の分岐鎖アルキル基が挙げられる。これらのうち、炭素原子数1〜8のアルキル基が好ましく、n−ブチル基、2−エチルヘキシル基がより好ましく、n−ブチル基が最も好ましい。
In the polyoxyalkylene compound represented by the general formula (2), R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, and the hydrocarbon group is an alkyl group having 1 to 30 carbon atoms; An aromatic group having 6 to 18 carbon atoms having a benzene ring such as a group, an alkylphenyl group, a phenyl group substituted with an alkylphenyl group, and a naphthyl group; and 2 to 18 carbon atoms such as an oleyl group and a linoleyl group Among them, an alkenyl group is preferably an alkyl group having 1 to 30 carbon atoms.
Specific examples of the alkyl group having 1 to 30 carbon atoms include methyl group, ethyl group, n-propyl group, n-butyl group, n-pentyl group, n-hexyl group, n-octyl group, and n-decyl group. Group, n-dodecyl group, n-tetradecyl group, n-hexadecyl group, n-octadecyl group and other linear alkyl groups; isopropyl group, sec-butyl group, tert-butyl group, neopentyl group, 1-ethylpropyl group, Examples thereof include branched alkyl groups such as 1-heptyldecyl group and 2-ethylhexyl group. Among these, an alkyl group having 1 to 8 carbon atoms is preferable, an n-butyl group and a 2-ethylhexyl group are more preferable, and an n-butyl group is most preferable.
前記一般式(2)で表されるポリオキシアルキレン化合物において、AOは炭素原子数2〜4のオキシアルキレン基を示し、具体的にはエチレンオキシ基、プロピレンオキシ基、ブチレンオキシ基が挙げられる。nはアルキレンオキサイドの付加モル数であって、0〜20の整数を表す。nが2以上の場合、オキシアルキレン基は同一のものであっても異なるものであってもよい。(AO)nが2種以上のアルキレンオキシ基から構成される場
合は、ブロック付加、ランダム付加のいずれであってもよいが、ブロック付加であることが好ましく、特に水素原子に連結する末端がエチレンオキシ基であることがより好ましい。
In the polyoxyalkylene compound represented by the general formula (2), AO represents an oxyalkylene group having 2 to 4 carbon atoms, and specific examples include an ethyleneoxy group, a propyleneoxy group, and a butyleneoxy group. n is the number of added moles of alkylene oxide, and represents an integer of 0 to 20. When n is 2 or more, the oxyalkylene groups may be the same or different. (AO) When n is composed of two or more types of alkyleneoxy groups, either block addition or random addition may be used, but block addition is preferred, and the terminal connected to the hydrogen atom is particularly ethylene. More preferred is an oxy group.
前記一般式(2)で表されるポリオキシアルキレン化合物の具体例としては、ポリエチレングリコールポリプロピレングリコールモノメチルエーテル、ポリエチレングリコールモノメチルエーテル、ポリエチレングリコールポリプロピレングリコールモノエチルエーテル、ポリエチレングリコールモノエチルエーテル、ポリエチレングリコールポリプロピレングリコールモノプロピルエーテル、ポリエチレングリコールモノプロピルエーテル、ポリエチレングリコールポリプロピレングリコールモノブチルエーテル、ポリエチレングリコールモノブチルエーテル等のポリオキシアルキレンアルキルエーテルが挙げられる。 Specific examples of the polyoxyalkylene compound represented by the general formula (2) include polyethylene glycol polypropylene glycol monomethyl ether, polyethylene glycol monomethyl ether, polyethylene glycol polypropylene glycol monoethyl ether, polyethylene glycol monoethyl ether, polyethylene glycol polypropylene glycol. Examples thereof include polyoxyalkylene alkyl ethers such as monopropyl ether, polyethylene glycol monopropyl ether, polyethylene glycol polypropylene glycol monobutyl ether, and polyethylene glycol monobutyl ether.
上記アルコキシシラン誘導体は、例えば前記アルコキシシラン、その加水分解物又はその重縮合物と上記一般式(2)で表されるポリオキシアルキレン化合物とを反応容器に仕込み、加熱して生成するアルコールを留去しながらエステル交換反応を行うことにより得ることができる。反応温度は通常50〜150℃程度である。また、上記のエステル交換反応に際しては、反応促進のために従来公知の触媒を使用することができる。また、前記
アルコキシシラン、その加水分解物又はその重縮合物と上記一般式(2)で表されるポリオキシアルキレン化合物の反応比率は前記アルコキシシラン、その加水分解物又はその重縮合物中のアルコキシ基の1当量に対し、上記一般式(2)で表されるポリオキシアルキレン化合物が0.3〜1当量であれば好ましく、0.5〜1当量であればより好ましい。
The alkoxysilane derivative is prepared, for example, by charging the alkoxysilane, its hydrolyzate or its polycondensate, and the polyoxyalkylene compound represented by the above general formula (2) into a reaction vessel, and heating it to stop the alcohol produced. It can be obtained by conducting a transesterification reaction while leaving. The reaction temperature is usually about 50 to 150 ° C. In the transesterification reaction, a conventionally known catalyst can be used for promoting the reaction. The reaction ratio of the alkoxysilane, its hydrolyzate or its polycondensate and the polyoxyalkylene compound represented by the above general formula (2) is the same as that of the alkoxysilane, its hydrolyzate or its polycondensate. The polyoxyalkylene compound represented by the general formula (2) is preferably 0.3 to 1 equivalent, more preferably 0.5 to 1 equivalent per 1 equivalent of the group.
