JP2010111537A - Method for producing concrete - Google Patents
Method for producing concrete Download PDFInfo
- Publication number
- JP2010111537A JP2010111537A JP2008285178A JP2008285178A JP2010111537A JP 2010111537 A JP2010111537 A JP 2010111537A JP 2008285178 A JP2008285178 A JP 2008285178A JP 2008285178 A JP2008285178 A JP 2008285178A JP 2010111537 A JP2010111537 A JP 2010111537A
- Authority
- JP
- Japan
- Prior art keywords
- concrete
- water
- hydraulic composition
- rheology modifier
- group
- 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
- 239000004567 concrete Substances 0.000 title claims abstract description 73
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000006254 rheological additive Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000004568 cement Substances 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000010276 construction Methods 0.000 claims abstract description 15
- 229920006317 cationic polymer Polymers 0.000 claims description 27
- 239000003638 chemical reducing agent Substances 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 21
- 238000004898 kneading Methods 0.000 claims description 15
- 125000004432 carbon atom Chemical group C* 0.000 claims description 13
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 4
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 23
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- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 6
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- YIOJGTBNHQAVBO-UHFFFAOYSA-N dimethyl-bis(prop-2-enyl)azanium Chemical class C=CC[N+](C)(C)CC=C YIOJGTBNHQAVBO-UHFFFAOYSA-N 0.000 description 5
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- KJIFKLIQANRMOU-UHFFFAOYSA-N oxidanium;4-methylbenzenesulfonate Chemical compound O.CC1=CC=C(S(O)(=O)=O)C=C1 KJIFKLIQANRMOU-UHFFFAOYSA-N 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 3
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- 150000001340 alkali metals Chemical class 0.000 description 3
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- 150000008051 alkyl sulfates Chemical class 0.000 description 3
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- 239000007795 chemical reaction product Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 238000011049 filling Methods 0.000 description 3
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- 150000002500 ions Chemical class 0.000 description 3
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- 239000002994 raw material Substances 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
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- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 2
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- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- PQPDDGPVZVCBAZ-UHFFFAOYSA-N ethyl-dimethyl-[3-(2-methylprop-2-enoyloxy)propyl]azanium Chemical class CC[N+](C)(C)CCCOC(=O)C(C)=C PQPDDGPVZVCBAZ-UHFFFAOYSA-N 0.000 description 1
- SFLDVYRLBRAQOZ-UHFFFAOYSA-O ethyl-dimethyl-[3-(prop-2-enoylamino)propyl]azanium Chemical class CC[N+](C)(C)CCCNC(=O)C=C SFLDVYRLBRAQOZ-UHFFFAOYSA-O 0.000 description 1
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- 235000011090 malic acid Nutrition 0.000 description 1
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- NHLUVTZJQOJKCC-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCN(C)C NHLUVTZJQOJKCC-UHFFFAOYSA-N 0.000 description 1
- GBCKRQRXNXQQPW-UHFFFAOYSA-N n,n-dimethylprop-2-en-1-amine Chemical compound CN(C)CC=C GBCKRQRXNXQQPW-UHFFFAOYSA-N 0.000 description 1
- QQGJWWNPACORPU-UHFFFAOYSA-N n,n-dimethylpropan-1-amine;prop-2-enamide Chemical compound NC(=O)C=C.CCCN(C)C QQGJWWNPACORPU-UHFFFAOYSA-N 0.000 description 1
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- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
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- 150000002482 oligosaccharides Chemical class 0.000 description 1
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- RAFRTSDUWORDLA-UHFFFAOYSA-N phenyl 3-chloropropanoate Chemical compound ClCCC(=O)OC1=CC=CC=C1 RAFRTSDUWORDLA-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- WSHYKIAQCMIPTB-UHFFFAOYSA-M potassium;2-oxo-3-(3-oxo-1-phenylbutyl)chromen-4-olate Chemical compound [K+].[O-]C=1C2=CC=CC=C2OC(=O)C=1C(CC(=O)C)C1=CC=CC=C1 WSHYKIAQCMIPTB-UHFFFAOYSA-M 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000011150 reinforced concrete Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NTVDGBKMGBRCKB-UHFFFAOYSA-M sodium;12-hydroxyoctadecanoate Chemical compound [Na+].CCCCCCC(O)CCCCCCCCCCC([O-])=O NTVDGBKMGBRCKB-UHFFFAOYSA-M 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 229950000244 sulfanilic acid Drugs 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- AIUAMYPYEUQVEM-UHFFFAOYSA-N trimethyl(2-prop-2-enoyloxyethyl)azanium Chemical class C[N+](C)(C)CCOC(=O)C=C AIUAMYPYEUQVEM-UHFFFAOYSA-N 0.000 description 1
- QXEDTOCFLFELQK-UHFFFAOYSA-N trimethyl(3-prop-2-enoyloxypropyl)azanium Chemical class C[N+](C)(C)CCCOC(=O)C=C QXEDTOCFLFELQK-UHFFFAOYSA-N 0.000 description 1
- USFMMZYROHDWPJ-UHFFFAOYSA-N trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium Chemical class CC(=C)C(=O)OCC[N+](C)(C)C USFMMZYROHDWPJ-UHFFFAOYSA-N 0.000 description 1
- UOASMSQZBFHQGX-UHFFFAOYSA-O trimethyl-[2-(prop-2-enoylamino)ethyl]azanium Chemical class C[N+](C)(C)CCNC(=O)C=C UOASMSQZBFHQGX-UHFFFAOYSA-O 0.000 description 1
- XVIGJPONQXWIOK-UHFFFAOYSA-N trimethyl-[3-(2-methylprop-2-enoyloxy)propyl]azanium Chemical class CC(=C)C(=O)OCCC[N+](C)(C)C XVIGJPONQXWIOK-UHFFFAOYSA-N 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- On-Site Construction Work That Accompanies The Preparation And Application Of Concrete (AREA)
- Preparation Of Clay, And Manufacture Of Mixtures Containing Clay Or Cement (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
Description
本発明はコンクリートの製造方法に関する。 The present invention relates to a method for producing concrete.
近年、鉄筋コンクリート造の建築現場では、部材断面の制約に伴う過密配筋化や、熟練技術者の不足等の理由からコンクリート構造物の品質確保に懸念が持たれている。コンクリート構造物の施工品質を確保するために、施工現場では流動性や充填性の高いコンクリートが望まれるケースが多い。また、河川、湧水、海岸周辺など施工箇所に水が多く存在する場合には、高い流動性と共に水中不分離性がコンクリートに求められる。 In recent years, reinforced concrete construction sites have been concerned about ensuring the quality of concrete structures due to overcrowding due to restrictions on the cross-section of members and lack of skilled engineers. In order to ensure the construction quality of concrete structures, there are many cases where concrete with high fluidity and filling properties is desired at the construction site. In addition, when there is a lot of water at construction sites such as rivers, springs, and coastal areas, concrete is required to have high fluidity and inseparability in water.
一方、コンクリート構造物の施工では、生コンクリート工場でコンクリートを生産し（いわゆるレディーミクストコンクリート）、ミキサー車で施工現場に輸送し、打設する方法が一般的である。流動性の高いコンクリートをこのように生コンクリート工場で生産して現場に打設する場合、製造後の経時に伴う材料分離や流動性の変化等に対応するため、普通コンクリートよりも物性管理を厳しくする必要が生じる。また、工場では特殊仕様のコンクリートを製造することになるため、工場全体の生産性にも影響する。 On the other hand, in the construction of concrete structures, it is common to produce concrete in a ready-mixed concrete factory (so-called ready-mixed concrete), transport to a construction site with a mixer car, and place it. When concrete with high fluidity is produced in a ready-mixed concrete factory and placed on site, physical property management is more stringent than ordinary concrete in order to cope with material separation and change in fluidity over time after production. Need to do. Also, since the factory manufactures concrete with special specifications, it affects the productivity of the factory as a whole.
特許文献１には、ＪＩＳ Ａ−５３０８記載のレディーミクストコンクリート（普通コンクリート）にセメント分散剤と不分離性混和剤とを混合して、コンクリートの調合を変化させることなく、材料分離抵抗性の非常に高い、スランプフロー３５ｃｍ以上の高流動性コンクリートを製造する方法が開示されている。 In Patent Document 1, a ready-mixed concrete (ordinary concrete) described in JIS A-5308 is mixed with a cement dispersant and a non-separable admixture so that the material separation resistance is extremely high without changing the concrete composition. A high flowable concrete with a slump flow of 35 cm or more is disclosed.
また、特許文献２には特定の多糖誘導体と高性能減水剤とを添加して得られるスランプフロー値が５０〜７０ｃｍの水硬性組成物が開示されている。
プラントで製造したコンクリートを用いて、施工現場でコンクリートの流動性を高めることが可能となれば、原料コンクリートの仕様変更なく、施工性の向上、品質の確保が達成できるので、多くの現場で採用されると予想される。しかしながら、特許文献１の技術も広く普及するまで至っていないのが現状であり、さらなる性能の向上が望まれている。すなわち、特許文献１の不分離性混和剤として記載されているヒドロキシエチルセルロース等を用いて、流動性が高く材料分離抵抗性の優れるコンクリートを得るためには、ヒドロキシエチルセルロース等を大量に配合する必要がある。しかし、ヒドロキシエチルセルロースを大量に配合するとセメント等の水硬性粉体の水和反応が抑制され、硬化遅延を起こすことがある。また、ブリーディング性や流動保持性の点でも性能向上が望まれる。 If the concrete fluidity can be increased at the construction site using concrete produced at the plant, it will be possible to improve the workability and ensure the quality without changing the specifications of the raw material concrete, so it is adopted at many sites. Expected to be. However, the technology of Patent Document 1 has not yet been widely spread, and further improvement in performance is desired. That is, in order to obtain a concrete having high fluidity and excellent material separation resistance by using hydroxyethyl cellulose described as the non-separable admixture of Patent Document 1, it is necessary to add a large amount of hydroxyethyl cellulose and the like. is there. However, when a large amount of hydroxyethyl cellulose is blended, the hydration reaction of hydraulic powder such as cement may be suppressed, and curing delay may occur. Further, improvement in performance is also desired in terms of bleeding property and fluidity retention.
さらに、各種のセルロース誘導体が本用途様に提案されているが、ポリマーであるセルロースを骨格とする限り、多くの水酸基を有するために、本質的な水和反応の遅延を改善するには至っていないのが現状である。 Furthermore, various cellulose derivatives have been proposed for this application. However, as long as cellulose as a polymer is used as a skeleton, it has not improved the delay of essential hydration reaction because it has many hydroxyl groups. is the current situation.
本発明の課題は、高い流動性を有し、材料分離抵抗性（耐ブリーディング性、水中不分離性等）に優れ、硬化遅延が少ないコンクリートを製造できる方法を提供することである。 An object of the present invention is to provide a method capable of producing concrete having high fluidity, excellent material separation resistance (bleeding resistance, underwater non-separation property, etc.) and less curing delay.
