WO2023070376A1 - 二氧化碳养护再生骨料残余二氧化碳气体含量的测试方法及装置 - Google Patents

二氧化碳养护再生骨料残余二氧化碳气体含量的测试方法及装置 Download PDF

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WO2023070376A1
WO2023070376A1 PCT/CN2021/126747 CN2021126747W WO2023070376A1 WO 2023070376 A1 WO2023070376 A1 WO 2023070376A1 CN 2021126747 W CN2021126747 W CN 2021126747W WO 2023070376 A1 WO2023070376 A1 WO 2023070376A1
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test
recycled aggregate
value
curing
tested
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PCT/CN2021/126747
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English (en)
French (fr)
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梁超锋
李然
候少丹
高越青
何智海
杨金城
田原
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绍兴文理学院
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Priority to PCT/CN2021/126747 priority Critical patent/WO2023070376A1/zh
Publication of WO2023070376A1 publication Critical patent/WO2023070376A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/38—Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass

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  • the invention relates to a method for testing the content of CO 2 gas, in particular to a method and device for testing the content of residual CO 2 gas in regenerated aggregates cured with CO 2 .
  • waste concrete to prepare recycled aggregates can not only absorb waste concrete, but also alleviate the increasing shortage of natural sand and gravel aggregates.
  • the porous old mortar attached to the surface of recycled aggregate the water absorption rate of recycled aggregate is high and the crushing value is large, which greatly limits the application of recycled aggregate in structural concrete.
  • CO 2 curing of recycled aggregates can significantly improve the physical and mechanical properties of recycled aggregates; at the same time, using CO 2 gas as a curing raw material gas to accelerate the carbonization of recycled aggregates can effectively absorb CO 2 waste gas emitted by industries such as steel and cement, It is an environmentally friendly method of strengthening recycled aggregates. However, the recycled aggregate is maintained with CO 2 gas, so that a certain amount of CO 2 gas remains inside the recycled aggregate.
  • CO 2 curing recycled aggregates When using CO 2 curing recycled aggregates to partially or completely replace natural aggregates to prepare recycled concrete, the residual CO 2 gas in CO 2 curing recycled aggregates will have two effects on the strength and durability of recycled concrete: 1) CO 2 curing regeneration Aggregate releases residual CO 2 gas, and then maintains the recycled concrete, improves the microstructure of the new interface transition zone of recycled concrete, and increases the strength of recycled concrete; 2) CO 2 curing recycled aggregate releases residual CO 2 gas, thereby reducing the pH value of recycled concrete, accelerating Corrosion of rebar embedded in recycled concrete. Therefore, the accurate determination of the residual CO 2 gas content in CO 2 cured recycled aggregates is of great significance for predicting the durability of recycled concrete prepared with CO 2 cured recycled aggregates.
  • the present invention provides a method and device for testing the residual CO gas content of CO2 curing regenerated aggregates.
  • the test method provided by the present invention has a clear test principle, a simple test method, and stable and reliable test data, thereby filling this field Whitespace.
  • the invention provides a method for testing the residual CO2 gas content of CO2 curing regenerated aggregates, comprising the following steps:
  • the standard test environment requirements are a temperature of 23°C ⁇ 2°C, air pressure 86kPa ⁇ 106kPa.
  • m CO2 is the mass of residual CO 2 gas in the CO 2 curing recycled aggregate to be measured, the unit is g;
  • Vw is the initial volume of deionized water in the CO2 curing regeneration aggregate solution to be tested, and the unit is L.
  • step 6 is also included: through parallel testing, obtain the residual CO 2 gas mass m CO2 of multiple groups of CO 2 curing recycled aggregate samples to be tested, and eliminate abnormal m CO 2 data according to the Grubbs criterion to obtain an effective m CO 2 test Data, the average value of effective m CO2 test data is used as the final test result.
  • the pH value of the deionized water is 6.7-7.2.
  • the accuracy of the pH meter is not lower than 0.01.
  • the protective gas is nitrogen, and the purity of the nitrogen is not lower than 99%.
  • the present invention provides a test device adopting the test method for CO2 gas content of residual regenerated aggregates in CO2 conservation as described in the above technical scheme, comprising a sealable test box (1), which is arranged in the test box (1)
  • the operating platform (8) on the inner bottom surface is arranged on the support (10) with a chassis (9) on the operating platform (8), and the pH meter (11) arranged on the support (10) is arranged on the
  • the container (12) on the chassis (9) the container (12) is arranged below the pH meter (11), and is arranged in the first operating hole (3) on the side wall of the test box (1). ), the air inlet (4), the second operation hole (5) and the air outlet (6), the top cover (2) that is arranged on the top of the test box (1), is arranged on the test box (1) inside the controller (7).
  • operating gloves are sealingly connected to the first operating hole (3) and the second operating hole (5).
  • the air inlet hole (4) is higher than the air outlet hole (6).
  • the chassis (9) is an electric rotating chassis, and the test box (1) and the top cover (2) are hermetically connected.
  • the pH meter (11) is a high-precision pH tester that can be read continuously.
