CN110015861A - A kind of cementitious composite dispersing agent - Google Patents
A kind of cementitious composite dispersing agent Download PDFInfo
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- CN110015861A CN110015861A CN201910206252.2A CN201910206252A CN110015861A CN 110015861 A CN110015861 A CN 110015861A CN 201910206252 A CN201910206252 A CN 201910206252A CN 110015861 A CN110015861 A CN 110015861A
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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
- 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
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
-
- 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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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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
- C04B2103/40—Surface-active agents, dispersants
- C04B2103/408—Dispersants
Abstract
The invention discloses a kind of cementitious composite dispersing agents, belong to technical field of chemical industry.The present invention solves the problems, such as to commonly use cement dispersants dispersion effect at present and influences interior mechanics performance.The present invention can keep low critical micelle concentration, and lipophilic group therein can be adsorbed on cement surface, and hydrophilic group can preferably improve the dispersion effect of cement in conjunction with water.It hydrolyzes the silicone hydroxyl generated and composite diffusion makees institute's hydroxyl in materials B and forms hydrogen bond, enhance the stability of dispersion, and improve internal connecting forces, the strong active group carboxyl of polarity in acrylic acid is introduced into wherein humic acid molecule, cooperate the influence of acrylic acid-grafted bring steric hindrance, improve the viscosity reducing effect of made siliceous processed material, improve the dispersibility being blended inside material, reduce the generation of precipitating and dispersion unevenness, improve cement cohesive strength, so that interior mechanics performance is further promoted after cement is blended.
Description
Technical field
The invention belongs to technical field of chemical industry, in particular to a kind of cementitious composite dispersing agent.
Background technique
Cement is used mostly at civil construction scene, water is added in cement, cement slurry is made, mix fine aggregate wherein
Mortar is obtained after sand, then mixing coarse aggregate rubble obtains concrete thereto, they are used in building element and building, fire resisting mostly
Wall etc. is many on the way, and dosage is also big.For these cement slurries, mortar and concrete, reacted by cement with water,
Intensity is generated by agglomerating and solidifying, so the operating characteristics after addition water reduces as time goes by.Especially
It has been strongly required to reduction concrete unit consumption of water since the socialization of the early stage deterioration problem of concrete component in 1981 to mention
Its high workability and durability, the cement additive that can having an immense impact on to cement composition quality and performance
Carry out technological innovation.
Cement dispersants, also known as water-reducing agent can reduce mixing and stirring for concrete under conditions of not influencing concrete flowability
Water consumption, or under conditions of not influencing water consumption increase concrete mix mobility, or both take into account, be that one kind has
The additive of diminishing and humidification.It the use of the main purpose of cement dispersants is in engineering to reduce concrete water amount, drop
Low water-cement ratio saves cement consumption, and improves its workability.
The mobile performance and intensity of concrete can be greatly improved after cement dispersants application, to improve the matter of engineering
Amount.Concrete is the maximum construction material of world's dosage, and cement dispersants have become essential addition in concrete production
Agent.Currently, developed countries and regions, cement dispersants dosage accounts for 80% or more in concrete.Cement dispersants mainly have following several
Kind: modified lignosulfonate water reducing agent；Naphthalene sulfonic acid-formaldehyde condensation product water-reducing agent；Melamine water reducing agent；Sulfamate subtracts
Aqua；Aliphatic water reducing agent；Carboxylic acid graft copolymer water-reducing agent.Polycarboxylate graft copolymer water-reducing agent is height novel at present
Performance water-reducing agent, it has the advantage that water-reducing rate is high, little loss of slump, later strength is high: 28d gain in strength 40% with
On.Volume is smaller, generally below 1%.Though mixing the Zeta potential value of the cement slurry of such water-reducing agent, its cement particle surface
It is so smaller than naphthalene system or melamine, but the slump was not lost substantially at 1 ~ 2 hour.The reason is that carboxylic acid ion meeting and cement slurry
Ca in body2+In conjunction with, slowed down hydration rate, due to hyrate it is relatively less without cause quickly reduce water-reducing agent concentration.In addition with
Polycarboxylate is related in the suction type of cement surface, its main side chain molecular architecture determine it cement surface spatially
Zigzag absorption, different from the Level Adsorption mode of naphthalene system, therefore more three-dimensional current potential protective effect, and can keep the long period
Stably dispersing state.Such water-reducing agent is suitable for high performance concrete.Its shortcomings that, is: poor compatibility, to concrete can be pre-
Opinion property is poor, such as: when poly carboxylic acid series water reducer and other additives are used in conjunction with, concrete slump loss is too fast and easily occurs
Phenomena such as fast hard, there are cement and chemical admixture consistency problem；In the concrete using high-performance water reducing agent, work as unit
Discharge reduction, when the slump increases, it occur frequently that following problems: water-reducing agent dosage is excessive, concrete is sticky too greatly, isolates
Excreting water phenomenon, pumping difficulties.And poly carboxylic acid series water reducer synthesis technology is complicated, and raw material is more expensive.