本発明は、下記工程（Ｉ）及び工程（II）を有するコンクリートの製造方法に関する。
工程（Ｉ）：プラントにて、水、水硬性粉体、骨材、及びコンクリート混和剤を混練りし、水セメント重量比が２５〜６５重量％の水硬性組成物（Ｉ）を調製する工程
工程（II）：コンクリート施工現場において、水硬性組成物（Ｉ）に一般式（ａ１）で表される化合物を含有するレオロジー改質剤を添加して、スランプフロー値が３５〜７５ｃｍである水硬性組成物（II）を調製する工程
The present invention relates to a method for producing concrete having the following steps (I) and (II).
Step (I): Step of preparing a hydraulic composition (I) having a water cement weight ratio of 25 to 65% by weight by kneading water, hydraulic powder, aggregate, and concrete admixture in a plant. Step (II): Water having a slump flow value of 35 to 75 cm by adding a rheology modifier containing a compound represented by the general formula (a1) to the hydraulic composition (I) at a concrete construction site. Step of preparing hard composition (II)
（式中、Ｒ1aは炭素数１０〜２６のアルキル基、Ｒ2aは炭素数１〜２２のアルキル基又はヒドロキシアルキル基、Ｒ3a、Ｒ4aは、それぞれ、炭素数１〜３のアルキル基又はヒドロキシアルキル基、Ｙはエチレン基又はプロピレン基、ｎは０又は１の数、Ｘ-はアニオン性芳香族化合物残基を表す。） Wherein R 1a is an alkyl group having 10 to 26 carbon atoms, R 2a is an alkyl group having 1 to 22 carbon atoms or a hydroxyalkyl group, and R 3a and R 4a are each an alkyl group having 1 to 3 carbon atoms or (Hydroxyalkyl group, Y represents an ethylene group or a propylene group, n represents a number of 0 or 1, and X − represents an anionic aromatic compound residue.)
本発明によれば、高い流動性を有し、材料分離抵抗性（耐ブリーディング性、水中不分離性等）に優れ、硬化遅延が少ないコンクリートを製造することができる。 According to the present invention, it is possible to produce a concrete having high fluidity, excellent material separation resistance (bleeding resistance, underwater non-separation property, etc.), and less curing delay.
＜工程（Ｉ）＞
本発明の工程（Ｉ）は水（Ｗ）、水硬性粉体（Ｃ）、骨材〔細骨材（Ｓ）及び粗骨材（Ｇ）〕、及びコンクリート混和剤〔以下、コンクリート混和剤（Ｉ）という〕を混練し、Ｗ／Ｃ（重量比）が２５〜６５％である水硬性組成物（Ｉ）を調製する工程である。Ｗ／Ｃは、〔水（Ｗ）の重量／水硬性粉体（Ｃ）の重量〕×１００（重量％）により算出される。
<Process (I)>
Process (I) of the present invention comprises water (W), hydraulic powder (C), aggregate [fine aggregate (S) and coarse aggregate (G)], and concrete admixture [hereinafter referred to as concrete admixture ( I)] is kneaded to prepare a hydraulic composition (I) having a W / C (weight ratio) of 25 to 65%. W / C is calculated by [weight of water (W) / weight of hydraulic powder (C)] × 100 (% by weight).
水（Ｗ）は、通常に用いるものが使用でき、水道水等が挙げられる。 As the water (W), those usually used can be used, and examples thereof include tap water.
水硬性粉体（Ｃ）は、水和反応により硬化する物性を有する粉体のことであり、セメント、石膏などが挙げられる。好ましくはセメントであり、またこれらに高炉スラグ、フライアッシュ、シリカヒューム等が添加されたものでもよい。その他、早強セメント、超早強セメント、高ビーライト系セメント、エコセメント等でもよい。 The hydraulic powder (C) is a powder having physical properties that hardens by a hydration reaction, and examples thereof include cement and gypsum. Cement is preferable, and blast furnace slag, fly ash, silica fume and the like may be added thereto. In addition, early strong cement, super early strong cement, high belite cement, eco-cement, etc. may be used.
骨材としては、細骨材（Ｓ）及び粗骨材（Ｇ）が挙げられる。骨材の使用量は、水硬性組成物において１０００〜２３００ｋｇ／ｍ3、１３５０〜２１５０ｋｇ／ｍ3、１５００〜１９００ｋｇ／ｍ3が好ましい。 Examples of the aggregate include fine aggregate (S) and coarse aggregate (G). The amount of aggregate, 1000~2300kg / m 3 in the hydraulic composition, 1350~2150kg / m 3, 1500~1900kg / m 3 is preferred.
細骨材（Ｓ）として、ＪＩＳ Ａ０２０３−２３０２で規定されるものが挙げられる。例えば細骨材としては、川、陸、山、海、石灰砂、珪砂及びこれらの砕砂、高炉スラグ細骨材、フェロニッケルスラグ細骨材、軽量細骨材（人工及び天然）及び再生細骨材等が挙げられる。細骨材（Ｓ）の使用量は、水硬性組成物において５００〜１１００ｋｇ／ｍ3、６００〜１０００ｋｇ／ｍ3、７００〜９００ｋｇ／ｍ3が好ましい。 Examples of the fine aggregate (S) include those defined in JIS A0203-2302. Examples of fine aggregates include rivers, land, mountains, sea, lime sand, silica sand and crushed sand, blast furnace slag fine aggregate, ferronickel slag fine aggregate, lightweight fine aggregate (artificial and natural) and regenerated fine bone. Materials and the like. The amount of the fine aggregate (S) is, 500~1100kg / m 3 in the hydraulic composition, 600~1000kg / m 3, 700~900kg / m 3 is preferred.
また、粗骨材（Ｇ）として、ＪＩＳ Ａ０２０３−２３０３で規定されるものが挙げられる。例えば粗骨材としては、川、陸、山、海、石灰砂利、これらの砕石、高炉スラグ粗骨材、フェロニッケルスラグ粗骨材、軽量粗骨材（人工及び天然）及び再生粗骨材等が挙げられる。粗骨材（Ｇ）の使用量は、水硬性組成物において５００〜１２００ｋｇ／ｍ3、７５０〜１１５０ｋｇ／ｍ3、８００〜１０００ｋｇ／ｍ3が好ましい。 Moreover, what is prescribed | regulated by JIS A0203-2303 is mentioned as a coarse aggregate (G). For example, as coarse aggregate, river, land, mountain, sea, lime gravel, crushed stone, blast furnace slag coarse aggregate, ferronickel slag coarse aggregate, lightweight coarse aggregate (artificial and natural), recycled coarse aggregate, etc. Is mentioned. The amount of coarse aggregate (G) is, 500~1200kg / m 3 in the hydraulic composition, 750~1150kg / m 3, 800~1000kg / m 3 is preferred.
コンクリート混和剤（Ｉ）としては、減水剤、高性能減水剤及び高性能ＡＥ減水剤から選ばれる１種以上が挙げられる。減水剤としては、具体的にはリグニンスルホン酸塩及びその誘導体、オキシカルボン酸塩、ポリオール誘導体が挙げられる。また、高性能減水剤及び高性能ＡＥ減水剤としては、工程（II）で使用するものと同じものから選択して使用できる。コンクリート混和剤（Ｉ）は、水硬性粉体（Ｃ）１００重量部に対して、固形分（有効分）で０．０１〜１．０重量部用いることが好ましく、０．０５〜０．５重量部がより好ましい。 As concrete admixture (I), 1 or more types chosen from a water reducing agent, a high performance water reducing agent, and a high performance AE water reducing agent are mentioned. Specific examples of the water reducing agent include lignin sulfonate and derivatives thereof, oxycarboxylate, and polyol derivatives. Moreover, as a high performance water reducing agent and a high performance AE water reducing agent, it can select and use from the same thing used by process (II). The concrete admixture (I) is preferably used in an amount of 0.01 to 1.0 part by weight in terms of solid content (effective part) with respect to 100 parts by weight of the hydraulic powder (C). Part by weight is more preferred.
工程（Ｉ）では、これらの材料を、Ｗ／Ｃ（重量比）が２５〜６５％、より好ましくは３５〜６０％、さらに好ましくは、４０〜５５％になるように配合し、混練を行い水硬性組成物（Ｉ）を調製する。この際の各材料の配合比率は、土木学会コンクリート標準示方書、建築工事標準仕様書に準じて得られた配合やＪＩＳ Ａ５３０８「レディミクストコンクリート」であることが好ましい。 In step (I), these materials are blended so that the W / C (weight ratio) is 25 to 65%, more preferably 35 to 60%, and still more preferably 40 to 55%, and kneading is performed. A hydraulic composition (I) is prepared. In this case, the blending ratio of each material is preferably a blend obtained according to the Japan Society of Civil Engineers Concrete Standard Specification and Building Construction Standard Specification or JIS A5308 “Ready Mixed Concrete”.
混練は、二軸ミキサー等の混練機を用いることができる。混練方法は、例えば、水硬性粉体（Ｃ）、細骨材（Ｓ）及び粗骨材（Ｇ）を空練り後、水（Ｗ）とコンクリート混和剤（Ｉ）を予め混合した混練水を添加し、混練する方法が挙げられる。 For the kneading, a kneader such as a twin screw mixer can be used. The kneading method is, for example, kneading water in which water (W) and a concrete admixture (I) are mixed in advance after kneading hydraulic powder (C), fine aggregate (S) and coarse aggregate (G). The method of adding and kneading is mentioned.
混練により得られる水硬性組成物（Ｉ）は、スランプ（ＪＩＳ Ａ １１０１）が８〜２３ｃｍであることが好ましく、さらには１５〜２１ｃｍが好ましい。スランプフロー値（ＪＩＳ Ａ１１５０）が２０〜７５ｃｍであることが好ましく、さらに、３５〜７０ｃｍであることがより好ましい。空気量（ＪＩＳ Ａ １１２８）が３．５〜６．０％であることが好ましい。 The hydraulic composition (I) obtained by kneading preferably has a slump (JIS A 1101) of 8 to 23 cm, more preferably 15 to 21 cm. The slump flow value (JIS A1150) is preferably 20 to 75 cm, and more preferably 35 to 70 cm. The amount of air (JIS A 1128) is preferably 3.5 to 6.0%.
＜工程（II）＞
工程（II）は、工程（Ｉ）で得られた水硬性組成物（Ｉ）に、前記一般式（ａ１）で表される化合物を含有するレオロジー改質剤を添加して、スランプフロー値が３５〜７５ｃｍである水硬性組成物（II）を調製する工程である。レオロジー改質剤と一緒にさらにカチオン性ポリマーやコンクリート混和剤を水硬性組成物（Ｉ）に添加しても良い。
<Process (II)>
In the step (II), a rheology modifier containing the compound represented by the general formula (a1) is added to the hydraulic composition (I) obtained in the step (I), and the slump flow value is increased. It is the process of preparing hydraulic composition (II) which is 35-75 cm. A cationic polymer or a concrete admixture may be further added to the hydraulic composition (I) together with the rheology modifier.
一般式（ａ１）中、Ｘ-はアニオン性芳香族化合物であり、好ましくはパラトルエンスルホン酸に由来するアニオン基である。 In general formula (a1), X − represents an anionic aromatic compound, preferably an anionic group derived from para-toluenesulfonic acid.