  • the present invention provides a method for testing the residual CO gas content of CO 2 cured recycled aggregates, which comprises the following steps: 1) Weigh a sample of the CO 2 cured recycled aggregate whose mass is m 1 and put it into a test box, and weigh it Take the deionized water that quality is m 2 and place in the container and put into the test box; 2) the air in the airtight test box is purged with protective gas, and the initial pressure and initial temperature of the airtight test box are adjusted , until it reaches and maintains the standard test environment requirement, the standard test environment requirement is a standard test with a temperature of 23 ° C ⁇ 2 ° C, and an air pressure of 86 kPa ⁇ 106 kPa; 3) use a pH meter to measure the initial pH value of the deionized water in the container; 4 ) Mix the sample of CO 2 curing recycled aggregate to be tested with deionized water to obtain the CO 2 curing recycled aggregate solution to be tested, use a pH meter to continuously monitor the pH
  • m CO2 is the mass of residual CO 2 gas in the CO 2 curing recycled aggregate to be measured, the unit is g;
  • Vw is the initial volume of deionized water in the CO2 curing regeneration aggregate solution to be tested, and the unit is L.
  • the test method provided by the present invention puts the CO2 conservation regeneration aggregate to be tested into deionized water to obtain the CO2 conservation regeneration aggregate solution to be tested.
  • OH) 2 dissolves OH - , so that the pH value of the CO 2 curing recycled aggregate solution to be tested increases; on the other hand, the residual CO 2 gas in the CO 2 curing recycled aggregate is released and dissolved in water to generate H + and HCO 3 - ; H + and OH - react to reduce the pH value of the CO 2 curing recycled aggregate solution to be tested, HCO 3 - and OH - further react to generate H 2 O and CO 3 2 , while CO 3 2 and the free Ca in the solution 2+ reaction generates CaCO 3 , which further reduces the pH value of the CO 2 curing recycled aggregate solution to be tested.
  • the pH value of the CO 2 cured recycled aggregate solution to be tested will tend to be stable.
  • the present invention calculates the amount of consumed H + by testing the difference between the maximum value and the stable value of the pH value of the CO2 curing recycled aggregate solution, and then calculates the CO2 curing recycled aggregate according to the chemical reaction formulas (2) and (3). residual amount of CO2 gas;
  • the test method for the residual CO 2 gas content of the CO 2 curing regenerated aggregate provided by the invention has a clear test principle, a simple test method, and stable and reliable test data.
  • the present invention provides a test device for testing the residual CO gas content of regenerated aggregates using CO conservation described in the above technical solution, including a test box 1 and an operating platform 8 arranged on the inner bottom surface of the test box 1 , set on the support 10 with the chassis 9 on the operating table 8, the pH meter 11 set on the support 10, the container 12 set on the chassis 9, the container 12 set on the pH meter 11 Below, the first operation hole 3, the air inlet 4, the second operation hole 5 and the air outlet 6 arranged on the side wall of the test box 1, the top cover 2 arranged on the top of the test box 1, set The controller 7 in the test box 1.
  • the test equipment provided by the invention is easy to operate, and the test data is stable and reliable. Thereby filling the gap in this field.
  • Fig. 1 is the CO of embodiment 1 Curing residual CO of regenerated aggregate The structural representation of the testing device of gas content;
  • Fig. 2 is the recycled aggregate of embodiment 1 (not CO 2 curing) solution pH value
  • Fig. 3 is the CO of embodiment 1 Curing regeneration aggregate solution pH value
  • test box 1 test box 1, top cover 2, first operating hole 3, air inlet 4, second operating hole 5, air outlet 6, controller 7, operating table 8, chassis 9, bracket 10, pH meter 11 , Container 12.
  • the present invention provides a kind of CO 2 maintenance regenerated aggregate residual CO 2 gas content test method, in that, comprising the following steps:
  • the air in the airtight test box is purged with protective gas, and the initial pressure and initial temperature of the airtight test box are adjusted until it reaches and maintains the standard test environment requirement.
  • the standard test environment requirement is a temperature of 23 °C ⁇ 2°C, air pressure 86kPa ⁇ 106kPa;
  • m CO2 is the mass of residual CO 2 gas in the CO 2 curing recycled aggregate to be measured, the unit is g;
  • Vw is the initial volume of deionized water in the CO2 curing regeneration aggregate solution to be tested, and the unit is L.
  • the particle size of the CO 2 -cured recycled aggregate sample to be tested is preferably 0.15-20 mm.
  • the preparation method of the CO2 conservation recycled aggregate sample to be tested preferably comprises the following steps:
  • the recycled aggregate and CO2 curing gas were carbonized to obtain the CO2- cured recycled aggregate sample to be tested.
  • the recycled aggregate in the present invention includes recycled coarse aggregate and recycled fine aggregate obtained by crushing waste concrete and waste mortar.
  • the particle size of the recycled aggregate sample is preferably 0.15-20 mm.
  • the present invention has no special requirements on the pressure, temperature and CO 2 gas volume concentration of the CO 2 curing.
  • the CO2 curing is preferably carried out in a closed environment.
  • the carbonization reaction of the CO 2 curing recycled aggregate is: the hydration product in the surface mortar of the recycled aggregate reacts with CO 2 gas.
  • the chemical reaction equation of the carbonization reaction is as shown in formula (4) ⁇ formula (7):
  • the regenerated aggregate sample to be tested with CO 2 curing with a mass of m 1 is put into a test box, and the deionized water with a mass of m 2 is weighed and placed in a container and put into the test box.
  • the pH value of the deionized water is preferably 6.7-7.2, more preferably 7.
