CN109320124A - A kind of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid and preparation method thereof - Google Patents
A kind of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid and preparation method thereof Download PDFInfo
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- CN109320124A CN109320124A CN201810976273.8A CN201810976273A CN109320124A CN 109320124 A CN109320124 A CN 109320124A CN 201810976273 A CN201810976273 A CN 201810976273A CN 109320124 A CN109320124 A CN 109320124A
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- grinding aid
- polycarboxylic acid
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- modified polycarboxylic
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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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2641—Polyacrylates; Polymethacrylates
- C04B24/2647—Polyacrylates; Polymethacrylates containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention belongs to building material technical fields, and in particular to a kind of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid and preparation method thereof.The present invention is led to be carried out in polymerization process in excessively unsaturated polymeric monomer and esterification monomer, addition nano-titanium dioxide is prepared, modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency of the present invention is high, and the cement granules of grinding have bigger specific surface area and smaller tail over.
Description
Technical field
The invention belongs to building material technical fields, and in particular to a kind of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid
Agent and preparation method thereof.
Background technique
The development of building trade proposes requirements at the higher level to the quantity and quality of cement.Exist in cement production process a large amount of
Power consumption, wherein grinding pow consumption accounts for 2/3rds of the total power consumption of manufacture of cement, and energy utilization rate is low, serious waste of resources.Cause
This, improving mill efficiency is the key that manufacture of cement energy-conservation of consumption reduction.Cement grinding aid is a kind of raising grinding efficiency, improves cement
Material grindability energy in production, and a kind of chemical addition agent of the little organic or inorganic of addition content.During finished ground cement,
Grinding aid can significantly improve mill efficiency, substantially reduce grinding pow consumption, improve the fineness and specific surface area of cement.Meanwhile grinding aid
Agent can also improve the early strength of cement, on the basis of not damaging cement self performance, reduce manufacture of cement cost, improve water
Mud production efficiency.Clinker and other mixing materials refine in grinding machine powder process with particle, and cement granules specific surface area increases
Electrically charged because of scission of link greatly, mutually absorption generates reunion between particle, is greatly reduced mill efficiency.Grinding aid acts on cement
Between the particle of material, the surface energy of particle is reduced, principle is to prevent particle aggregation, improves its mobility, improves grinding effect
Rate, thus energy-saving and emission-reduction.This greatly reduces grinding time and energy consumption.Currently, cement grinding aid usually selects alkanol
Or alcamines (such as glycerine, ethylene glycol, triethanolamine, triisopropanolamine etc.) is used as raw material and simply compounding preparation
At.Nowadays, such grinding aid cannot fully meet cement high-performance, the demand of high-quality, and its performance is also unstable, fit
Answering property is poor, and with the rise of the chemical raw materials such as petroleum, the price of compounding production grinding aid also rises steadily.Therefore, it synthesizes
Performance is stable, adaptable organic polymer cement grinding aid reinforcing agent just seems imperative.Poly carboxylic acid series concrete is additional
Agent is a kind of synthesis macromolecular organic compound, is had been widely used in the cement compositions such as concrete, mortar, cement slurry.It grinds
Study carefully discovery, poly carboxylic acid series concrete additive equally has grind -aiding effect, with traditional alcamines grinding aid phase simply compounded
Than synthesis polymeric polycarboxylic acid series cement grinding aid has the effects that performance is stable, have grinding aid concurrently and improves cement performance.Than
Such as, CN101798198 is esterified, then by polyoxyethylene ether, the poly- second of allyl using polyoxyethylene ether and unsaturated carboxylic acid
Glycol, (methyl) Sodium Allyl Sulfonate, polyalcohol and water copolymerization polycarboxylic-acid cement grinding aid.CN102134300 will not
Polycarboxylic-acid cement grinding aid is made in saturation polyethers, unsaturated sulfonic acid synthetic reaction.US6005057 uses styrene, maleic acid
Acid anhydride, the copolymerization of maleic anhydride polyalkylene glycol monoalkyl ether-ether form a kind of polycarboxylic-acid cement grinding aid.However, above-described water
Its grinding aid limited efficacy of cement grinding aids, powder efficient utilization need to be further increased.
