CN106380110A - Graphene oxide modified cement grinding aid and preparation method thereof - Google Patents
Graphene oxide modified cement grinding aid and preparation method thereof Download PDFInfo
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- CN106380110A CN106380110A CN201610801348.XA CN201610801348A CN106380110A CN 106380110 A CN106380110 A CN 106380110A CN 201610801348 A CN201610801348 A CN 201610801348A CN 106380110 A CN106380110 A CN 106380110A
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- grinding aid
- graphene oxide
- cement grinding
- cement
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- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/52—Grinding aids; Additives added during grinding
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a graphene oxide modified cement grinding aid. The graphene oxide modified cement grinding aid comprises, by weight, 35-55% of polymeric polylol, 2-5% of acrylate, 3-6% of aminopolyethylene glycol, 1-3% of tetraisopropyl titanate, 3-8% of a polycarboxylate superplasticizer, 1-2% of sodium dodecyl benzene sulfonate, 1-2% of polyoxyethylene fatty alcohol sodium sulfate, 5-10% of triethanolamine, 5-10% of triisopropanolamine, 1-5% of an aqueous solution of graphene oxide, and the balance of industrial wastewater. The invention also relates to a preparation method of the grinding aid. The graphene oxide is used to modify the cement grinding aid, the milling efficiency is substantially improved when the admixture of the graphene oxide is small, and milled cement particles have large specific surface area and small residue on sieve; the graphene oxide modified cement grinding aid substantially enhances the early strength of cement; ground cement has excellent adaptability to a water reducer; and the graphene oxide modified cement grinding aid effectively utilizes industrial wastewater, is friendly to environment, and has no pollution.
Description
Technical field
The invention belongs to the technical field of construction material and in particular to a kind of graphene oxide modification cement grinding aid and its
Preparation method.
Background technology
Since 21 century, China's economic development is rapid, which also promotes the development of building industry and its related industry, and China becomes
For manufacture of cement first big country.There is substantial amounts of power consumption, wherein to account for manufacture of cement total for grinding pow consumption in cement production process
2/3rds of power consumption, energy utilization rate is low, serious waste of resources.Therefore, improving mill efficiency is manufacture of cement energy-conservation of consumption reduction
Key.Cement grinding aid is a kind of raising grinding efficiency, improves material grindability energy in manufacture of cement, and addition content is little
A kind of chemical addition agent of organic or inorganic.During finished ground cement, grinding aid can significantly improve mill efficiency, substantially reduces
Grinding pow consumption, improves fineness and the specific surface area of cement.Meanwhile, grinding aid can also improve the early strength of cement, is not damaging
On the basis of cement self performance, reduce manufacture of cement cost, improve manufacture of cement efficiency.Clinker and other mixing materials exist
In grinding machine powder process, with grain refine, the increase of cement granules specific surface area is electrically charged because of scission of link, mutually adsorbs between granule
Produce and reunite, so that mill efficiency is greatly reduced.Grinding aid acts between the granule of cement material, reduces the surface energy of particle,
Its principle is to prevent particle aggregation, improves its mobility, improves mill efficiency, thus energy-saving and emission-reduction.At present, used by cement plant
Grinding aid is generally alcohol-based liquid grinding aid.
Currently, nearly 7,000,000 tons of the annual discharge of wastewater of China, centralized pollution control wastewater discharge is only 0.4 hundred million tons, accounts for
The 0.1% of wastewater emission amount, still has substantial amounts of waste water not processed, brings immense pressure to environmental improvement.Textile industry waste water is arranged
Put and account for the 9.1% of total discharge of wastewater, in sewage, mainly contain additional various slurries in oils and fatss, salt and the course of processing, dye
The inorganic matters such as material, surfactant, auxiliary agent and soda acid, sulfide, all kinds of salt compounds, wherein alkali, sulfide, all kinds of
Salt compounds environmental pollution is very big, and affects its own existence of the mankind.The water reuse that textile production is produced
In manufacture of cement, can effectively solve textile industry waste water handling problem, and the surfactant comprising in waste water can
To promote the grinding of cement, the solution not only improving waste water handling problem achieves twice laid again.
Graphene is the intensity highest of discovery so far, toughness is best, specific surface area is maximum material.Graphene oxide
（GO）It is the oxidized reaction of graphite and the later product of ultrasonic disperse, have that specific surface area is larger, surface functional group type is enriched
Feature, stable dispersion can have the good compatibility in aqueous and with macromolecule.Graphene oxide is applied to poly-
Compound organic material and mineral-type materials are the focuses that contemporary scientific is studied, and have obtained card in the applied research of cement-based material
The porosity of hardened paste can effectively being reduced in fact, improving microstructure, thus being favorably improved the mechanical property of cement.
