CN109133710A - A kind of naphthalene water reducer matching preparation method for subtracting jelly - Google Patents
A kind of naphthalene water reducer matching preparation method for subtracting jelly Download PDFInfo
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- CN109133710A CN109133710A CN201811061682.1A CN201811061682A CN109133710A CN 109133710 A CN109133710 A CN 109133710A CN 201811061682 A CN201811061682 A CN 201811061682A CN 109133710 A CN109133710 A CN 109133710A
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- water reducer
- sodium
- naphthalene water
- jelly
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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
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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
- 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
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
Abstract
The present invention provides a kind of naphthalene water reducer matching preparation methods for subtracting jelly.Naphthalene water reducer matching is prepared with subtracting jelly by following parts by weight of component: 30-50 parts of polyalcohol amine ester compounds, 0.01-0.05 parts of bleeding agent, 0.08-0.4 parts of lubricant, 0.04-0.08 parts of emulsifying dispersant, 0.02-0.1 parts of sulfate radical precipitating reagent, surplus is water, 100 parts of gross mass；Above-mentioned each component is sufficiently stirred 0.5 hour in a kettle, i.e. acquisition naphthalene water reducer matching is with subtracting jelly.The present invention subtracts jelly using the method preparation that alcamines minor comonomer polymerize to obtain with unsaturated acid anhydride the higher hydramine ester polymer of molecular weight, it is to subtract jelly to have compared with severely sterically resistance ability, have certain guarantor to collapse ability, there is preferable matching with naphthalene water reducer, the workability of concrete can be significantly improved, and any surface finish after concrete setting can be made bright.
Description
Technical field
The present invention relates to building material technical field, it is related specifically to a kind of naphthalene water reducer matching and is prepared with jelly is subtracted
Method.
Background technique
Concrete subtracts the concrete admixture that jelly is a new generation, is used cooperatively with other additives such as water-reducing agents, can
The workability energy for preferably improving concrete, reduces the gel material content in concrete.But in practical applications, commonly subtract glue
Matching between agent and other additives especially cement water reducing agent restricts the large-scale promotion for subtracting jelly there are limitation
Using.Particularly, it is more prominent commonly to subtract the problem that matching is poor between jelly and naphthalene water reducer, it is difficult to which acquisition subtracts glue dispersion
Effect.
Naphthalene water reducer is made by the substances such as naphthalene sulfonate and formaldehyde through condensation reaction, mainly passes through electrostatic repulsion for cement
Particle dispersion, i.e., surface has the cement granules of positive charge when the anion sulfonic group in diminishing agent molecule is adsorbed in aquation initial stage
On, formed absorption electric double layer, keep cement granules mutually exclusive, it is therefore prevented that the generation of cohesion.But the suction type is stub
Formula absorption, naphthalene water reducer molecular weight is smaller in addition, and space multistory repulsion ability is weaker, and diminishing agent molecule is easily detached from cement granules
Surface, and as the diminishing agent molecule that hydration reaction be adsorbed in cement particle surface is easy to be wrapped by, macroscopically show
It is big for concrete gradual loss.
The common jelly that subtracts mainly uses hydramine cationoid minor comonomer, passes through the electronegative flocculation of electrostatic repulsion dispersion train
Structure, dispersibility is weaker, is matched with naphthalene water reducer in use, the substance of two kinds of small-molecular-weights is difficult to be cooperated.For
The problem of small molecule dispersion performance deficiency can be made to subtract jelly and obtained certain steric hindrance using the thinking that polymerize hydramine
Effect, greatly enhances the ability of disperse cement particles.At this stage, polyalcohol amine ester compounds preparation subtract jelly research it is still few
See, but it has the characteristics that stronger dispersion effect, determine that its Later development will increasingly be taken seriously, using also will more
Come more extensive.
Patent CN105174774A discloses a kind of concrete and subtracts jelly, this subtracts in jelly each component by weight
It matches as follows: 100-120 parts of melamine, 400-500 parts of formaldehyde, 300-400 parts of water, 80-100 parts of salicylic acid.Subtracted using this
Jelly reduces Cost of Concrete, improves the performance of concrete under the premise of intensity remains unchanged.