  • the mass ratio of the CO 2 -cured recycled aggregate sample to be tested to deionized water is preferably 5:4.
  • the present invention uses protective gas to purge the air in the airtight test box, and adjusts the initial pressure and initial temperature of the airtight test box until it reaches and maintains the standard test environment requirement, and the standard test environment requirement is a temperature of 23°C ⁇ 2°C, air pressure 86kPa ⁇ 106kPa.
  • the protective gas is preferably nitrogen, and the purity of the nitrogen is preferably 99.99%.
  • the present invention uses a pH meter to measure the initial pH of the water in the container.
  • the accuracy of the pH meter is preferably not lower than 0.01.
  • the present invention mixes the sample of the CO2 - cured recycled aggregate to be tested with deionized water to obtain the CO2- cured recycled aggregate solution to be tested, and continuously monitors the pH value of the CO2 - cured recycled aggregate solution to be measured with a pH meter, and calculates the pH value
  • the data is stored synchronously in the processor and the test is stopped when the pH value remains stable.
  • the CO 2 curing regenerated aggregate sample to be measured is mixed with deionized water, it is preferable to put the measured CO 2 curing regenerated aggregate sample into deionized water.
  • the present invention determines the maximum value and the stable value of the pH from the change curve of the pH value of the CO2 conservation regeneration aggregate solution to be measured, and calculates the residual CO2 gas of the CO2 conservation regeneration aggregate sample to be measured according to the formula (1) Mass m CO2 :
  • m CO2 is the mass of residual CO 2 gas in the CO 2 curing recycled aggregate to be measured, the unit is g;
  • Vw is the initial volume of deionized water in the CO2 curing regeneration aggregate solution to be tested, and the unit is L.
  • the present invention provides a test device adopting the test method for the CO2 gas content of the residual CO2 in regenerated aggregates described in the above technical solution, comprising a test box 1 and an operating platform arranged on the inner bottom surface of the test box 1 8.
  • a test box 1 Set on the support 10 with chassis 9 on the operating table 8, the pH meter 11 set on the support 10, the container 12 set on the chassis 9, the container 12 set on the pH test Below the instrument 11, the first operation hole 3, the air inlet 4, the second operation hole 5 and the air outlet 6 arranged on the side wall of the test box 1 are arranged on the top cover of the test box 1 2.
  • the controller 7 arranged in the test box 1 .
  • the test device provided by the present invention includes a test box 1, and as a specific embodiment of the present invention, the test box 1 is in the shape of a cube.
  • the test device provided by the present invention comprises an operating table 8 arranged on the inner bottom surface of the test box 1, and a support 10 with a chassis 9 is arranged on the operating table 8.
  • the chassis 9 The chassis is electrically swivel.
  • the chassis 9 when the chassis 9 is an electric rotating chassis, it can be used to ensure the uniformity of the CO 2 curing recycled aggregate solution to be measured.
  • the test device provided by the present invention includes a pH meter 11 arranged on a support 10.
  • the pH meter 11 is a sustainable reading and high-precision pH tester, and the pH meter 11 is fixedly connected. on the bracket 10.
  • the pH meter is in signal connection with the processor.
  • the test device provided by the present invention includes a container 12 arranged on the chassis 9 , and the container 12 is arranged below the pH meter 11 .
  • the test device provided by the present invention includes a first operation hole 3 , an air inlet 4 , a second operation hole 5 and an air outlet 6 arranged on the side wall of the test box 1 .
  • the first operation hole 3 and the air inlet 4 are arranged on the side wall of the test box 1
  • the second operation hole 5 and the air outlet 6 are arranged on the first
  • the operation hole 3 and the air inlet hole 4 are arranged on the other side wall corresponding to the side wall.
  • operating gloves are sealed and connected to the first operating hole 3 and the second operating hole 5 .
  • the first operation hole 3 and the second operation hole 5 are used to mix the CO 2 -cured recycled aggregate sample to be tested with deionized water.
  • the air inlet hole 4 is higher than the air outlet hole 6 .
  • the test device provided by the present invention includes a bottom cover 2 arranged above the test box 1 , and as a specific embodiment of the present invention, the test box 1 and the top cover 2 are hermetically connected.
  • the test device provided by the present invention includes a controller 7 arranged in the test chamber 1.
  • the controller 7 is used to control the temperature in the test chamber 1 and the pressure of the shielding gas.
  • the protective gas is preferably nitrogen.
  • the test device shown in Figure 1 includes a test box 1, the top of the test box 1 is sealed with a top cover 2, wherein the first operating The hole 3 and the air inlet hole 4 are provided with a second operation hole 5 and an air outlet hole 6 on the other side wall; the above-mentioned first operation hole 3 and the second operation hole 5 are sealed and connected with operation gloves.
  • the height of the air inlet hole 4 is higher than the air outlet hole 6 .
  • the test box 1 is provided with a controller 7 and an operating table 8, the controller 7 is a controller 7 for controlling the temperature and the protective gas in the test box, and the operating table 8 is provided with a support with a chassis 9 10.
  • a pH meter 11 is fixed on the bracket 10, a container 12 is placed on the chassis 9, and the container 12 is placed below the pH meter 11.
  • the chassis 9 is an electric rotating chassis.
  • the pH meter 11 is a pH meter with continuous reading and high precision.
