CN101294942A - Method and device for measuring free calcium oxide in cement or coal ash by microwave heating - Google Patents
Method and device for measuring free calcium oxide in cement or coal ash by microwave heating Download PDFInfo
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- CN101294942A CN101294942A CNA2008101500254A CN200810150025A CN101294942A CN 101294942 A CN101294942 A CN 101294942A CN A2008101500254 A CNA2008101500254 A CN A2008101500254A CN 200810150025 A CN200810150025 A CN 200810150025A CN 101294942 A CN101294942 A CN 101294942A
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- calcium oxide
- free calcium
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- flyash
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Abstract
The invention discloses a method and device for measuring free calcium oxide in cement or fly ash by microwave heating; the method comprises the following steps: the cement or the fly ash and a free calcium oxide dissolving-out agent are placed in a ground conical flask; after the refluxing heating is carried out in a microwave oven, the free calcium oxide is dissolved out, and the content of the free calcium oxide in the sample is finally determined by dipping benzoic acid standard solution; the device comprises that: a heating power knob and a heating time knob are connected with the microwave oven, the internal cavity of the microwave oven is provided with the conical flask, a condensing tube is inserted into the upper end of the conical flask, the upper end of the condensing tube is communicated with a circulating cooling water tank, the lower end thereof is communicated with a circulating pump, and the internal cavity of the conical flask is provided with the cement or the fly ash sample and free calcium oxide dissolving-out medium; by adopting the microwave oven as a heating source, the heating speed is fast, the heating is started from the inner part of the solution with convenient operation, the dissolving-out speed of the free calcium oxide is obviously improved, the dissolving-out times are reduced, the measuring speed is improved, the microwave heating has high heat efficiency and can save energy and the device has long service life.
Description
Technical field
The present invention relates to the free calcium oxide content in cement, the flyash is carried out method for measuring and device, be specifically related to method and device that free calcium oxide in cement or the flyash is measured in microwave heating.
Background technology
As everyone knows, free calcium oxide in the cement is related to cement and concrete volume stability problem, is the project of strict control in the technology of producing cement national standard, therefore in cement production process, the mensuration of free calcium oxide content is indispensable test item in the cement clinker.
And in the high-calcium fly ass of calcium oxide content greater than 10% (weight), the existence of free calcium oxide is for the application of high-calcium fly ass in cement and concrete brings hidden danger.According to the technical standard of the relevant high-calcium fly ass of country, most of high-calcium fly ass can not directly add in cement or the concrete and uses, and need carry out modification to high-calcium fly ass and handle.Therefore need before high-calcium fly ass uses in construction work the content of free calcium oxide in the high-calcium fly ass is measured.
The fast measuring of free calcium oxide for timely control cement quality, forecasts that in advance soundness of cement is significant, also has realistic meanings for the processing modified production of high-calcium fly ass.According to the characteristics and the requirement of actual production process, The faster the better for free calcium oxide mensuration.
The mensuration of free calcium oxide has glycerine-Ethanol Method, ethylene glycol-Ethanol Method etc. in traditional cement or the flyash.All be traditional type of heating in all free calcium oxide assay methods, the outstanding problem that exists is that measuring speed is slow, electrical heating wire is short serviceable life, the free calcium oxide dissolution efficiency is low, because measuring speed is slow, can not measure synchronously with producing, after often causing product to form, its testing result just can be come out, and is late testing result, can not in time adjust some composition for flow production line and brings irremediable defective.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can improve firing rate, accelerate the dissolution rate and the dissolution rate of free calcium oxide, just in minutes can detect the content of free calcium oxide, the method for free calcium oxide in cement or the flyash is measured in the microwave heating that can adjust the product composition at any time.
Another object of the present invention provides a kind of fast detecting and goes on a tour from the device of calcium oxide content.