本発明に用いられるレオロジー改質剤では、増粘する温度領域を広くできる点で、炭化水素基Ｒ1の長さが異なる４級カチオン基が２種以上存在することが好ましく、そのためには、４級カチオン基の炭化水素基Ｒ1の長さが異なる一般式（ａ１）の化合物を２種以上併用することが好ましい。これは、水への溶解性とレオロジー改質の効果の点からも好ましい。 In the rheology modifier used in the present invention, it is preferable that two or more quaternary cation groups having different lengths of the hydrocarbon group R 1 are present in that the temperature range for thickening can be widened. It is preferable to use two or more compounds of the general formula (a1) in which the length of the quaternary cationic group R 1 is different. This is also preferable from the viewpoints of solubility in water and the effect of rheology modification.
一般式（ａ１）で表される化合物の製造方法としては、（ｉ）３級アミンをアニオン性芳香族化合物の酸型で中和しそこにエチレンオキサイド（以下、ＥＯという）を反応させる方法、（ii）４級塩型化合物とアニオン性芳香族化合物の混合物を脱塩する方法、（iii）４級塩型化合物の対イオンを芳香族アニオン基で対イオン交換する方法などが挙げられる。これらの製造工程では、ハロゲン元素は元々含まれないか、または系外に除去されるので、金属が存在する部分に使用しても腐食を起こさないことから、これらの製造法が好ましい。 As a method for producing the compound represented by the general formula (a1), (i) a method in which a tertiary amine is neutralized with an acid type of an anionic aromatic compound and ethylene oxide (hereinafter referred to as EO) is reacted therewith, (Ii) A method of desalting a mixture of a quaternary salt type compound and an anionic aromatic compound, (iii) a method of counter-ion exchange of a counter ion of a quaternary salt type compound with an aromatic anion group, and the like. In these production steps, halogen elements are not originally contained or removed from the system, and therefore, these production methods are preferred because they do not cause corrosion even when used in a portion where a metal exists.
また、本発明に用いられるレオロジー改質剤は、前記一般式（ａ１）で表される化合物の性能を大きく妨げない範囲で、その他の成分を含有することができる。その他の成分としては、例えば、樹脂石鹸、飽和もしくは不飽和脂肪酸、ヒドロキシステアリン酸ナトリウム、ラウリルサルフェート、アルキルベンゼンスルホン酸（塩）、アルカンスルホネート、ポリオキシアルキレンアルキル（フェニル）エーテル、ポリオキシアルキレンアルキル（フェニル）エーテル硫酸エステル（塩）、ポリオキシアルキレンアルキル（フェニル）エーテルリン酸エステル（塩）、蛋白質材料、アルケニルコハク酸、α−オレフィンスルホネート等のＡＥ剤；グルコン酸、グルコヘプトン酸、アラボン酸、リンゴ酸、クエン酸等のオキシカルボン酸系、デキストリン、単糖類、オリゴ糖類、多糖類等の糖系、糖アルコール系等の遅延剤；起泡剤；増粘剤；珪砂；ＡＥ減水剤；塩化カルシウム、亜硝酸カルシウム、硝酸カルシウム、臭化カルシウム、沃化カルシウム等の可溶性カルシウム塩、塩化鉄、塩化マグネシウム等の塩化物等、硫酸塩、水酸化カリウム、水酸化ナトリウム、炭酸塩、チオ硫酸塩、蟻酸（塩）、アルカノールアミン等の早強剤又は促進剤；発泡剤；樹脂酸（塩）、脂肪酸エステル、油脂、シリコーン、パラフィン、アスファルト、ワックス等の防水剤；高炉スラグ；流動化剤；ジメチルポリシロキサン系、ポリアルキレングリコール脂肪酸エステル系、鉱油系、油脂系、オキシアルキレン系、アルコール系、アミド系等の消泡剤；防泡剤；亜硝酸塩、燐酸塩、酸化亜鉛等の防錆剤；メチルセルロース、ヒドロキシエチルセルロース等のセルロース系、β−１，３−グルカン、キサンタンガム、ウエランガム等の天然物系、ポリアクリル酸アミド、ポリエチレングリコール、オレイルアルコールのＥＯ付加物もしくはこれとビニルシクロヘキセンジエポキシドとの反応物等の合成系等の水溶性高分子、合成繊維として、ポリアセタール繊維、ナイロン繊維、アラミド繊維、ポリエステル繊維、アクリル繊維、ビニロン繊維、ポリプロピレン繊維、ポリエチレン繊維等の合繊繊維、レーヨン繊維等の再生繊維等の爆裂防止用繊維が挙げられる。 In addition, the rheology modifier used in the present invention can contain other components as long as the performance of the compound represented by the general formula (a1) is not significantly impaired. Other components include, for example, resin soap, saturated or unsaturated fatty acid, sodium hydroxystearate, lauryl sulfate, alkylbenzene sulfonic acid (salt), alkane sulfonate, polyoxyalkylene alkyl (phenyl) ether, polyoxyalkylene alkyl (phenyl) ) AE agents such as ether sulfate (salt), polyoxyalkylene alkyl (phenyl) ether phosphate (salt), protein material, alkenyl succinic acid, α-olefin sulfonate; gluconic acid, glucoheptonic acid, alabonic acid, malic acid Retarders such as oxycarboxylic acids such as citric acid, dextrin, monosaccharides, oligosaccharides and polysaccharides, sugar alcohols, etc .; foaming agents; thickeners; silica sand; AE water reducing agents; calcium chloride, Calcium nitrite, glass Soluble calcium salts such as calcium, calcium bromide and calcium iodide, chlorides such as iron chloride and magnesium chloride, sulfate, potassium hydroxide, sodium hydroxide, carbonate, thiosulfate, formic acid (salt), alkanol Fastening agents or accelerators such as amines; foaming agents; waterproofing agents such as resin acids (salts), fatty acid esters, oils and fats, silicones, paraffins, asphalts, waxes; blast furnace slag; fluidizing agents; dimethylpolysiloxanes, polyalkylenes Antifoaming agents such as glycol fatty acid esters, mineral oils, fats and oils, oxyalkylenes, alcohols and amides; antifoaming agents; rust inhibitors such as nitrites, phosphates and zinc oxides; methylcellulose, hydroxyethylcellulose, etc. Cellulose, natural products such as β-1,3-glucan, xanthan gum, welan gum, polyacrylic acid Water-soluble polymers such as EO adducts of amide, polyethylene glycol, oleyl alcohol, or a reaction product of this with vinylcyclohexene diepoxide, synthetic fibers such as polyacetal fiber, nylon fiber, aramid fiber, polyester fiber, acrylic Explosion-preventing fibers such as fibers, synthetic fibers such as vinylon fibers, polypropylene fibers and polyethylene fibers, and regenerated fibers such as rayon fibers.
本発明のレオロジー改質剤中の一般式（ａ１）で表される化合物の含有量は、好ましくは１０〜１００重量％、より好ましくは２０〜１００重量％である。本発明のレオロジー改質剤の固形分中の一般式（ａ１）で表される化合物の固形分の比率は５０重量％以上が好ましい。工程（II）におけるレオロジー改質剤、更にレオロジー改質剤中の一般式（ａ１）で表される化合物の添加量が多いと粘性が高くなり、材料分離抵抗性が向上する。 The content of the compound represented by the general formula (a1) in the rheology modifier of the present invention is preferably 10 to 100% by weight, more preferably 20 to 100% by weight. The ratio of the solid content of the compound represented by the general formula (a1) in the solid content of the rheology modifier of the present invention is preferably 50% by weight or more. If the addition amount of the rheology modifier in the step (II) and the compound represented by the general formula (a1) in the rheology modifier is large, the viscosity increases and the material separation resistance is improved.
工程（II）におけるレオロジー改質剤の添加量は、目的とする増粘の程度に応じ適宜決めればよいが、例えば水硬性組成物（Ｉ）で用いた水硬性粉体量（Ｃ）１００重量部に対して、一般式（ａ１）で表される化合物が好ましくは０．０１〜５重量部、より好ましくは０．０５〜３重量部、更に好ましくは０．１〜２重量部となる量が適している。 The addition amount of the rheology modifier in the step (II) may be appropriately determined according to the target degree of thickening. For example, the amount of hydraulic powder (C) used in the hydraulic composition (I) is 100 wt. The amount of the compound represented by the general formula (a1) is preferably 0.01 to 5 parts by weight, more preferably 0.05 to 3 parts by weight, and still more preferably 0.1 to 2 parts by weight with respect to parts. Is suitable.
工程（II）では、レオロジー改質剤と共に、更に、カチオン性ポリマーを水硬性組成物（Ｉ）に添加することが好ましい。カチオン性ポリマーとしては、カチオン性窒素を含むカチオン性ポリマー、更に、分子中に４級塩構造を有するポリマー、なかでもカチオン性窒素が、第４級窒素であるカチオン性ポリマーが挙げられる。 In step (II), it is preferable to add a cationic polymer to the hydraulic composition (I) together with the rheology modifier. Examples of the cationic polymer include a cationic polymer containing cationic nitrogen, a polymer having a quaternary salt structure in the molecule, and a cationic polymer in which the cationic nitrogen is quaternary nitrogen.
カチオン性ポリマーとしては、ジメチルアミノエチル（メタ）アクリレート、ジメチルアミノプロピル（メタ）アクリレート、（メタ）アクリルアミドエチルジメチルアミン、（メタ）アクリルアミドプロピルジメチルアミン、アリルアミン、アリルメチルアミン、アリルジメチルアミン、ジアリルアミン、ジアリルメチルアミン等のホモポリマー、及びこれらのモノマーと他のモノマーとから得られる共重合体が挙げられ、いずれも中和型でも未中和型でも使用できる。 Examples of cationic polymers include dimethylaminoethyl (meth) acrylate, dimethylaminopropyl (meth) acrylate, (meth) acrylamide ethyl dimethylamine, (meth) acrylamide propyl dimethylamine, allylamine, allylmethylamine, allyldimethylamine, diallylamine, Examples include homopolymers such as diallylmethylamine, and copolymers obtained from these monomers and other monomers, both of which can be used as neutralized or non-neutralized types.
また、カチオン性ポリマーとしては、ジエチレントリアミン、トリエチレンテトラミン、テトラエチレンペンタミン、ジプロピレントリアミン、トリプロピレンテトラミン等のポリアルキレンポリアミンおよび、ポリアルキレンポリアミンに炭素数２〜４のアルキレンオキサイドを付加させたポリマーが挙げられ、いずれも中和型でも未中和型でも使用できる。 In addition, examples of cationic polymers include polyalkylene polyamines such as diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine, and tripropylenetetramine, and polymers obtained by adding alkylene oxides having 2 to 4 carbon atoms to polyalkylenepolyamine. Any of neutralized and non-neutralized types can be used.
その他にもポリエチレンイミンおよびポリエチレンイミンに炭素数２〜４のアルキレンオキサイドを付加させたポリマーをカチオン性ポリマーとして使用できる。 In addition, polyethyleneimine and a polymer obtained by adding a C2-C4 alkylene oxide to polyethyleneimine can be used as the cationic polymer.