  • the test first place the container 12 filled with deionized water on the base 9, put the probe of the pH meter into the deionized water to test the initial pH, put the sample to be tested into the test box 1, seal the test box, and pass the controller 7. Purge with nitrogen, and adjust the test temperature to 23°C and air pressure to 101.3kPa. Put the sample to be tested into the container through the test operation gloves, and monitor the pH value of the CO2 curing recycled aggregate solution through the processor. In order to ensure the uniformity of the solution, the rotating base will rotate at a constant speed. When the pH of the solution remained constant, the test was terminated.
  • test steps are:
  • the content of residual CO 2 gas in the pores of CO 2 cured recycled aggregate was calculated by the change of pH value of the sample solution of CO 2 cured recycled aggregate. Due to the release of residual CO 2 gas, the pH of the 10-20mm particle size CO 2 curing recycled aggregate solution dropped from a maximum of 10.00 to 9.36, and the pH of the 5-10mm particle size CO 2 curing recycled aggregate solution dropped from a maximum value of 10.02 to 9.21.

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Abstract

一种CO 2养护再生骨料残余CO 2气体含量的测试方法及装置，该测试方法为首先将待测CO 2养护再生骨料样品和去离子水放入测试箱（1）内，然后用保护气体对密闭的测试箱（1）中的空气进行吹扫达到标准测试要求，使用pH计（11）测出容器（12）中去离子水的初始pH；将待测CO 2养护再生骨料样品和去离子水混合得到待测CO 2养护再生骨料溶液，用pH计（11）持续监测待测CO 2养护再生骨料溶液的pH值，由待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH的最大值与稳定值，根据公式计算待测CO 2养护再生骨料样品残余CO 2气体的质量。该测试方法简单，测试数据稳定可靠。

Description

二氧化碳养护再生骨料残余二氧化碳气体含量的测试方法及装置 技术领域
本发明涉及一种CO 2气体含量的测试方法，尤其涉及是一种CO 2养护再生骨料残余CO 2气体含量的测试方法及装置。
背景技术
随着城镇化的推进，老旧建筑物和基础设施的拆除产生了大量的废弃混凝土，其随意处置严重影响市容市貌，并污染环境和空气。利用废弃混凝土制备再生骨料，不仅可消纳废弃混凝土，而且可缓解天然砂石骨料日益紧缺的问题。但由于再生骨料表面附着多孔老砂浆，再生骨料吸水率高，压碎值大，较大程度限制了再生骨料在结构混凝土中的应用。
CO 2养护再生骨料，可显著提高再生骨料的物理力学性能；同时，以CO 2气体作为加速再生骨料碳化强化的养护原料气，可有效吸收钢铁、水泥等工业排放的CO 2废气，是一种环境友好的再生骨料强化方法。但用CO 2气体养护再生骨料，使再生骨料内部残留一定量的CO 2气体。
当利用CO 2养护再生骨料部分或全部置换天然骨料制备再生混凝土时，CO 2养护再生骨料残留的CO 2气体会对再生混凝土强度和耐久性产生两方面影响：1)CO 2养护再生骨料释放残留CO 2气体，继而养护再生混凝土，改善再生混凝土新界面过渡区微观结构，提高再生混凝土强度；2)CO 2养护再生骨料释放残留CO 2气体，进而降低再生混凝土pH值，加速埋置于再生混凝土内的钢筋腐蚀。因此，CO 2养护再生骨料中残余CO 2气体的含量的准确测定对预测以CO 2养护再生骨料制备得到的再生混凝土耐久性意义重大。
但是现有技术中缺少有效测量CO 2养护再生骨料残余CO 2气体含量的方法。
发明内容
有鉴于此，本发明提供了一种CO 2养护再生骨料残余CO 2气体含量的测试方法及装置，本发明提供的测试方法测试原理明确，测试方法简单，测试数据稳定可靠，从而填补该领域的空白。
本发明提供了一种CO 2养护再生骨料残余CO 2气体含量的测试方法，包括以下步骤：
1)称量待测CO 2养护再生骨料样品的质量，记为m 1，将所述待测CO 2养护再生骨料样品放入可密闭测试箱内，称取质量为m 2的去离子水置于容器中并放入可密闭测试箱内；
