CN106866018A - A kind of air entrained concrete activity excitant and preparation method thereof - Google Patents
A kind of air entrained concrete activity excitant and preparation method thereof Download PDFInfo
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- CN106866018A CN106866018A CN201611193630.0A CN201611193630A CN106866018A CN 106866018 A CN106866018 A CN 106866018A CN 201611193630 A CN201611193630 A CN 201611193630A CN 106866018 A CN106866018 A CN 106866018A
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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
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Abstract
The invention discloses a kind of air entrained concrete activity excitant and preparation method thereof, matched by weight by following components and constituted：Purified water, bodied ferric sulfate, hydroxy succinic acid, the monoester disodium salts of sulfosuccinic acid AEO 9, N, N bis- (polyoxyethylene) P toluenesulfonic acids acid amides, high-strength αsemiwatergypsum, the sulfonic acid of 1 amino anthraquinones 2,3,5 syringol, chromium nanoparticle, the tectoquinone of 1 amino 2,2 ((nitrobenzophenone of 4 chlorine 2) azo) oxo butyramides of N (4 ethoxyl phenenyl) 3, the anthraquinone formic acid of 1 amino, 4 nitro 2.The invention advantage is：Volume has excitation no more than the 20% of desulfurization flyash quality for air entrained concrete construction material；There is excitation for the normal concrete mixed with flyash, miberal powder, it is possible to increase the compression strength of air entrained concrete construction material and normal concrete；With stable chemical nature, it is applicable that wide, pH value range is wide, firm rate is high；The consumption of cement is reduced, flyash, the incorporation of miberal powder is improved.
Description
Technical field
The invention belongs to additives for building materials field, more particularly to a kind of air entrained concrete activity excitant and its preparation
Method.
Background technology
The coal consumption of production of construction materials industry sustainable growth, causes AND ENERGY RESOURCES CONSUMPTION IN CHINA rapidly to increase, the thermoelectricity dress of China
Machine capacity showed explosive growth from 2002, therefore, carbon dioxide, sulfur dioxide (SO2) emissions also increased within past 8 years
2.5 times are grown.Often consuming 40 tons of coals will produce 0.1 ton of carbon dioxide, sulfur dioxide, and the random discharge of Ash Field of Thermal Power Plant is not
It is only huge, while also creating flyash (containing heavy metal, radioactive substance) pollution, air pollution, water pollution, soil dirt
The environmental disruption and social influence of many aspects such as dye, human health damage and geological disaster.Therefore, increase to flyash
The research and development dealt carefully with and comprehensively utilize seem and become more and more important.
Used in aerated bricks are produced by high-effect exciting agent, it is possible to reduce pollution and resource that manufacture of cement is brought
Consumption, as it is a kind of substitute cement construction material exciting agent, have broad application prospects.
A kind of ground slag air entrained concrete of patent CN 102351454 excites stabilizer, based on desulfurated plaster and MgO
Component is wanted, is modified component with the sodium sulphate no more than 5%wt and the quick lime no more than 5%wt, improve the levigate ore deposit of large dosage
The early strength and volume stability of slag aerated concrete.
The slag-fly ash complex solid exciting agents of patent CN 102627426 and its production method, the exciting agent include hydrogen
Sodium oxide molybdena, sodium carbonate and low modulus liquid soluble glass and modifying agent (polyacrylamide or Quadrafos are composite modified), improve and add
Gas concrete strength 20-30%, strengthens air entrained concrete durability.
Domestic majority admixture activity excitant contains potassium, sodium ion at present, can not while admixture activity is improved
Increase the potential hazard of alkali-aggregate reaction generation with avoiding, while generation of saltouing may be caused, destroy air entrained concrete itself
Structure, influences air entrained concrete presentation quality.