Patent CN106116224A discloses a kind of multifunctional concrete synergist, specifically by the raw material system of following parts by weight
At: 26-42 parts of diisopropyl ethanolamine, 2-8 parts of pentaerythrite, wooden sodium sulfonate 15-26 parts, cetyl trimethyl hydroxide
8-16 parts of ammonium, 1-6 parts of xanthan gum, 5-13 parts of alkyl glycosides, 40-80 parts of water.The multifunctional concrete synergist can reduce water
Mud dosage enough enhances the intensity of concrete, improves concrete durability and anti-thawing, improves impervious.
Patent CN105906230A discloses a kind of high performance concrete and subtracts jelly and preparation method thereof with multi-functional, by changing
Property polyethers, mixing hydramine, mixed alcohol, unsaturated acids, modified siloxane, initiator and water composition.The high-performance of the invention is mixed
Solidifying soil subtracts that be able to maintain strength grade of concrete while jelly reduces gel material content used in concrete constant with multi-functional,
And the durabilities such as frost resistance and anti-carbonation that can improve coagulation scholar.
It is different from the above patent, the present invention introduces polyalcohol amine ester in subtracting sizing agent component, i.e. alcamines minor comonomer polymerize
As the method for high molecular polymer, makes to subtract sizing agent component and have certain steric hindrance effect, significantly improve and subtract jelly to water
The dispersion effect of mud particle；Originally it is good with naphthalene water reducer matching to subtract jelly, concrete workability can be improved, and reach reduction glue
The purpose of gel material dosage.
Summary of the invention
It is of the invention to be to provide a kind of naphthalene water reducer matching with subtracting jelly preparation method.
Design philosophy of the invention is to be conceived to the dispersibility for improving and subtracting jelly, and especially steric hindrance ability is set out,
The alcamines monomer polymerization of small molecule is formed into alkanolamine ester high molecular polymer, increases certain steric hindrance to subtract sizing agent component
Effect, further increase subtract jelly subtract glue dispersibility.
The present invention using alcamines minor comonomer polymerize under certain process conditions formed the higher alkanolamine ester of molecular weight gather
The method for closing object, and during cationic polymerizable compound, unsaturated acids anhydride compound is introduced as main polymer chain knot
The important component of structure avoids initial stage as far as possible and subtracts jelly and water-reducing agent competitive Adsorption using the hysteresis quality that it is hydrolyzed, and can
To make up the deficiency that naphthalene water reducer protects ability difference of collapsing.
Hydramine ester polymer prepared by the present invention, steric hindrance ability is stronger, makes up naphthalene water reducer molecule and lacks space
The deficiency of steric hindrance.In the synthesis process, cationic minor comonomer is also introduced, the absorption dispersibility of polymer is improved.
Present invention introduces bleeding agents, subtract jelly when improving the mixed effect between each component, and use can be improved and mix
The stirring and mixing effect of solidifying soil each component especially naphthalene water reducer；The lubricant of introducing can not only significantly improve concrete and easily
Property, and any surface finish after concrete setting can be made bright；It is used cooperatively, is subtracted using the air entraining agent and defoaming agent of low bleed air volume
Few air pocket generates, and reduces the influence to concrete strength performance, it is ensured that concrete surface exists without obvious bubble.In component
Sulfate radical precipitating reagent is introduced, the problem of bring sulfate radical excess due to using naphthalene water reducer is inhibited；Sulfate radical can excessively be made
At generating false set in cement slurry because being settled out gypsum crystal, and excessive sulfate radical will lead to it is a large amount of form entringite,
The slurry for hardening cement initial stage generates swelling stress, weakens intensity；In addition, barium salt can act on being formed with sulfate radical with lead salt
The fillable hydration reaction of precipitating during the gap that is formed, it is helpful to the growth of intensity.