Content of the invention
For solving the above problems, the present invention provides a kind of graphene oxide modification cement grinding aid, and this grinding aid grinding is imitated
Rate is high, and after grinding water mud is excellent with water reducer adaptability, effectively utilizes industrial wastewater, environmental protection.
Present invention simultaneously provides the preparation method of this cement grinding aid.
The present invention is achieved through the following technical solutions：
A kind of graphene oxide modification cement grinding aid, is made up of following mass percent：Polymerized polyalcohol 35-55%, acrylic acid
Ester 2-5%, amino-polyethyleneglycols 3-6%, tetraisopropyl titanate 1-3%, polycarboxylate water-reducer 3-8%, dodecylbenzene sodium sulfonate 1-
2%, polyoxyethylenated alcohol sodium sulfate 1-2%, triethanolamine 5-10%, triisopropanolamine 5-10%, graphene oxide water solution
1-5%, balance of industrial wastewater.
Preferably, grinding aid is made up of following materials in percentage by mass：Polymerized polyalcohol 44%, acrylate 2%, amino gathers
Ethylene glycol 3%, tetraisopropyl titanate 1%, polycarboxylate water-reducer 5%, dodecylbenzene sodium sulfonate 2%, fatty alcohol-polyoxyethylene ether sulfur
Sour sodium 1%, triethanolamine 10%, triisopropanolamine 10%, graphene oxide water solution 2%, industrial wastewater 20%.
Preferably, the concentration of graphene oxide described above is 1-5mg/ml, and described industrial wastewater gives up for textile industry
Water.
The preparation method of this cement grinding aid, comprises the following steps：
（1）By polymerized polyalcohol, acrylate and amino-polyethyleneglycols heating in water bath to 70 DEG C～100 DEG C, add metatitanic acid four different
Propyl ester, stirs 10-20 minute, ultrasonic disperse 10-20min, reacts 1-3h；
（2）Maintain 70 DEG C～100 DEG C of bath temperature, add industrial wastewater, mix homogeneously；
（3）Sequentially add dodecylbenzene sodium sulfonate, polyoxyethylenated alcohol sodium sulfate, triethanolamine, triisopropanolamine and
Polycarboxylate water-reducer, stirs and dissolves to whole；
（4）Graphene oxide solution is added, heating in water bath, to 60-90 DEG C, stands 10-24h after ultrasonic disperse 10-30min, obtains
Cement grinding aid.
The useful achievement of the present invention is：
The present invention utilizes graphene oxide modification cement grinding aid, and graphene oxide just can significantly improve powder when volume is less
Mill efficiency, the cement granules of grinding have bigger specific surface area and less tailing over；Significantly enhance the early strength of cement；
After grinding water mud is excellent with water reducer adaptability；Efficiently utilize industrial wastewater, product is environmentally friendly, pollution-free.
In the cement pulverizing course of equal time, this product tails over compared with blank sample label PC42.5 cement 0.045mm
Reduce 8%-12%, 0.08mm tails over reduction 10%-20%, specific surface area improves 8%-10%, 3 days intensity improves 4-6Mpa, and 28 days strong
Degree improves 4-8Mpa.There is certain improvement compared with the adaptability of commercially available prod after grinding water mud and water reducer, liquidity value added reduces,
It is effectively improved the bad bleeding causing of adaptability, is layered, takes off bottom phenomenon, water-reducing rate improves 3-5%.
Specific embodiment
Essence for a better understanding of the present invention, enters to advance to technical scheme below by specific embodiment
The elaboration of one step.
Embodiment 1
A kind of preparation method of type graphene oxide modification cement grinding aid, comprises the following steps, following percentage ratio is quality
Percentage ratio：
（1）Take 35% polymerized polyalcohol, 2% acrylate and 70 DEG C of 3% amino-polyethyleneglycols heating in water bath, add 1% metatitanic acid four
Isopropyl ester, mechanical agitation 10min, then ultrasonic disperse 10min is to after uniformly, and water-bath 1h obtains hydramine ester type compound.
（2）Maintain 70 DEG C of bath temperature, hydramine ester type compound adds 34% textile waste, mix homogeneously, joins
Become solution.
（3）In the solution having configured, it is proportionally added into the dodecylbenzene sodium sulfonate 1% measuring, aliphatic alcohol polyethenoxy
Ether sodium sulfate 1%, triethanolamine 10%, triisopropanolamine 9%, polycarboxylate water-reducer 3%, it is evenly stirred until whole dissolvings；
（4）Add the graphene oxide solution 1% (concentration is 1mg/ml) of metering, heating in water bath to 60 DEG C, ultrasonic disperse 10min；
Last solution left standstill 10h, after standing, obtains final product cement grinding aid after the assay was approved.Have no irritating odor after testing, solid content closes
Lattice, pH value are qualified, chloride ion content is qualified, comply fully with the requirement of GB/T26748-2011.