2)用保护气体对密闭测试箱中的空气进行吹扫，并对密闭测试箱的初始压力和初始温度进行调节，直至其达到并保持标准测试环境要求，所述标准测试环境要求为温度23℃±2℃，气压86kPa～106kPa。
3)测试容器中去离子水的初始pH值；
4)将待测CO 2养护再生骨料样品和去离子水混合得到待测CO 2养护再生骨料溶液，持续监测待测CO 2养护再生骨料溶液的pH值，将监测所得pH值数据同步存储于处理器中，直至pH值保持稳定时停止测试；
5)由待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH值的最大值与稳定值，并根据公式(1)计算待测CO 2养护再生骨料样品残余CO 2气体的质量m CO2：
Figure PCTCN2021126747-appb-000001
式(1)中：m CO2为待测CO 2养护再生骨料残余CO 2气体的质量，单位为g；
Figure PCTCN2021126747-appb-000002
为所述待测CO 2养护再生骨料溶液pH值最大时，所述待测CO 2养护再生骨料溶液OH -的摩尔数，单位为mol；
Figure PCTCN2021126747-appb-000003
为所述待测CO 2养护再生骨料溶液pH值稳定时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
V w为所述待测CO 2养护再生骨料溶液的去离子水初始体积，单位为L。
优选的，还包括步骤6)：通过平行测试，得到多组待测CO 2养护再生骨料样品残余CO 2气体质量m CO2，依据格拉布斯准则，剔除异常m CO2数据，得到有效m CO2测试数据，采用有效m CO2测试数据的平均值作为最终测试结果。
优选的，所述去离子水的pH值为6.7～7.2。
优选的，所述pH计的精度不低于0.01。
优选的，所述保护气体为氮气，所述氮气的纯度不低于99％。
本发明提供了一种采用如上述技术方案所述CO 2养护再生骨料残余CO 2气体含量的测试方法的测试装置，包括可密闭测试箱(1)，设置于所述测试箱(1)的内部底面上的操作台(8)，设置于所述操作台(8)上带底盘(9)的支架(10)，设置于所述支架(10)上的pH计(11)，设置于所述底盘(9)上的容器(12)，所述容器(12)设置于所述pH计(11)的下方，设置于所述测试箱(1)的侧壁上的第一操作孔(3)、进气孔(4)、第二操作孔(5)和出气孔(6)，设置于所述测试箱(1)的上方的顶盖(2)，设置于所述测试箱(1)内的控制器(7)。
优选的，所述第一操作孔(3)和所述第二操作孔(5)上均密封连接有操作手套。
优选的，所述进气孔(4)的高度高于出气孔(6)。
优选的，所述底盘(9)为电动旋转底盘，所述测试箱(1)和顶盖(2)密封连接。
优选的，所述pH计(11)为可持续测读且高精度的pH测试仪。
本发明提供了一种CO 2养护再生骨料残余CO 2气体含量的测试方法，包括以下步骤：1)称取质量为m 1的待测CO 2养护再生骨料样品放入测试箱内，称取质量为m 2的去离子水置于容器中并放入测试箱内；2)用保护气体对密闭的测试箱中的空气进行吹扫，并对密闭测试箱的初始压力和初始温度进行调节，直至其达到并保持标准测试环境要求，所述标准测试环境要求为温度23℃±2℃标准测试，气压86kPa～106kPa；3)使用pH计测得容器中去离子水的初始pH值；4)将待测CO 2养护再生骨料样品和去离子水混合得到待测CO 2养护再生骨料溶液，用pH计持续监测待测CO 2养护再生骨料溶液的pH值，并将pH值数据同步存储于处理器中，当pH值保持稳定时停止测试；5)由所述待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH的最大值与稳定值，并根据公式(1)计算待测CO 2养护再生骨料样品残余CO 2气体的质量m CO2：
Figure PCTCN2021126747-appb-000004
式(1)中：m CO2为待测CO 2养护再生骨料残余CO 2气体的质量，单位为g；
Figure PCTCN2021126747-appb-000005
为所述待测CO 2养护再生骨料溶液pH最大时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
Figure PCTCN2021126747-appb-000006
为所述待测CO 2养护再生骨料溶液pH稳定时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
V w为所述待测CO 2养护再生骨料溶液的去离子水初始体积，单位为L。
本发明提供的测试方法将待测CO 2养护再生骨料放入去离子水中，得到待测CO 2养护再生骨料溶液，一方面CO 2养护再生骨料因未完全碳化的碱性物质Ca(OH) 2溶解出OH -，使待测CO 2养护再生骨料溶液pH值增大；另一方面CO 2养护再生骨料内残留的CO 2气体释出并溶于水中，生成H +和HCO 3 -；H +和OH -反应降低待测CO 2养护再生骨料溶液的pH值，HCO 3 -与OH -进一步反应生成H 2O和CO 3 2，而CO 3 2与溶液中游离的Ca 2+反应生成CaCO 3，进一步降低待测CO 2养护再生骨料溶液的pH值。当CO 2养护再生骨料内残留CO 2气体消耗完后，待测CO 2养护再生骨料溶液pH值将趋于稳定。本发明通过测试CO 2养护再生骨料溶液pH的最大值与稳定值的差值，计算消耗H +的量，进而根据化学反应公式(2)和(3)计算出CO 2养护再生骨料的CO 2气体的残留量；
CO 2+H 2O＝2H ++CO 3 2-   (2)；
H ++OH -＝H 2O   (3)。