The content of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of air entrained concrete activity excitant, by following components
Proportioning is constituted by weight：240.106~465.940 parts of purified water, 32.482~74.716 parts of bodied ferric sulfate, hydroxyl amber
35.969~144.300 parts of amber acid, 31.237~48.892 parts of Disodium Sulfosuccinate AEO-9 Ester, (the polyoxy second of N, N- bis-
Alkene) 34.856~91.609 parts of-P- toluenesulfonic acids acid amides, 37.133~98.620 parts of high-strength alpha-half hydrated gypsum, 1- amino anthraquinones-
34.921~57.852 parts of 2- sulfonic acid, 3,5- 31.962~76.643 parts of syringol, chromium nanoparticle 39.184~
94.777 parts, 32.184~74.694 parts of 1- amino-2-methyls anthraquinone, 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- second
Phenyl) 22.856~65.839 parts of -3- oxos butyramide, 1- amino -4- nitro -2- anthraquinones formic acid 23.351~59.169
Part, N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-Beta-alanine methyl esters 34.768~
74.290 parts, 2- [[4- (dimethylamino) phenyl] azo] -6- methoxyl group -3- methylbenzothiazoles chloride 41.377~
85.612 parts, mass concentration for 31.226ppm~298.698ppm cetyl acid -1,2- ethylidene ester 64.686~
118.421 parts.
Further, matched by weight by following components and constituted：241.106~464.940 parts of purified water, polymerised sulphur
33.482~73.716 parts of sour iron, 36.969~143.300 parts of hydroxy succinic acid, Disodium Sulfosuccinate AEO-9 Ester
32.237~47.892 parts, 35.856~90.609 parts of N, N- bis- (polyoxyethylene)-P- toluenesulfonic acids acid amides, high-strength α-half water stone
38.133~97.620 parts of cream, 35.921~56.852 parts of 1- amino anthraquinones -2- sulfonic acid, 3,5- syringol 32.962~
75.643 parts, 40.184~93.777 parts of chromium nanoparticle, 33.184~73.694 parts of 1- amino-2-methyls anthraquinone, 2- ((4-
Chloro- 2- nitrobenzophenones) azo) 23.856~64.839 parts of-N- (4- ethoxyl phenenyls) -3- oxos butyramide, 1- amino -4- nitre
24.351~58.169 parts of base -2- anthraquinones formic acid, N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo]
Phenyl] 35.768~73.290 parts of-Beta-alanine methyl esters, 2- [[4- (dimethylamino) phenyl] azo] -6- methoxyl group -3- first
42.377~84.612 parts of base benzothiazole chloride, mass concentration is the cetyl of 32.226ppm~297.698ppm
65.686~117.421 parts of acid -1,2- ethylidene ester.
Further, the invention also discloses a kind of preparation method of air entrained concrete activity excitant, by weight
Meter, comprises the following steps：
1st step：In band stirring heated type reactor, purified water and bodied ferric sulfate are added, start band stirring heated type reaction
Mixer in device, setting speed is 33.113rpm~79.844rpm, is started with the rotary drum in stirring heated type reactor
Heater, makes temperature rise to 48.101 DEG C~49.333 DEG C, adds hydroxy succinic acid to stir, and carries out Esterification catalytic reaction
25.810~36.622 minutes, add Disodium Sulfosuccinate AEO-9 Ester, be passed through flow for 24.726m3/min~
The oxygen of 65.399m3/min 0.33~0.98 hour；Afterwards N, (the polyoxy second of N- bis- are added in band stirring heated type reactor
Alkene)-P- toluenesulfonic acid acid amides, it is again started up, with the drum heater in stirring heated type reactor, rising to temperature
65.101 DEG C~98.333 DEG C, 25.726~36.755 minutes are incubated, add high-strength alpha-half hydrated gypsum, adjustment band stirring heated type
The pH value of solution is 4.818~8.9169 in reactor, is incubated 25.726~265.755 minutes；
2nd step：Chromium nanoparticle separately is taken, by chromium nanoparticle at power is for ultrasonic wave under 5.65138KW~11.09755KW
Reason 0.31~0.98 hour, attrition grinding, and by 420.361~520.821 eye mesh screens；Chromium nanoparticle is added to another
In individual band stirring heated type reactor, it is the 1- amino-2-methyl anthraquinones of 35.252ppm~265.190ppm to add mass concentration
Dispersion chromium nanoparticle, starts with the drum heater in stirring heated type reactor, makes solution temperature 4.8726 × 10
DEG C~8.9333 × 10 DEG C between, start band stir heated type reactor in mixer, and with 4.8101 × 102rpm~
8.9844 × 102rpm speed stirring, adjustment pH value between 4.8138~8.9755, insulated and stirred 5.65 × 10-1~
11.09×10-1Hour；Stop reaction afterwards and stand 5.65 × 10~11.09 × 10 minutes, go the removal of impurity；Suspension is added