To achieve the above object, technical scheme is as follows:
A kind of naphthalene water reducer matching preparation method for subtracting jelly, it is characterised in that: the naphthalene water reducer matching is used
Subtract jelly to be prepared by following parts by weight of component:
30-50 parts of polyalcohol amine ester compounds, 0.01-0.05 parts of bleeding agent,
0.08-0.4 parts of lubricant, 0.04-0.08 parts of emulsifying dispersant,
0.02-0.1 parts of sulfate radical precipitating reagent, surplus is water, 100 parts of gross mass；
Above-mentioned each component is sufficiently stirred 0.5 hour in a kettle, i.e. acquisition naphthalene water reducer matching is with subtracting jelly；
Wherein: polyalcohol amine ester compounds contain following parts by weight of component:
50-70 parts of alcamine compound, 20-40 parts of unsaturated acid anhydride,
Cationic minor comonomer 1-6 parts, 0.1-2 parts of catalyst,
1-5 parts of neutralizer, 100 parts of gross mass；
Preparation method is as follows:
1), by 50-70 parts of alcamine compound, 20-40 parts of unsaturated acid anhydride, cationic minor comonomer 1-6 parts of investments reaction
In kettle, stir evenly；
2), temperature is controlled at 30-70 DEG C, puts into catalyst 0.1-2 parts, continues stirring 1-4 hours；
3), the reaction time terminates, and when controlling 20-30 DEG C of temperature, is added neutralizer 1-5 parts, is separated by filtration catalyst carrier,
Obtain polyalcohol amine ester compounds.
The alcamine compound is butylethanolamine, methyl diethanolamine, L- phosphatidyl-ethanolamine, N- (3- amino
Propyl) diethanol amine, n,N-diisopropylethanolamine, dodecyl benzene sulfonic acid triethanolamine, N- (2- amino -4- nitrobenzophenone)
Ethanol amine, 1,2-, bis- lauroyl phosphatidyl-ethanolamine, valiolamine, cetamiphen, Monoethanolamine Oleate, oleic acid triethanolamine
One kind of amine, N- phenylethanol amine, hydroiodic acid triethanolamine, Ecamsule triethanolamine, biacetyl ethanol amine, tert-butyl ethanol amine
Or several compositions；Preferred molecular weight is big, has the alcamine compound of certain space steric hindrance ability；Preferred mass is than for 1:1's
The composition of valiolamine and Ecamsule triethanolamine.
The unsaturated acid anhydride is acrylic anhydride, crotonic anhydride, 2- butene-1-base succinic anhydride, isobutenyl succinic
Acid anhydrides, Radix Angelicae Sinensis acid anhydrides, maleic anhydride, last of the ten Heavenly stems enetutanedioic acid anhydride, 15 alkenyl succinic anhydrides, dodecenylsuccinic acid acid anhydride,
(2- methyl -2- propylene -1- base) succinic anhydride, itaconic anhydride, one kind of 4- methacryloxyethyl trimellitic anhydride or
Several compositions；Preferred molecular weight is big, has the unsaturated acid anhydride of certain space steric hindrance ability；Preferred mass is than (the 2- first for 1:1
Base -2- propylene -1- base) succinic anhydride and 4- methacryloxyethyl trimellitic anhydride composition.
The cationic minor comonomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methylacryoyloxyethyl diformazan
Base benzyl ammonium chloride, methacryl hydroxypropyltrimonium chloride, methacryloxypropyl amido trimethyl silane, 2- acryloyl group
Oxygroup ethoxytrimethylsilane, acryloxyethyldimethyl benzyl ammonium chloride, N- hexyl-N- methacryloxy-N,
N- dimethylamino ammonium bromide, chlorination glycidol trimethyl ammonium, benzyl vinyl trimethyl ammonium chloride, choline chloride, eight alkyl three
Ammonio methacrylate, tetradecyl trimethyl ammonium chloride, decyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, 18
One or more of compositions of alkyl trimethyl ammonium chloride；Preferred mass is than the methylacryoyloxyethyl trimethyl ammonia chloride for 1:1
The composition of ammonium and octadecyltrimethylammonium chloride.
The catalyst is solid super-strong acid, specifically loads to oxygen by one or both of sulfate, persulfate
Change and is made on one of zirconium, iron oxide or titanium oxide carrier through high temperature；The sulfate by sodium sulphate, sodium thiosulfate,
Sodium bisulfate, copper sulphate, ammonium sulfate, potassium sulfate, magnesium sulfate, the one or more of of zinc sulfate form；Preferred mass is than for 1:1's
The composition of sodium sulphate and sodium thiosulfate；The persulfate is by ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate, persulfuric acid
One or more of compositions of hydrogen potassium, Potassium Monopersulfate；Preferred mass is than the potassium hydrogen persulfate and Potassium Monopersulfate for 1:1
Composition.
The neutralizer be sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide,
Ethanol amine, diethanol amine, triethanolamine, the one or more of of triisopropanolamine form；The alcamines object of preferred cationic monomer
Matter；Composition of the preferred mass than triethanolamine and triisopropanolamine for 1:1.