カチオン性ポリマーとしては、カチオン性窒素を含むものが好ましく、更に当該カチオン性ポリマーのカチオン性窒素に、炭素数１〜２２のアルキル基、炭素数２〜８のオキシアルキレン基を含んでなるポリオキシアルキレン基、水素原子及び下記式（ｂ１） As the cationic polymer, those containing cationic nitrogen are preferable, and polyoxygen containing an alkyl group having 1 to 22 carbon atoms and an oxyalkylene group having 2 to 8 carbon atoms in the cationic nitrogen of the cationic polymer. An alkylene group, a hydrogen atom and the following formula (b1)
で表される基〔ここで、Ｒ1b〜Ｒ5bは、同一でも異なっていても良く、それぞれ水素原子又は炭素数１〜２２のアルキルもしくはアルケニル基であり、Ｚは−Ｏ−又は−ＮＹ−（Ｙは水素原子又は炭素数１〜１０のアルキル基）であり、ｎは１〜１０の数である。ただし、Ｒ1b及びＲ3bはポリマー構造中に取り込まれていても良く、その場合はＲ1b及びＲ3bは存在しない。〕から選ばれる基が結合しているものが好ましい。 Wherein R 1b to R 5b may be the same or different and each represents a hydrogen atom or an alkyl or alkenyl group having 1 to 22 carbon atoms, and Z is —O— or —NY—. (Y is a hydrogen atom or a C1-C10 alkyl group), and n is a number of 1-10. However, R 1b and R 3b may be incorporated in the polymer structure, in which case R 1b and R 3b are not present. A group to which a group selected from the above is bonded is preferable.
一般式（ｂ１）で表される基の由来となる化合物としては、メタクリロイルオキシエチルトリメチルアンモニウム塩、メタクリロイルオキシエチルジメチルエチルアンモニウム塩、メタクリロイルオキシプロピルトリメチルアンモニウム塩、メタクリロイルオキシプロピルジメチルエチルアンモニウム塩、メタクリルアミドエチルトリメチルアンモニウム塩、メタクリルアミドエチルジメチルエチルアンモニウム塩、メタクリルアミドプロピルトリメチルアンモニウム塩、メタクリルアミドプロピルジメチルエチルアンモニウム塩、アクリロイルオキシエチルトリメチルアンモニウム塩、アクリロイルオキシエチルジメチルエチルアンモニウム塩、アクリロイルオキシプロピルトリメチルアンモニウム塩、アクリロイルオキシプロピルジメチルエチルアンモニウム塩、アクリルアミドエチルトリメチルアンモニウム塩、アクリルアミドエチルジメチルエチルアンモニウム塩、アクリルアミドプロピルトリメチルアンモニウム塩、アクリルアミドプロピルジメチルエチルアンモニウム塩等が挙げられ、これらはアルキル硫酸塩、中でもエチル硫酸塩、メチル硫酸塩が好ましい。 Compounds derived from the group represented by the general formula (b1) include methacryloyloxyethyltrimethylammonium salt, methacryloyloxyethyldimethylethylammonium salt, methacryloyloxypropyltrimethylammonium salt, methacryloyloxypropyldimethylethylammonium salt, methacrylamide Ethyltrimethylammonium salt, methacrylamideamidodimethylethylammonium salt, methacrylamideamidopropyltrimethylammonium salt, methacrylamidopropyldimethylethylammonium salt, acryloyloxyethyltrimethylammonium salt, acryloyloxyethyldimethylethylammonium salt, acryloyloxypropyltrimethylammonium salt, Acryloyloxypropyl dimethyl Examples include ethylammonium salt, acrylamidoethyltrimethylammonium salt, acrylamidoethyldimethylethylammonium salt, acrylamidopropyltrimethylammonium salt, acrylamidopropyldimethylethylammonium salt, and the like. These are alkyl sulfates, among which ethyl sulfate and methyl sulfate are preferable. .
また、カチオン性ポリマーのカチオン性窒素が、ジアリルジアルキルアンモニウム塩、好ましくはジアリルジメチルアンモニウム塩に由来するポリマーもまた好適であり、具体的には、ジアリルジメチルアンモニウム塩とアクリル酸系モノマーとの共重合体等が挙げられる。 In addition, a polymer in which the cationic nitrogen of the cationic polymer is derived from a diallyldialkylammonium salt, preferably a diallyldimethylammonium salt is also suitable. Specifically, a copolymer of a diallyldimethylammonium salt and an acrylic monomer is used. Examples include coalescence.
また、カチオン性ポリマーとしては、カチオン基を有する（メタ）アクリル酸系モノマー、カチオン基を有するスチレン系モノマー、ビニルピリジン系モノマー、ビニルイミダゾリン系モノマー、及びジアリルジアルキルアミン系モノマーからなる群から選ばれるモノマーに由来する構造を有するものが挙げられる。 The cationic polymer is selected from the group consisting of a (meth) acrylic acid monomer having a cationic group, a styrene monomer having a cationic group, a vinylpyridine monomer, a vinylimidazoline monomer, and a diallyldialkylamine monomer. What has the structure derived from a monomer is mentioned.
カチオン性ポリマーの対イオンとしては、ハロゲンイオン、硫酸イオン、アルキル硫酸イオン、リン酸イオン、有機酸イオン等のアニオン性イオンが挙げられる。 Examples of the counter ion of the cationic polymer include anionic ions such as halogen ions, sulfate ions, alkyl sulfate ions, phosphate ions, and organic acid ions.
カチオン性ポリマーの具体例としては、ポリアリルトリメチルアンモニウム塩等のポリアリルトリアルキルアンモニウム塩、ポリ（ジアリルジメチルアンモニウム塩）、ポリメタクリロイルオキシエチルジメチルエチルアンモニウム塩、ポリメタクリルアミドプロピルトリメチルアンモニウム塩、カチオン化でん粉、カチオン化セルロース、カチオン化ヒドロキシエチルセルロース等であり、これらは４級塩構造を有するモノマーを重合して得ても、対応するポリマーを４級化剤で４級化して得ても良い。これらは、ホモポリマーでなくてもよく、必要に応じて共重合可能なモノマーとの共重合物としても良い。具体的には、ジアリルジメチルアンモニウム塩−ＳＯ2共重合体、ジアリルジメチルアンモニウム塩−アクリルアミド共重合体、ジアリルジメチルアンモニウム塩−アクリル酸−アクリルアミド共重合物、メタクリロイルオキシエチルジメチルエチルアンモニウム塩−ビニルピロリドン共重合体、メタクリルアミドプロピルトリメチルアンモニウム塩−ビニルピロリドン共重合体、等が挙げられる。これらは、未反応モノマー、副生物、異なるカチオン化密度のポリマーを含んでいてもよい。これらは２種以上併用することができる。 Specific examples of the cationic polymer include polyallyltrialkylammonium salts such as polyallyltrimethylammonium salt, poly (diallyldimethylammonium salt), polymethacryloyloxyethyldimethylethylammonium salt, polymethacrylamidopropyltrimethylammonium salt, cationization Starch, cationized cellulose, cationized hydroxyethyl cellulose and the like may be obtained by polymerizing a monomer having a quaternary salt structure, or may be obtained by quaternizing a corresponding polymer with a quaternizing agent. These may not be homopolymers, and may be a copolymer with a copolymerizable monomer as required. Specifically, diallyldimethylammonium salt-SO 2 copolymer, diallyldimethylammonium salt-acrylamide copolymer, diallyldimethylammonium salt-acrylic acid-acrylamide copolymer, methacryloyloxyethyldimethylethylammonium salt-vinylpyrrolidone copolymer Examples thereof include a polymer and a methacrylamidopropyltrimethylammonium salt-vinylpyrrolidone copolymer. These may contain unreacted monomers, by-products, polymers of different cationization densities. These can be used in combination of two or more.
上記の中でも、ポリジメチルアミノエチルメタクリレートジエチル硫酸塩、ポリ（ジアリルジメチルアンモニウム塩）、ポリメタクリロイルオキシエチルジメチルエチルアンモニウム塩、ポリメタクリルアミドプロピルトリメチルアンモニウム塩、メタクリロイルオキシエチルジメチルエチルアンモニウム塩−ビニルピロリドン共重合体、及びメタクリルアミドプロピルトリメチルアンモニウム塩−ビニルピロリドン共重合体から選ばれるカチオン性ポリマーが好ましく、更にこれらの中でも、レオロジー改質効果の観点から、対イオンがアルキル硫酸イオンであるもの、中でもエチル硫酸塩、メチル硫酸塩がより好ましい。 Among them, polydimethylaminoethyl methacrylate diethyl sulfate, poly (diallyldimethylammonium salt), polymethacryloyloxyethyldimethylethylammonium salt, polymethacrylamidopropyltrimethylammonium salt, methacryloyloxyethyldimethylethylammonium salt-vinylpyrrolidone copolymer Preferred is a cationic polymer selected from a polymer and a methacrylamide propyltrimethylammonium salt-vinyl pyrrolidone copolymer, and among these, from the viewpoint of rheology modification effect, those whose counter ion is an alkyl sulfate ion, especially ethyl sulfate More preferred are salts and methyl sulfate.
カチオン性ポリマーの分子量は、１０００以上が好ましく、１０００〜３００万が更に好ましく、この点で一般式（ａ１）で表される化合物とは区別される。この分子量は、ゲル・パーミエーション・クロマトグラフィーにより、以下の条件で測定された重量平均分子量である。
カラム：α−M（東ソー製） ２本連結
溶離液：０．１５ｍｏｌ／Ｌ硫酸Ｎａ、１％酢酸水溶液
流速 ：１．０ｍＬ／ｍｉｎ
温度 ：４０℃
検出器：ＲＩ
分子量標準はプルランを使用
The molecular weight of the cationic polymer is preferably 1000 or more, more preferably 1000 to 3 million, and is distinguished from the compound represented by the general formula (a1) in this respect. This molecular weight is a weight average molecular weight measured under the following conditions by gel permeation chromatography.
Column: α-M (manufactured by Tosoh Corp.) 2 linked Eluent: 0.15 mol / L Na sulfate 1% acetic acid aqueous solution Flow rate: 1.0 mL / min
Temperature: 40 ° C
Detector: RI
Pullulan is used as molecular weight standard
カチオン性ポリマーは、カチオン化密度が０．５〜１０ｍｅｑ／ｇ、更に１〜９ｍｅｑ／ｇ、より更に３〜８ｍｅｑ／ｇであることが、スラリー調製直後及び経時的な粘弾性維持の点から好ましい。カチオン化密度は、後述の実施例の方法により測定することができる。 The cationic polymer preferably has a cationization density of 0.5 to 10 meq / g, more preferably 1 to 9 meq / g, and even more preferably 3 to 8 meq / g from the viewpoint of maintaining viscoelasticity immediately after slurry preparation and over time. . The cationization density can be measured by the method of Examples described later.
工程（II）におけるカチオン性ポリマーの添加量は、所望とする流動性に応じて適宜決定することができるが、水硬性粉体（Ｃ）１００重量部に対して、好ましくは０．００１〜１．０重量部、より好ましくは０．０２〜０．２重量部である。工程（II）におけるカチオン性ポリマーの添加量が多いと材料分離抵抗性が向上する。 Although the addition amount of the cationic polymer in the step (II) can be appropriately determined according to the desired fluidity, it is preferably 0.001-1 with respect to 100 parts by weight of the hydraulic powder (C). 0.0 part by weight, more preferably 0.02 to 0.2 part by weight. When the addition amount of the cationic polymer in the step (II) is large, the material separation resistance is improved.
