CN114262173A - Preparation method of enhanced fly ash grinding aid - Google Patents
Preparation method of enhanced fly ash grinding aid Download PDFInfo
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- CN114262173A CN114262173A CN202111671343.7A CN202111671343A CN114262173A CN 114262173 A CN114262173 A CN 114262173A CN 202111671343 A CN202111671343 A CN 202111671343A CN 114262173 A CN114262173 A CN 114262173A
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- fly ash
- additive
- grinding aid
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- 239000010881 fly ash Substances 0.000 title claims abstract description 60
- 238000000227 grinding Methods 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 37
- 230000000996 additive effect Effects 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 235000019738 Limestone Nutrition 0.000 claims abstract description 11
- 239000010440 gypsum Substances 0.000 claims abstract description 11
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 11
- 239000006028 limestone Substances 0.000 claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 14
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 8
- -1 alcohol amine Chemical class 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000012024 dehydrating agents Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000004568 cement Substances 0.000 description 37
- 239000000463 material Substances 0.000 description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 15
- 239000002245 particle Substances 0.000 description 12
- 239000011575 calcium Substances 0.000 description 9
- 230000036571 hydration Effects 0.000 description 9
- 238000006703 hydration reaction Methods 0.000 description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005242 forging Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 150000003841 chloride salts Chemical class 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000002801 charged material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of an enhanced fly ash grinding aid, which comprises the following steps: the preparation method comprises the steps of preparing the additive A, preparing the additive B, mixing the additive A, the additive B, gypsum and limestone according to a certain proportion, and stirring to obtain the enhanced fly ash grinding aid.
Description
Technical Field
The invention belongs to the technical field of grinding aid preparation, and relates to a preparation method of an enhanced fly ash grinding aid.
Background
The cement grinding comprises two modes of separate grinding and mixed grinding, and the mixed grinding mode is commonly used at present. When mixed grinding is carried out, the performance of clinker cannot be fully exerted due to the difference of the abrasion resistance of the clinker and the mixed material in the cement, and the waste of resources is caused. In addition, when cement clinker and mixed materials are added into a mill together for grinding, the materials generate static electricity due to violent and frequent friction and impact between the materials and a grinding body, and the charged materials are adsorbed on the surfaces of steel balls and the grinding body, so that the cement mill has serious ball wrapping and forging phenomena, and the yield and the quality of cement are greatly reduced. In order to solve the problems, the conventional common method is a method for adding a cement grinding aid, the conventional cement grinding aid is mainly prepared by compounding triethanolamine and various chloride salts, the chloride salts have strong corrosivity, when the cement mixed with the cement grinding aid is used, the corrosion phenomenon to building steel can be greatly improved, the building strength is reduced, the service life of a building is greatly shortened, and meanwhile, the conventional grinding aid is low in activity, low in grinding efficiency and high in use cost in the use process.
Disclosure of Invention
The invention aims to provide a preparation method of an enhanced fly ash grinding aid.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of an enhanced fly ash grinding aid is characterized by comprising the following steps:
(1) mixing an alcohol amine internal compound and a carboxylic acid compound in a certain molar ratio in a distillation flask by using concentrated sulfuric acid as a catalyst, and reacting for 6-8h at a certain temperature;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) putting 20 meshes of fly ash into an ultrasonic stirrer, and adding a certain amount of Ca (OH) into the ultrasonic stirrer2And a certain amount of CaCO3；
(4) Adjusting the ultrasonic stirrer to keep the ultrasonic stirrer at a certain frequency, stirring for 3 hours at a certain temperature, and drying to obtain an additive B;
(5) and mixing the additive A, the additive B, gypsum and limestone according to a certain proportion, and stirring to obtain the enhanced fly ash grinding aid.
Further, the alcohol amine internal compound is triethanolamine, and the carboxylic acid compound is glacial acetic acid.
Further, the certain proportion in the step (1) is specifically 1:1, the certain temperature in the step (1) is specifically 130-140 ℃.