本発明で使用するコンクリート用養生剤において、(A)脂肪酸エステル混合物と(B)アルコキシシラン誘導体の配合割合は、質量比で5〜95:95〜5の範囲内で使用でき、より好ましくは20〜95:80〜5、50〜95:50〜5、70〜95:30〜5、最も好ましくは70〜90:30〜10にて使用することができる。 In the concrete curing agent used in the present invention, the blending ratio of (A) fatty acid ester mixture and (B) alkoxysilane derivative can be used within a range of 5 to 95:95 to 5 by mass ratio, more preferably 20 ~ 95: 80-5, 50-95: 50-5, 70-95: 30-5, most preferably 70-90: 30-10.
本発明で使用するコンクリート用養生剤において、前記(A)脂肪酸エステル混合物と(B)アルコキシシラン誘導体に加え、水硬性組成物に一般に使用されるその他の成分を含んでいても良い。他に含まれ得るその他の成分としては、汎用的に使用される防水剤、耐水剤、撥水剤、消泡剤、養生剤、収縮低減剤が挙げられる。これら併用されるその他の成分の配合比は、質量比で前記(A)脂肪酸エステル混合物と(B)アルコキシシラン誘導体の総質量:併用されるその他の成分の総質量=50:50〜99:1の割合で、好ましくは70:30〜99:1である。 The concrete curing agent used in the present invention may contain other components generally used in hydraulic compositions in addition to the (A) fatty acid ester mixture and (B) alkoxysilane derivative. Other components that may be included include water-proofing agents, water-resistant agents, water-repellent agents, antifoaming agents, curing agents, and shrinkage reducing agents that are used for general purposes. The compounding ratio of these other components used in combination is, in mass ratio, the total mass of the (A) fatty acid ester mixture and (B) alkoxysilane derivative: the total mass of other components used in combination = 50: 50 to 99: 1. The ratio is preferably 70:30 to 99: 1.
[セメント系硬化体 及び セメントモルタル又はコンクリートの養生方法]
本発明においてセメント系硬化体とは、セメント類に細骨材及び水を混合したセメントモルタル或いは更に粗骨材を配合したコンクリートの硬化体であり、各種混和材料から選ばれる1種又は2種以上を更に配合したものでもよい。
本発明に用いられるセメント類としては、水硬性を有するものであればよく、例えば、普通ポルトランドセメントや早強ポルトランドセメント等のポルトランドセメント、エコセメント、高炉セメントやフライアッシュセメント等の混合セメント、アルミナセメント、太平洋セメント(株)製「スーパージェットセメント」(商品名)や住友大阪セメント(株)製「ジェットセメント」(商品名)等の超速硬セメント、半水石膏、高炉スラグ等の潜在水硬性物質が挙げられ、これらから選ばれる一種又は二種以上を用いることができる。
[Cemented hardened body and cement mortar or concrete curing method]
In the present invention, the cement-based cured body is a cement cured mortar in which fine aggregates and water are mixed with cement or further mixed with coarse aggregate, and one or more selected from various admixtures. May be further blended.
The cement used in the present invention is not particularly limited as long as it has hydraulic properties, for example, portland cement such as ordinary portland cement and early-strength portland cement, eco-cement, mixed cement such as blast furnace cement and fly ash cement, and alumina. Latent hydraulic properties such as cement, "super jet cement" (trade name) manufactured by Taiheiyo Cement Co., Ltd. and super fast cement such as "jet cement" (trade name) manufactured by Sumitomo Osaka Cement Co., Ltd., hemihydrate gypsum, blast furnace slag, etc. A substance is mentioned and 1 type, or 2 or more types chosen from these can be used.