In order to overcome the deficiencies in the prior art, technical scheme of the present invention is to solve like this: the method for free calcium oxide in cement or the flyash is measured in a kind of microwave heating, its special character is load weighted cement or flyash 0.3 gram～0.5 gram together are loaded in the ground conical flask for 15 milliliters～22 milliliters with free calcium oxide stripping agent mixed liquor, after backflow is heated in micro-wave oven, 2～5 minutes heat time heating times, by the benzoic acid standard solution titration, finally determine the content of the free calcium oxide in the sample after the free calcium oxide stripping.
The method of free calcium oxide in cement or the flyash is measured in described microwave heating, it is characterized in that described free calcium oxide stripping agent is glycerine or ethylene glycol, or ethylene glycol-alcohol mixture, preferentially select for use ethylene glycol-alcohol mixture to mix according to 2: 1 volume ratio.
At least 450 watts of described microwave heating power selection, 3～4 minutes heat time heating times; Cement or flyash sample weight are 0.4065 gram～0.4542 gram; 18 milliliters～20 milliliters of the mixed liquors of ethylene glycol-ethanol.
After the described free calcium oxide process microwave heating stripping, determine the content of free calcium oxide in the sample or adopt conductance measurement or additive method to determine the content of free calcium oxide after the titration of employing standard benzoic acid solution.
The device of the method for free calcium oxide in microwave heating fast measuring cement or the flyash, comprise be respectively arranged with on the micro-wave oven heating power knob and heat time heating time knob, its special character is that microwave cavity is equipped with conical flask, a condenser pipe is inserted in the upper end of described conical flask, its condenser pipe upper end is connected with the recirculated cooling water case, its lower end and water circulating pump are connected, and the conical flask inner chamber is equipped with cement or flyash sample and free calcium oxide dissolution medium.
The method and apparatus of free calcium oxide is based on microwave free calcium oxide dissolution medium such as glycerine, ethylene glycol in cement and the flyash are had strong absorption is ultimate principle in a kind of microwave heating fast measuring cement or the flyash, basically do not change the dissolution medium of traditional free calcium oxide, adopt the method for microwave heating, when greatly having accelerated firing rate, under microwave action, the dissolution rate of calcium oxide is also accelerated simultaneously, finally realizes the fast measuring of free calcium oxide in cement or the flyash.
Characteristics of the present invention are:
At first the present invention adopt micro-wave oven be the heating thermal source, firing rate is fast, is traditional more than ten times of type of heating firing rate.
Secondly, because laboratory glass wares are little to microwave absorbing, heating of the present invention is inner from solution, and the glass container temperature is lower, does not have the problem that adds thermo-lag after stopping to heat, and is easy to operate.And traditional heating is first heating glass container, again by the liquid in the glass container heating glass container, makes the glass container temperature be higher than the liquid in container temperature, and exists and significantly to add thermal hysteresis, is awkward unfavorable mensuration.
The 3rd, under microwave action and do not have in the ethylene glycol of the same temperature of microwave action or glycerine stripping cement or the flyash free calcium oxide compare, under microwave action, the free calcium oxide dissolution rate obviously improves, and this is for reducing the stripping number of times, and it is significant to improve finding speed.
The 4th, microwave heating thermal efficiency height, energy-conservation than classic method, the device long service life.
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention.
Embodiment
Accompanying drawing is embodiments of the invention
Below in conjunction with drawings and Examples content of the present invention is described further:
Its concrete grammar is undertaken by following step:
(1) preparation of dissolution fluid
The dissolution fluid of free calcium oxide can adopt the potpourri of glycerine, ethylene glycol or ethylene glycol ethanol in cement or the flyash, and is consistent with traditional free calcium oxide dissolution medium.Usually adopt ethylene glycol-alcohol mixeding liquid, mix the back according to 2: 1 volume ratios and use;
(2) load weighted cement or flyash 0.3 gram～0.5 gram sample are placed the flask (or ground conical flask) that has ground, ethylene glycol-the alcohol mixeding liquid of adding prior process naoh treatment and adding indicator is 18 milliliters～22 milliliters then, and the ground flask is placed in the household microwave oven hall.At family expenses micro-wave oven top drilling, the glass serpentine condenser therefrom passes the ground flask interior with placing the micro-wave oven hall and is connected;
(3) set 2～5 minutes heat time heating times, heating power is opened microwave heating greater than 450 watts, after heating finishes automatically, takes out the ground flask, uses the benzoic acid standard solution titration;
(4) the consumer product by the benzoic acid standard solution calculate sample go out in the content of free calcium oxide.