Summary of the invention
The object of the present invention is to provide a kind of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aids and preparation method thereof, lead to
It crosses and is carried out in polymerization process in unsaturated polymeric monomer and esterification monomer, addition nano-titanium dioxide is prepared, and the present invention is modified
Polycarboxylic acids alkanolamine ester high-molecular cement grinding aid mill efficiency is high, and the cement granules of grinding have bigger specific surface area and smaller
Tail over.
The technical solution of the present invention is as follows:
A kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, comprising the following steps:
(1) it stirs evenly after mixing triethanolamine by a mole mass ratio with methyl methacrylate, then heats up, stirring
Esterification is carried out under the conditions of mixing obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) unsaturated polymeric monomer methacrylic acid polyoxyethylene ether, esterification monomer and water are added in reactor, unlatching is stirred
It mixes;Then closed reactor opens heating, and when temperature reaches 80 DEG C -90 DEG C, initiator and chain-transferring agent is added;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water drop at this time
When no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor when temperature rises to vertex for temperature, when
When temperature continues to drop to 55~60 DEG C, temperature lowering water is closed, when reactor temperature drops to 35~45 DEG C naturally, blowing,
Obtain modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid.
Preferably, the molar ratio of triethanolamine and methyl methacrylate is 1:1 in step (1).
Preferably, 60~70 DEG C are warming up in step (1).
Preferably, it is 5~6h that time control is stirred to react in step (1).
Preferably, each component additional amount in step (3) are as follows: 60~70 parts by weight of methacrylic acid polyoxyethylene ether, esterification
15~25 parts by weight of monomer, 1~3 parts by weight of initiator, 1~2 parts by weight of chain-transferring agent.
Preferably, speed of agitator is 70~90r/min in step (3).
Preferably, the initiator is one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
Preferably, the chain-transferring agent is 2- thioacetic acid or 3- mercaptopropionic acid.
Preferably, in step (4) weight of nano-titanium dioxide account for the methacrylic acid polyoxyethylene ether weight 1~
15%.
The obtained modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid of above method preparation.
Beneficial effects of the present invention are as follows:
The present invention in unsaturated polymeric monomer and esterification monomer by carrying out in polymerization process, addition nano-titanium dioxide preparation
It forms, modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency of the present invention is high, and the cement granules of grinding have bigger
Specific surface area and smaller tail over.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described in further detail, but do not constituted pair
Any restrictions of the invention.
Embodiment 1
A kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, comprising the following steps:
(1) it stirs evenly, then heats to after mixing triethanolamine by a mole mass ratio 1:1 with methyl methacrylate
60 DEG C, esterification is carried out under agitation, and reaction time control is 5h, obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) by 66 parts by weight unsaturation polymeric monomer methacrylic acid polyoxyethylene ether, the above-mentioned esterification monomer of 22 parts by weight and
Water is added in reactor, opens stirring, and adjusting mixing speed is 70r/min;Then closed reactor opens heating, works as temperature
When reaching 80 DEG C -90 DEG C, 1.5 parts by weight initiator ammonium persulfates and 1 parts by weight chain-transferring agent 2- Thioglycolic acid is added;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water drop at this time
When no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor when temperature rises to vertex for temperature, control
Nano-titanium dioxide weight processed accounts for the 10% of methacrylic acid polyoxyethylene ether weight, when temperature continues to drop to 55~60 DEG C
When, close temperature lowering water, when reactor temperature drops to 35~45 DEG C naturally, blowing to get arrive modified polycarboxylic acid alkanolamine ester
High-molecular cement grinding aid.
Modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency manufactured in the present embodiment is high, the cement of grinding
Grain has biggish specific surface area and lesser tails over.