本发明提供的CO 2养护再生骨料残余CO 2气体含量的测试方法，测试原理明确，测试方法简单，测试数据稳定可靠。
本发明提供了一种采用上述技术方案所述CO 2养护再生骨料残余CO 2气体含量的测试方法的测试装置，包括测试箱1，设置于所述测试箱1的内部底面上的操作台8，设置于所述操作台8上带底盘9的支架10，设置于所述支架10上的pH计11，设置于所述底盘9上的容器12，所述 容器12设置于所述pH计11的下方，设置于所述测试箱1的侧壁上的第一操作孔3、进气孔4、第二操作孔5和出气孔6，设置于所述测试箱1上方的顶盖2，设置于所述测试箱1内的控制器7。
本发明提供的测试设备操作简单，测试数据稳定可靠。从而填补该领域的空白。
说明书附图
图1为实施例1的CO 2养护再生骨料残余CO 2气体含量的测试装置的结构示意图；
图2为实施例1的再生骨料(未CO 2养护)溶液pH值；
图3为实施例1的CO 2养护再生骨料溶液pH值；
图1中：测试箱1、顶盖2、第一操作孔3、进气孔4、第二操作孔5、出气孔6、控制器7、操作台8、底盘9、支架10、pH计11、容器12。
具体实施方式
本发明提供了一种CO 2养护再生骨料残余CO 2气体含量的测试方法，在于，包括以下步骤：
1)称取质量为m 1的待测CO 2养护再生骨料样品放入测试箱内，称取质量为m 2的去离子水置于容器中并放入测试箱内；
2)用保护气体对密闭的测试箱中的空气进行吹扫，并对密闭测试箱的初始压力和初始温度进行调节，直至其达到并保持标准测试环境要求，所述标准测试环境要求为温度23℃±2℃，气压86kPa～106kPa；
3)使用pH计测出容器中去离子水的初始pH；
4)将待测CO 2养护再生骨料样品放入去离子水中得到待测CO 2养护再生骨料溶液，用pH计持续监测待测CO 2养护再生骨料溶液的pH值，并将pH值数据同步存储于处理器中，当pH值保持稳定时停止测试；
5)由所述待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH的最大值与稳定值，并根据公式(1)计算待测CO 2养护再生骨料样品残余CO 2气体的质量m CO2：
Figure PCTCN2021126747-appb-000007
式(1)中：m CO2为待测CO 2养护再生骨料残余CO 2气体的质量，单位为g；
Figure PCTCN2021126747-appb-000008
为所述待测CO 2养护再生骨料溶液pH最大时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
Figure PCTCN2021126747-appb-000009
为所述待测CO 2养护再生骨料溶液pH稳定时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
V w为所述待测CO 2养护再生骨料溶液的去离子水初始体积，单位为L。
在本发明中，所述待测CO 2养护再生骨料样品的粒径优选为0.15～20mm。
在本发明中，所述待测CO 2养护再生骨料样品的制备方法优选包括以下步骤：
将再生骨料和CO 2养护气体进行碳化反应，得到待测CO 2养护再生骨料样品。
本发明所述再生骨料包括由废弃混凝土和废弃砂浆破碎所得再生粗骨料和再生细骨料。在本发明中，所述再生骨料样品的粒径优选为0.15～20mm。本发明对所述CO 2养护的压力、温度和CO 2气体体积浓度没有特殊要求。在本发明中，所述CO 2养护优选在密闭环境中进行。
在本发明中，所述CO 2养护再生骨料的碳化反应为：再生骨料表层砂浆中的水化产物与CO 2气体发生碳化反应。在本发明中，所述碳化反应的化学反应方程如式(4)～式(7)所示：
Ca(OH) 2+CO 2→CaCO 3+H 2O(4)；
3CaO·2SiO 2·3H 2O+3CO 2→3CaCO 3+2SiO 2·3H 2O(5)；
3CaO·Al 2O 3·3CaSO 4·32H 2O+3CO 2→Al 2O 3·xH 2O+3(CaSO 4·2H 2O)+3CaCO 3+(26-x)H 2O(6)；
3CaO·Al 2O 3·CaSO 4·18H 2O+3CO2→Al 2O 3·xH 2O+CaSO 4·2H2O+3CaCO 3+(16-x)H 2O(7)。
本发明称取质量为m 1的待测CO 2养护再生骨料样品放入测试箱内，称取质量为m 2的去离子水置于容器中并放入测试箱内。
在本发明中，所述水去离子的pH值优选为6.7～7.2，更优选为7。
在本发明中，所述待测CO 2养护再生骨料样品和去离子水的质量比优选为5:4。
本发明用保护气体对密闭测试箱中的空气进行吹扫，并对密闭测试箱的初始压力和初始温度进行调节，直至其达到并保持标准测试环境要求，所述标准测试环境要求为温度23℃±2℃，气压86kPa～106kPa。
在本发明中，所述保护气体优选为氮气，所述氮气的纯度优选为99.99％。
本发明使用pH计测出容器中水的初始pH。
在本发明中，所述pH计的精度优选不低于0.01。
本发明将待测CO 2养护再生骨料样品和去离子水混合得到待测CO 2养护再生骨料溶液，用pH计持续监测待测CO 2养护再生骨料溶液的pH值，并将pH值数据同步存储于处理器中，当pH值保持稳定时停止测试。
本发明将待测CO 2养护再生骨料样品和去离子水混合时优选将所述测CO 2养护再生骨料样品放入去离子水中。
本发明由所述待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH的最大值与稳定值，并根据公式(1)计算待测CO 2养护再生骨料样品残余CO 2气体的质量m CO2：
Figure PCTCN2021126747-appb-000010