Embodiment 2
A kind of preparation method of type graphene oxide modification cement grinding aid, comprises the following steps, following percentage ratio is quality
Percentage ratio：
（1）Take 55% polymerized polyalcohol, 5% acrylate and 100 DEG C of 6% amino-polyethyleneglycols heating in water bath, add metatitanic acid four isopropyl
Ester 3%, mechanical agitation 20min, then ultrasonic disperse 20min is to after uniformly, and water-bath 2h obtains hydramine ester type compound.
（2）Maintain 100 DEG C of bath temperature, add in hydramine ester type compound, 4% textile waste, mix homogeneously,
Wiring solution-forming.
（3）In the solution having configured, it is proportionally added into the dodecylbenzene sodium sulfonate 2% measuring, aliphatic alcohol polyethenoxy
Ether sodium sulfate 2%, triethanolamine 5%, triisopropanolamine 5%, polycarboxylate water-reducer 8%, it is evenly stirred until whole dissolvings；
（4）Add the graphene oxide solution 5% (concentration is 5mg/ml) of metering, heating in water bath to 90 DEG C, ultrasonic disperse 30min；
Last solution left standstill 24h, after standing, obtains final product cement grinding aid after the assay was approved.Have no irritating odor after testing, solid content closes
Lattice, pH value are qualified, chloride ion content is qualified, comply fully with the requirement of GB/T26748-2011.
Embodiment 3
A kind of preparation method of type graphene oxide modification cement grinding aid, comprises the following steps, following percentage ratio is quality hundred
Divide ratio：
（1）Take 44% polymerized polyalcohol, 2% acrylate and 90 DEG C of 3% amino-polyethyleneglycols heating in water bath, add metatitanic acid four isopropyl
Ester 1%, mechanical agitation 20min, then ultrasonic disperse 20min is to after uniformly, and water-bath 3h obtains hydramine ester type compound.
（2）Maintain 90 DEG C of bath temperature, hydramine ester type compound adds 20% textile waste, mix homogeneously, joins
Become solution.
（3）In the solution having configured, it is proportionally added into the dodecylbenzene sodium sulfonate 2% measuring, aliphatic alcohol polyethenoxy
Ether sodium sulfate 1%, triethanolamine 10%, triisopropanolamine 10%, polycarboxylate water-reducer 5%, it is evenly stirred until whole dissolvings；
（4）Add the graphene oxide solution 2% (concentration is 2mg/ml) of metering, heating in water bath to 90 DEG C, ultrasonic disperse 20min；
Last solution left standstill 24h, after standing, obtains final product cement grinding aid after the assay was approved.Have no irritating odor after testing, solid content closes
Lattice, pH value are qualified, chloride ion content is qualified, comply fully with the requirement of GB/T26748-2011.It is designated as grinding aid D.
Comparative example 1
A kind of larger grinding aid of commercially available shared market share, its main component is triethanolamine and polyalcohols grinding aid, note
For grinding aid A.
Comparative example 2
A kind of preparation method of graphene oxide modification cement grinding aid, step is identical with embodiment 3, and difference is, body
The addition of non-oxidation Graphene in system, i.e. no step（4）, other steps, all with embodiment 3, are designated as grinding aid B.
Comparative example 3
A kind of graphene oxide modification cement grinding aid and preparation method thereof, step is identical with embodiment 3, and difference is,
The addition of fat-free polyoxyethylenated alcohol sodium sulfate in system, other steps, all with embodiment 3, are designated as grinding aid C.
Above-mentioned 4 kinds of grinding aids are used for PC 42.5 cement ball-milling, each proportioning such as table 1, the chemical component table of clinker is shown in
Table 2.Gypsum Fibrosum is the natural gypsum.Ball-milling technology：Mill feed material 5kg every time, using the Ceramic Balls of a diameter of 5cm, the filling of abrading-ball
Measure as 100kg, the rotating speed of grinding machine is 50r/min, and grinding time is 30min.Under identical grinding time, the mixing of each grinding aid
Dosage is 0.03%.
Table 1 PC42.5 experimental raw formula
Table 2 raw material chemical analyses
Below the result of grinding is analyzed, table 3 and table 4 are grinding aid grinding aid performance and the cement performance survey of PC42.5 respectively
The result of examination, grinding aid A is poor with the compatibility of additive, has more serious bleeding, is layered, takes off bottom phenomenon, grinding aid B is with outward
Plus the compatibility of agent is general, there is slight bleeding, be layered, take off bottom phenomenon, grinding aid C is general with the compatibility of additive, has light
Micro- bleeding, be layered, take off bottom phenomenon, grinding aid D is good with the compatibility of additive, no bleeding, be layered, take off bottom phenomenon.