The bleeding agent is sulfated castor oil, sodium alkyl benzene sulfonate, alkyl sulfate sodium, sodium secondary alkyl sulfonate, secondary
Alkyl sulfate sodium, Negel, the one or more of of sulfamic acid sodium form；It is preferred that water-soluble preferable, band phenyl ring knot
The sodium alkyl benzene sulfonate of structure.
The lubricant is that organosiloxane lubricant, hydrocarbon lubricants are constituted, specially dimethyl silicone polymer, poly-
Methyl phenyl siloxane, polydiethylsiloxane, polyethylene wax, oxidized polyethylene wax, the one or more of of chlorinated paraffin form；
It is preferred that compounded lubricant；Preferred mass is than the polymethylphenylsiloxane and oxidic polyethylene Wax composition for 1:1.
The emulsifying dispersant is α-sodium olefin sulfonate, aromatic polyvinylether, polyethylene glycol monooleate, octadecanol
Polyoxyethylene ether, polyoxyethylene laurel ether, polyoxyethylene sorbitol acid anhydride tristearate, nonylphenol polyoxyethylene ether, castor oil
One or more of compositions of polyoxyethylene ether；It is preferred that with the preferable α-sodium olefin sulfonate of naphthalene water reducer matching.
The sulfate radical precipitating reagent is barium nitrate, barium chloride, barium hydroxide, barium acetate, barium sulphide, three hydration thiocyanic acids
Barium, barium iodide, barium acetate, butyric acid barium, barium propionate, lead chloride, plumbi nitras, lead oxalate, lead formate, lead acetate, lead bromate, secondary second
One or more of compositions of lead plumbate；It is preferred that organic-inorganic barium salt is used in combination；Preferred mass is than the barium nitrate and lead acetate for 3:1
Composition.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention polymerize to obtain the higher hydramine ester polymer of molecular weight with unsaturated acid anhydride using alcamines minor comonomer
Method preparation subtract sizing agent component, the alkanolamine ester polymer architecture have preferable designability, have compared with severely sterically hinder ability；
Important component of the unsaturated acids anhydride compound of selection as polymer backbone conformation, using its hydrolyze hysteresis quality,
Avoiding initial stage as far as possible subtracts jelly and water-reducing agent competitive Adsorption, and has certain guarantor and collapse ability, has preferably with naphthalene water reducer
Matching；Introduce cationic minor comonomer, dispersion effect of the enhancing polyalcohol amine ester large molecule for negative electrical charge cement aggregation；
2, present invention introduces bleeding agent, subtract when improving the mixed effect between each component, and use can be improved jelly with
The stirring and mixing effect of concrete each component especially naphthalene water reducer；
3, present invention introduces lubricant can not only significantly improve the workability of concrete, and after concrete setting capable of being made
Any surface finish it is bright；
4, the present invention is used cooperatively using emulsifying dispersant and defoaming agent, reinforces concrete compactness, improves strong concrete
Degree, it is ensured that concrete is apparently without obvious bubble；
5, the present invention introduces sulfate radical precipitating reagent in component, and sulfate radical is inhibited excessively to will cause in cement slurry because of precipitating
Out gypsum crystal and the case where generate false set, reduce excessive sulfate radical will lead to it is a large amount of formed entringite generate swelling stresses and
The problem of weakening intensity；In addition, precipitating reagent and sulfate radical act on the sky formed during the fillable hydration reaction of the precipitating to be formed
Gap, it is helpful to the growth of intensity.
Specific embodiment
Clear, complete description further is carried out to technical solution of the present invention below with reference to embodiment.
Embodiment 1 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 50 parts of composition of the valiolamine of mass ratio 1:1 and Ecamsule triethanolamine, 40 parts of acrylic anhydride,
In 5 parts of investment reaction kettles of methylacryloxyethyldimethyl benzyl ammonium chloride, stir evenly；
2), temperature is controlled to the group of sodium sulphate and sodium thiosulfate that the cured mass ratio 1:1 of iron oxide is put at 60 DEG C
That closes object bakes and banks up with earth 1.8 parts of object, continues stirring 3.5 hours；
3), the reaction time terminates, and when controlling 20 DEG C of temperature, is added 3.2 parts of diethanol amine, is separated by filtration catalyst carrier,
Obtain polyalcohol amine ester compounds.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: 30 parts of polyalcohol amine ester compounds, alkane
0.05 part of base benzene sulfonic acid sodium salt, the polymethylphenylsiloxane of mass ratio 1:1 with 0.4 part of oxidic polyethylene Wax composition, α-alkenyl
0.08 part of sodium sulfonate, 0.1 part of barium nitrate, surplus is water, 100 parts of gross mass.Above-mentioned each component is sufficiently stirred 0.5 in a kettle
Hour, i.e., the matching of acquisition naphthalene water reducer is with subtracting jelly.