式(1)中：m CO2为待测CO 2养护再生骨料残余CO 2气体的质量，单位为g；
Figure PCTCN2021126747-appb-000011
为所述待测CO 2养护再生骨料溶液pH最大时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
Figure PCTCN2021126747-appb-000012
为所述待测CO 2养护再生骨料溶液pH稳定时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
V w为所述待测CO 2养护再生骨料溶液的去离子水初始体积，单位为L。
本发明提供了一种采用上述技术方案所述的CO 2养护再生骨料残余 CO 2气体含量的测试方法的测试装置，包括测试箱1，设置于所述测试箱1的内部底面上的操作台8，设置于所述操作台8上带底盘9的支架10，设置于所述支架10上的pH计11，设置于所述底盘9上的容器12，所述容器12设置于所述pH测试仪11的下方，设置于所述测试箱1的侧壁上的第一操作孔3、进气孔4、第二操作孔5和出气孔6，设置于所述测试箱1的上方的顶盖2，设置于所述测试箱1内的控制器7。
本发明提供的测试装置包括测试箱1，作为本发明的一个具体实施例，所述测试箱1为立方体形。
本发明提供的测试装置包括设置于所述测试箱1的内部底面上的操作台8，所述操作台8上设置带底盘9的支架10，作为本发明的一个具体实施例，所述底盘9为电动旋转底盘。在本发明中，所述底盘9为电动旋转底盘时，能够用于确保所述待测CO 2养护再生骨料溶液的均匀性。
本发明提供的测试装置包括设置于支架10的pH计11，作为本发明的一个具体实施例，所述pH计11为可持续测读且高精度的pH测试仪，所述pH计11固定连接在所述支架10上。在本发明中，所述pH计与处理器信号连接。
本发明提供的测试装置包括设置于所述底盘9上的容器12，所述容器12设置于所述pH计11的下方。
本发明提供的测试装置包括设置于测试箱1的侧壁上的第一操作孔3、进气孔4、第二操作孔5和出气孔6。作为本发明的一个具体实施例，所述第一操作孔3和进气孔4设置于所述测试箱1的一侧壁上，所述第二操作孔5和出气孔6设置于与第一操作孔3和进气孔4设置的侧壁相对应的另一侧壁上。
作为本发明的一个具体实施例，所述第一操作孔3和所述第二操作孔5上均密封连接有操作手套。所述第一操作孔3和所述第二操作孔5用于将所述待测CO 2养护再生骨料样品和去离子水混合。
作为本发明的一个具体实施例，所述进气孔4的高度高于出气孔6。
本发明提供的测试装置包括设置于所述测试箱1上方的底盖2，作为本发明的一个具体实施例，所述测试箱1和顶盖2密封连接。
本发明提供的测试装置包括设置于所述测试箱1内的控制器7，作为 本发明的一个具体实施例，所述控制器7用于控制测试箱1内的温度和保护气体的压力，在本发明中，所述保护气体优选为氮气。
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
采用图1所示的测试装置进行测试，其中，图1所示的测试装置，包括测试箱1，所述测试箱1的上方密封连接有顶盖2，其中一侧壁上设有第一操作孔3和进气孔4，另一侧壁上设有第二操作孔5和出气孔6；上述第一操作孔3和第二操作孔5上均密封连接有操作手套。所述进气孔4的高度要高于出气孔6。所述测试箱1内设有控制器7和操作台8，所述控制器7是用于控制测试箱内温度和保护气体的控制器7，所述操作台8上设有带底盘9的支架10，所述支架10上固定有pH计11，所述底盘9上放置有容器12，上述pH计11下方为容器12。所述底盘9为电动旋转底盘。所述pH计11为可持续测读且高精度的pH计。
测试时，首先将装有去离子水的容器12放在底座9上，将pH计探头放入去离子水中测试初始pH，将待测样品放入测试箱1内后密封测试箱，通过控制器7用氮气吹扫，并调节试验要求温度23℃和气压101.3kPa。通过试验操作手套将待测样品放入容器内，通过处理器监测CO 2养护再生骨料溶液pH值。为保证溶液的均匀性，旋转底座将匀速转动。当溶液pH保持恒定，结束测试。
测试步骤为：
取4组试样，分别为粒径为5～10mm、10～20mm的再生骨料(未CO 2养护)，粒径为5～10mm、10～20mm的CO 2养护再生骨料。
每组骨料各取200g，并将160g(160mL)去离子水加到容器内，用pH计测得去离子水的初始pH，后将再生骨料放入容器，再次用pH计监测并存储待测样品溶液的pH值，pH值测量结果如图2、图3所示。
由图2可见，再生骨料(未CO 2养护)的两种粒径样品的pH在初期急剧上升，之后随时间增长而缓慢增大，最后趋于稳定，这主要归因于再生 骨料附着砂浆中的Ca(OH) 2等碱性物质不断释出OH -所致。
由图3可见，在3min时，CO 2养护再生骨料的两组溶液pH达到最大值，两种粒径CO 2养护再生骨料溶液的pH值基本相等，为10左右；随后，两者的pH值随时间的增长而降低，并趋于稳定。与再生骨料(未CO 2养护)溶液pH值曲线(图2)对比，CO 2养护再生骨料溶液pH曲线下降的原因是CO 2养护再生骨料孔隙中残留的CO 2气体溶于去离子水中，降低了溶液的pH。在溶液静置24h时，5～10mm和10～20mm两种粒径的CO 2养护再生骨料样品溶液pH值分别为9.21和9.36。
通过CO 2养护再生骨料样品溶液pH值的变化来计算CO 2养护再生骨料孔隙中残留CO 2气体的含量。因残留CO 2气体的释出，10～20mm粒径CO 2养护再生骨料溶液的pH由最大值10.00下降至9.36，5～10mm粒径CO 2养护再生骨料溶液pH由最大值10.02下降至9.21。
a)粒径为10～20mmCO 2养护再生骨料残留CO 2气体计算：
