WO2020192140A1 - Accélérateur liquide de solubilisation à haute intensité et procédé de préparation associé - Google Patents

Accélérateur liquide de solubilisation à haute intensité et procédé de préparation associé Download PDF

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Publication number
WO2020192140A1
WO2020192140A1 PCT/CN2019/118048 CN2019118048W WO2020192140A1 WO 2020192140 A1 WO2020192140 A1 WO 2020192140A1 CN 2019118048 W CN2019118048 W CN 2019118048W WO 2020192140 A1 WO2020192140 A1 WO 2020192140A1
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WO
WIPO (PCT)
Prior art keywords
acid
strength
solubilizing liquid
add
setting agent
Prior art date
Application number
PCT/CN2019/118048
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English (en)
Chinese (zh)
Inventor
官梦芹
郭鑫祺
李祥河
蒋卓君
陈晓彬
林添兴
郭元强
Original Assignee
科之杰新材料集团有限公司
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 科之杰新材料集团有限公司 filed Critical 科之杰新材料集团有限公司
Priority to ZA2020/01354A priority Critical patent/ZA202001354B/en
Publication of WO2020192140A1 publication Critical patent/WO2020192140A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/38—Polysaccharides or derivatives thereof

Definitions

  • the invention belongs to the technical field of building materials, and specifically relates to a high-strength solubilizing liquid accelerator and a preparation method thereof.
  • Accelerating agent is a new type of chemical admixture that can quickly set and harden cement concrete.
  • the shotcrete In order to increase the thickness of a shotcrete spray layer, the shotcrete must be mixed with an accelerator to shorten the time interval between two shots and improve The early strength of shotcrete reduces the rebound amount of shotcrete and guarantees the stability of the project quality. It is mainly used for bolting and shotcrete support in tunnels, shafts, slope protection and other projects, as well as in the process of plugging and repairing.
  • the purpose of the present invention is to provide a high-strength solubilizing liquid quick-setting admixture and a preparation method thereof, so as to solve the problems of poor stability of the existing quick-setting admixtures, easy stratification and precipitation, and the production concentration cannot be increased.
  • the preparation method of the complexing enhancer is to add ethylenediaminetetraacetic acid to the reaction kettle, turn on the stirring device, and then add alcoholamine and catalyst all at once to react, and at a temperature of 70-100°C, Reacting for 1 to 4 hours to prepare the complex enhancer, wherein the molar ratio of ethylenediaminetetraacetic acid and alcohol amine is 1:0.5-2, and the amount of catalyst is 0.5 to 0.5 of the total mass of ethylenediaminetetraacetic acid and alcohol amine. 3.0%.
  • the alcohol amine is at least one of monoethanolamine, diethanolamine, triethanolamine, triisopropanolamine and diethanolmonoisopropanolamine.
  • the catalyst is p-toluenesulfonic acid and/or concentrated sulfuric acid.
  • the initiator is ammonium persulfate.
  • the molecular weight regulator is at least one of thioglycolic acid, mercaptopropionic acid and mercaptoethanol.
  • the pH adjusting agent is at least one of concentrated sulfuric acid, p-toluenesulfonic acid, citric acid, tartaric acid, salicylic acid, oxalic acid, and hydrofluoric acid.
  • the method for preparing a high-strength solubilizing liquid quick-setting agent specifically includes the following steps: firstly, the stabilizer and water are added to the reaction kettle for stirring, and then the pH adjuster is added and stirred uniformly, and then added separately Stir aluminum sulfate, aluminum citrate, hydroxyethyl cellulose and complexing enhancer. After the materials are completely stirred and evenly mixed, react for 1.0-4.0h at a temperature of 40-80°C. After the reaction is completed, the product High-strength solubilizing liquid accelerator.