また、工程（II）では、レオロジー改質剤と共に、更に、高性能減水剤及び高性能ＡＥ減水剤から選ばれるコンクリート混和剤〔以下、高性能（ＡＥ）減水剤という〕を水硬性組成物（Ｉ）に添加することが好ましい。高性能（ＡＥ）減水剤としては、ＪＩＳ Ａ ６２０４に規定される減水率１８％以上のコンクリート用化学混和剤が好適に用いられ、具体的には、ナフタレン、メラミン、フェノール、尿素およびアニリンの何れかのメチロール化物およびスルホン化物の群から選ばれる１種又は２種以上の化合物のホルムアルデヒド縮合物が挙げられる。例えば、ナフタレンスルホン酸金属塩ホルムアルデヒド縮合物［例えば花王（株）製マイテイ１５０］、メラミンスルホン酸金属塩ホルムアルデヒド縮合物［例えば花王（株）製マイテイ１５０−Ｖ２］、フェノールスルホン酸ホルムアルデヒド化合物（特許第１０９７６４７号に記載の化合物等）、フェノール・スルファニル酸ホルムアルデヒド共縮合物（特開平１−１１３４１９号公報に記載の化合物等）等である。さらにまた他の例として、エチレン系不飽和モノカルボン酸、そのアルキレンオキシド付加物又はその誘導体、並びにエチレン系不飽和ジカルボン酸、そのアルキレンオキシド付加物又はその誘導体からなる群より選ばれる１種又は２種以上を含有する単量体を重合して得られる重合体又は共重合体（特公平２−７９０１号公報、特開平３−７５２５２号公報、特公平２−８９８３号公報などに記載の化合物等）が挙げられる。 In the step (II), a concrete admixture selected from a high performance water reducing agent and a high performance AE water reducing agent (hereinafter referred to as a high performance (AE) water reducing agent) is added to the hydraulic composition (in addition to the rheology modifier). It is preferable to add to I). As a high performance (AE) water reducing agent, a chemical admixture for concrete having a water reduction rate of 18% or more specified in JIS A 6204 is preferably used. Specifically, any of naphthalene, melamine, phenol, urea and aniline Examples thereof include formaldehyde condensates of one or more compounds selected from the group of methylolated products and sulfonated products. For example, a naphthalenesulfonic acid metal salt formaldehyde condensate [for example, Mighty 150 manufactured by Kao Corporation], a melamine sulfonic acid metal salt formaldehyde condensate [for example, Mighty 150-V2 manufactured by Kao Corporation], a phenolsulfonic acid formaldehyde compound (patent no. No. 1097647, etc.) and phenol / sulfanilic acid formaldehyde cocondensates (compounds described in JP-A No. 1-113419). As still another example, one or two selected from the group consisting of an ethylenically unsaturated monocarboxylic acid, an alkylene oxide adduct or derivative thereof, and an ethylenically unsaturated dicarboxylic acid, an alkylene oxide adduct or derivative thereof Polymers or copolymers obtained by polymerizing monomers containing at least seeds (compounds described in JP-B-2-7901, JP-A-3-75252, JP-B-2-8983, etc.) ).
また、本発明において用いられる高性能（ＡＥ）減水剤としては、下記一般式（ｃ１）で表される単量体と、下記一般式（ｃ２）及び（ｃ３）で表される化合物の中から選ばれる一種以上を含有する単量体とを重合して得られる、オキシアルキレン基を有する水溶性ビニル共重合体がより好ましく用いられる（例えば花王（株）製マイテイ３０００）。こうした高性能減水剤については、例えば特開平７−２２３８５２号公報に記載がある。 Moreover, as a high performance (AE) water reducing agent used in the present invention, among monomers represented by the following general formula (c1) and compounds represented by the following general formulas (c2) and (c3) A water-soluble vinyl copolymer having an oxyalkylene group obtained by polymerizing a monomer containing one or more selected monomers is more preferably used (for example, Mighty 3000 manufactured by Kao Corporation). Such a high-performance water reducing agent is described, for example, in JP-A-7-223852.
［式中、
R1c，R2c：水素原子又はメチル基
m1：０〜２の数
AO：炭素数２〜３のオキシアルキレン基
ｎ：平均付加モル数であり、２〜300の数
Ｘ：水素原子又は炭素数１〜３のアルキル基
を表す。］
[Where:
R 1c , R 2c : hydrogen atom or methyl group
m1: Number from 0 to 2
AO: C2-C3 oxyalkylene group n: Average addition mole number, 2-300 number X: Represents a hydrogen atom or C1-C3 alkyl group. ]
［式中、
R3c，R4c，R5c：水素原子、メチル基又は(ＣＨ2)m2ＣＯＯＭ2
R6c：水素原子又はメチル基
M1，M2，Ｙ：水素原子、アルカリ金属、アルカリ土類金属（１／２原子）、アンモニウム、アルキルアンモニウム又は置換アルキルアンモニウム
m2：０〜２の数
を表す。］
[Where:
R 3c , R 4c , R 5c : hydrogen atom, methyl group or (CH 2 ) m2 COOM 2
R 6c : hydrogen atom or methyl group
M 1 , M 2 , Y: hydrogen atom, alkali metal, alkaline earth metal (1/2 atom), ammonium, alkylammonium or substituted alkylammonium
m2 represents a number from 0 to 2. ]
上記の好ましい高性能減水剤として用いられる共重合体において、上記一般式（ｃ１）で表される単量体としては、メトキシポリエチレングリコール、メトキシポリエチレンポリプロピレングリコール、エトキシポリエチレングリコール、エトキシポリエチレンポリプロピレングリコール、プロポキシポリエチレングリコールおよびプロポキシポリエチレンポリプロピレングリコール等の片末端アルキル封鎖ポリアルキレングリコールとアクリル酸、メタクリル酸又は脂肪酸の脱水素（酸化）反応物とのエステル化物や、アクリル酸、メタクリル酸又は脂肪酸の脱水素（酸化）反応物へのＥＯ、プロピレンオキサイド（以下、ＰＯという）付加物が用いられる。またポリアルキレングリコールのモノマーの繰り返し単位としては、ＥＯ単独、ＰＯ単独、ＥＯとＰＯのランダム、ブロック、交互付加の何れでも用いることができる。ポリアルキレングリコールのモノマーの繰り返し単位の平均付加モル数が、上記特開平７−２２３８５２号公報に記載の場合のように１１０〜３００であると、硬化遅延の短縮、高流動性、高充填性、高分離低減性の面でより好ましい。 In the copolymer used as the preferred high performance water reducing agent, the monomer represented by the general formula (c1) includes methoxypolyethylene glycol, methoxypolyethylenepolypropyleneglycol, ethoxypolyethyleneglycol, ethoxypolyethylenepolypropyleneglycol, propoxy Deesterification (oxidation) of acrylic acid, methacrylic acid or fatty acid, esterification product of one-end alkyl-blocked polyalkylene glycol such as polyethylene glycol and propoxy polyethylene polypropylene glycol and dehydrogenation (oxidation) reaction product of acrylic acid, methacrylic acid or fatty acid ) Adduct of EO and propylene oxide (hereinafter referred to as PO) to the reaction product is used. As the repeating unit of the polyalkylene glycol monomer, any one of EO alone, PO alone, random, block and alternating addition of EO and PO can be used. When the average added mole number of the repeating unit of the polyalkylene glycol monomer is 110 to 300 as described in JP-A-7-223852, the curing delay is shortened, high fluidity, high filling property, It is more preferable in terms of high separation reduction.
上記一般式（ｃ２）で表される化合物としては、不飽和モノカルボン酸系単量体として、アクリル酸、メタクリル酸、クロトン酸、又はこれらのアルカリ金属塩、アルカリ土類金属塩（１／２原子）、アンモニウム塩、アミン塩、置換アミン塩が挙げられる。また、不飽和ジカルボン酸系単量体として、無水マレイン酸、マレイン酸、無水イタコン酸、イタコン酸、無水シトラコン酸、シトラコン酸、フマル酸、又はこれらのアルカリ金属塩、アルカリ土類金属塩（１／２原子）、アンモニウム塩、アミン塩、置換アミン塩が挙げられる。 Examples of the compound represented by the general formula (c2) include, as unsaturated monocarboxylic acid monomers, acrylic acid, methacrylic acid, crotonic acid, or alkali metal salts and alkaline earth metal salts thereof (1/2 Atom), ammonium salts, amine salts, substituted amine salts. Further, as the unsaturated dicarboxylic acid monomer, maleic anhydride, maleic acid, itaconic anhydride, itaconic acid, citraconic anhydride, citraconic acid, fumaric acid, or alkali metal salts or alkaline earth metal salts thereof (1 / 2 atom), ammonium salts, amine salts, substituted amine salts.
また、上記一般式（ｃ３）で表される化合物としては、アリルスルホン酸、メタリルスルホン酸、又はこれらのアルカリ金属塩、アルカリ土類金属塩（１／２原子）、アンモニウム塩、アミン塩、置換アミン塩が挙げられる。 Examples of the compound represented by the general formula (c3) include allyl sulfonic acid, methallyl sulfonic acid, or alkali metal salts, alkaline earth metal salts (1/2 atoms), ammonium salts, amine salts, Substituted amine salts are mentioned.
さらに、本発明において用いられる高性能（ＡＥ）減水剤としては、下記一般式（ｄ１）で表される単量体１と、下記一般式（ｄ２）で表される単量体２及び下記一般式（ｄ３）で表される単量体３を含む混合単量体とを、ｐＨ７以下で共重合して得られるリン酸エステル系重合体が好適に用いられる。かかるリン酸エステル系重合体は、特開２００６−５２３８１号を参照することができる。 Furthermore, as the high performance (AE) water reducing agent used in the present invention, the monomer 1 represented by the following general formula (d1), the monomer 2 represented by the following general formula (d2), and the following general formula A phosphate ester polymer obtained by copolymerizing the mixed monomer containing the monomer 3 represented by the formula (d3) at a pH of 7 or less is preferably used. JP, 2006-52381, A can be referred to for such a phosphate ester system polymer.