Further, the fly ash, Ca (OH) in the step (3)2And CaCO3The adhesive is specifically divided into the following components in parts by mass: 20 parts of fly ash and 40 parts of Ca (OH)2And 35 parts of CaCO3。
Further, the certain frequency in the step (4) is specifically 20-40KHz, and the certain temperature is specifically 20-30 ℃.
Further, the mass parts of the additive A, the additive B, the gypsum and the limestone in the step (5) are as follows: 5: 30: 5: 5.
the invention has the beneficial effects that:
the grinding aid prepared by the invention has high activity, greatly improves the grinding efficiency, ensures that the cement cannot be over-ground in the grinding process, and simultaneously has the phenomenon of ball wrapping and forging.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a flow chart of a preparation method of an enhanced fly ash grinding aid of the invention.
Detailed Description
Example 1: the preparation method of the enhanced fly ash grinding aid comprises the following steps:
(1) mixing triethanolamine and glacial acetic acid in a distillation flask according to a molar ratio of 1:1 by taking concentrated sulfuric acid as a catalyst, and reacting for 6-8h at the temperature of 130-;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) 20 parts of 20-mesh fly ash was put into an ultrasonic stirrer, and 40 parts of Ca (OH) was added to the ultrasonic stirrer2And 35 parts of CaCO3；
(4) Adjusting the ultrasonic mixer to keep the ultrasonic mixer at the frequency of 20-40KHz, stirring for 3h at the temperature of 20-30 ℃, and drying to obtain an additive B;
(5) and mixing 5 parts of additive A, 30 parts of additive B, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain the enhanced fly ash grinding aid.
Example 2:
(1) mixing triethanolamine and glacial acetic acid in a distillation flask according to a molar ratio of 1:1 by taking concentrated sulfuric acid as a catalyst, and reacting for 6-8h at the temperature of 130-;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) 20 parts of 20-mesh fly ash was put into an ultrasonic stirrer, and 40 parts of Ca (OH) was added to the ultrasonic stirrer2And 35 parts of CaCO3；
(4) Adjusting the ultrasonic mixer to keep the ultrasonic mixer at the frequency of 20-40KHz, stirring for 3h at the temperature of 20-30 ℃, and drying to obtain an additive B;
(5) and mixing 5 parts of additive A, 20 parts of additive B, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain the fly ash grinding aid.
Example 3:
(1) mixing triethanolamine and glacial acetic acid in a distillation flask according to a molar ratio of 1:1 by taking concentrated sulfuric acid as a catalyst, and reacting for 6-8h at the temperature of 130-;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) 20 parts of 20-mesh fly ash is put into an ultrasonic stirrer, and added into the ultrasonic stirrer40 parts of Ca (OH)2And 35 parts of CaCO3；
(4) Adjusting the ultrasonic mixer to keep the ultrasonic mixer at the frequency of 20-40KHz, stirring for 3h at the temperature of 20-30 ℃, and drying to obtain an additive B;
(5) and mixing 5 parts of additive A, 40 parts of additive B, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain the fly ash grinding aid.
Example 4:
(1) mixing triethanolamine and glacial acetic acid in a distillation flask according to a molar ratio of 1:1 by taking concentrated sulfuric acid as a catalyst, and reacting for 6-8h at the temperature of 130-;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) 20 parts of 20-mesh fly ash was put into an ultrasonic stirrer, and 40 parts of Ca (OH) was added to the ultrasonic stirrer2And 35 parts of CaCO3；
(4) Adjusting the ultrasonic mixer to keep the ultrasonic mixer at the frequency of 20-40KHz, stirring for 3h at the temperature of 20-30 ℃, and drying to obtain an additive B;
(5) and mixing 5 parts of additive A, 50 parts of additive B, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain the fly ash grinding aid.