Summary of the invention
The technical problems to be solved by the invention: it for common cementitious composite dispersing agent dispersion effect at present and influences internal
The problem of mechanical property, provides a kind of cementitious composite dispersing agent.
Above-mentioned technical problem is solved, the present invention is using technical solution as described below:
A kind of cementitious composite dispersing agent, according to the mass fraction, including following component: 3 ~ 7 parts of fillers, 20 ~ 45 parts of composite diffusions are made
Materials A, 12 ~ 20 parts of composite diffusions make materials B.
The composite diffusion makees the preparation method of materials A, includes the following steps:
(1) in 25 ~ 35 DEG C, 1:7 ~ 12:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst mixing, leads to nitrogen protection,
Stirring, obtains mixing, takes mixing that 1,1,1,3,3,5, the 5- seven methylsiloxane mixing of mixing quality 30 ~ 55% is added, is warming up to 60
~ 70 DEG C, heat preservation is warming up to 80 ~ 95 DEG C, and reflux obtains reactant, reactant is taken to wash, dry, silane treatment object is obtained, in 50 ~ 65
DEG C, it takes silane treatment object 5:2:12 in mass ratio ~ 18 that dimethylaminoethyl methacrylate is added and is mixed, lead to nitrogen protection,
Heat preservation, discharging, obtains reaction material, takes reaction material 1:3 ~ 5 in mass ratio to be cleaned with mixing washing lotion, is dried in vacuo, derives from and make siliceous list
Body；
(2) in 30 ~ 45 DEG C, 4 ~ 8:3:60 ~ 80 are derived from silicon-containing monomer processed, acrylamide, water mixing in mass ratio, lead to nitrogen and protect
Shield is warming up to 60 ~ 75 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 8 ~ 15% is added is mixed, heat preservation,
It is cooling, reaction solution is obtained, 1:2 in mass ratio ~ 4 is extracted reaction solution and acetone mixing is added, filter, take filter residue to be freeze-dried, material must be lyophilized,
Take freeze-drying material 6 ~ 10:3:1 in mass ratio that carbon boron carrier, additive mixing is added, shearing dispersion makees materials A to get composite diffusion.
Catalyst in the step (1): 1:40 ~ 60 take chloroplatinic acid, isopropanol mixing in mass ratio, refrigerate to get urging
Agent.
Mixing washing lotion in the step (1): 3 ~ 6:5 takes ether, ethanol solution mixing to wash to get mixing by volume
Liquid.
Carbon boron carrier in the step (2): 3:0.2:13 ~ 18 take boric acid, xanthan gum, citric acid solution mixed in mass ratio
It closes, is heat-treated in 80 ~ 100 DEG C, obtains gelinite, take gelinite to heat in high temperature furnace with 700 ~ 800 DEG C, obtain presoma, take forerunner
For body with 1200 ~ 1500 DEG C in vacuum drying oven, heat treatment obtains micro mist, takes micro mist 1:7 in mass ratio ~ 16 that dopamine solution, room is added
Temperature is impregnated, filtering, collects filter residue and drying to get carbon boron carrier.
Additive in the step (2): 3 ~ 6:1 in mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
The composite diffusion makees the preparation of materials B: 1:35 ~ 55 take potassium acrylate, NaOH solution to be mixed in mass ratio,
Liquid must be mixed, takes mixed liquid 3 ~ 7:2 in mass ratio that humic acid potassium mixing is added, is warming up to 70 ~ 85 DEG C, mixed liquid quality 0.1 is added in heat preservation
The potassium acrylate mixing of ~ 0.4% initiator, the acrylamide of mixed liquid quality 40 ~ 60%, mixed liquid quality 30 ~ 55%, heat preservation, in 65
~ 80 DEG C of rotary evaporations, vacuum concentration obtain concentrate, and 1:2 ~ 4:0.1 in mass ratio takes gellan gum, sucrose, magnesium citrate mixing to grind
Mill obtains dry blend, and 1:40 ~ 60 in mass ratio take dry blend, water mixing, and in 80 ~ 90 DEG C, shearing dispersion is stored at room temperature swelling, obtains
Glue, in mass ratio 4 ~ 8:3:0.1 take concentrate, sizing material, auxiliary material mixing, and shearing dispersion makees materials B to get composite diffusion.
The initiator: sodium peroxydisulfate, potassium peroxydisulfate, any one in ammonium persulfate.
The auxiliary material: 5 ~ 8:1:1 in mass ratio takes hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary
Material.