Shown in accompanying drawing 1, device comprise be connected with respectively on the micro-wave oven 8 heating power knob 4 and heat time heating time knob 5, be equipped with conical flask 7 on the supporter 6 of microwave cavity, a condenser pipe 1 is inserted in the upper end of described conical flask 7, its condenser pipe 1 upper end and recirculated cooling water case 2 is connected, its lower end and water circulating pump 3 are connected, conical flask 7 inner chambers are equipped with cement or flyash sample and free calcium oxide dissolution medium.Water circulating pump 3 provides recirculated water for reflux condensing tube 1, realizes the purpose of condensation.
After heating finishes, utilize the benzoic acid standard solution to carry out the free calcium oxide Determination on content and calculate.
Embodiment 1:
Getting the cement fineness is 10.4% (85 tm screen tail over) 0.4065 gram, add 20 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 70% of one kilowatt of microwave power, by microwave heating 3 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 3.54%, the standard method error is-0.01%.
Embodiment 2:
Getting the cement fineness is 10.4% (85 tm screen tail over) 0.4143 gram, add 20 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 50% of one kilowatt of microwave power, heated 4 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 3.56%, the standard method error is+0.01%.
Embodiment 3:
Getting the cement fineness is 10.4% (85 tm screen tail over) 0.4542 gram, add 20 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 100% of one kilowatt of microwave power, heated 2 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 3.54%, the standard method error is-0.01%.
Embodiment 4:
Getting fineness of pulverized-coal ash is 18.3% (85 tm screen tail over) 0.4434 gram, add 20 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 100% of one kilowatt of microwave power, heated 2 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 2.36%, the standard method error is-0.02%.
Embodiment 5:
Getting fineness of pulverized-coal ash is 18.3% (85 tm screen tail over) 0.4748 gram, add 20 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 80% of one kilowatt of microwave power, heated 4 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 2.38%, the standard method error is-0.00%.
Embodiment 6:
Getting fineness of pulverized-coal ash is 18.3% (85 tm screen tail over) 0.4089 gram, add 15 milliliters of ethylene glycol-ethanolic solutions, after placing the ground conical flask, select 50% of one kilowatt of microwave power, heated 5 minutes, back standard benzoic acid solution titration, recording free calcium oxide content is 2.37%, the standard method error is-0.01%.
Claims (4)
1, the method for free calcium oxide in cement or the flyash is measured in a kind of microwave heating, it is characterized in that carrying out according to the following steps:
1., be that 0.3 gram～0.5 gram together is loaded in the ground conical flask for 15 milliliters～22 milliliters with free calcium oxide stripping agent mixed liquor with load weighted cement or flyash sample weight, described free calcium oxide stripping agent is glycerine or ethylene glycol, or ethylene glycol-alcohol mixture, preferentially select ethylene glycol-alcohol mixture for use;
2., after the heating that in micro-wave oven, refluxes, be 2～5 minutes its heat time heating time;
3., treat to pass through the benzoic acid standard solution titration after the free calcium oxide stripping content of the free calcium oxide in finally definite sample.
2, the method for free calcium oxide in cement or the flyash is measured in microwave heating according to claim 1, at least 450 watts of the microwave heating power selection of the heating that it is characterized in that refluxing in the micro-wave oven, 3～4 minutes heat time heating times; Cement or flyash sample weight are 0.4065 gram～0.4542 gram; 18 milliliters～20 milliliters of the mixed liquors of ethylene glycol-ethanol.
3, the method for free calcium oxide in cement or the flyash is measured in microwave heating according to claim 1, after it is characterized in that free calcium oxide is through the microwave heating stripping, determine the content of free calcium oxide in the sample or adopt conductance measurement or additive method to determine the content of free calcium oxide after the titration of employing standard benzoic acid solution.