N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-Beta-alanine methyl esters, adjustment pH value exists
Between 1.726~2.399, sediment purifying water elution is formed, by centrifuge in rotating speed 4.361 × 103Rpm~9.821
×103Solid content is obtained under rpm, 2.190 × 102DEG C~3.844 × 102Dried at a temperature of DEG C, 8.361 × 10 are crossed after grinding3
~9.821 × 103Mesh sieve, it is standby；
3rd step：It is another to take chromium nanoparticle after the treatment of 1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the 2nd step, mixing
Using the irradiation of 60Co- gamma Rays after uniform, the energy of 60Co- gamma Rays irradiation for 22.430MeV~
50.999MeV, dosage are 70.41kGy~110.781kGy, irradiation time is 34.670~59.546 minutes, obtain proterties and change
1- amino anthraquinones -2- the sulfonic acid of change, 3,5- syringol and chromium nanoparticle mixture；By 1- amino anthraquinones -2- sulfonic acid,
3,5- syringol and chromium nanoparticle mixture are placed in another band stirring heated type reactor, are started band stirring and are heated
Drum heater in formula reactor, 33.18 DEG C~79.399 DEG C of design temperature starts with stirring heated type reactor
Mixer, rotating speed is 25.726rpm~420.138rpm, and pH is adjusted between 4.8430~8.9999, dehydration 34.844~
It is 48.810 minutes, standby；
4th step：1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the chromium nanometer that the proterties that 3rd step is obtained changes are micro-
Grain is well mixed, adds in the 1- amino-2-methyl anthraquinones that mass concentration is 35.252ppm~265.190ppm, and cocurrent is added to
In the band stirring heated type reactor of the 1st step, flow acceleration is 170.176mL/min~898.185mL/min；Start band stirring
Heated type reacts mechanical stirrer, and setting speed is 39.553rpm~79.804rpm；Stirring 4.8113~8.9999 minutes；Again plus
Enter 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- ethoxyl phenenyls) -3- oxo butyramides, start band stirring heated type anti-
The drum heater in device is answered, 69.751 DEG C~106.379 DEG C are warming up to, pH is adjusted between 4.8252~8.9190, led to
Enter oxygen ventilation amount for 24.113m3/ min~65.622m3/ min, insulation stands 59.749~89.743 minutes；It is again started up band
Stirring heated type reaction mechanical stirrer, rotating speed is 34.867rpm~79.65rpm, adds 1- amino -4- nitro -2- anthraquinone first
Acid, makes the hydrophobic-hydrophilic balance threshold value of its reaction solution be 5.65138~11.09755, and cause pH be adjusted to 4.8751~
Between 8.9379, insulation stands 58.188~98.437 minutes；
5th step：Start with the mixer in stirring heated type reactor, setting speed is 31.454rpm~98.386rpm, side
To N- ethyls-N- is added in band stirring heated type reactor, [[(5- nitro -2,1- benzisothiazole -3- bases) is even for 4- on stirring side
Nitrogen] phenyl]-Beta-alanine methyl esters, start with the drum heater in stirring heated type reactor, setting band stirring is heated
Temperature in formula reactor is 4.122 × 102DEG C~9.870 × 102DEG C, after being incubated 58.188~98.437 minutes, add 2-
[[4- (dimethylamino) phenyl] azo] -6- methoxyl group -3- methylbenzothiazole chlorides, Esterification catalytic reaction 25.810~
36.399 minutes；Cetyl acid -1,2- ethylidene esters are added afterwards, are started and are added with the rotary drum in stirring heated type reactor
Hot device, it is 109.122 DEG C~165.870 DEG C to set with the temperature in stirring heated type reactor, pH adjusted to 4.8113~
Between 8.9622, pressure is 0.31607MPa~0.32550MPa, and the reaction time is 0.424~0.949 hour；It is depressurized to afterwards
0MPa, is cooled to 54.31751 DEG C~59.31190 DEG C dischargings, that is, obtain a kind of air entrained concrete activity excitant.
Further, the particle diameter of the chromium nanoparticle is 39.940 μm~49.716 μm.
Further, the invention also discloses a kind of application of air entrained concrete activity excitant；This is commercially mixed with aerating
Solidifying soil activity excitant is mainly used in the application that active component in building foundation material production aerated bricks excites aspect.
Further, the building foundation material be the solidifying concrete in end, brick fuel, imogolite, lime-fly-ash loess, triphase soil,
At least one in high strength RC.