The filler: 5 ~ 8:1:1 in mass ratio takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide mixing to grind
Mill is to get filler.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is introduced with acrylamide, dimethyl diallyl ammonium chloride etc. for raw material with good surface and interface activity
Organic functional silicon base, the polymer with good amphipathic surface-active is made, low critical micelle concentration can be kept, it is therein
Lipophilic group can be adsorbed on cement surface, and hydrophilic group reduces interfacial free energy in conjunction with water, can increase solids and be moistened by water
Wet degree, is formed simultaneously electric double layer, so that it is separate because of electrostatic repulsion between solid particle, can preferably it facilitate to water
The improvement of mud dispersion effect；
(2) present invention prepares carbon boron carrier, with good adsorptivity, energy using boric acid, citric acid, dopamine as raw material
It is enough that ion is adsorbed in system, so that system partial charge is uneven, improve electrostatic repulsion effect, and particle
Itself also contains a small amount of hydroxyl isopolarity group, and when being cured moisture reduction, viscosity resistance increases, and causes electron transfer
It is hindered, can lead to electron transfer rate and be greatly reduced, and conductivity declines, the silicone hydroxyl and composite diffusion for hydrolyzing generation are made
Hydrogen bond is formed in materials B between institute's hydroxyl, constitutes monomolecular film, reduces the surface energy of blend, mixture can be substantially reduced
Suction-operated between material, enhances the stability of peptizaiton, and improves internal connecting forces, improves when being applied to cement to whole
The influence of mechanics performance；
(3) the strong active group carboxyl of polarity in acrylic acid is introduced into humic acid molecule therein by the present invention, improves its dispersion
Property stability, can strong ionogen, and in cement Blending Processes so that material particles surface have negative electrical charge, increase
Its strong internal oiliness molecule repulsion, cooperates the influence of acrylic acid-grafted bring steric hindrance, the cohesion between cement may make to make
While with reducing, dispersion performance is enhanced, and is conducive to disperse then to dissociate in the case where surface active ingredient acts on, is avoided occurring
Agglomeration effect, and rapid dispersion can be permeated during cement mixing, the viscosity reducing effect of made siliceous processed material is improved, because
And can reduce precipitating while improving the dispersibility being blended inside material and disperse uneven generation, the gellan gum of addition
Can the effectively stable calcium ion received in suspended dispersed cement in system, and add magnesium citrate can play chelating
Agent effect, the metal ion through chelation can play catalytic effect in the solidification process of cement, improve cement cohesive strength,
So that internal mechanical property is further promoted after cement blending processing, thus use value is high, has a extensive future.
Specific embodiment
Catalyst: 1:40 ~ 60 take chloroplatinic acid, isopropanol mixing in mass ratio, in 2 ~ 5 DEG C of refrigerator cold-storages to get catalyst.
Mixing washing lotion: the ethanol solution mixing that 3 ~ 6:5 takes ether by volume, volume fraction is 70% is washed to get mixing
Liquid.
Initiator: sodium peroxydisulfate, potassium peroxydisulfate, any one in ammonium persulfate.
Auxiliary material: 5 ~ 8:1:1 in mass ratio takes hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary material.
The preparation of carbon boron carrier: 3:0.2:13 ~ 18 take boric acid, xanthan gum, the citric acid that mass fraction is 20% in mass ratio
Solution mixing, in 80 ~ 100 DEG C of 20 ~ 45min of heat treatment, obtain gelinite, take gelinite in high temperature furnace with 700 ~ 800 DEG C heat 20 ~
35min obtains presoma, takes presoma in vacuum drying oven with 1200 ~ 1500 DEG C, is heat-treated 1 ~ 3h, obtains micro mist, take micro mist by quality
Than the dopamine solution that mass fraction 12% is added in 1:7 ~ 16,1 ~ 3h of soaking at room temperature, it is dry in 65 ~ 80 DEG C of baking ovens to collect filter residue for filtering
It is dry to get carbon boron carrier.
Filler: 5 ~ 8:1:1 in mass ratio takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide to mix, and grinding 1 ~
3h is to get filler.