  • a complexing enhancer is prepared by esterifying ethylenediaminetetraacetic acid and an alcohol amine, which is used in the synthesis of a liquid accelerator, which can improve the overall strength of concrete.
  • hydroxyethyl cellulose is used to synthesize liquid quick-setting agent, and the complexation enhancer, stabilizer and hydroxyethyl cellulose are combined in the solution to form a cross-linked network structure, which can achieve good solubilization Effectively, the product concentration can be as high as 80%, and there will be no stratification or precipitation. The product has a good dissolution effect and can reduce the transportation cost of the liquid accelerator.
  • step (3) Add 2.00g of the stabilizer prepared in step (2) and 60.00g of water into the reaction kettle for stirring, then add 5.00g of concentrated sulfuric acid, and then add 37.00g of aluminum sulfate and 8.00g of aluminum citrate, respectively , 6.00g of hydroxyethyl cellulose and 12.00g of the complexing enhancer prepared in step (1) are stirred. After the materials are completely stirred and evenly mixed, they will react for 3.0h at a temperature of 50°C to obtain a high-strength solubilization Type liquid quick-setting agent KZJ-1.
  • step (3) Add 3.00g of the stabilizer prepared in step (2) and 20.00g of water to the reaction kettle for stirring, then add 6.00g of hydrofluoric acid, and after stirring, add 32.00g of aluminum sulfate and 7.00g of citric acid, respectively
  • Aluminum, 8.00g of hydroxyethyl cellulose and 10.00g of the complexing enhancer prepared in step (1) are stirred. After the materials are completely stirred and evenly mixed, they are reacted for 1.5 hours at a temperature of 70°C to obtain a high-strength enhancement.
  • Dissolved liquid quick-setting agent KZJ-3 Dissolved liquid quick-setting agent KZJ-3.
  • step (3) Add 2.60g of the stabilizer prepared in step (2) and 50.00g of water to the reactor and stir, then add 10.00g of concentrated sulfuric acid, and after stirring, add 36.00g of aluminum sulfate and 10.00g of aluminum citrate respectively , 3.00g of hydroxyethyl cellulose and 15.00g of the complexing enhancer prepared in step (1) are stirred. After the materials are completely stirred and uniform, the reaction is carried out for 2.0h at a temperature of 80°C to obtain a high-strength solubilization Type liquid quick-setting agent KZJ-4.
  • Ammonium persulfate aqueous solution (Ammonium persulfate is 2.60g, water is 10.00g) and mercaptopropionic acid aqueous solution (Mercaptopropionic acid is 1.20g, water is 10.00g), dripping time is 2.5h, drip After completion, the stabilizer is prepared by keeping the temperature at 35°C for 2.0h;
  • step (3) Add 2.50g of the stabilizer prepared in step (2) and 40.00g of water to the reaction kettle for stirring, then add 7.00g of oxalic acid, and then add 35.00g of aluminum sulfate and 9.00g of citric acid, respectively Aluminum, 7.00g of hydroxyethyl cellulose and 11.00g of the complexing enhancer prepared in step (1) are stirred evenly. After the materials are fully stirred, the reaction is carried out for 2.0h at a temperature of 40°C to obtain a high-strength enhancement. Dissolved liquid quick-setting agent KZJ-5.
  • the high-strength solubilizing liquid accelerator prepared in Example 1 to Example 5 was tested, and Conch P.O 42.5 ordinary Portland cement was selected. According to GB/T35159-2017 "Accelerating Agent for Shotcrete", the obtained high-strength solubilizing liquid accelerator was tested for cement slurry setting water time and cement mortar strength. The amount of accelerator is calculated as the percentage of cement weight.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