Embodiment 2 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 57 parts of methyl diethanolamine, (2- methyl -2- propylene -1- base) succinic anhydride and 4- methyl of mass ratio 1:1
30 parts of the composition of acryloyl-oxyethyl trimellitic anhydride, the 6 parts of investment reactions of acryloxyethyldimethyl benzyl ammonium chloride
In kettle, stir evenly；
2), temperature is controlled at 70 DEG C, what investment titanium oxide solidify potassium sulfate bakes and banks up with earth 2 parts of object, continues to stir 4 hours；
3), the reaction time terminates, control 25 DEG C of temperature when, be added 5 parts of potassium carbonate, be separated by filtration catalyst carrier to get
To polyalcohol amine ester compounds.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: 35 parts of polyalcohol amine ester compounds, sulphur
Acidification 0.04 part of castor oil, 0.35 part of dimethyl silicone polymer, 0.07 part of aromatic polyvinylether, the barium nitrate of mass ratio 3:1 and
0.09 part of the composition of lead acetate, surplus are water, 100 parts of gross mass.It is small that above-mentioned each component is sufficiently stirred 0.5 in a kettle
When, i.e., the matching of acquisition naphthalene water reducer is with subtracting jelly.
Embodiment 3 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 60 parts of L- phosphatidyl-ethanolamine, 2- butene-1-32.5 parts of base succinic anhydride, the metering system of mass ratio 1:1
In 3 parts of investment reaction kettles of acyloxyethyl trimethyl ammonium chloride and the composition of octadecyltrimethylammonium chloride, stir evenly；
2), temperature is controlled at 55 DEG C, the investment cured hydrogen persulfate sodium of zirconium oxide bakes and banks up with earth 1.5 parts of object, continues to stir
3.5 hour；
3), the reaction time terminates, and when controlling 27 DEG C of temperature, is added 3 parts of sodium hydroxide, is separated by filtration catalyst carrier, i.e.,
Obtain polyalcohol amine ester compounds.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: 40 parts of polyalcohol amine ester compounds, alkane
It is 0.03 part of base sodium sulfovinate, 0.3 part of polydiethylsiloxane, 0.06 part of octadecanol polyoxyethylene ether, 0.08 part of barium chloride, remaining
Measuring is water, 100 parts of gross mass.Above-mentioned each component is sufficiently stirred 0.5 hour in a kettle, i.e. acquisition naphthalene water reducer matching is used
Subtract jelly.
Embodiment 4 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 69 parts of n,N-diisopropylethanolamine, 20 parts of Radix Angelicae Sinensis acid anhydrides, N- hexyl-N- methacryloxy-N, N-
In 5.5 parts of investment reaction kettles of dimethylamino ammonium bromide, stir evenly；
2), temperature is controlled at 45 DEG C, the investment cured sodium sulphate of titanium oxide bakes and banks up with earth 1.6 parts of object, and it is small to continue stirring 2
When；
3), the reaction time terminates, and when controlling 28 DEG C of temperature, is added 3.9 parts of ethanol amine, is separated by filtration catalyst carrier, i.e.,
Obtain polyalcohol amine ester compounds.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: is 45 parts of polyalcohol amine ester compounds, secondary
0.02 part of alkyl sulfate sodium, 0.25 part of polyethylene wax, 0.06 part of octadecanol polyoxyethylene ether, 0.07 part of lead oxalate, surplus
For water, 100 parts of gross mass.Above-mentioned each component is sufficiently stirred 0.5 hour in a kettle, i.e. acquisition naphthalene water reducer matching is with subtracting
Jelly.