〔式中、Ｒ1d、Ｒ2dは、それぞれ水素原子又はメチル基、Ｒ3は水素原子又は-ＣＯＯ(ＡＯ)nＸ、ＡＯは炭素数２〜４のオキシアルキレン基又はオキシスチレン基、ｎはＡＯの全平均付加モル数であり、３〜２００の数、Ｘは水素原子又は炭素数１〜１８のアルキル基を表す。〕 [Wherein R 1d and R 2d are each a hydrogen atom or a methyl group, R 3 is a hydrogen atom or —COO (AO) n X, AO is an oxyalkylene group or oxystyrene group having 2 to 4 carbon atoms, n is It is the total average addition mole number of AO, the number of 3-200, X represents a hydrogen atom or a C1-C18 alkyl group. ]
〔式中、Ｒ4dは水素原子又はメチル基、Ｒ5dは炭素数２〜１２のアルキレン基、ｍ１は１〜３０の数、Ｍは水素原子、アルカリ金属又はアルカリ土類金属（１／２原子）を表す。〕 [Wherein R 4d is a hydrogen atom or a methyl group, R 5d is an alkylene group having 2 to 12 carbon atoms, m1 is a number of 1 to 30, M is a hydrogen atom, an alkali metal or an alkaline earth metal (1/2 atom ). ]
〔式中、Ｒ6d、Ｒ8dは、それぞれ水素原子又はメチル基、Ｒ7d、Ｒ9dは、それぞれ炭素数２〜１２のアルキレン基、ｍ２、ｍ３は、それぞれ１〜３０の数、Ｍは水素原子、アルカリ金属又はアルカリ土類金属（１／２原子）を表す。〕 [Wherein R 6d and R 8d are each a hydrogen atom or a methyl group, R 7d and R 9d are each an alkylene group having 2 to 12 carbon atoms, m2 and m3 are each a number from 1 to 30, and M is hydrogen. Represents an atom, alkali metal or alkaline earth metal (1/2 atom). ]
これらの高性能（ＡＥ）減水剤のうち、工程（II）では、ポリカルボン酸系ＥＯ付加物を主成分とする高性能（ＡＥ）減水剤、あるいは上記リン酸エステル系重合体を主成分とする高性能（ＡＥ）減水剤が好適である。 Among these high performance (AE) water reducing agents, in step (II), the high performance (AE) water reducing agent mainly composed of a polycarboxylic acid-based EO adduct or the above-mentioned phosphate ester-based polymer as a main component. High performance (AE) water reducing agents are preferred.
工程（II）における高性能（ＡＥ）減水剤の添加量は、所望とする流動性に応じて適宜決定することができるが、水硬性粉体（Ｃ）１００重量部に対して、好ましくは０．０１〜１重量部、より好ましくは０．０５〜０．５重量部である。 The addition amount of the high performance (AE) water reducing agent in the step (II) can be appropriately determined according to the desired fluidity, but is preferably 0 with respect to 100 parts by weight of the hydraulic powder (C). 0.01 to 1 part by weight, more preferably 0.05 to 0.5 part by weight.
工程（II）におけるレオロジー改質剤の水硬性組成物（Ｉ）への添加は、水溶液または粉末のどちらの状態でも可能である。また、予めレオロジー改質剤と、カチオン性ポリマー及び／又は高性能（ＡＥ）減水剤とを混合した混合物を添加しても良い。さらにレオロジー改質剤、カチオン性ポリマー、及び高性能（ＡＥ）減水剤のそれぞれあるいは混合物を、一時に全量添加する方法、あるいは数回に分割して添加する方法のどちらを採用することもできる。 The rheology modifier in step (II) can be added to the hydraulic composition (I) in either an aqueous solution or a powder state. Moreover, you may add the mixture which mixed the rheology modifier previously with the cationic polymer and / or the high performance (AE) water reducing agent. Furthermore, it is possible to employ either a method in which each or a mixture of the rheology modifier, the cationic polymer, and the high performance (AE) water reducing agent or a mixture thereof is added all at once, or a method in which the rheology modifier is added in several portions.
レオロジー改質剤を水硬性組成物（Ｉ）に添加後、混練することで水硬性組成物（II）が得られる。混練は、二軸ミキサー、等の混練機、ミキサー車の混練り装置を用いることができる。本発明では、工程（Ｉ）で調製した水硬性組成物（Ｉ）をアジテーター車で施工現場に搬送し、工程（II）の少なくとも一部を、アジテータ車内の水硬性組成物（Ｉ）へのレオロジー改質剤の添加により行うことができる。 After adding the rheology modifier to the hydraulic composition (I), the hydraulic composition (II) is obtained by kneading. For kneading, a kneader such as a twin-screw mixer or a kneading device for a mixer truck can be used. In the present invention, the hydraulic composition (I) prepared in the step (I) is transported to the construction site by an agitator vehicle, and at least a part of the step (II) is transferred to the hydraulic composition (I) in the agitator vehicle. This can be done by adding a rheology modifier.
工程（II）では、計量の手間を省き、投入作業の簡便性をはかるために、レオロジー改質剤を、該レオロジー改質剤を収容した水溶性包装体として用いることが好ましい。その際、レオロジー改質剤は粉末状のものが好ましい。また、レオロジー改質剤は、一般式（ａ１）で表される化合物と共に、他の成分とを含有することもできる。レオロジー改質剤は、更にカチオン性ポリマー及び／又は高性能（ＡＥ）減水剤を含有することが好ましい。レオロジー改質剤に配合されるカチオン性ポリマー、高性能（ＡＥ）減水剤等の成分は粉末状ものが好ましい。工程（II）では、レオロジー改質剤を収容した水溶性包装体を用いることが好ましい。水溶性包装体は、水溶性材料でレオロジー改質剤を包装してなるものであり、形状は問わない。また、密封されていなくてもよく、開放容器に収容した状態の水溶性包装体を使用してもよい。かかる水溶性包装体を、アジテーター車、又は攪拌機内に投入することが好ましい。 In the step (II), it is preferable to use the rheology modifier as a water-soluble package containing the rheology modifier, in order to save the labor of weighing and simplify the charging operation. In that case, the rheology modifier is preferably in powder form. The rheology modifier can also contain other components in addition to the compound represented by the general formula (a1). The rheology modifier preferably further contains a cationic polymer and / or a high performance (AE) water reducing agent. Components such as a cationic polymer and a high performance (AE) water reducing agent blended in the rheology modifier are preferably in powder form. In step (II), it is preferable to use a water-soluble package containing a rheology modifier. The water-soluble package is formed by packaging a rheology modifier with a water-soluble material, and may have any shape. Moreover, it does not need to be sealed, and a water-soluble package in a state of being accommodated in an open container may be used. Such a water-soluble package is preferably put into an agitator vehicle or a stirrer.
水溶性包装体には、例えば、水溶性樹脂であるポリビニルアルコールを原料としたシートを袋状に成型したものや、例えば、特開平５−９９００に記載されているような水難溶性ないし不溶性のカルボキシメチルセルロース（ＣＭＣ）またはカルボキシエチルセルロース繊維と、水難溶性ないし不溶性の無機粉体と、パルプ等の製紙用繊維とを混抄したシートに、アルカリ可溶性ないし解砕性の重合体を一体化したアルカリ崩壊性のシートを袋状に成型したものを用いることができる。水溶性包装体を構成する水溶性材料の厚みは、１０〜１５０μｍ程度が適当であり、好ましくは１５〜５０μｍである。また、これら水溶性包装体を構成する水溶性材料は、農薬、染料、顔料、ワックス、トイレ殺菌剤等にも使用されるが、中でもセメントへの遅延性が小さいものが好ましい。 Examples of the water-soluble packaging include a sheet made of polyvinyl alcohol, which is a water-soluble resin, as a raw material, and a poorly water-soluble or insoluble carboxy as described in JP-A-5-9900. Alkali-disintegrating, in which an alkali-soluble or disintegratable polymer is integrated into a sheet obtained by mixing methylcellulose (CMC) or carboxyethylcellulose fibers, a poorly water-soluble or insoluble inorganic powder, and papermaking fibers such as pulp. A sheet formed into a bag shape can be used. About 10-150 micrometers is suitable for the thickness of the water-soluble material which comprises a water-soluble package, Preferably it is 15-50 micrometers. The water-soluble materials constituting these water-soluble packaging bodies are also used for agricultural chemicals, dyes, pigments, waxes, toilet disinfectants, and the like, and among them, those having a small delay to cement are preferable.
水硬性組成物（II）は、ＪＩＳ Ａ １１５０に規定するスランプフロー値が３５〜７５ｃｍの範囲であり、より好ましくは４０〜７０ｃｍ、さらに好ましくは５０〜６８ｃｍである。スランプフロー値は、フレッシュコンクリートの流動性を示す指標の一つであり、スランプコーンを引き上げた後の試料の直径の広がりで表す。スランプフロー値が５０ｃｍを超え、単位粉体量が５００ｋｇを超えるコンクリートでは、練り上がり後、流動性が安定する時間で測定することが好ましい。例えば、練り上がり後、５〜１５分の間が望ましい。 As for hydraulic composition (II), the slump flow value prescribed | regulated to JISA1150 is the range of 35-75 cm, More preferably, it is 40-70 cm, More preferably, it is 50-68 cm. The slump flow value is one of indexes indicating the fluidity of fresh concrete, and is represented by the spread of the diameter of the sample after the slump cone is pulled up. For concrete with a slump flow value exceeding 50 cm and a unit powder amount exceeding 500 kg, it is preferable to measure in a time during which the fluidity is stabilized after kneading. For example, it is desirable to be between 5 and 15 minutes after kneading.
また、水硬性組成物（II）は、スランプ値（ＪＩＳ Ａ １１０１）が１０〜２５ｃｍ、さらには１５〜２５ｃｍ、１８〜２５ｃｍであることがより好ましい。また、空気量（ＪＩＳ Ａ １１２８）が３．５〜６％であることが好ましい。 The hydraulic composition (II) has a slump value (JIS A 1101) of 10 to 25 cm, more preferably 15 to 25 cm, and more preferably 18 to 25 cm. Further, the amount of air (JIS A 1128) is preferably 3.5 to 6%.
本発明の製造方法は、生コンクリート工場で生産されたレディーミクストコンクリートとして水硬性組成物（Ｉ）を調製し、コンクリート施工現場で工程（II）を行う方法として実施できる。レディーミクストコンクリートを用いることで、水硬性組成物（Ｉ）として安定した物性のコンクリートが得られる。工程（Ｉ）と工程（II）の間にミキサー車等による輸送工程を有しても、輸送中のコンクリート物性管理は普通セメントの条件で行えばよく、特別な管理は不要である。さらに、工程（II）を施工現場で行うことで、輸送中のコンクリート物性変化に対してしても、レオロジー改質剤と高性能（ＡＥ）減水剤の添加量の微調整で対応できる。また、工程（II）の直後にコンクリート打設を開始できるため、流動性の高いコンクリートの流動性保持等の管理が容易になる。流動性保持の観点から、水硬性組成物組成物（II）の打設は、工程（II）の後、９０分以内に開始することが好ましい。なお、工程（Ｉ）の終了後、直ちに工程（II）を行うことができるが、上記の通り、ミキサー車等による輸送等を考慮すると、適当な間隔（３０分間等）をおいた後、施工現場で工程（II）を行うことが好ましい。また、打設の終了は、工程（II）の後、２１０分以内であることが好ましい。 The production method of the present invention can be implemented as a method of preparing the hydraulic composition (I) as ready-mixed concrete produced in a ready-mixed concrete factory and performing the step (II) at a concrete construction site. By using ready-mixed concrete, concrete having stable physical properties can be obtained as the hydraulic composition (I). Even if there is a transportation process using a mixer truck or the like between the process (I) and the process (II), the physical properties of the concrete during transportation may be controlled under the condition of ordinary cement, and no special management is required. Furthermore, by performing the process (II) at the construction site, it is possible to cope with changes in the physical properties of the concrete during transportation by fine adjustment of the addition amount of the rheology modifier and the high performance (AE) water reducing agent. Moreover, since the concrete pouring can be started immediately after the step (II), it becomes easy to maintain the fluidity of the highly fluid concrete. From the viewpoint of maintaining fluidity, the placement of the hydraulic composition (II) is preferably started within 90 minutes after the step (II). In addition, although the process (II) can be performed immediately after the completion of the process (I), as described above, after taking an appropriate interval (30 minutes, etc.) in consideration of transportation by a mixer truck, etc. It is preferable to perform step (II) on site. Moreover, it is preferable that the completion | finish of casting is less than 210 minutes after process (II).