前述のコンクリート用養生剤を、硬化したセメント系硬化体(セメントモルタル又はコンクリート硬化体)の表面に施工することにより、該養生剤が硬化体表面から表層に含浸され、本発明のセメント系硬化体を得ることができる。具体的にはセメント系硬化体の仕上げ時の仕上げ補助として、または、セメント系硬化体の硬化脱型後、硬化体に前述のコンクリート用養生剤を施工する。該コンクリート用養生剤の施工方法は、セメント系硬化体の表面に施工できる方法であれば特に限定されるものではなく、散布、塗布、吹付け、噴霧等で行うことが可能であり、ローラ、刷毛又はブラシ等による塗布、噴霧器等による噴霧等のように、セメント系硬化体の表面に均一に施工できるものが好ましい。
前記コンクリート用養生剤をセメント系硬化体に対して塗布する際、通常その表面に対して50〜300g/m2程度を使用する。50gより少ないと、仕上げ時のスムーズな
コテ均し及び水分の逸散防止効果が得られにくくなる虞があり、300gを超えると過剰な量で付着強度の低下が懸念される。また、対象となるセメント系硬化体としてはモルタルおよびコンクリートのいずれも含まれる。
By applying the above-mentioned curing agent for concrete on the surface of a hardened cement-based cured body (cement mortar or concrete cured body), the curing agent is impregnated on the surface layer from the surface of the cured body, and the cement-based cured body of the present invention Can be obtained. Specifically, the above-mentioned curing agent for concrete is applied to the hardened body as a finishing aid when finishing the hardened cementitious body, or after hardening and demolding of the hardened cementitious body. The method for applying the curing agent for concrete is not particularly limited as long as it can be applied to the surface of the cement-based cured body, and can be performed by spraying, coating, spraying, spraying, and the like. Those that can be applied uniformly to the surface of the hardened cementitious body are preferred, such as application with a brush or brush, spraying with a sprayer, or the like.
When the concrete curing agent is applied to a cement-based cured body, usually about 50 to 300 g / m 2 is used with respect to the surface. If the amount is less than 50 g, there is a concern that it will be difficult to obtain smooth scouring and moisture dissipation prevention effects at the time of finishing, and if it exceeds 300 g, there is a concern that the adhesion strength will be reduced by an excessive amount. Moreover, both mortar and concrete are included as a cementitious hardened | cured material used as object.
本発明のセメント系硬化体は、硬化初期において乾燥が抑制され強度発現が促進されるとともに収縮をも低減された硬化体となり、また、長期にわたって乾燥が抑制され且つ防水性が維持された硬化体とすることができる。そして本発明のセメントモルタル又はコンクリートの養生方法を適用することにより、適用初期には硬化体の乾燥を抑制し強度発現を促進するとともに収縮をも低減し、長期にわたって硬化体の乾燥を抑制しつつ防水性を維持することが可能となる。
上述の効果(高い強度、収縮低減性及び吸水防止性の向上)が得られる理由は明らかではないが、養生剤に不飽和結合の数が異なる脂肪酸エステルを組み合わせて脂肪酸エステル混合物の形態として用いることにより、硬化体表面に配列したときに各々の分子間立体反発を緩和し、緻密な層を形成しているものと推察される。これが高い養生効果と吸水防止性に寄与し、さらには炭酸ガスや塩化物イオンの侵入抑制にも貢献しているものと推察される。
またアルコキシシラン誘導体は、親水性と疎水性のバランスが最適化された構造を有し、セメント系硬化体表面から数cm内部までの表層部分へと浸透するのに適した構造となっている。そのため、該誘導体が硬化体の表層部分における水分保持に寄与し、前述の脂肪酸エステル混合物が有する外部からの水分の浸入防止と高い養生効果の実現と相まって、セメント系硬化体の乾燥抑制と防水性の維持、さらには炭酸ガスや塩化物イオンの侵入抑制における相乗効果の発現につながると推察される。
The cement-based cured body of the present invention is a cured body in which drying is suppressed in the initial stage of curing, strength development is promoted, and shrinkage is reduced, and drying is suppressed over a long period of time and waterproofness is maintained. It can be. And, by applying the cement mortar or concrete curing method of the present invention, at the initial stage of application, the drying of the cured body is suppressed, the strength development is promoted and the shrinkage is also reduced, and the drying of the cured body is suppressed over a long period of time. It becomes possible to maintain waterproofness.
The reason why the above-mentioned effects (high strength, shrinkage reduction and improvement in water absorption prevention) are obtained is not clear, but a fatty acid ester having a different number of unsaturated bonds is used in combination with a curing agent as a form of a fatty acid ester mixture. Thus, it is presumed that when arranged on the surface of the cured body, each intermolecular steric repulsion is relaxed and a dense layer is formed. It is presumed that this contributes to a high curing effect and water absorption prevention, and also contributes to the suppression of intrusion of carbon dioxide and chloride ions.
Further, the alkoxysilane derivative has a structure in which the balance between hydrophilicity and hydrophobicity is optimized, and has a structure suitable for penetrating into the surface layer portion from the cement-based cured body surface to the inside of several centimeters. Therefore, the derivative contributes to moisture retention in the surface layer portion of the cured body, and is coupled with the prevention of moisture penetration from the outside and the realization of a high curing effect possessed by the above-mentioned fatty acid ester mixture, and drying suppression and waterproofness of the cement-based cured body It is presumed that this will lead to the development of a synergistic effect in the maintenance of carbon dioxide and further the suppression of infiltration of carbon dioxide and chloride ions.
次に、実施例に基づいて本発明をより詳しく説明するが、本発明は下記の実施例に限定されるものではない。 Next, the present invention will be described in more detail based on examples, but the present invention is not limited to the following examples.