Additive: 3 ~ 6:1 in mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
Composite diffusion makees the preparation method of materials A, includes the following steps:
(1) in 25 ~ 35 DEG C, 1:7 ~ 12:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst to mix in reaction kettle, leads to
Nitrogen protection obtains mixing with 600 ~ 900r/min, 35 ~ 60min of magnetic agitation, and mixing is taken to be added the 1,1 of mixing quality 30 ~ 55%,
The mixing of 1,3,3,5,5- seven methylsiloxane, is warming up to 60 ~ 70 DEG C, keeps the temperature 35 ~ 55min, is warming up to 80 ~ 95 DEG C, and flow back 2 ~ 4h,
Reactant is obtained, takes reactant to be washed with water 2 ~ 4 times, obtains silane treatment object, in 50 ~ 65 DEG C, take silane treatment object in mass ratio 5:
2:12 ~ 18 is added dimethylaminoethyl methacrylate and is mixed in reaction kettle, leads to nitrogen protection, keeps the temperature 55 ~ 65h, and discharging obtains
Reaction material, take reaction material 1:3 ~ 5 in mass ratio with mixing washing lotion clean after, in 45 ~ 55 DEG C vacuum drying 20 ~ for 24 hours, contain derived from system
Silicon monomer；
(2) in 30 ~ 45 DEG C, 4 ~ 8:3:60 ~ 80 are derived from silicon-containing monomer processed, acrylamide, water and mix in reaction kettle in mass ratio, lead to
Nitrogen protection is warming up to 60 ~ 75 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 8 ~ 15% is added is mixed,
2 ~ 4h is kept the temperature, cooled to room temperature obtains reaction solution, extracts reaction solution 1:2 in mass ratio ~ 4 and acetone mixing is added, filter, take filter
Dry 4 ~ the 8h of -40 DEG C of freeze driers of slag use, must be lyophilized material, take freeze-drying material 6 ~ 10:3:1 in mass ratio that carbon boron carrier is added, adds
Add agent to mix, 8 ~ 15min of dispersion is sheared with 2000 ~ 4000r/min and makees materials A to get composite diffusion.
Composite diffusion makees the preparation of materials B: the NaOH that 1:35 ~ 55 take potassium acrylate in mass ratio, mass fraction is 6% is molten
Liquid is mixed in ice-water bath, with 500 ~ 800r/min, 35 ~ 60min of magnetic agitation, obtains mixed liquid, and mixed liquid 3 ~ 7:2 in mass ratio is taken to be added
Humic acid potassium mixing, is warming up to 70 ~ 85 DEG C, keeps the temperature 20 ~ 45min, and the initiator of mixed liquid quality 0.1 ~ 0.4% is added, mixes liquid quality
The potassium acrylate mixing of 40 ~ 60% acrylamide, mixed liquid quality 30 ~ 55%, keeps the temperature 1 ~ 3h, in 65 ~ 80 DEG C of rotary evaporations, vacuum
The 25 ~ 45% of original volume are concentrated into, concentrate is obtained, 1:2 ~ 4:0.1 in mass ratio takes gellan gum, sucrose, magnesium citrate mixed in mortar
It closes, 1 ~ 3h is ground with 350 ~ 550r/min, obtain dry blend, 1:40 ~ 60 in mass ratio take dry blend, water mixing, in 80 ~ 90 DEG C,
7 ~ 12min of dispersion is sheared with 1200 ~ 2500r/min, 1 ~ 3h of swelling is stored at room temperature, obtains glue, 4 ~ 8:3:0.1 in mass ratio takes dense
Contracting object, sizing material, auxiliary material mixing shear 7 ~ 13min of dispersion with 1500 ~ 2500r/min and make materials B to get composite diffusion.
A kind of cementitious composite dispersing agent, according to the mass fraction, including following component: 3 ~ 7 parts of fillers, 20 ~ 45 parts compound point
Dissipate make materials A, 12 ~ 20 parts of composite diffusions make materials B.
Embodiment 1
Catalyst: 1:40 in mass ratio takes chloroplatinic acid, isopropanol mixing, in 2 DEG C of refrigerator cold-storages to get catalyst.
Mixing washing lotion: the ethanol solution mixing that 3:5 takes ether by volume, volume fraction is 70% is to get mixing washing lotion.
Initiator: sodium peroxydisulfate.
Auxiliary material: 5:1:1 in mass ratio takes hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary material.
The preparation of carbon boron carrier: 3:0.2:13 in mass ratio takes boric acid, xanthan gum, mass fraction molten for 20% citric acid
Liquid mixing, in 80 DEG C of heat treatment 20min, obtains gelinite, gelinite is taken, with 700 DEG C of heating 20min, to obtain presoma in high temperature furnace,
It takes presoma in vacuum drying oven with 1200 DEG C, is heat-treated 1h, obtains micro mist, take micro mist 1:7 in mass ratio that mass fraction 12% is added
Dopamine solution, soaking at room temperature 1h, filtering collect filter residue in 65 DEG C of oven dryings to get carbon boron carrier.
Filler: 5:1:1 in mass ratio takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide mixing, grinds 1h,
Up to filler.