Embodiment 5 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 68 parts of cetamiphen, 27 parts of last of the ten Heavenly stems enetutanedioic acid anhydride, 2 parts of benzyl vinyl trimethyl ammonium chloride investments are anti-
It answers in kettle, stirs evenly；
2), temperature is controlled at 40 DEG C, the investment cured sodium thiosulfate of zirconium oxide bakes and banks up with earth 0.5 part of object, continues to stir
1.5 hour；
3), the reaction time terminates, and at control 29 DEG C of temperature, the triethanolamine and triisopropanolamine of mass ratio 1:1 is added
2.5 parts of composition, catalyst carrier is separated by filtration to get polyalcohol amine ester compounds are arrived.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: 47 parts of polyalcohol amine ester compounds, alkane
0.03 part of base sodium naphthalene sulfonate, 0.15 part of chlorinated paraffin, 0.05 part of polyoxyethylene sorbitol acid anhydride tristearate, lead bromate 0.04
Part, surplus is water, 100 parts of gross mass.0.5 hour, i.e. acquisition naphthalene water reducer is sufficiently stirred in above-mentioned each component in a kettle
Matching is with subtracting jelly.
Embodiment 6 (dosage of each component is parts by weight)
1, the preparation of polyalcohol amine ester compounds: preparation method carries out as follows:
1), by 70 parts of tert-butyl ethanol amine, 27.9 parts of 4- methacryloxyethyl trimellitic anhydride, choline chloride 1
In part investment reaction kettle, stir evenly；
2), temperature is controlled at 30 DEG C, puts into the potassium hydrogen persulfate and monopersulfate of the cured mass ratio 1:1 of titanium oxide
The composition of potassium bakes and banks up with earth 0.1 part of object, continues stirring 1 hour；
3), the reaction time terminates, control 30 DEG C of temperature when, be added 1 part of sodium methoxide, be separated by filtration catalyst carrier to get
To polyalcohol amine ester compounds.
2, subtract the preparation of jelly: subtracting jelly and be prepared by following parts by weight of component: 50 parts of polyalcohol amine ester compounds, ammonia
0.01 part of base sodium sulfonate, 0.08 part of composition of the dimethyl silicone polymer of mass ratio 1:1 and polyethylene wax, castor oil polyoxy second
0.04 part of alkene ether, 0.02 part of lead formate, surplus is water, 100 parts of gross mass.Above-mentioned each component is sufficiently stirred 0.5 in a kettle
Hour, i.e., the matching of acquisition naphthalene water reducer is with subtracting jelly.
Example test result
Test is using C30 concrete as object (table 1), and cement uses 42.5 ordinary portland cement of Huaxing, and sand is thin
The river sand that modulus is 2.4 is spent, stone is the continuous grading rubble of 5-25mm, and water-reducing agent is 3 kinds of different naphthalene water reducers, label
For naphthalene water reducer A, naphthalene water reducer B and naphthalene water reducer C.By the embodiment 1-6 concrete prepared subtract jelly be applied to it is mixed
In solidifying soil, and from do not add and subtract the blank example of jelly, different naphthalene water reducer situations compare.Coagulation scholar's mix physical performance according to
GB/T50080 " Standard for test methods of properties of ordinary concrete mixture standard " tests；Concrete strength is according to GB/T50081
" standard for test methods of mechanical properties of ordinary concrete " tests.
1 C30 concrete mix of table
| Cement | Flyash | Sand | Stone | Water | Water-reducing agent |
| 300 | 80 | 850 | 1020 | 160 | 7.7 |
Do not change the match ratio of concrete, concrete is added and subtracts jelly, volume is the 0.5% of gel material content, is used
Concrete prepared by embodiment 1,3,5 subtracts jelly progress concrete test concrete mixture characteristic test result and is shown in Table 2.
2 concrete performance experimental result of table
Be added in concrete it can be seen from test result in table 2 it is of the invention subtract jelly after, concrete initially collapses
Degree/divergence and the 1h slump/divergence all make moderate progress, and 7d, 8d and 64d compression strength enhance, and the present invention
Subtract jelly and naphthalene water reducer matching performance is preferable, all there is good adaptability from various different naphthalene water reducers.
Concrete mix is adjusted, cement consumption is reduced, subtracts jelly with concrete prepared by embodiment 2,4,6 and carries out coagulation
Soil test, concrete adjustment match ratio are shown in Table 3, and concrete mixture characteristic and mechanical property test the results are shown in Table 4 (blank example adopted
With first wife's composition and division in a proportion, other embodiments are all made of match ratio after adjustment).