[コンクリート用養生剤]
<脂肪酸エステル混合物>
以下の実施例及び比較例で使用した式(1)R1CO−O−R2で表される脂肪酸エステル混合物の組成を表1に示す。
<Fatty acid ester mixture>
Table 1 shows the composition of the fatty acid ester mixture represented by the formula (1) R 1 CO—O—R 2 used in the following Examples and Comparative Examples.
[アルコキシシラン誘導体]
以下の実施例で使用したアルコキシシラン誘導体を以下の手順にて調製した。なお文中、アルコキシシランに対するポリオキシアルキレン化合物(以降、ポリアルキレングリコールとも称する)のモル比率とは、アルコキシシラン構造中のアルコキシ基1モルに対するポリオキシアルキレン化合物の仕込みモル比である。
[Alkoxysilane derivatives]
The alkoxysilane derivative used in the following examples was prepared by the following procedure. In the text, the molar ratio of the polyoxyalkylene compound (hereinafter also referred to as polyalkylene glycol) to the alkoxysilane is the charged molar ratio of the polyoxyalkylene compound to 1 mole of the alkoxy group in the alkoxysilane structure.
(製造例1:アルコキシシラン誘導体(化合物B−1)の製造方法)
撹拌機、温度計、コンデンサー、留出物回収槽及び窒素導入管を備え付けた反応容器にテトラエトキシシラン401部、ポリエチレングリコールモノブチルエーテル(ポリエチレングリコールの繰り返し単位の平均が3であるもの)1593部(アルコキシシランに対するモル比率:4)及びトリエチルアミン5部を仕込んだ。反応器内を窒素気流下とし、140℃まで2時間かけて昇温後、同温にて7時間撹拌し、生成するエタノールを留出
させながら反応させた。反応の終点はエタノールの回収量により判断し、淡黄色液体(化合物B−1)1569部(収率95%)を得た。
(Production Example 1: Production method of alkoxysilane derivative (compound B-1))
In a reaction vessel equipped with a stirrer, thermometer, condenser, distillate collection tank and nitrogen introduction tube, 401 parts of tetraethoxysilane, 1593 parts of polyethylene glycol monobutyl ether (average of polyethylene glycol repeating units is 3) A molar ratio to alkoxysilane: 4) and 5 parts of triethylamine were charged. The reactor was placed in a nitrogen stream, heated to 140 ° C. over 2 hours, stirred at the same temperature for 7 hours, and reacted while distilling the produced ethanol. The end point of the reaction was judged by the amount of ethanol recovered to obtain 1569 parts (yield 95%) of a pale yellow liquid (Compound B-1).
(製造例2:アルコキシシラン誘導体(化合物B−2)の製造方法)
トリエチルアミンの仕込み量、装置および製造手順は製造例1に従い、テトラエトキシシラン317部、ポリエチレングリコールモノブチルエーテルのかわりにポリエチレングリコールモノ−2−エチルヘキシルエーテル(ポリエチレングリコールの繰り返し単位の平均が3であるもの)1601部(アルコキシシランに対するモル比率:4)を用いて、化合物B−2(1560部、収率95%)を得た。
(Production Example 2: Production method of alkoxysilane derivative (compound B-2))
Charge amount, apparatus and production procedure of triethylamine are in accordance with Production Example 1, 317 parts of tetraethoxysilane, polyethylene glycol mono-2-ethylhexyl ether instead of polyethylene glycol monobutyl ether (the average of polyethylene glycol repeating units is 3) Using 1601 parts (molar ratio to alkoxysilane: 4), compound B-2 (1560 parts, yield 95%) was obtained.
(製造例3:アルコキシシラン誘導体(化合物B−3)の製造方法)
トリエチルアミンの仕込み量、装置および製造手順は製造例1に従い、テトラエトキシシランのかわりにエトキシシラン重縮合物(平均重合度5)1087部、ポリエチレングリコールモノブチルエーテル(ポリエチレングリコールの繰り返し単位の平均が3であるもの)908部(アルコキシシランに対するモル比率:3)を用いて、化合物B−3(1707部、収率95%)を得た。
(Production Example 3: Method for producing alkoxysilane derivative (compound B-3))
The amount of triethylamine charged, the apparatus and the production procedure were the same as in Production Example 1. Instead of tetraethoxysilane, 1087 parts of ethoxysilane polycondensate (average polymerization degree 5), polyethylene glycol monobutyl ether (average of polyethylene glycol repeating units was 3) Compound B-3 (1707 parts, 95% yield) was obtained using 908 parts (something) (molar ratio to alkoxysilane: 3).
上記脂肪酸エステル混合物:混合物A−1、比較混合物C−1及びC−2、並びに、上記調製したアルコキシシラン誘導体:化合物B−1〜B−3を用いて後述の表3に示す実施例及び比較例の養生剤とし、以下の手順にて製造したフレッシュコンクリートの硬化体に適用し、各種性能を評価した。なお比較例1として養生剤を使用していない硬化体(ブランク)も合わせて評価した。 Examples and comparisons shown in Table 3 below using the fatty acid ester mixture: mixture A-1, comparative mixtures C-1 and C-2, and the prepared alkoxysilane derivatives: compounds B-1 to B-3 It applied to the hardening body of the fresh concrete manufactured with the following procedures as an example of a curing agent, and various performances were evaluated. As Comparative Example 1, a cured body (blank) that did not use a curing agent was also evaluated.