Additive: 3:1 in mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
Composite diffusion makees the preparation method of materials A, includes the following steps:
(1) in 25 DEG C, 1:7:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst to mix in reaction kettle, leads to nitrogen and protects
Shield, with 600r/min magnetic agitation 35min, obtains mixing, takes mixing that 1,1,1,3,3,5,5- seven methyl of mixing quality 30% is added
Siloxanes mixing, is warming up to 60 DEG C, keeps the temperature 35min, is warming up to 80 DEG C, and flow back 2h, obtains reactant, reactant is taken to be washed with water 2
It is secondary, silane treatment object is obtained, in 50 DEG C, takes silane treatment object 5:2:12 in mass ratio that dimethylaminoethyl methacrylate is added in anti-
It answers kettle to be mixed, leads to nitrogen protection, keep the temperature 55h, discharging obtains reaction material, takes reaction material 1:3 in mass ratio clear with mixing washing lotion
After washing, in 45 DEG C of vacuum drying 20h, derived from silicon-containing monomer processed；
(2) in 30 DEG C, 4:3:60 in mass ratio is derived from silicon-containing monomer processed, acrylamide, water and mixes in reaction kettle, leads to nitrogen and protects
Shield is warming up to 60 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 8% is added is mixed, and keeps the temperature 2h, natural
It is cooled to room temperature, obtains reaction solution, extract reaction solution 1:2 in mass ratio and acetone mixing is added, filter, take -40 DEG C of filter residue use freezings dry
The dry 4h of dry machine, must be lyophilized material, take freeze-drying material 6:3:1 in mass ratio that carbon boron carrier, additive mixing is added, with 2000r/min
Shearing dispersion 8min makees materials A to get composite diffusion.
Composite diffusion makees the preparation of materials B: 1:35 in mass ratio take potassium acrylate, mass fraction be 6% NaOH solution in
Ice-water bath mixing, with 500r/min magnetic agitation 35min, obtains mixed liquid, takes mixed liquid 3:2 in mass ratio that humic acid potassium mixing is added,
70 DEG C are warming up to, 20min is kept the temperature, the initiator of mixed liquid quality 0.1%, the acrylamide of mixed liquid quality 40%, mixed liquid quality is added
30% potassium acrylate mixing, heat preservation 1h are concentrated in vacuo to the 25% of original volume, obtain concentrate, by quality in 65 DEG C of rotary evaporations
It takes gellan gum, sucrose, magnesium citrate to mix in mortar than 1:2:0.1,1h is ground with 350r/min, obtains dry blend, in mass ratio
1:40 takes dry blend, water mixing, in 80 DEG C, shears dispersion 7min with 1200r/min, is stored at room temperature swelling 1h, glue is obtained, by matter
Amount takes concentrate, sizing material, auxiliary material mixing than 4:3:0.1, shears dispersion 7min with 1500r/min and makees materials to get composite diffusion
B。
A kind of cementitious composite dispersing agent, according to the mass fraction, including following component: 3 parts of fillers, 20 parts of composite diffusion effects
Material A, 12 parts of composite diffusions make materials B.
Embodiment 2
Catalyst: 1:50 in mass ratio takes chloroplatinic acid, isopropanol mixing, in 3 DEG C of refrigerator cold-storages to get catalyst.
Mixing washing lotion: the ethanol solution mixing that 4:5 takes ether by volume, volume fraction is 70% is to get mixing washing lotion.
Initiator: potassium peroxydisulfate.
Auxiliary material: 6:1:1 in mass ratio takes hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary material.
The preparation of carbon boron carrier: 3:0.2:15 in mass ratio takes boric acid, xanthan gum, mass fraction molten for 20% citric acid
Liquid mixing, in 90 DEG C of heat treatment 35min, obtains gelinite, gelinite is taken, with 750 DEG C of heating 30min, to obtain presoma in high temperature furnace,
It takes presoma in vacuum drying oven with 1400 DEG C, is heat-treated 2h, obtains micro mist, take micro mist 1:11 in mass ratio that mass fraction 12% is added
Dopamine solution, soaking at room temperature 2h, filtering, collect filter residue in 75 DEG C of oven dryings to get carbon boron carrier.
Filler: 7:1:1 in mass ratio takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide mixing, grinds 2h,
Up to filler.
Additive: 5:1 in mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
Composite diffusion makees the preparation method of materials A, includes the following steps:
(1) in 30 DEG C, 1:10:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst to mix in reaction kettle, leads to nitrogen and protects
Shield, with 750r/min magnetic agitation 45min, obtains mixing, takes mixing that 1,1,1,3,3,5,5- seven methyl of mixing quality 40% is added
Siloxanes mixing, is warming up to 65 DEG C, keeps the temperature 50min, is warming up to 90 DEG C, and flow back 3h, obtains reactant, reactant is taken to be washed with water 3
It is secondary, silane treatment object is obtained, in 60 DEG C, takes silane treatment object 5:2:15 in mass ratio that dimethylaminoethyl methacrylate is added in anti-
It answers kettle to be mixed, leads to nitrogen protection, keep the temperature 60h, discharging obtains reaction material, takes reaction material 1:4 in mass ratio clear with mixing washing lotion
After washing, in 50 DEG C of vacuum drying 22h, derived from silicon-containing monomer processed；
(2) in 40 DEG C, 6:3:70 in mass ratio is derived from silicon-containing monomer processed, acrylamide, water and mixes in reaction kettle, leads to nitrogen and protects
Shield is warming up to 70 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 11% is added is mixed, and keeps the temperature 3h, natural
It is cooled to room temperature, obtains reaction solution, extract reaction solution 1:3 in mass ratio and acetone mixing is added, filter, take -40 DEG C of filter residue use freezings dry
The dry 6h of dry machine, must be lyophilized material, take freeze-drying material 8:3:1 in mass ratio that carbon boron carrier, additive mixing is added, with 3000r/min
Shearing dispersion 11min makees materials A to get composite diffusion.