Table 3 PC42.5 grinding aid grinding aid performance test
Table 4 PC42.5 cement performance is tested
Grinding-aid effect compares, D> B > C >A>Blank, such as table 3, grinding aid D of the present invention, 0.045mm tail over reduction about 10%,
0.08mm tails over reduction about 18%, and specific surface area improves about 9%, significantly reduces and tails over, improves the specific surface area of cement.
Mechanical property compares, D> B > C >A>Blank, such as table 4, grinding aid D of the present invention, 3 days intensity raising 6Mpa, 28
Its intensity improves 8Mpa.There is certain improvement compared with the adaptability of commercially available prod after grinding water mud and water reducer, liquidity value added drops
Low, it is effectively improved the bad bleeding causing of adaptability, be layered, take off bottom phenomenon.
Claims (5)
1. a kind of graphene oxide modification cement grinding aid is it is characterised in that be made up of following mass percent：Polymerized polyalcohol
35-55%, acrylate 2-5%, amino-polyethyleneglycols 3-6%, tetraisopropyl titanate 1-3%, polycarboxylate water-reducer 3-8%, dodecane
Base benzene sulfonic acid sodium salt 1-2%, polyoxyethylenated alcohol sodium sulfate 1-2%, triethanolamine 5-10%, triisopropanolamine 5-10%, oxidation
Graphene aqueous solution 1-5%, balance of industrial wastewater.
2. cement grinding aid according to claim 1 is it is characterised in that be made up of following materials in percentage by mass：Polymerization
Polyhydric alcohol 44%, acrylate 2%, amino-polyethyleneglycols 3%, tetraisopropyl titanate 1%, polycarboxylate water-reducer 5%, detergent alkylate
Sodium sulfonate 2%, polyoxyethylenated alcohol sodium sulfate 1%, triethanolamine 10%, triisopropanolamine 10%, graphene oxide water solution
2%, industrial wastewater 20%.
3. cement grinding aid according to claim 1 is it is characterised in that the concentration of described graphene oxide is 1-5mg/
ml.
4. cement grinding aid according to claim 1 is it is characterised in that described industrial wastewater is textile industry waste water.
5. the preparation method of the cement grinding aid described in a kind of one of claim 1-4 is it is characterised in that comprise the following steps：
（1）By polymerized polyalcohol, acrylate and amino-polyethyleneglycols heating in water bath to 70 DEG C～100 DEG C, add metatitanic acid four different
Propyl ester, stirs 10-20 minute, ultrasonic disperse 10-20min, reacts 1-3h；
（2）Maintain 70 DEG C～100 DEG C of bath temperature, add industrial wastewater, mix homogeneously；
（3）Sequentially add dodecylbenzene sodium sulfonate, polyoxyethylenated alcohol sodium sulfate, triethanolamine, triisopropanolamine and
Polycarboxylate water-reducer, stirs and dissolves to whole；
（4）Graphene oxide solution is added, heating in water bath, to 60-90 DEG C, stands 10-24h after ultrasonic disperse 10-30min, obtains
Cement grinding aid.
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Cited By (5)
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| CN107216058A (en) * | 2017-04-24 | 2017-09-29 | 浙江博力建材科技有限公司 | A kind of graphene cement grinding aid and preparation method thereof |
| CN107235649A (en) * | 2017-05-17 | 2017-10-10 | 常州第六元素材料科技股份有限公司 | A kind of cement grinding aid and preparation method thereof |
| CN114907031A (en) * | 2022-05-26 | 2022-08-16 | 昌德新材科技股份有限公司 | Cement raw material additive, application thereof and cement production process |
| CN115181544A (en) * | 2022-07-01 | 2022-10-14 | 惠州市鑫业建材有限公司 | Grinding additive of blocky lime and lime grinding method |
| CN117209192A (en) * | 2023-11-07 | 2023-12-12 | 中石化西南石油工程有限公司 | Early-strength toughening type polycarboxylic acid dispersing agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216058A (en) * | 2017-04-24 | 2017-09-29 | 浙江博力建材科技有限公司 | A kind of graphene cement grinding aid and preparation method thereof |
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| CN115181544A (en) * | 2022-07-01 | 2022-10-14 | 惠州市鑫业建材有限公司 | Grinding additive of blocky lime and lime grinding method |
| CN117209192A (en) * | 2023-11-07 | 2023-12-12 | 中石化西南石油工程有限公司 | Early-strength toughening type polycarboxylic acid dispersing agent and preparation method thereof |
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| CN106380110B (en) | 2018-06-26 |
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Effective date of registration: 20200518 Address after: 100020 room 213, 2f, building 1, No.5 (Xiyuan), Huahua Road, Chaoyang District, Beijing Patentee after: Fenglebao chemical materials (Beijing) Co., Ltd Address before: The central nanxinzhuang Ji'nan Road, No. 336 of 250022 cities in Shandong Province Patentee before: University of Jinan |