Further, a kind of air entrained concrete activity excitant is used cooperatively with double spike, a kind of aerating coagulation
Native activity excitant is 1 with double spike fit quality ratio:460.300~900.892；The double spike is：2-[[1-(2,
The chloro- 4- sulfophenyls of 5- bis-) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] -1-naphthalene sulfonic aicd sodium salt (9CL),
4- (5- amino -3- methyl isophthalic acids-phenyl -1H- pyrazoles -4- bases azo) -2,5- dichloro-s-benzene sulfonic acid list lithium salts, two [5- chloros -
3- [(4,5- dihydro -3- methyl -5- oxo -1- phenyl -1H- pyrazoles -4- bases) azo] -2- hydroxy benzene sulfonic acids base]-chromic acid base second
One kind in three kinds of hydramine sodium salt, the double spike is common commercial goods.
A kind of air entrained concrete activity excitant and preparation method thereof, the advantage is that disclosed in patent of the present invention：
(1) a kind of air entrained concrete activity excitant of the present invention, the volume in air entrained concrete construction material are being used
No more than the 20% of desulfurization flyash quality, there is excitation for air entrained concrete construction material；
(2) a kind of air entrained concrete activity excitant of the present invention, has for the normal concrete mixed with flyash, miberal powder
Excitation, it is possible to increase the compression strength of air entrained concrete construction material and normal concrete；
(3) a kind of air entrained concrete activity excitant of the present invention have stable chemical nature, be applicable wide, pH value range it is wide,
Firm rate is high；
(4) a kind of air entrained concrete activity excitant of the present invention will not produce precipitation after use, be mixed aerating is kept
In the case that solidifying soil construction material and normal concrete compression strength are constant, the consumption of cement is reduced, improve flyash, miberal powder
Incorporation, reduces the material cost of air entrained concrete construction material and normal concrete, and preparation method of the present invention is simple, need to only press
Added after mixing according to ratio in concrete, told at once, prepared by completion, operation cost is low.
Brief description of the drawings
Fig. 1 be a kind of air entrained concrete activity excitant under differential responses time conditions in testing experiment embodiment with it is right
Shearing impact Strength Changes figure as usual.
Fig. 2 be a kind of air entrained concrete activity excitant under differential responses time conditions in testing experiment embodiment with it is right
Compression shear strength variation diagram is socketed as usual.
Fig. 3 be a kind of air entrained concrete activity excitant under differential responses time conditions in testing experiment embodiment with it is right
Peel strength variation diagram as usual.
Specific embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit of the invention and essence, the modification and replacement made to the inventive method, step or condition belong to the present invention
Scope.If not specializing, the conventional meanses that technological means used is well known to those skilled in the art in embodiment.
Embodiment 1
A kind of air entrained concrete activity excitant of the present invention is prepared according to following steps, and is counted by weight：
1st step：In band stirring heated type reactor, 240.106 parts of purified water is added, 32.482 parts of bodied ferric sulfate starts
With the mixer in stirring heated type reactor, setting speed is 33.113rpm, turning in starting with stirring heated type reactor
Drum heater, makes temperature rise to 48.101 DEG C, adds 35.969 parts of hydroxy succinic acid to stir, and carries out Esterification catalytic reaction
25.810 minutes, 31.237 parts of Disodium Sulfosuccinate AEO-9 Ester is added, be passed through flow for 24.726m3The oxygen of/min
0.33 hour；Afterwards N, N- bis- (polyoxyethylene)-P- toluenesulfonic acids acid amides 34.856 are added in band stirring heated type reactor
Part, it is again started up, with the drum heater in stirring heated type reactor, temperature is risen to 65.101 DEG C, it is incubated 25.726 points
Clock, adds 37.133 parts of high-strength alpha-half hydrated gypsum, and pH value of the adjustment with solution in stirring heated type reactor is 4.818, insulation
25.726 minutes；
2nd step：Separately take 39.184 parts of chromium nanoparticle, by chromium nanoparticle power be 5.65138KW under ultrasonication
0.31 hour, attrition grinding, and by 420.361 eye mesh screens；Chromium nanoparticle is added to another band stirring heated type anti-