Composite diffusion makees the preparation of materials B: 1:45 in mass ratio take potassium acrylate, mass fraction be 6% NaOH solution in
Ice-water bath mixing, with 650r/min magnetic agitation 50min, obtains mixed liquid, takes mixed liquid 5:2 in mass ratio that humic acid potassium mixing is added,
80 DEG C are warming up to, 30min is kept the temperature, the initiator of mixed liquid quality 0.3%, the acrylamide of mixed liquid quality 50%, mixed liquid quality is added
45% potassium acrylate mixing, heat preservation 2h are concentrated in vacuo to the 30% of original volume, obtain concentrate, by quality in 75 DEG C of rotary evaporations
It takes gellan gum, sucrose, magnesium citrate to mix in mortar than 1:3:0.1,1 ~ 3h is ground with 450r/min, dry blend is obtained, by quality
Dry blend, water mixing are taken than 1:50, in 85 DEG C, dispersion 10min is sheared with 1800r/min, swelling 2h is stored at room temperature, obtains glue,
6:3:0.1 in mass ratio takes concentrate, sizing material, auxiliary material mixing, shears dispersion 10min with 2000r/min to get composite diffusion work
Materials B.
A kind of cementitious composite dispersing agent, according to the mass fraction, including following component: 5 parts of fillers, 30 parts of composite diffusion effects
Material A, 16 parts of composite diffusions make materials B.
Embodiment 3
Catalyst: 1:60 in mass ratio takes chloroplatinic acid, isopropanol mixing, in 5 DEG C of refrigerator cold-storages to get catalyst.
Mixing washing lotion: the ethanol solution mixing that 6:5 takes ether by volume, volume fraction is 70% is to get mixing washing lotion.
Initiator: ammonium persulfate.
Auxiliary material: 8:1:1 in mass ratio takes hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary material.
The preparation of carbon boron carrier: 3:0.2:18 in mass ratio takes boric acid, xanthan gum, mass fraction molten for 20% citric acid
Liquid mixing, in 100 DEG C of heat treatment 45min, obtains gelinite, gelinite is taken, with 800 DEG C of heating 35min, to obtain presoma in high temperature furnace,
It takes presoma in vacuum drying oven with 1500 DEG C, is heat-treated 3h, obtains micro mist, take micro mist 1:16 in mass ratio that mass fraction 12% is added
Dopamine solution, soaking at room temperature 3h, filtering, collect filter residue in 80 DEG C of oven dryings to get carbon boron carrier.
Filler: 8:1:1 in mass ratio takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide mixing, grinds 3h,
Up to filler.
Additive: 6:1 in mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
Composite diffusion makees the preparation method of materials A, includes the following steps:
(1) in 35 DEG C, 1:12:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst to mix in reaction kettle, leads to nitrogen and protects
Shield, with 900r/min magnetic agitation 60min, obtains mixing, takes mixing that 1,1,1,3,3,5,5- seven methyl of mixing quality 55% is added
Siloxanes mixing, is warming up to 70 DEG C, keeps the temperature 55min, is warming up to 95 DEG C, and flow back 4h, obtains reactant, reactant is taken to be washed with water 4
It is secondary, silane treatment object is obtained, in 65 DEG C, takes silane treatment object 5:2:18 in mass ratio that dimethylaminoethyl methacrylate is added in anti-
It answers kettle to be mixed, leads to nitrogen protection, keep the temperature 65h, discharging obtains reaction material, takes reaction material 1:5 in mass ratio clear with mixing washing lotion
After washing, for 24 hours in 55 DEG C of vacuum drying, derived from silicon-containing monomer processed；
(2) in 45 DEG C, 8:3:80 in mass ratio is derived from silicon-containing monomer processed, acrylamide, water and mixes in reaction kettle, leads to nitrogen and protects
Shield is warming up to 75 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 15% is added is mixed, and keeps the temperature 4h, natural
It is cooled to room temperature, obtains reaction solution, extract reaction solution 1:4 in mass ratio and acetone mixing is added, filter, take -40 DEG C of filter residue use freezings dry
The dry 8h of dry machine, must be lyophilized material, take freeze-drying material 10:3:1 in mass ratio that carbon boron carrier, additive mixing is added, with 4000r/min
Shearing dispersion 15min makees materials A to get composite diffusion.