製造例１（ａ−１の製造）
反応槽にヘキサデシルジメチルアミン３９．１ｋｇ、オクタデシルジメチルアミン１００．４ｋｇを仕込み、６５℃に昇温した。イオン交換水４８７．２ｋｇ、ｐ−トルエンスルホン酸の７０％水溶液１２２．７ｋｇを仕込み、攪拌した後、更にイオン交換水２７ｋｇを仕込み、１時間攪拌し均一化させた。得られた混合水溶液の全量を６５℃まで昇温し、攪拌後、系内を窒素置換した。ＥＯ２７．４ｋｇを仕込み、３時間、６５℃で反応させた。その後、反応器内の残圧を系外にブローし、６５℃で２００ｔｏｒｒ（２６．７ｋＰａ）、３０分間の脱気を行った。さらに、ｐ−トルエンスルホン酸の７０％水溶液３２．３ｋｇを仕込み、４８重量％ＮａＯＨ水溶液８．０ｋｇで中和し、さらにカチオン性ポリマー〔ポリジメチルアミノエチルメタクリレートジエチル硫酸塩（重量平均分子量１２万、カチオン化密度３．６ｍｅｑ／ｇ）の３５重量％水溶液〕１５５．４ｋｇ、消泡剤０．５ｋｇ（ＦＳアンチフォームＱ１−１１８３：東レ・ダウコーニング社製）を仕込み均一化させ、目的とするジメチルヒドロキシエチルアルキルアンモニウムｐ−トルエンスルホネート及びカチオン性ポリマーを含む混合水溶液約１ｔを得た。混合水溶液の分析値は、ｐＨ７．２、水分６６．８％、原料アミン反応率９９％であった。
Production Example 1 (Production of a-1)
The reaction vessel was charged with 39.1 kg of hexadecyldimethylamine and 100.4 kg of octadecyldimethylamine and heated to 65 ° C. 487.2 kg of ion-exchanged water and 122.7 kg of a 70% aqueous solution of p-toluenesulfonic acid were added and stirred, and then 27 kg of ion-exchanged water was further added and stirred for 1 hour to homogenize. The total amount of the obtained mixed aqueous solution was raised to 65 ° C., and after stirring, the system was purged with nitrogen. 27.4 kg of EO was charged and reacted at 65 ° C. for 3 hours. Thereafter, the residual pressure in the reactor was blown out of the system, and deaeration was performed at 65 ° C. for 200 torr (26.7 kPa) for 30 minutes. Further, 32.3 kg of a 70% aqueous solution of p-toluenesulfonic acid was charged, neutralized with 8.0 kg of a 48% by weight aqueous NaOH solution, and a cationic polymer [polydimethylaminoethyl methacrylate diethyl sulfate (weight average molecular weight 120,000, 35 wt% aqueous solution with a cationization density of 3.6 meq / g)] 155.4 kg, defoaming agent 0.5 kg (FS Antifoam Q1-1183, manufactured by Toray Dow Corning Co., Ltd.), and homogenized to obtain the desired dimethyl About 1 t of a mixed aqueous solution containing hydroxyethylalkylammonium p-toluenesulfonate and a cationic polymer was obtained. The analysis values of the mixed aqueous solution were pH 7.2, moisture 66.8%, and raw material amine reaction rate 99%.
次に、槽内温度９０℃に設定した横型円筒ジャケット式真空乾燥機（高砂化工機株式会社製、容量：３．１３６ｍ３、直径１．１ｍ×長さ３．５ｍ、動力１１ｋＷ、粉砕棒サイズ：φ３５×３．３８ｍ、）に、前記混合水溶液１ｔを投入した。攪拌速度６．４ｒｐｍ、減圧度０．０７０ＭＰａ、乾燥時間１２時間の条件で乾燥させた後、乾燥物が室温になるまで６時間冷却した。乾燥物の水分量を計測し、水分量が１重量％以下になった乾燥物を粉砕機（ミル）で粉砕し、目的とするレオロジー改質剤ａ−１〔一般式（１）で表される化合物及びカチオン性ポリマーを含有する粉末状組成物〕を得た。 Next, a horizontal cylindrical jacket type vacuum dryer set at a temperature of 90 ° C. (manufactured by Takasago Kako Co., Ltd., capacity: 3.136 m 3 , diameter 1.1 m × length 3.5 m, power 11 kW, grinding rod size) : Φ35 × 3.38 m) was added to the mixed aqueous solution 1t. After drying under the conditions of a stirring speed of 6.4 rpm, a reduced pressure of 0.070 MPa, and a drying time of 12 hours, the product was cooled for 6 hours until the dried product reached room temperature. The moisture content of the dried product was measured, and the dried product having a moisture content of 1% by weight or less was pulverized with a pulverizer (mill), and the desired rheology modifier a-1 [represented by the general formula (1) And a powdery composition containing a cationic polymer].
製造例（ａ−２の製造）
フラスコに水５０ｇ、ｐ−トルエンスルホン酸１水和物９５．１ｇ、イソプロピルアルコール（ＩＰＡ）８５．０ｇを仕込み、６０℃に昇温、攪拌して溶解した。混合調整溶液を５０から６０℃に保ち、予め融解させておいた硬化牛脂ジメチルアミン１４５．４ｇを、６０℃に保持して３時間かけて滴下した。滴下終了後、６０℃でさらに１時間攪拌後、硬化牛脂ジメチルアミンのｐ−トルエンスルホン酸塩のＩＰＡ／水−混合溶液（１）３７５．５ｇを得た。次に、２Ｌのオートクレーブに、混合溶液（１）３７５ｇを仕込み、攪拌後、系内を窒素置換した。６５℃まで昇温し、ＥＯ２８．６ｇを仕込み、３時間反応させた。反応器内の残圧を系外にブローし、４５℃で２００ｔｏｒｒ（２６．７ｋＰａ）、３０分間の脱気をした。さらに、ｐＨ調整（ｐ−トルエンスルホン酸１水和物、ＩＰＡ）を行い、目的とするレオロジー改質剤（ａ−２）（ジメチルヒドロキシエチルアルキルアンモニウムｐ−トルエンスルホネートのＩＰＡ／水−混合溶液）３９０ｇを得た。
Production example (production of a-2)
A flask was charged with 50 g of water, 95.1 g of p-toluenesulfonic acid monohydrate, and 85.0 g of isopropyl alcohol (IPA), and heated to 60 ° C. and stirred to dissolve. The mixed adjustment solution was kept at 50 to 60 ° C., and 145.4 g of hardened beef tallow dimethylamine previously melted was added dropwise over 3 hours while maintaining the temperature at 60 ° C. After completion of the dropwise addition, the mixture was further stirred at 60 ° C. for 1 hour, to obtain 375.5 g of an IPA / water-mixed solution (1) of p-toluenesulfonate of cured beef tallow dimethylamine. Next, 375 g of the mixed solution (1) was charged into a 2 L autoclave. After stirring, the system was purged with nitrogen. The temperature was raised to 65 ° C., and 28.6 g of EO was charged and reacted for 3 hours. The residual pressure in the reactor was blown out of the system, and degassed at 45 ° C. for 200 torr (26.7 kPa) for 30 minutes. Furthermore, pH adjustment (p-toluenesulfonic acid monohydrate, IPA) is performed, and the intended rheology modifier (a-2) (IPA / water-mixed solution of dimethylhydroxyethylalkylammonium p-toluenesulfonate) 390 g was obtained.
表１に、以下の実施例及び比較例で用いたレオロジー改質剤を示す。 Table 1 shows the rheology modifiers used in the following examples and comparative examples.
また、表２に、以下の実施例で用いたコンクリート混和剤を示す。 Table 2 shows concrete admixtures used in the following examples.
実施例１
表３の配合１で、セメント（Ｃ）、細骨材（Ｓ）及び粗骨材（Ｇ）を100リットルの強制２軸ミキサーに投入後、２０℃にて１０秒間空練りを行った。次いで水道水（Ｗ）に、コンクリート混和剤をその添加量が表３の通りとなるように加えた混練水を加え６０秒間本練りを行い、水硬性組成物（Ｉ）を調製した〔工程（Ｉ）〕。
Example 1
In Formulation 1 of Table 3, cement (C), fine aggregate (S), and coarse aggregate (G) were put into a 100 liter forced biaxial mixer, and then kneaded at 20 ° C. for 10 seconds. Next, the tap water (W) was mixed with kneaded water in which the amount of the concrete admixture was added as shown in Table 3, and kneaded for 60 seconds to prepare a hydraulic composition (I) [Step ( I)].
得られた水硬性組成物（Ｉ）を練り舟に排出し、コンクリートの運搬時間を想定して３０分間静置した。その後、傾胴式ミキサーに水硬性組成物（Ｉ）を移し、レオロジー改質剤を表４の量で添加し９０秒間混練し、水硬性組成物（II）を得た〔工程（II）〕。 The obtained hydraulic composition (I) was discharged into a kneading boat and allowed to stand for 30 minutes assuming a concrete transportation time. Thereafter, the hydraulic composition (I) was transferred to a tilt-type mixer, and the rheology modifier was added in the amount shown in Table 4 and kneaded for 90 seconds to obtain a hydraulic composition (II) [Step (II)]. .
水硬性組成物（Ｉ）は、スランプ値、流動性としてスランプフロー値を、水硬性組成物（II）は、スランプ値、流動性としてスランプフロー値、材料分離抵抗性としてブリーディング量、圧縮強度（材齢１日）を測定した。また、水硬性組成物（Ｉ）の空気量については、空気量調整剤（マイテイＡＥ０２、花王製）および消泡剤（市販品：脂肪酸エステル系）を使用し、４．５±１．５％になるように調整した。各評価は以下の方法で行った（試験温度は２０℃）。結果を表５に示す。 The hydraulic composition (I) has a slump value and a slump flow value as fluidity, and the hydraulic composition (II) has a slump value and a slump flow value as fluidity, a bleeding amount as a material separation resistance, and a compressive strength ( Material age 1 day) was measured. Moreover, about the air quantity of hydraulic composition (I), an air quantity regulator (Mighty AE02, Kao make) and an antifoamer (commercial item: fatty acid ester type) are used, and 4.5 ± 1.5% It was adjusted to become. Each evaluation was performed by the following method (test temperature is 20 ° C.). The results are shown in Table 5.