Comparative example 1:
(1) mixing triethanolamine and glacial acetic acid in a distillation flask according to a molar ratio of 1:1 by taking concentrated sulfuric acid as a catalyst, and reacting for 6-8h at the temperature of 130-;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) mixing 5 parts of additive A, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain a grinding aid;
comparative example 2:
(1) 20 parts of 20-mesh fly ash was put into an ultrasonic stirrer, and 40 parts of Ca (OH) was added to the ultrasonic stirrer2And 35 parts of CaCO3；
(2) Adjusting the ultrasonic mixer to keep the ultrasonic mixer at the frequency of 20-40KHz, stirring for 3h at the temperature of 20-30 ℃, and drying to obtain an additive B;
(3) and mixing 20 parts of additive B, 5 parts of gypsum and 5 parts of limestone, and stirring to obtain the fly ash grinding aid.
Example 5:
(1) mixing 65 parts of cement clinker with the enhanced fly ash grinding aid prepared in example 1 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 1 sample;
(2) mixing 65 parts of cement clinker with the fly ash grinding aid prepared in example 2 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 2 sample;
(3) mixing 65 parts of cement clinker with the fly ash grinding aid prepared in example 3 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 3 sample;
(4) mixing 65 parts of cement clinker with the fly ash grinding aid prepared in example 4 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 4 sample;
(5) mixing 65 parts of cement clinker with the grinding aid prepared in the comparative example 1 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 5 sample;
(6) and mixing 65 parts of cement clinker with the fly ash grinding aid prepared in the comparative example 2 to prepare 3kg of material, and grinding the material in a phi 500mmX500mm standard experimental mill for 30min to obtain a No. 6 sample.
(7) The results of the stability, standard consistency, setting time and strength tests at 3d and 28d on samples Nos. 1-6 are as follows:
table 1: effect of grinding aid on Cement physical Properties
As can be seen from Table 1, after the grinding aid disclosed by the invention is used, the 45um screen residue is obviously reduced, which shows that the addition of the grinding aid disclosed by the invention reduces the content of particles, the grinding efficiency is greatly improved, the stability of cement is not influenced by the grinding aid disclosed by the invention, and the cement is ensured to have good stability;
as can be seen from Table 1, with the increase of the blending amount of the fly ash, the water consumption of the standard consistency is continuously increased, because the fly ash particles are much smaller than the cement particles, the moisture for wrapping the fly ash particles is naturally increased, and when the blending amount of the fly ash is increased, the moisture required for wrapping the fly ash particles is greatly more than the moisture which can be released by the water reducing effect of the fly ash particles, which is expressed as the increase of the water consumption of the standard consistency;
as can be seen from Table 1, the setting time of the cement paste is obviously prolonged along with the increase of the mixing amount of the fly ash, which shows that the mixing amount of the fly ash can delay the hydration of the cement, the setting time of the fly ash slurry with large mixing amount is longer, the fly ash replaces part of the cement in equal amount, the particles of the fly ash are relatively fine and are filled in the gaps of the cement particles, the contact between the cement particles and water and between the cement particles is reduced, the concentration of the cement is diluted, the less the amount of the cement is, the less the generated hydration products are, the setting of the cement is delayed, and simultaneously the fly ash can prevent C from being mixed with the cement3The hydration of A, soluble calcium ions in the fly ash are adsorbed on the surface of the aluminum-rich layer, so that the hydration activity of cement is reduced, the hydration speed is slowed, and the initial setting time and the final setting time of slurry are prolonged;
as can be seen from Table 1, with the increase of the amount of the fly ash, the early-stage reduction amplitude of the compressive strength of the cement mortar is increased, the later-stage reduction amplitude of the compressive strength is improved, and the influence on the flexural strength is relatively small. The reason is that after the fly ash replaces part of cement, the mineral proportion of cement clinker in the system is reduced, the effective water-cement ratio for controlling the hydration speed of the cement is relatively increased, and Ca in the solution2+The concentration is reduced, the total hydration speed in a cement-fly ash system is reduced, the connection between generated hydration product particles is not tight enough, and the early strength is correspondingly reduced, so that the early strength reduction amplitude is continuously increased along with the increase of the mixing amount of the fly ash, but the fly ash volcanic ash reaction is carried out in the later period, and the fly ash is subjected to the coal ash volcanic ash reactionThe filling effect and the micro-aggregate effect of the particles are exerted, so that the structure of the slurry tends to be compact, and the cross and connection degree among hydration products tend to be good, so that the reduction of the later strength is improved.