The adjustment of 3 C30 concrete mix of table
| Cement | Flyash | Sand | Stone | Water | Water-reducing agent | Subtract jelly |
| 300 | 80 | 850 | 1020 | 160 | 8 | 0 |
| 270 | 80 | 860 | 1030 | 157 | 8 | 1.7 |
Concrete performance experimental result after table 4 adjusts
It can be seen from test data in table 4 in the case where cement consumption reduces by 10%, concrete of the invention is added
Subtract the concrete workability of jelly still better than the blank sample for using first wife's composition and division in a proportion, and 28d intensity is enhanced with 60d intensity.
And it is of the invention subtract jelly and naphthalene water reducer matching performance is preferable, all have from various different naphthalene water reducers good suitable
It should be able to power.
In conclusion of the invention subtracted jelly and can be significantly improved the workability of concrete mix with prepared by naphthalene system,
Promote the compression strength of concrete；The present invention also can reduce the 10% of cement consumption, greatly in the case where guaranteeing concrete strength
It is big to reduce production cost, it realizes making full use of for raw material, brings huge economic benefit for society；It is of the invention subtract jelly with
Polycarboxylate water-reducer matching performance is preferable, all has good adaptability from various different polycarboxylate water-reducers.
All features disclosed in this specification or disclosed all formulas and volume, in addition to mutually exclusive feature and/
Or it other than formula, volume, can combine in any way.It is any disclosed in this specification (including claim, abstract)
Feature can be replaced by other alternative features that are equivalent or have similar purpose unless specifically stated.It removes and non-specifically chats
It states, each feature is an example in a series of equivalent or similar characteristics.
Described above is only the non-limiting embodiment of invention, a large amount of embodiment can also be derived, for this field
Those of ordinary skill for, not departing from the invention design and under the premise of do not make creative work, can also do
The embodiment of several modifications and improvements out, these are all within the scope of protection of the present invention.
Claims (10)
1. a kind of naphthalene water reducer matching preparation method for subtracting jelly, it is characterised in that: the naphthalene water reducer matching is with subtracting
Jelly is prepared by following parts by weight of component:
30-50 parts of polyalcohol amine ester compounds, 0.01-0.05 parts of bleeding agent,
0.08-0.4 parts of lubricant, 0.04-0.08 parts of emulsifying dispersant,
0.02-0.1 parts of sulfate radical precipitating reagent, surplus is water, 100 parts of gross mass；
Above-mentioned each component is sufficiently stirred 0.5 hour in a kettle, i.e. acquisition naphthalene water reducer matching is with subtracting jelly；
Wherein: polyalcohol amine ester compounds contain following parts by weight of component:
50-70 parts of alcamine compound, 20-40 parts of unsaturated acid anhydride,
Cationic minor comonomer 1-6 parts, 0.1-2 parts of catalyst,
1-5 parts of neutralizer, 100 parts of gross mass；
Preparation method is as follows:
1), by 50-70 parts of alcamine compound, 20-40 parts of unsaturated acid anhydride, in cationic minor comonomer 1-6 parts of investment reaction kettles,
It stirs evenly；
2), temperature is controlled at 30-70 DEG C, puts into catalyst 0.1-2 parts, continues stirring 1-4 hours；
3), the reaction time terminates, control 20-30 DEG C of temperature when, be added neutralizer 1-5 parts, be separated by filtration catalyst carrier to get
To polyalcohol amine ester compounds.
2. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: the alcohol
Aminated compounds be butylethanolamine, methyl diethanolamine, L- phosphatidyl-ethanolamine, N- (3- aminopropyl) diethanol amine, N,
N- diisopropyl ethanolamine, dodecyl benzene sulfonic acid triethanolamine, N- (2- amino -4- nitrobenzophenone) ethanol amine, 1,2- February
Osmanthus acyl phosphatidyl-ethanolamine, valiolamine, cetamiphen, Monoethanolamine Oleate, triethanolamine oleate, N- phenylethanol
Amine, hydroiodic acid triethanolamine, Ecamsule triethanolamine, biacetyl ethanol amine, the one or more of of tert-butyl ethanol amine form.