Embodiment 2
A kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, comprising the following steps:
(1) it stirs evenly, then heats to after mixing triethanolamine by a mole mass ratio 1:1 with methyl methacrylate
62 DEG C, esterification is carried out under agitation, and reaction time control is 6h, obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) by 65 parts by weight unsaturation polymeric monomer methacrylic acid polyoxyethylene ether, the above-mentioned esterification monomer of 20 parts by weight and
Water is added in reactor, opens stirring, and adjusting mixing speed is 75r/min;Then closed reactor opens heating, works as temperature
When reaching 80 DEG C -90 DEG C, 2 parts by weight initiator sodium peroxydisulfates and 1 parts by weight chain-transferring agent 2- Thioglycolic acid is added;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water drop at this time
When no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor when temperature rises to vertex for temperature, control
Nano-titanium dioxide weight processed accounts for the 5% of methacrylic acid polyoxyethylene ether weight, when temperature continues to drop to 55~60 DEG C,
Close temperature lowering water, when reactor temperature drops to 35~45 DEG C naturally, blowing to get arrive modified polycarboxylic acid alkanolamine ester high score
Sub- cement grinding aid.
Modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency manufactured in the present embodiment is high, the cement of grinding
Grain has biggish specific surface area and lesser tails over.
Embodiment 3
A kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, comprising the following steps:
(1) it stirs evenly, then heats to after mixing triethanolamine by a mole mass ratio 1:1 with methyl methacrylate
70 DEG C, esterification is carried out under agitation, and reaction time control is 5h, obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) by 60 parts by weight unsaturation polymeric monomer methacrylic acid polyoxyethylene ether, the above-mentioned esterification monomer of 18 parts by weight and
Water is added in reactor, opens stirring, and adjusting mixing speed is 90r/min;Then closed reactor opens heating, works as temperature
When reaching 80 DEG C -90 DEG C, 1.2 parts by weight initiator ammonium persulfates are added and 1 parts by weight chain-transferring agent 3- dredges base propionic acid;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water drop at this time
When no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor when temperature rises to vertex for temperature, control
Nano-titanium dioxide weight processed accounts for the 12% of methacrylic acid polyoxyethylene ether weight, when temperature continues to drop to 55~60 DEG C
When, close temperature lowering water, when reactor temperature drops to 35~45 DEG C naturally, blowing to get arrive modified polycarboxylic acid alkanolamine ester
High-molecular cement grinding aid.
Modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency manufactured in the present embodiment is high, the cement of grinding
Grain has biggish specific surface area and lesser tails over.
Embodiment 4
A kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, comprising the following steps:
(1) it stirs evenly, then heats to after mixing triethanolamine by a mole mass ratio 1:1 with methyl methacrylate
68 DEG C, esterification is carried out under agitation, and reaction time control is 5.5h, obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) by 60 parts by weight unsaturation polymeric monomer methacrylic acid polyoxyethylene ether, the above-mentioned esterification monomer of 25 parts by weight and
Water is added in reactor, opens stirring, and adjusting mixing speed is 80r/min;Then closed reactor opens heating, works as temperature
When reaching 80 DEG C -90 DEG C, 2.5 parts by weight initiator potassium persulfates and 2 parts by weight chain-transferring agent 2- Thioglycolic acids are added;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water drop at this time
When no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor when temperature rises to vertex for temperature, control
Nano-titanium dioxide weight processed accounts for the 15% of methacrylic acid polyoxyethylene ether weight, when temperature continues to drop to 55~60 DEG C
When, close temperature lowering water, when reactor temperature drops to 35~45 DEG C naturally, blowing to get arrive modified polycarboxylic acid alkanolamine ester
High-molecular cement grinding aid.
Modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid mill efficiency manufactured in the present embodiment is high, the cement of grinding
Grain has biggish specific surface area and lesser tails over.