pH值为10时，OH -的浓度为1×10 -4mol/L，pH为9.36时，OH -的浓度为1×10 -4.64mol/L，则此过程消耗的OH -为：
(1×10 -4-1×10 -4.64)×0.16＝1.233×10 -5mol，
依据化学反应方程式(2)和(3)计算残留CO 2气体含量：
H ++OH -＝H 2O   (3)；
CO 2+H 2O＝2H ++CO 3 2-   (2)；
消耗的CO 2质量m CO2＝0.617×10 -5mol×44g/mol＝0.271×10 -3g，因CO 2气体在23℃和101.3kPa大气压下的密度为ρ CO2＝1.810g/L，故消耗的CO 2气体体积为：
V CO2＝0.271×10 -3g÷1.810g/L＝0.150mL；
则每千克10～20mmCO 2养护再生骨料残留CO 2气体为0.750mL或1.355×10 -3g。
b)粒径为5～10mmCO 2养护再生骨料残留CO 2气体计算
pH值为10.02时，OH -浓度为1×10 -3.98mol/L，pH为9.19时，OH -浓度为1×10 -4.81mol/L，消耗的OH -为：
(1×10 -3.98-1×10 -4.81)×0.16＝1.428×10 -5mol
则依据化学反应方程式(2)(3)计算残留CO2气体含量：
H ++OH -＝H 2O；
CO 2+H 2O＝2H ++CO 3 2-；
则消耗CO 2质量为m CO2＝0.714×10 -5mol×44g/mol＝0.314×10 -3g。因CO 2气体在23℃和101.3kPa大气压下的密度为ρ CO2＝1.810g/L，故消耗的CO 2气体体积为：
V CO2＝0.314×10 -3g÷1.810g/L＝0.173ml
则每千克5～10mm碳化再生骨料残留CO 2气体为0.867ml或1.57×10 -3g。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

  1. 一种CO 2养护再生骨料残余CO 2气体含量的测试方法，包括以下步骤：
    1)称量待测CO 2养护再生骨料样品的质量，记为m 1，将所述待测CO 2养护再生骨料样品放入可密闭测试箱内，称取质量为m 2的去离子水置于容器中并放入可密闭测试箱内；
    2)用保护气体对密闭测试箱中的空气进行吹扫，并对密闭测试箱的初始压力和初始温度进行调节，直至其达到并保持标准测试环境要求，所述标准测试环境要求为温度23℃±2℃，气压86kPa～106kPa。
    3)测试容器中去离子水的初始pH值；
    4)将待测CO 2养护再生骨料样品和去离子水混合得到待测CO 2养护再生骨料溶液，持续监测待测CO 2养护再生骨料溶液的pH值，将监测所得pH值数据同步存储于处理器中，直至pH值保持稳定时停止测试；
    5)由待测CO 2养护再生骨料溶液pH值的变化曲线图，确定pH值的最大值与稳定值，并根据公式(1)计算待测CO 2养护再生骨料样品残余CO 2气体的质量m CO2：
    Figure PCTCN2021126747-appb-100001
    式(1)中：m CO2为待测CO 2养护再生骨料残余CO 2气体的质量，单位为g；
    Figure PCTCN2021126747-appb-100002
    为所述待测CO 2养护再生骨料溶液pH值最大时，所述待测CO 2养护再生骨料溶液OH -的摩尔数，单位为mol；
    Figure PCTCN2021126747-appb-100003
    为所述待测CO 2养护再生骨料溶液pH值稳定时，所述待测CO 2养护再生骨料溶液内OH -的摩尔数，单位为mol；
    V w为所述待测CO 2养护再生骨料溶液的去离子水初始体积，单位为L。
  2. 根据权利要求1所述的测试方法，其特征在于：还包括步骤6)：通过平行测试，得到多组待测CO 2养护再生骨料样品残余CO 2气体质量 m CO2，依据格拉布斯准则，剔除异常m CO2数据，得到有效m CO2测试数据，采用有效m CO2测试数据的平均值作为最终测试结果。
  3. 根据权利要求1所述的测试方法，其特征在于：所述去离子水的pH值为6.7～7.2。
  4. 根据权利要求1所述的测试方法，其特征在于：所述pH计的精度不低于0.01。
  5. 根据权利要求1所述的测试方法，其特征在于：所述保护气体为氮气，所述氮气的纯度不低于99％。
  6. 一种采用如权利要求1～5任一项所述CO 2养护再生骨料残余CO 2气体含量的测试方法的测试装置，其特征在于：包括可密闭测试箱(1)，设置于所述测试箱(1)的内部底面上的操作台(8)，设置于所述操作台(8)上带底盘(9)的支架(10)，设置于所述支架(10)上的pH计(11)，设置于所述底盘(9)上的容器(12)，所述容器(12)设置于所述pH计(11)的下方，设置于所述测试箱(1)的侧壁上的第一操作孔(3)、进气孔(4)、第二操作孔(5)和出气孔(6)，设置于所述测试箱(1)的上方的顶盖(2)，设置于所述测试箱(1)内的控制器(7)。
  7. 根据权利要求6所述的测试装置，其特征在于：所述第一操作孔(3)和所述第二操作孔(5)上均密封连接有操作手套。
  8. 根据权利要求6所述的测试装置，其特征在于：所述进气孔(4)的高度高于出气孔(6)。
  9. 根据权利要求6所述的测试装置，其特征在于：所述底盘(9)为电动旋转底盘，所述测试箱(1)和顶盖(2)密封连接。
  10. 根据权利要求3所述的测试装置，其特征在于：所述pH计(11)为可持续测读且高精度的pH测试仪。
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