[試験用フレッシュコンクリートの製造]
コンクリートの仕様は呼び強度30MPaとし、スランプ:8±2.5cm、空気量:4.5±1.5%とした。試験用コンクリートの配合を表2に示す。練り混ぜ方法は、公称容量1m3の水平二軸強制練りミキサを用いて、各バッチのコンクリート製造量を0.
8m3×1バッチとし、まずセメントと細骨材をミキサへ投入し10秒練り、その後練り
混ぜ水、混和剤と粗骨材を投入して120秒間練り混ぜ、その後排出し、以降の試験の供した。
[Manufacture of fresh concrete for testing]
The specifications of the concrete were nominal strength 30 MPa, slump: 8 ± 2.5 cm, air amount: 4.5 ± 1.5%. Table 2 shows the composition of the test concrete. The kneading method uses a horizontal biaxial forced kneading mixer with a nominal capacity of 1 m 3 , and the amount of concrete produced in each batch is set to 0. 0.
Make 8m 3 × 1 batch, first put cement and fine aggregate into mixer and knead for 10 seconds, then mix water, admixture and coarse aggregate, mix for 120 seconds, then discharge, Provided.
[養生剤を用いたコンクリート試験評価]
<コンクリートの圧縮強度試験>
前記の手順にて作製したフレッシュコンクリートで、圧縮強度試験用の供試体(φ10cm×20cm)を作製し、圧縮強度試験を行った。供試体は作製の翌日に脱型し、供試体全面(上面、底面、側面)に表3に示す各養生剤を均一に塗布(150g/m2)し、
温度20℃、湿度60%の環境下にて気中養生を行った。圧縮強度試験はJIS A 1108(コンクリートの圧縮強度試験方法)に準拠し、改質剤塗布後、材齢7日及び材齢28日における圧縮強度を測定した。結果を表3に示す。
[Concrete test evaluation using curing agent]
<Compressive strength test of concrete>
A specimen (φ10 cm × 20 cm) for compressive strength test was prepared from the fresh concrete prepared by the above procedure, and a compressive strength test was performed. The specimen was demolded the day after production, and each curing agent shown in Table 3 was uniformly applied (150 g / m 2 ) to the entire specimen surface (top, bottom, side),
In-air curing was performed in an environment of temperature 20 ° C. and humidity 60%. The compressive strength test was based on JIS A 1108 (Concrete compressive strength test method), and after applying the modifier, the compressive strength at a material age of 7 days and a material age of 28 days was measured. The results are shown in Table 3.
<乾燥質量減少率、長さ変化率>
前記の手順にて作製したフレッシュコンクリートで、乾燥質量減少率ならびに長さ変化率測定用のコンクリート供試体(縦10cm×横10cm×高さ40cm)を作製し、乾燥質量減少率の測定を行った。供試体は材齢3日で脱枠し、脱枠直後に作製したコンクリート供試体上面に表3に示す各養生剤を塗布(150g/m2)したのち、供試体の質量
を測定し、乾燥質量減少率の基点とした。またモールドゲージ方法にて供試体の寸法を測定し、これを長さ変化率の基準値とした。以降供試体を温度20℃、湿度60%の条件にて保管し、材齢28日における乾燥質量減少率および長さ変化率を後述の式を用いて算出した。
ここで、乾燥質量減少率の値が小さい供試体ほど、供試体中の水分逸散を抑制できていることを意味する。また長さ変化率の値は、養生剤を塗布していない供試体(比較例1)の長さ変化率の値より小さいほど、供試体の乾燥収縮を抑制していることを意味する。結果を表3に示す。
<Dry weight loss rate, length change rate>
A concrete specimen (10 cm long × 10 cm wide × 40 cm height) for measuring the dry mass reduction rate and the length change rate was produced from the fresh concrete produced by the above procedure, and the dry mass reduction rate was measured. . The specimen was unframed at the age of 3 days, and after applying each curing agent shown in Table 3 (150 g / m 2 ) on the upper surface of the concrete specimen prepared immediately after the deframement, the mass of the specimen was measured and dried. It was used as the base point of mass reduction rate. Moreover, the dimension of the specimen was measured by the mold gauge method, and this was used as the reference value for the rate of change in length. Thereafter, the specimen was stored under the conditions of a temperature of 20 ° C. and a humidity of 60%, and the dry mass reduction rate and length change rate at the age of 28 days were calculated using the formulas described below.
Here, the smaller the value of the dry mass reduction rate means that the moisture dissipation in the test sample can be suppressed. Moreover, the value of the length change rate means that the smaller the value of the length change rate of the specimen to which the curing agent is not applied (Comparative Example 1), the more the drying shrinkage of the specimen is suppressed. The results are shown in Table 3.