4, the device of the method for free calcium oxide in a kind of claim 1 described microwave heating fast measuring cement or the flyash, comprise and be respectively arranged with heating power knob (4) and knob heat time heating time (5) on the micro-wave oven (8), it is characterized in that being equipped with on micro-wave oven (8) the inner chamber supporter (6) conical flask (7), a condenser pipe (1) is inserted in the upper end of described conical flask (7), its condenser pipe (1) upper end is connected with recirculated cooling water case (2), its lower end and water circulating pump (3) are connected, and conical flask (7) inner chamber is equipped with cement or flyash sample and free calcium oxide dissolution medium.
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| CN2008101500254A CN101294942B (en) | 2008-06-10 | 2008-06-10 | Method and device for measuring free calcium oxide in cement or coal ash by microwave heating |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010063144A1 (en) * | 2008-12-02 | 2010-06-10 | 浙江泰德新材料有限公司 | Microwave heater and its application in chemical reaction |
| CN102401822A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Determination method of free calcium oxide in furnace slag |
| CN102507546A (en) * | 2011-09-28 | 2012-06-20 | 吉林恒联精密铸造科技有限公司 | Method for detecting content of calcium oxide in limestone |
| CN104198651A (en) * | 2014-09-09 | 2014-12-10 | 青岛润鑫伟业科贸有限公司 | Method for determining free calcium oxide in cement |
| CN105738560A (en) * | 2016-04-18 | 2016-07-06 | 河北钢铁股份有限公司 | Method for measuring content of calcium oxide in calcium-containing alloy |
| CN105891197A (en) * | 2014-12-01 | 2016-08-24 | 登封市嵩基水泥有限公司 | Method for measuring free calcium by using potassium nitrate to replace strontium nitrate as catalyst |
| CN113588399A (en) * | 2021-07-29 | 2021-11-02 | 宝武集团环境资源科技有限公司 | Quick digestion method for free calcium oxide in metallurgical dust and mud |
| CN113800841A (en) * | 2021-09-16 | 2021-12-17 | 四川杭加坤正新型材料有限公司 | Lime-free aerated concrete product and production method thereof |
-
2008
- 2008-06-10 CN CN2008101500254A patent/CN101294942B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010063144A1 (en) * | 2008-12-02 | 2010-06-10 | 浙江泰德新材料有限公司 | Microwave heater and its application in chemical reaction |
| AU2008364687B2 (en) * | 2008-12-02 | 2011-12-08 | Beijing Sijiantong Technology & Development Co., Ltd | Microwave heater and its application in chemical reaction |
| US8946605B2 (en) | 2008-12-02 | 2015-02-03 | Zhejiang Twrd New Material Co., Ltd. | Microwave heating device and its application in chemical reactions |
| CN102401822A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Determination method of free calcium oxide in furnace slag |
| CN102507546A (en) * | 2011-09-28 | 2012-06-20 | 吉林恒联精密铸造科技有限公司 | Method for detecting content of calcium oxide in limestone |
| CN104198651A (en) * | 2014-09-09 | 2014-12-10 | 青岛润鑫伟业科贸有限公司 | Method for determining free calcium oxide in cement |
| CN105891197A (en) * | 2014-12-01 | 2016-08-24 | 登封市嵩基水泥有限公司 | Method for measuring free calcium by using potassium nitrate to replace strontium nitrate as catalyst |
| CN105738560A (en) * | 2016-04-18 | 2016-07-06 | 河北钢铁股份有限公司 | Method for measuring content of calcium oxide in calcium-containing alloy |
| CN113588399A (en) * | 2021-07-29 | 2021-11-02 | 宝武集团环境资源科技有限公司 | Quick digestion method for free calcium oxide in metallurgical dust and mud |
| CN113800841A (en) * | 2021-09-16 | 2021-12-17 | 四川杭加坤正新型材料有限公司 | Lime-free aerated concrete product and production method thereof |
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|---|---|
| CN101294942B (en) | 2010-11-17 |
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