Answer in device, it is 32.184 parts of the 1- amino-2-methyls anthraquinone of 35.252ppm to add mass concentration, disperses chromium nanoparticle, is started
With the drum heater in stirring heated type reactor, make solution temperature at 4.8726 × 10 DEG C, start band stirring heated type
Mixer in reactor, and with 4.8101 × 102The speed stirring of rpm, adjustment pH value 4.8138, insulated and stirred 5.65 ×
10-1Hour；Stop reaction afterwards and stand 5.65 × 10 minutes, go the removal of impurity；Suspension is added into N- ethyls-N- [4- [(5- nitre
Base -2,1- benzisothiazole -3- bases) azo] phenyl] 34.768 parts of-Beta-alanine methyl esters, adjustment pH value is in 1.726, formation
Sediment purifying water elution, by centrifuge in rotating speed 4.361 × 103Solid content is obtained under rpm, 2.190 × 102DEG C temperature
The lower drying of degree, crosses 8.361 × 10 after grinding3Mesh sieve, it is standby；
3rd step：After separately taking the treatment of 34.921 parts of 1- amino anthraquinones -2- sulfonic acid, 31.962 parts of 3,5- syringol and the 2nd step
39.184 parts of chromium nanoparticle, is irradiated after being well mixed using 60Co- gamma Rays, the energy of 60Co- gamma Rays irradiation
Measure for 22.430MeV, dosage be 70.41kGy, irradiation time be 34.670 minutes, obtain proterties change 1- amino anthraquinones -2-
Sulfonic acid, 3,5- syringol and chromium nanoparticle mixture；By 1- amino anthraquinones -2- sulfonic acid, 3,5- syringol
It is placed in another band stirring heated type reactor with chromium nanoparticle mixture, is started with the rotary drum in stirring heated type reactor
Formula heater, 33.18 DEG C of design temperature starts with the mixer in stirring heated type reactor, and rotating speed is 25.726rpm, pH
4.8430 are adjusted to, are dehydrated 34.844 minutes, it is standby；
4th step：1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the chromium nanometer that the proterties that 3rd step is obtained changes are micro-
Grain is well mixed, adds in 32.184 parts of the 1- amino-2-methyls anthraquinone that mass concentration is 35.252ppm, and cocurrent adds to the 1st step
Band stirring heated type reactor in, flow acceleration is 170.176mL/min；Start band stirring heated type reaction mechanical stirrer,
Setting speed is 39.553rpm；Stirring 4.8113 minutes；Add 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- ethoxies
Base phenyl) 22.856 parts of -3- oxos butyramide, start with the drum heater in stirring heated type reactor, it is warming up to
69.751 DEG C, pH is adjusted to 4.8252, is passed through oxygen ventilation amount for 24.113m3/ min, insulation stands 59.749 minutes；Again
Start band stirring heated type reaction mechanical stirrer, rotating speed is 34.867rpm, adds 1- amino -4- nitro -2- anthraquinone formic acid
23.351 parts, make the hydrophobic-hydrophilic balance threshold value of its reaction solution be 5.65138, and cause that pH is adjusted to 4.8751, insulation stands
58.188 minutes；
5th step：Start with the mixer in stirring heated type reactor, setting speed is 31.454rpm, is stirred to band while stirring
Mix addition N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-β-ammonia in heated type reactor
34.768 parts of base methyl propionate, starts with the drum heater in stirring heated type reactor, and setting band stirring heated type is anti-
It is 4.122 × 10 to answer the temperature in device2DEG C, after being incubated 58.188 minutes, add 2- [[4- (dimethylamino) phenyl] azo] -6-
41.377 parts of methoxyl group -3- methylbenzothiazoles chloride, carries out Esterification catalytic reaction 25.810 minutes；Add afterwards
64.686 parts of cetyl acid -1, the 2- ethylidene ester of 31.226ppm, starts and adds with the rotary drum in stirring heated type reactor
Hot device, it is 109.122 DEG C to set with the temperature in stirring heated type reactor, and pH is adjusted to 4.8113, and pressure is
0.31607MPa, the reaction time is 0.424 hour；0MPa is depressurized to afterwards, 54.31751 DEG C of dischargings are cooled to, that is, obtain one kind
Air entrained concrete activity excitant.
The particle diameter of wherein described chromium nanoparticle is 39.940 μm.
In the application, a kind of air entrained concrete activity excitant needs to be used cooperatively with double spike, a kind of aerating
Concrete active exciting agent is 1 with double spike fit quality ratio:460.300；The double spike is：2- [[1- (2,5- bis-
Chloro- 4- sulfophenyls) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] -1-naphthalene sulfonic aicd sodium salt (9CL), it is described
Double spike 2- [[1- (the chloro- 4- sulfophenyls of 2,5- bis-) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] -
1-naphthalene sulfonic aicd sodium salt (9CL) is common commercial goods.