《乾燥質量減少率》
乾燥質量減少率(%)={[試験後の供試体の質量−試験前の供試体の質量]/[試験前の供試体の質量]}×100
《長さ変化率》
長さ変化率(10-6)=[試験後の各供試体の長さ(mm)−試験前の供試体の長さ(mm)]/[試験前の供試体の長さ(mm)]
《Dry weight loss rate》
Dry mass reduction rate (%) = {[mass of specimen after test−mass of specimen before test] / [mass of specimen before test]} × 100
《Length change rate》
Length change rate (10 −6 ) = [length of each specimen after test (mm) −length of specimen before test (mm)] / [length of specimen before test (mm)]
<吸水防止性能試験>
前記手順にして作製したフレッシュコンクリートで試験板(縦1,000mm×横1,000mm×厚さ100mm、図1参照)を作製し、吸水防止性能の測定に適用した。表3に示す各養生剤を試験板表面に塗布(150g/m2)した後、該試験板を単管パイプ
で組み立てた試験板設置枠を用いて屋外放置した(図2参照)。
材齢28日の時点で、試験板1表面の6箇所に太さの異なる2つの円柱が組み合わさってできた漏斗形状のガラス器具2を粘着剤3を用いて設置(接着)した(図1(B)参照)。なおこのガラス器具2の試験板1と接する太い円柱部分の径2aは27mmφ、この太い円柱部分の長さ2cは40mm、細い円柱部分の径2bは12mmφ、細い円柱部分の長さ2dは115mmである。図1(A)にガラス器具の接着箇所(試験点):上部A点〜C点、下部D〜F点を示す。設置したガラス器具2の内部をイオン交換水で満たし、パラフィン製フィルムでガラス器具2の開口部2−1を覆い密封した。試験点A〜Fのそれぞれにつき、48時間経過後のイオン交換水の吸水量を測定し、上部試験点(A点〜C点)と、下部試験点(D点〜E点)のそれぞれの単位面積(1cm2)当たりの吸水量の
平均値(単位吸水量)を求めた。結果を表3に示す。
<Water absorption prevention performance test>
A test plate (length 1000 mm × width 1,000 mm × thickness 100 mm, see FIG. 1) was prepared from the fresh concrete prepared according to the above procedure, and applied to the measurement of water absorption prevention performance. After applying each curing agent shown in Table 3 to the surface of the test plate (150 g / m 2 ), the test plate was left outdoors using a test plate installation frame assembled with a single pipe pipe (see FIG. 2).
At the age of 28 days, a funnel-shaped
なお、吸水防止性能は、養生剤を塗布していないブランクの試験板(比較例1)と比較して、単位吸水量の値が少ないほど、供試体中への水分浸入を抑制できていることを意味する。さらに、上部と下部の単位吸水量の値が同等であるものは、所定の性能が均一に得られていることを示している。 It should be noted that the water absorption prevention performance is such that, as the unit water absorption value is smaller, the moisture intrusion into the specimen can be suppressed as compared with the blank test plate (Comparative Example 1) to which no curing agent is applied. Means. Furthermore, the unit water absorption values of the upper part and the lower part that are equal indicate that the predetermined performance is obtained uniformly.
<炭酸ガスの浸透抑制性能試験>
前記手順にして作製したフレッシュコンクリートでJIS A 1153(コンクリートの促進中性化試験方法)に準拠して試験体(10×10×20cm)を作製し、試験体全面(上面、底面、側面)に表3に示す各緻密層形成剤を均一に塗布(150g/m2)
し、各試験体を温度20℃、湿度60%の条件にて保管した。材齢1週間経過後、温度20℃、湿度60%、CO2濃度5%促進養生を行い、JIS A 1152(コンクリー
トの中性化深さの測定方法)に準拠し、試験体の28日後の中性化深さ(炭酸ガス浸透性)を測定した。
<Permeation suppression performance test for carbon dioxide>
A test specimen (10 × 10 × 20 cm) is prepared from the fresh concrete prepared according to the above procedure in accordance with JIS A 1153 (accelerated neutralization test method for concrete), and the entire test specimen (top, bottom, side) is prepared. Uniformly apply each dense layer forming agent shown in Table 3 (150 g / m 2 )
Each specimen was stored under conditions of a temperature of 20 ° C. and a humidity of 60%. After one week of material age, temperature curing 20 ° C, humidity 60%, CO 2 concentration 5% accelerated curing, in accordance with JIS A 1152 (measurement of the carbonation depth of concrete), 28 days after the specimen The neutralization depth (carbon dioxide permeability) was measured.