Comparative example 1
A kind of biggish grinding aid of commercially available shared market share, main component are triethanolamine and polyalcohols grinding aid
Agent is denoted as grinding aid A.
Comparative example 2
A kind of preparation method of polycarboxylic acids alkanolamine ester high-molecular cement grinding aid, step is identical with embodiment 1, difference
It is, without the addition of nano-titanium dioxide in system, is denoted as grinding aid B.
Performance test
6 kinds of grinding aids in above-described embodiment 1~4 and comparative example 1~2 are respectively used to commercially available 42.5 cement ball-milling of PC,
Ball-milling technology: each mill feed material 5kg uses diameter for the Ceramic Balls of 5cm, and the loading of abrading-ball is 100kg, the revolving speed of grinding machine
For 50r/min, grinding time 30min.Under identical grinding time, the addition content of each grinding aid is 0.03%, will not
The cement of grinding aid is added as blank group, the grinding aid the performance test results of grinding aid are as shown in table 1.
1 grinding aid grinding aid performance test of table
By the contrast test of above embodiments and comparative example and blank group it is found that the present invention is due to unsaturated big single
Body and esterification monomer carry out in polymerization process, and addition nano-titanium dioxide is prepared, and modified polycarboxylic acid alkanolamine ester of the present invention is high
Molecule cement grinding aid mill efficiency is high, and the cement granules of grinding have bigger specific surface area and smaller tail over.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid, which comprises the following steps:
(1) it stirs evenly after mixing triethanolamine by a mole mass ratio with methyl methacrylate, then heats up, in stirring bar
Esterification is carried out under part obtains esterification monomer;
(2) nano-titanium dioxide is dissolved in deionized water and obtains nano titanium oxide dispersion;
(3) unsaturated polymeric monomer methacrylic acid polyoxyethylene ether, esterification monomer and water are added in reactor, open stirring;
Then closed reactor opens heating, and when temperature reaches 80 DEG C -90 DEG C, initiator and chain-transferring agent is added;
(4) when reactor temperature is begun to ramp up, polymerization reaction is had begun in reactor, opens temperature lowering water cooling at this time,
When temperature rises to vertex, when no longer rising and beginning to decline, nano titanium oxide dispersion is added into reactor, works as temperature
When continuing to drop to 55~60 DEG C, close temperature lowering water, when reactor temperature drops to 35~45 DEG C naturally, blowing to get
To modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid.
2. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that the molar ratio of triethanolamine and methyl methacrylate is 1:1 in step (1).
3. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that step is warming up to 60~70 DEG C in (1).
4. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that it is 5~6h that time control is stirred to react in step (1).
5. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is, each component additional amount in step (3) are as follows: 60~70 parts by weight of methacrylic acid polyoxyethylene ether, esterification monomer 15~
25 parts by weight, 1~3 parts by weight of initiator, 1~2 parts by weight of chain-transferring agent.
6. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that speed of agitator is 70~90r/min in step (3).
7. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that the initiator is one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
8. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that the chain-transferring agent is 2- thioacetic acid or 3- mercaptopropionic acid.
9. a kind of preparation method of modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid according to claim 1, special
Sign is that the weight of nano-titanium dioxide accounts for the 1~15% of the methacrylic acid polyoxyethylene ether weight in step (4).
10. the obtained modified polycarboxylic acid alkanolamine ester high-molecular cement grinding aid of any method preparation described in claim 1 to 9
Agent.
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CN111689715A (en) * | 2020-05-26 | 2020-09-22 | 贵州石博士科技有限公司 | Yield-increasing reinforced cement grinding aid and preparation method thereof |
CN115286749A (en) * | 2022-08-22 | 2022-11-04 | 上海抚佳精细化工有限公司 | Polycarboxylic acid polymer and preparation method and application thereof |
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CN115286749A (en) * | 2022-08-22 | 2022-11-04 | 上海抚佳精细化工有限公司 | Polycarboxylic acid polymer and preparation method and application thereof |
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