L'invention concerne un accélérateur liquide de solubilisation à haute intensité et son procédé de préparation, l'accélérateur liquide comprenant au moins les matières premières suivantes en parties en poids : 30 à 40 parties de sulfate d'aluminium, 5 à 10 parties de citrate d'aluminium, 2 à 8 parties d'hydroxyéthyl cellulose, 1 à 10 parties de régulateurs de pH, 5 à 15 parties d'exhausteurs de complexation, 0,5 à 3 parties d'agents de stabilisation et le reste d'eau. Avec l'introduction d'hydroxyéthyl cellulose pour synthétiser l'accélérateur liquide et la combinaison des activateurs de complexation, des agents de stabilisation et de la cellulose d'hydroxyéthyle dans la solution, une structure réticulaire réticulée est formée, un bon effet de solubilisation peut être obtenu, la concentration de produit atteint 80 %, la survenue de phénomènes de stratification et de séparation par précipitation n'est pas possible, l'effet de dissolution du produit est bon, et le coût de transport de l'accélérateur de liquide peut être réduit.
PCT/CN2019/118048 2019-03-25 2019-11-13 Accélérateur liquide de solubilisation à haute intensité et procédé de préparation associé WO2020192140A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
ZA2020/01354A ZA202001354B (en) 2019-03-25 2020-03-03 High-strength highly-soluble liquid accelerator and method of preparing same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910229343.8 2019-03-25
CN201910229343.8A CN109879631B (zh) 2019-03-25 2019-03-25 一种高强增溶型液体速凝剂及其制备方法

Publications (1)

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WO2020192140A1 true WO2020192140A1 (fr) 2020-10-01

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CN (1) CN109879631B (fr)
WO (1) WO2020192140A1 (fr)
ZA (1) ZA202001354B (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109879631B (zh) * 2019-03-25 2021-08-31 科之杰新材料集团有限公司 一种高强增溶型液体速凝剂及其制备方法
CN111961455B (zh) * 2020-07-26 2022-07-12 青岛大学 一种热致硬水凝胶油井堵水剂的制备方法

Citations (6)

* Cited by examiner, † Cited by third party
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US20140066546A1 (en) * 2010-11-29 2014-03-06 Construction Research & Technology Gmbh Powdered Accelerator
CN105254208A (zh) * 2015-10-16 2016-01-20 徐�明 一种添加纤维素的无碱液体速凝剂及其制备方法
CN105669909A (zh) * 2015-12-28 2016-06-15 江苏中铁奥莱特新材料有限公司 一种增强型聚丙烯酰胺系水泥助磨剂的制备方法
CN109020292A (zh) * 2018-08-16 2018-12-18 科之杰新材料集团有限公司 一种环保增强型无碱液体速凝剂的制备方法
CN109354434A (zh) * 2018-11-30 2019-02-19 山西黄河新型化工有限公司 一种液体无碱速凝剂及其制备方法
CN109879631A (zh) * 2019-03-25 2019-06-14 科之杰新材料集团有限公司 一种高强增溶型液体速凝剂及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3600155B2 (ja) * 2000-05-25 2004-12-08 電気化学工業株式会社 液体急結剤、それを用いた急結性セメントコンクリート、及びその製造方法
CN102786256A (zh) * 2012-09-05 2012-11-21 江苏南瓷绝缘子有限公司 喷射混凝土用液体速凝剂及其应用
CN103396027B (zh) * 2013-07-25 2016-04-06 北京市建筑工程研究院有限责任公司 一种新型无碱液体速凝剂的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140066546A1 (en) * 2010-11-29 2014-03-06 Construction Research & Technology Gmbh Powdered Accelerator
CN105254208A (zh) * 2015-10-16 2016-01-20 徐�明 一种添加纤维素的无碱液体速凝剂及其制备方法
CN105669909A (zh) * 2015-12-28 2016-06-15 江苏中铁奥莱特新材料有限公司 一种增强型聚丙烯酰胺系水泥助磨剂的制备方法
CN109020292A (zh) * 2018-08-16 2018-12-18 科之杰新材料集团有限公司 一种环保增强型无碱液体速凝剂的制备方法
CN109354434A (zh) * 2018-11-30 2019-02-19 山西黄河新型化工有限公司 一种液体无碱速凝剂及其制备方法
CN109879631A (zh) * 2019-03-25 2019-06-14 科之杰新材料集团有限公司 一种高强增溶型液体速凝剂及其制备方法

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ZA202001354B (en) 2020-12-23
CN109879631A (zh) 2019-06-14

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