Composite diffusion makees the preparation of materials B: 1:55 in mass ratio take potassium acrylate, mass fraction be 6% NaOH solution in
Ice-water bath mixing, with 800r/min magnetic agitation 60min, obtains mixed liquid, takes mixed liquid 7:2 in mass ratio that humic acid potassium mixing is added,
85 DEG C are warming up to, 45min is kept the temperature, the initiator of mixed liquid quality 0.4%, the acrylamide of mixed liquid quality 60%, mixed liquid quality is added
55% potassium acrylate mixing, heat preservation 3h are concentrated in vacuo to the 45% of original volume, obtain concentrate, by quality in 80 DEG C of rotary evaporations
It takes gellan gum, sucrose, magnesium citrate to mix in mortar than 1:4:0.1,3h is ground with 550r/min, obtains dry blend, in mass ratio
1:60 takes dry blend, water mixing, in 90 DEG C, shears dispersion 12min with 2500r/min, is stored at room temperature swelling 3h, obtains glue, press
Mass ratio 8:3:0.1 takes concentrate, sizing material, auxiliary material mixing, shears dispersion 13min with 2500r/min to get composite diffusion effect
Expect B.
A kind of cementitious composite dispersing agent, according to the mass fraction, including following component: 7 parts of fillers, 45 parts of composite diffusion effects
Material A, 20 parts of composite diffusions make materials B.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that filler.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that composite diffusion makees materials A.
Comparative example 3: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that composite diffusion makees materials B.
Comparative example 4: the cementitious composite dispersing agent of company, Suzhou City production.
Embodiment is tested with cementitious composite dispersing agent obtained by comparative example according to GB/T14825-2006, test result
As shown in table 1.
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Viscosity (20s-1) | 581 | 573 | 572 | 574 | 589 | 770 | 780 |
| Mobility (mL/s) | 1.21 | 1.23 | 1.26 | 1.24 | 1.21 | 0.31 | 0.34 |
| Dispersibility | Soluble, uniformity is good | Soluble, uniformity is good | Soluble, uniformity is good | Soluble, uniformity is good | Soluble, uniformity is good | It not readily dissolves, uniformity is poor | It not readily dissolves, uniformity is poor |
| Stability (for 24 hours) | Without precipitating | Without precipitating | Without precipitating | Without precipitating | Without precipitating | There is precipitating to occur | There is precipitating to occur |
In summary, cementitious composite dispersing agent of the invention is more preferable compared to commercial product effect, is worth promoting.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of cementitious composite dispersing agent, according to the mass fraction, which is characterized in that including following component: 3 ~ 7 parts of fillers, 20 ~ 45
Composite diffusion makees materials A to part, 12 ~ 20 parts of composite diffusions make materials B.
2. a kind of cementitious composite dispersing agent according to claim 1, which is characterized in that the composite diffusion makees the system of materials A
Preparation Method includes the following steps:
(1) in 25 ~ 35 DEG C, 1:7 ~ 12:0.03 in mass ratio takes the bromo- 1- butylene of 4-, toluene, catalyst mixing, leads to nitrogen protection,
Stirring, obtains mixing, takes mixing that 1,1,1,3,3,5, the 5- seven methylsiloxane mixing of mixing quality 30 ~ 55% is added, is warming up to 60
~ 70 DEG C, heat preservation is warming up to 80 ~ 95 DEG C, and reflux obtains reactant, reactant is taken to wash, dry, silane treatment object is obtained, in 50 ~ 65
DEG C, it takes silane treatment object 5:2:12 in mass ratio ~ 18 that dimethylaminoethyl methacrylate is added and is mixed, lead to nitrogen protection,
Heat preservation, discharging, obtains reaction material, takes reaction material 1:3 ~ 5 in mass ratio to be cleaned with mixing washing lotion, is dried in vacuo, derives from and make siliceous list
Body；
(2) in 30 ~ 45 DEG C, 4 ~ 8:3:60 ~ 80 are derived from silicon-containing monomer processed, acrylamide, water mixing in mass ratio, lead to nitrogen and protect
Shield is warming up to 60 ~ 75 DEG C, and the two NSC 18620 hydrochloric acid sodium of azo that self-control silicon-containing monomer quality 8 ~ 15% is added is mixed, heat preservation,
It is cooling, reaction solution is obtained, 1:2 in mass ratio ~ 4 is extracted reaction solution and acetone mixing is added, filter, take filter residue to be freeze-dried, material must be lyophilized,
Take freeze-drying material 6 ~ 10:3:1 in mass ratio that carbon boron carrier, additive mixing is added, shearing dispersion makees materials A to get composite diffusion.