<塩化物イオン浸透抑制性能試験>
前記手順にして作製したフレッシュコンクリートで試験体(10×10×40cm)を作製し、試験体全面(上面、底面、側面)に表3に示す各緻密層形成剤を均一に塗布(150g/m2)し、各試験体を温度20℃、湿度60%の条件にて保管した。材齢1週間
経過後より、各試験体を40℃の5%NaCl水溶液を3日間噴霧したのち、4日間湿度60%で乾燥させるという塩水噴霧乾湿繰り返しサイクルを1ヶ月間継続し、JIS A
1171(ポリマーセメントモルタルの試験方法)に準拠し、28日後の塩分浸透深さを測定した。
<Chlorine ion penetration inhibition performance test>
A test specimen (10 × 10 × 40 cm) was prepared from the fresh concrete prepared according to the above procedure, and each dense layer forming agent shown in Table 3 was uniformly applied to the entire specimen surface (upper surface, bottom surface, side surface) (150 g / m 2 ) and each specimen was stored under conditions of a temperature of 20 ° C. and a humidity of 60%. After one week of material age, each test specimen was sprayed with a 5% NaCl aqueous solution at 40 ° C. for 3 days and then dried at 60% humidity for 4 days.
In accordance with 1171 (Testing method for polymer cement mortar), the salt penetration depth after 28 days was measured.
表3に示すように、脂肪酸エステル混合物(A−1)とアルコキシシラン誘導体(B−1〜B−3)とを含有するコンクリート用養生剤を適用したセメント系硬化体(実施例1〜実施例3)は、養生剤を用いていないブランクの硬化体(比較例1)、並びに長鎖モノ不飽和脂肪酸残基の割合が多い脂肪酸エステル混合物(C−1)及び長鎖ジ不飽和脂肪酸残基の割合が多い脂肪酸エステル混合物(C−2)を含有する養生剤を適用した硬化体(比較例2及び比較例3)に比べ、圧縮強度が高く、乾燥質量減少率及び長さ変化率が低く、吸水防止性を示す単位吸水量の値も小さいとする結果となった。特に、比較例2及び比較例3の硬化体においては単位吸水量の上部と下部の値の差が大きいものの、実施例1〜3の硬化体は単位吸水量の上部と下部の値に殆ど差がないとする結果となり、本発明の硬化体が、適用した箇所(場所)によらず所定の性能が均一に得られた硬化体であるとする
結果となった。
さらに、上記コンクリート用養生材を適用した硬化体(実施例1〜実施例3)は、比較例の硬化体と比べ、いずれも炭酸ガスや塩化物イオンの浸透性(拡散性)も抑えられたものとなっているとする結果が得られた。
尚、実施例1〜実施例3は比較例1に比べて、圧縮強度が9〜10%向上しているが、これは、実施例1〜実施例3のセメント硬化体が比較例1のセメント硬化体と比べ、硬化体表層内部が緻密な構造となっていることを示唆するものであり、これにより炭酸ガスや塩化物イオンの浸透性(拡散性)の抑制につながったものとみられる。
As shown in Table 3, a cement-based cured body to which a curing agent for concrete containing a fatty acid ester mixture (A-1) and an alkoxysilane derivative (B-1 to B-3) is applied (Example 1 to Example). 3) is a hardened blank (Comparative Example 1) that does not use a curing agent, and a fatty acid ester mixture (C-1) and a long-chain diunsaturated fatty acid residue having a large proportion of long-chain monounsaturated fatty acid residues. Compared with the hardened material (Comparative Example 2 and Comparative Example 3) to which the curing agent containing the fatty acid ester mixture (C-2) containing a large proportion is applied, the compression strength is high, and the dry mass reduction rate and the length change rate are low. As a result, the unit water absorption value indicating the water absorption preventing property was also small. In particular, in the cured bodies of Comparative Example 2 and Comparative Example 3, although the difference between the upper and lower values of the unit water absorption is large, the cured bodies of Examples 1 to 3 are almost different in the upper and lower values of the unit water absorption. As a result, the cured product of the present invention was determined to be a cured product having a predetermined performance uniformly obtained regardless of the place (location) applied.
Furthermore, the hardened bodies (Examples 1 to 3) to which the above concrete curing material was applied were all suppressed in the permeability (diffusibility) of carbon dioxide and chloride ions as compared with the hardened bodies of the comparative examples. The result was assumed to be.
The compressive strength of Examples 1 to 3 is 9 to 10% higher than that of Comparative Example 1. This is because the hardened cement of Examples 1 to 3 is the cement of Comparative Example 1. This suggests that the inside of the surface of the cured body has a dense structure compared to the cured body, and this seems to have led to the suppression of the permeability (diffusibility) of carbon dioxide and chloride ions.