The grinding aid prepared by the method has high activity, greatly improves the grinding efficiency, prevents the cement from being over-ground in the grinding process, prevents the phenomenon of ball wrapping and forging, greatly reduces the using amount of the cement and reduces the construction cost.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A preparation method of an enhanced fly ash grinding aid is characterized by comprising the following steps:
(1) mixing an alcohol amine internal compound and a carboxylic acid compound in a certain molar ratio in a distillation flask by using concentrated sulfuric acid as a catalyst, and reacting for 6-8h at a certain temperature;
(2) recovering the dehydrating agent and unreacted raw materials by reduced pressure distillation to finally obtain an additive A;
(3) putting 20-mesh fly ash into an ultrasonic stirrer, and adding a certain amount of fly ash into the ultrasonic stirrer;
(4) adjusting the ultrasonic stirrer to keep the ultrasonic stirrer at a certain frequency, stirring for 3 hours at a certain temperature, and drying to obtain an additive B;
(5) and mixing the additive A, the additive B, gypsum and limestone according to a certain proportion, and stirring to obtain the enhanced fly ash grinding aid.
2. The preparation method of the enhanced fly ash grinding aid as claimed in claim 1, wherein the alcohol amine internal compound is triethanolamine and the carboxylic acid compound is glacial acetic acid.
3. The preparation method of the enhanced fly ash grinding aid according to claim 1, wherein a certain proportion in the step (1) is specifically 1:1, the certain temperature in the step (1) is specifically 130-140 ℃.
4. The preparation method of the enhanced fly ash grinding aid according to claim 1, wherein the fly ash in the step (3) and the additive are specifically divided into the following components in parts by mass: 20 parts of fly ash, 40 parts of fly ash and 35 parts of fly ash.
5. The preparation method of the enhanced fly ash grinding aid as claimed in claim 1, wherein the certain frequency in step (4) is specifically 20-40KHz, and the certain temperature is specifically 20-30 ℃.
6. The preparation method of the enhanced fly ash grinding aid according to claim 1, wherein the additive A, the additive B, the gypsum and the limestone in the step (5) are prepared in the following mass parts: 5: 30: 5: 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111671343.7A CN114262173A (en) | 2021-12-31 | 2021-12-31 | Preparation method of enhanced fly ash grinding aid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111671343.7A CN114262173A (en) | 2021-12-31 | 2021-12-31 | Preparation method of enhanced fly ash grinding aid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372409A (en) * | 2008-05-07 | 2009-02-25 | 赵洪义 | Solid non-chlorate cement grinding aid |
| CN102060462A (en) * | 2010-12-10 | 2011-05-18 | 山东宏艺科技股份有限公司 | Preparation method of enforced flyash cement grinding aid |
| CN102503218A (en) * | 2011-10-18 | 2012-06-20 | 沈阳建筑大学 | Enhanced powder cement grinding aid |
| CN112876125A (en) * | 2021-03-26 | 2021-06-01 | 唐山冀东水泥外加剂有限责任公司 | Cement grinding aid and high early strength cement using same |
-
2021
- 2021-12-31 CN CN202111671343.7A patent/CN114262173A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372409A (en) * | 2008-05-07 | 2009-02-25 | 赵洪义 | Solid non-chlorate cement grinding aid |
| CN102060462A (en) * | 2010-12-10 | 2011-05-18 | 山东宏艺科技股份有限公司 | Preparation method of enforced flyash cement grinding aid |
| CN102503218A (en) * | 2011-10-18 | 2012-06-20 | 沈阳建筑大学 | Enhanced powder cement grinding aid |
| CN112876125A (en) * | 2021-03-26 | 2021-06-01 | 唐山冀东水泥外加剂有限责任公司 | Cement grinding aid and high early strength cement using same |
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