・スランプ値：ＪＩＳ Ａ １１０１
・スランプフロー値：ＪＩＳ Ａ １１５０
・ブリーディング量：ＪＩＳ Ａ １１２３
・圧縮強度：ＪＩＳ Ａ １１０８
・ Slump value: JIS A 1101
・ Slump flow value: JIS A 1150
・ Bleeding amount: JIS A 1123
・ Compressive strength: JIS A 1108
表３中の使用材料は以下の通りである。
・水（Ｗ）：水道水
・セメント（Ｃ）：普通ポルトランドセメント（太平洋セメント株式会社製普通ポルトランドセメントと住友大阪セメント株式会社製普通ポルトランドセメントの１：１混合物）、密度３．１６ｇ／ｃｍ3
・細骨材（Ｓ）：君津産 山砂（密度２．６０ｇ／ｃｍ3、粗粒率２．６３）
・粗骨材（Ｇ）：鳥形山産 石灰砕石（密度２．７０ｇ／ｃｍ3、粗粒率７．０３、最大寸法２０ｍｍ）
The materials used in Table 3 are as follows.
Water (W): Tap water Cement (C): Ordinary Portland cement (1: 1 mixture of ordinary Portland cement manufactured by Taiheiyo Cement Co., Ltd. and ordinary Portland cement manufactured by Sumitomo Osaka Cement Co., Ltd.), density 3.16 g / cm 3
· Fine aggregate (S): Kimitsu producing pit sand (density 2.60 g / cm 3, Sotsuburitsu 2.63)
・ Coarse aggregate (G): lime crushed stone from Torigatayama (density 2.70 g / cm 3 , coarse grain ratio 7.03, maximum dimension 20 mm)
ここで、実施例１−１及び比較例１−１の工程（II）では、レオロジー改質剤は、ポリビニルアルコールフィルムからなる１３．５ｃｍ（長さ）×１０ｃｍ（幅）の粉体包装用袋に封入して水硬性組成物（Ｉ）に添加した。 Here, in the step (II) of Example 1-1 and Comparative Example 1-1, the rheology modifier is a 13.5 cm (length) × 10 cm (width) powder packaging bag made of a polyvinyl alcohol film. And added to the hydraulic composition (I).
実施例１−１、１−２は、比較例１−１に比べて工程（II）においてスランプフロー値の低下が少ない。コンクリートを施工する段階で、スランプフロー値が低下するとポンプ圧送性が低下したり、充填作業に支障を来すので、スランプフロー値の低下が少ない方が好ましい。また、比較例１−１の材齢１日の圧縮強度やブリーディング量については、凝結遅延の影響が認められ、実施例１−１、１−２に及ばない結果となった。材齢１日の圧縮強度は、硬化遅延の指標になり、型枠を外す時期を決める目安となる。材齢１日の圧縮強度が大きい方が、型枠を確実に早い時期に外すことができ、次の工程に早く取り掛かることができるので好ましい。また、ブリーディング量は材料分離を表す。ある程度のブリーディング量はコテ均しをする際にやり易くなるので問題にならないが、比較例１−１のようにブリーディング量が大きくなると材料分離を起こしていることになる。 In Examples 1-1 and 1-2, the decrease in the slump flow value in the step (II) is smaller than that in Comparative Example 1-1. When the slump flow value is lowered at the concrete construction stage, the pumpability is lowered or the filling operation is hindered. Therefore, it is preferable that the slump flow value is less lowered. Moreover, about the compressive strength and bleeding amount of the material age 1 day of the comparative example 1-1, the influence of the setting delay was recognized and it became a result which does not reach Example 1-1, 1-2. The compressive strength at one day of age is an index of hardening delay and is a guideline for determining when to remove the formwork. A higher compressive strength per day is preferable because the mold can be reliably removed early and the next process can be started quickly. The bleeding amount represents material separation. A certain amount of bleeding is not a problem because it is easy to do when leveling the iron, but when the amount of bleeding increases as in Comparative Example 1-1, material separation occurs.
実施例２
実施例１と同様に、ただしコンクリート配合は表６の配合２の通りとし、コンクリート混和剤の種類を表７のように変更して、水硬性組成物（Ｉ）を得た〔工程（Ｉ）〕。傾胴式ミキサーに水硬性組成物（Ｉ）を移し、レオロジー改質剤及びコンクリート混和剤を表７の量で添加し１８０秒間混練し、水硬性組成物（II）を得た〔工程（II）〕。この水硬性組成物（II）は、水中不分離コンクリートとして好適である。
Example 2
As in Example 1, except that the concrete composition was as shown in composition 6 in Table 6, and the type of the concrete admixture was changed as shown in Table 7 to obtain a hydraulic composition (I) [Step (I) ]. The hydraulic composition (I) was transferred to a tilting-type mixer, the rheology modifier and the concrete admixture were added in the amounts shown in Table 7, and kneaded for 180 seconds to obtain a hydraulic composition (II) [Step (II ]]. This hydraulic composition (II) is suitable as underwater non-separable concrete.
この水硬性組成物（II）について、以下に示す試験法にしたがって、材料分離抵抗性として懸濁物質量（ＳＳ）の測定を、また、圧縮強度（材齢３日）の測定を行った。また、水硬性組成物（Ｉ）、（II）のスランプ値及び流動性としてスランプフロー値を実施例１と同様に測定した。その結果を表８に示す。 About this hydraulic composition (II), according to the test method shown below, the amount of suspended solids (SS) was measured as material separation resistance, and the compressive strength (material age 3 days) was measured. Moreover, the slump flow value was measured in the same manner as in Example 1 as the slump value and fluidity of the hydraulic compositions (I) and (II). The results are shown in Table 8.
１．懸濁物質量（ＳＳ）：「土木学会、水中不分離性コンクリート設計施行指針（案）、水中不分離性コンクリートの水中分離度試験方法（案）」に基づいて評価した。評価基準は以下の通りである。
Ａ：１５％以下
Ｂ：１５％超３０％以下
Ｃ：３０％超６０％以下
Ｄ：６０％超
1. Suspended substance amount (SS): Evaluated based on "Japan Society of Civil Engineers, Underwater inseparable concrete design enforcement guidelines (draft), Underwater separability concrete test method (draft)". The evaluation criteria are as follows.
A: 15% or less B: Over 15% over 30% C: Over 30% over 60% D: Over 60%
２．圧縮強度（材齢３日）：「土木学会、水中不分離性コンクリート設計施行指針（案）、水中不分離性コンクリートの圧縮強度試験用水中作製供試体の作り方（案）」に基づいて評価した。 2. Compressive strength (age 3 days): Evaluated based on "Japan Society of Civil Engineers, Underwater inseparable concrete design enforcement guidelines (draft), How to make underwater specimen for compressive strength test of underwater inseparable concrete (draft)" .
表６中の使用材料は以下の通りである。
水（Ｗ）：水道水
セメント（Ｃ）：普通ポルトランドセメント、市販品、密度３．１６ｇ／ｃｍ3
細骨材（Ｓ）：千葉県君津産山砂、表乾密度２．６２ｇ／ｃｍ3、粗粒率２．５７
粗骨材（Ｇ）：高知県鳥形山産石灰砕石、表乾密度２．７１ｇ／ｃｍ3、粗粒率７．０３、最大寸法２０ｍｍ
The materials used in Table 6 are as follows.
Water (W): tap water cement (C): ordinary portland cement, commercially available, density 3.16g / cm 3
Fine aggregate (S): Kimitsu mountain sand, Chiba prefecture, surface dry density 2.62 g / cm 3 , coarse grain ratio 2.57
Coarse aggregate (G): lime crushed stone from Mt. Torigata, Kochi Prefecture, surface dry density 2.71 g / cm 3 , coarse grain ratio 7.03, maximum dimension 20 mm
ここで、実施例２−１及び比較例２−１の工程（II）では、レオロジー改質剤及びセメント混和剤の両方を、ポリビニルアルコールフィルムからなる１３．５ｃｍ（長さ）×１０ｃｍ（幅）の粉体包装用袋に封入して水硬性組成物（Ｉ）に添加した。 Here, in step (II) of Example 2-1 and Comparative Example 2-1, both the rheology modifier and the cement admixture were 13.5 cm (length) × 10 cm (width) made of a polyvinyl alcohol film. Were encapsulated in a powder packaging bag and added to the hydraulic composition (I).
表８から明らかなように、実施例２−１、２−２は、水中での材料分離抵抗性に優れると同時に、３日後の水中作製供試体の強度発現も同時に優れた結果が得られている。これに対し比較例２−１では、材料分離抵抗性を得るために所定の添加量を加えると、未硬化を起こし型枠を外す事ができなかった。また、比較例２−１は、セルロース系のポリマーを使用しているため、コンクリートの流動性の低下を引き起こしやすく、スランプフロー値が５０ｃｍを超える高流動性が得られなかった。 As is clear from Table 8, Examples 2-1 and 2-2 are excellent in material separation resistance in water, and at the same time, the strength expression of the underwater preparation specimen after 3 days is also excellent. Yes. On the other hand, in Comparative Example 2-1, when a predetermined addition amount was added in order to obtain material separation resistance, it was not cured and the mold could not be removed. Moreover, since the comparative example 2-1 uses the cellulosic polymer, it was easy to cause the fall of the fluidity | liquidity of concrete, and the high fluidity | liquidity whose slump flow value exceeds 50 cm was not obtained.
Claims (5)
工程（Ｉ）：プラントにて、水、水硬性粉体、骨材、及びコンクリート混和剤を混練りし、水セメント重量比が２５〜６５重量％の水硬性組成物（Ｉ）を調製する工程
工程（II）：コンクリート施工現場において、水硬性組成物（Ｉ）に一般式（ａ１）で表される化合物を含有するレオロジー改質剤を添加して、スランプフロー値が３５〜７５ｃｍである水硬性組成物（II）を調製する工程
（式中、Ｒ1aは炭素数１０〜２６のアルキル基、Ｒ2aは炭素数１〜２２のアルキル基又はヒドロキシアルキル基、Ｒ3a、Ｒ4aは、それぞれ、炭素数１〜３のアルキル基又はヒドロキシアルキル基、Ｙはエチレン基又はプロピレン基、ｎは０又は１の数、Ｘ-はアニオン性芳香族化合物残基を表す。） The manufacturing method of the concrete which has the following process (I) and process (II).
Step (I): Step of preparing a hydraulic composition (I) having a water cement weight ratio of 25 to 65% by weight by kneading water, hydraulic powder, aggregate, and concrete admixture in a plant. Step (II): Water having a slump flow value of 35 to 75 cm by adding a rheology modifier containing a compound represented by the general formula (a1) to the hydraulic composition (I) at a concrete construction site. Step of preparing hard composition (II)
Wherein R 1a is an alkyl group having 10 to 26 carbon atoms, R 2a is an alkyl group having 1 to 22 carbon atoms or a hydroxyalkyl group, and R 3a and R 4a are each an alkyl group having 1 to 3 carbon atoms or (Hydroxyalkyl group, Y represents an ethylene group or a propylene group, n represents a number of 0 or 1, and X − represents an anionic aromatic compound residue.)
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| JP2015063884A (en) * | 2013-08-30 | 2015-04-09 | 太平洋マテリアル株式会社 | Construction method with special concrete |
| JP2015113243A (en) * | 2013-12-10 | 2015-06-22 | 花王株式会社 | Hydraulic composition |
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| CN107879654A (en) * | 2017-11-27 | 2018-04-06 | 黎芷杉 | A kind of special swelling agent of traffic engineering and its production method |
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