3. the naphthalene water reducer according to claim 1 matching preparation method for subtracting jelly, it is characterised in that: it is described not
Saturation acid anhydrides is acrylic anhydride, and crotonic anhydride, 2- butene-1-base succinic anhydride, isobutenyl succinic anhydride, Radix Angelicae Sinensis acid anhydrides is suitable
Anhydride maleique, last of the ten Heavenly stems enetutanedioic acid anhydride, 15 alkenyl succinic anhydrides, dodecenylsuccinic acid acid anhydride, (2- methyl -2- propylene -1-
Base) succinic anhydride, itaconic anhydride, one or more of compositions of 4- methacryloxyethyl trimellitic anhydride.
4. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: the sun
Ion minor comonomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methylacryloxyethyldimethyl benzyl ammonium chloride, first
Base acryloyl hydroxypropyltrimonium chloride, methacryloxypropyl amido trimethyl silane, 2- acryloyl group oxygroup ethyoxyl front three
Base silane, acryloxyethyldimethyl benzyl ammonium chloride, N- hexyl-N- methacryloxy-N, N- dimethylamino bromination
Ammonium, chlorination glycidol trimethyl ammonium, benzyl vinyl trimethyl ammonium chloride, choline chloride, eight alkyl trimethyl ammonium chlorides, 14
Alkyl trimethyl ammonium chloride, decyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, octadecyltrimethylammonium chloride
One or more of compositions.
5. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: described urges
Agent is solid super-strong acid, and specially one or both of sulfate, persulfate load to zirconium oxide, iron oxide or oxidation
It is made on one of titanium carrier through high temperature；The sulfate is sodium sulphate, sodium thiosulfate, sodium bisulfate, copper sulphate, sulphur
Sour ammonium, potassium sulfate, magnesium sulfate, the one or more of of zinc sulfate form；The persulfate be ammonium persulfate, sodium peroxydisulfate,
Potassium peroxydisulfate, potassium hydrogen persulfate, the one or more of of Potassium Monopersulfate form.
6. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: in described
With agent be sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, ethanol amine, diethanol amine,
One or more of compositions of triethanolamine, triisopropanolamine.
7. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: the infiltration
Saturating agent is sulfated castor oil, sodium alkyl benzene sulfonate, alkyl sulfate sodium, sodium secondary alkyl sulfonate, secondary alkyl sulphate sodium, alkyl
One or more of compositions of sodium naphthalene sulfonate, sulfamic acid sodium.
8. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: the profit
Lubrication prescription be organosiloxane lubricant, hydrocarbon lubricants constitute, specially dimethyl silicone polymer, polymethylphenylsiloxane,
Polydiethylsiloxane, polyethylene wax, oxidized polyethylene wax, the one or more of of chlorinated paraffin form.
9. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: the cream
Change dispersing agent by α-sodium olefin sulfonate, aromatic polyvinylether, polyethylene glycol monooleate, octadecanol polyoxyethylene ether, polyoxy
Ethylene laurel ether, polyoxyethylene sorbitol acid anhydride tristearate, nonylphenol polyoxyethylene ether, one kind of castor oil polyoxyethylene ether
Or several compositions.
10. the naphthalene water reducer matching preparation method for subtracting jelly according to claim 1, it is characterised in that: described
Sulfate radical precipitating reagent is barium nitrate, barium chloride, barium hydroxide, barium acetate, barium sulphide, three hydration barium rhodanides, barium iodide, acetic acid
One kind or several of barium, butyric acid barium, barium propionate, lead chloride, plumbi nitras, lead oxalate, lead formate, lead acetate, lead bromate, secondary lead acetate
Kind composition.
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| CN110204240A (en) * | 2019-07-16 | 2019-09-06 | 江苏苏博特新材料股份有限公司 | A kind of organic amphiprotic polymeric activity excitant and preparation method thereof and its application in large dosage admixture cement-based material |
| CN110386773A (en) * | 2019-06-28 | 2019-10-29 | 浙江老虎山建材有限公司 | A kind of concrete subtracts the preparation method of jelly |
| CN111825368A (en) * | 2019-04-18 | 2020-10-27 | 安徽海盾建材有限公司 | Concrete with good workability and preparation method thereof |
| CN113121771A (en) * | 2019-12-30 | 2021-07-16 | 江苏苏博特新材料股份有限公司 | Air-entraining modified naphthalene water reducer and preparation method thereof |
| CN115819005A (en) * | 2022-11-15 | 2023-03-21 | 安徽海螺材料科技股份有限公司 | Modified alcohol amine efficient cement grinding aid and preparation method thereof |
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