1・・・試験板
2・・・ガラス器具
2−1・・・開口部
3・・・粘着剤
DESCRIPTION OF
Claims (4)
R1CO−O−R2 (1)
(式中、R1COは炭素原子数12〜24の脂肪酸残基を表し、その全脂肪酸残基中、炭
素原子数16〜24の長鎖飽和脂肪酸残基の割合が3〜40質量%、炭素原子数16〜24の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、炭素原子数16〜24の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であり、そして炭素原子数16〜24の長鎖トリ不飽和脂肪酸残基の割合が0〜10質量%の割合であり、R2は炭素原子数1〜8
のアルキル基を表す。)
R3O−(AO)n−H (2)
(式中、R3は炭素原子数が1〜18の炭化水素基を表し、AOは炭素原子数2〜4のオ
キシアルキレン基を表し、nは1〜20の整数を表す。) Reacting a fatty acid ester mixture (A) represented by the following general formula (1), an alkoxysilane, its hydrolyzate or its polycondensate, and a polyoxyalkylene compound represented by the following general formula (2) A cement-based cured product obtained by impregnating a surface curing layer from the surface with a curing agent for concrete containing the alkoxysilane derivative (B) obtained by the above.
R 1 CO—O—R 2 (1)
(In the formula, R 1 CO represents a fatty acid residue having 12 to 24 carbon atoms, and the proportion of long-chain saturated fatty acid residues having 16 to 24 carbon atoms in the total fatty acid residues is 3 to 40% by mass, The proportion of long-chain monounsaturated fatty acid residues having 16 to 24 carbon atoms is 30 to 50% by mass, the proportion of long-chain diunsaturated fatty acid residues having 16 to 24 carbon atoms is 20 to 40% by mass, and a percentage ratio of 0 mass% of long chain tri-unsaturated fatty acid residues of carbon atoms 16 to 24, R 2 is 1 to 8 carbon atoms
Represents an alkyl group. )
R 3 O— (AO) n —H (2)
(In the formula, R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, AO represents an oxyalkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 to 20).
脂肪酸残基中、炭素原子数18の長鎖飽和脂肪酸残基の割合が10質量%未満、炭素原子数18の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、そして炭素原子数18の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%である、請求項1記載のセメント系硬化体。 In the fatty acid ester mixture (A) represented by the general formula (1), R 1 CO has a ratio of long-chain saturated fatty acid residues having 18 carbon atoms in the total fatty acid residues of less than 10% by mass, carbon The proportion of long-chain monounsaturated fatty acid residues having 18 atoms is 30 to 50% by mass, and the proportion of long-chain diunsaturated fatty acid residues having 18 carbon atoms is 20 to 40% by mass. Cement-based hardened body.
R1CO−O−R2 (1)
(式中、R1COは炭素原子数12〜24の脂肪酸残基を表し、その全脂肪酸残基中、炭
素原子数16〜24の長鎖飽和脂肪酸残基の割合が3〜40質量%、炭素原子数16〜24の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、炭素原子数16〜24の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%であり、そして炭素原子数16〜24の長鎖トリ不飽和脂肪酸残基の割合が0〜10質量%の割合であり、R2は炭素原子数1〜8
のアルキル基を表す。)
R3O−(AO)n−H (2)
(式中、R3は炭素原子数が1〜18の炭化水素基を表し、AOは炭素原子数2〜4のオ
キシアルキレン基を表し、nは1〜20の整数を表す。) Reacting a fatty acid ester mixture (A) represented by the following general formula (1), an alkoxysilane, its hydrolyzate or its polycondensate, and a polyoxyalkylene compound represented by the following general formula (2) A curing method for cement mortar or concrete, comprising applying a curing agent for concrete containing the alkoxysilane derivative (B) obtained by the method to the cement-based cured body surface.
R 1 CO—O—R 2 (1)
(In the formula, R 1 CO represents a fatty acid residue having 12 to 24 carbon atoms, and the proportion of long-chain saturated fatty acid residues having 16 to 24 carbon atoms in the total fatty acid residues is 3 to 40% by mass, The proportion of long-chain monounsaturated fatty acid residues having 16 to 24 carbon atoms is 30 to 50% by mass, the proportion of long-chain diunsaturated fatty acid residues having 16 to 24 carbon atoms is 20 to 40% by mass, and a percentage ratio of 0 mass% of long chain tri-unsaturated fatty acid residues of carbon atoms 16 to 24, R 2 is 1 to 8 carbon atoms
Represents an alkyl group. )
R 3 O— (AO) n —H (2)
(In the formula, R 3 represents a hydrocarbon group having 1 to 18 carbon atoms, AO represents an oxyalkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 to 20).
脂肪酸残基中、炭素原子数18の長鎖飽和脂肪酸残基の割合が10質量%未満、炭素原子数18の長鎖モノ不飽和脂肪酸残基の割合が30〜50質量%、そして炭素原子数18の長鎖ジ不飽和脂肪酸残基の割合が20〜40質量%である、請求項3記載のセメントモルタル又はコンクリートの養生方法。 In the fatty acid ester mixture (A) represented by the general formula (1), R 1 CO has a ratio of long-chain saturated fatty acid residues having 18 carbon atoms in the total fatty acid residues of less than 10% by mass, carbon The proportion of long-chain monounsaturated fatty acid residues having 18 atoms is 30 to 50% by mass, and the proportion of long-chain diunsaturated fatty acid residues having 18 carbon atoms is 20 to 40% by mass. Cement mortar or concrete curing method.
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