3. a kind of cementitious composite dispersing agent according to claim 2, which is characterized in that the catalyst in the step (1): press
Mass ratio 1:40 ~ 60 take chloroplatinic acid, isopropanol mixing, refrigerate to get catalyst.
4. a kind of cementitious composite dispersing agent according to claim 2, which is characterized in that the mixing washing lotion in the step (1):
3 ~ 6:5 takes ether, ethanol solution mixing to get mixing washing lotion by volume.
5. a kind of cementitious composite dispersing agent according to claim 2, which is characterized in that the carbon boron carrier in the step (2):
3:0.2:13 ~ 18 take boric acid, xanthan gum, citric acid solution mixing in mass ratio, are heat-treated in 80 ~ 100 DEG C, obtain gelinite, take
Gelinite is heated in high temperature furnace with 700 ~ 800 DEG C, is obtained presoma, is taken presoma in vacuum drying oven with 1200 ~ 1500 DEG C, at heat
Reason, obtain micro mist, take micro mist 1:7 in mass ratio ~ 16 be added dopamine solution, soaking at room temperature, filtering, collect filter residue and drying to get
Carbon boron carrier.
6. a kind of cementitious composite dispersing agent according to claim 2, which is characterized in that the additive in the step (2): press
3 ~ 6:1 of mass ratio takes microcrystalline wax, stearic acid mixing to get additive.
7. a kind of cementitious composite dispersing agent according to claim 1, which is characterized in that the composite diffusion makees the system of materials B
Standby: 1:35 ~ 55 take potassium acrylate, NaOH solution to be mixed in mass ratio, obtain mixed liquid, and mixed liquid 3 ~ 7:2 in mass ratio is taken to be added
Humic acid potassium mixing, is warming up to 70 ~ 85 DEG C, and heat preservation is added the initiator of mixed liquid quality 0.1 ~ 0.4%, mixes liquid quality 40 ~ 60%
The potassium acrylate mixing of acrylamide, mixed liquid quality 30 ~ 55%, heat preservation, in 65 ~ 80 DEG C of rotary evaporations, vacuum concentration must be concentrated
Object, in mass ratio 1:2 ~ 4:0.1 take gellan gum, sucrose, magnesium citrate mixed grinding, obtain dry blend, and 1:40 ~ 60 in mass ratio take
Dry blend, water mixing, in 80 ~ 90 DEG C, shearing dispersion is stored at room temperature swelling, obtains glue, 4 ~ 8:3:0.1 in mass ratio takes concentration
Object, sizing material, auxiliary material mixing, shearing dispersion make materials B to get composite diffusion.
8. a kind of cementitious composite dispersing agent according to claim 7, which is characterized in that the initiator: sodium peroxydisulfate, over cure
Any one in sour potassium, ammonium persulfate.
9. a kind of cementitious composite dispersing agent according to claim 7, which is characterized in that the auxiliary material: 5 ~ 8:1:1 in mass ratio
Take hydroxyapatite, polyvinylpyrrolidone, lecithin mixing to get auxiliary material.
10. a kind of cementitious composite dispersing agent according to claim 1, which is characterized in that the filler: 5 ~ 8:1 in mass ratio:
1 takes talcum powder, polyvinyl alcohol, cetyl trimethylammonium bromide mixed grinding to get filler.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299747A (en) * | 2019-11-20 | 2021-02-02 | 株洲市中建新材料有限公司 | Cement dispersant with high dispersibility |
| CN113087438A (en) * | 2021-04-06 | 2021-07-09 | 杭州邦利建材有限公司 | High-performance compound water reducing agent and preparation method thereof |
| CN115477519A (en) * | 2022-10-13 | 2022-12-16 | 中路交科科技股份有限公司 | High-impermeability shield tunnel synchronous grouting material, preparation and use method |
-
2019
- 2019-03-19 CN CN201910206252.2A patent/CN110015861A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299747A (en) * | 2019-11-20 | 2021-02-02 | 株洲市中建新材料有限公司 | Cement dispersant with high dispersibility |
| CN113087438A (en) * | 2021-04-06 | 2021-07-09 | 杭州邦利建材有限公司 | High-performance compound water reducing agent and preparation method thereof |
| CN113087438B (en) * | 2021-04-06 | 2022-06-21 | 杭州邦利建材有限公司 | High-performance compound water reducing agent and preparation method thereof |
| CN115477519A (en) * | 2022-10-13 | 2022-12-16 | 中路交科科技股份有限公司 | High-impermeability shield tunnel synchronous grouting material, preparation and use method |
| CN115477519B (en) * | 2022-10-13 | 2023-11-17 | 中路交科科技股份有限公司 | High-impermeability shield tunnel synchronous grouting material, preparation and use methods |
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