Embodiment 2
A kind of air entrained concrete activity excitant of the present invention is prepared according to following steps, and is counted by weight：
1st step：In band stirring heated type reactor, 465.940 parts of purified water is added, 74.716 parts of bodied ferric sulfate starts
With the mixer in stirring heated type reactor, setting speed is 79.844rpm, turning in starting with stirring heated type reactor
Drum heater, makes temperature rise to 49.333 DEG C, adds 144.300 parts of hydroxy succinic acid to stir, and carries out catalyzing esterification anti-
Answer .36.622 minutes, add 48.892 parts of Disodium Sulfosuccinate AEO-9 Ester, be passed through flow for 65.399m3/ min's
Oxygen 0.98 hour；Afterwards N, N- bis- (polyoxyethylene)-P- toluenesulfonic acid acid amides are added in band stirring heated type reactor
91.609 parts, it is again started up with the drum heater in stirring heated type reactor, temperature is risen to 98.333 DEG C, insulation
36.755 minutes, 98.620 parts of high-strength alpha-half hydrated gypsum is added, pH value of the adjustment with solution in stirring heated type reactor is
8.9169, it is incubated 265.755 minutes；
2nd step：Separately take 94.777 parts of chromium nanoparticle, by chromium nanoparticle power be 11.09755KW under ultrasonication
0.98 hour, attrition grinding, and by 520.821 eye mesh screens；Chromium nanoparticle is added to another band stirring heated type anti-
Answer in device, it is 74.694 parts of the 1- amino-2-methyls anthraquinone of 265.190ppm to add mass concentration, disperses chromium nanoparticle, is opened
Drum heater in the dynamic heated type reactor with stirring, makes solution temperature at 8.9333 × 10 DEG C, starts band stirring and is heated
Mixer in formula reactor, and with 8.9844 × 102The speed stirring of rpm, adjustment pH value is in 8.9755, insulated and stirred
11.09×10-1Hour；Stop reaction afterwards and stand 11.09 × 10 minutes, go the removal of impurity；Suspension is added into N- ethyls-N-
[4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl] 74.290 parts of-Beta-alanine methyl esters, adjustment pH value exists
2.399, sediment purifying water elution is formed, by centrifuge in rotating speed 9.821 × 103Solid content is obtained under rpm,
3.844×102Dried at a temperature of DEG C, 9.821 × 10 are crossed after grinding3Mesh sieve, it is standby；
3rd step：After separately taking the treatment of 57.852 parts of 1- amino anthraquinones -2- sulfonic acid, 76.643 parts of 3,5- syringol and the 2nd step
94.777 parts of chromium nanoparticle, is irradiated after being well mixed using 60Co- gamma Rays, the energy of 60Co- gamma Rays irradiation
Measure for 50.999MeV, dosage be 110.781kGy, irradiation time be 59.546 minutes, obtain proterties change 1- amino anthraquinones-
2- sulfonic acid, 3,5- syringol and chromium nanoparticle mixture；By 1- amino anthraquinones -2- sulfonic acid, 3,5- dimethoxy benzenes
Phenol and chromium nanoparticle mixture are placed in another band stirring heated type reactor, turning in starting with stirring heated type reactor
Drum heater, 79.399 DEG C of design temperature starts with the mixer in stirring heated type reactor, and rotating speed is
420.138rpm, pH are adjusted to 8.9999, are dehydrated 48.810 minutes, standby；
4th step：1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the chromium nanometer that the proterties that 3rd step is obtained changes are micro-
Grain is well mixed, adds in 74.694 parts of the 1- amino-2-methyls anthraquinone that mass concentration is 265.190ppm, and cocurrent adds to the 1st
In the band stirring heated type reactor of step, flow acceleration is 898.185mL/min；Start band stirring heated type reactor stirring
Machine, setting speed is 79.804rpm；Stirring 8.9999 minutes；Add 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- second
Phenyl) 65.839 parts of -3- oxos butyramide, start with the drum heater in stirring heated type reactor, it is warming up to
106.379 DEG C, pH is adjusted to 8.9190, is passed through oxygen ventilation amount for 65.622m3/ min, insulation stands 89.743 minutes；Again
Start band stirring heated type reaction mechanical stirrer, rotating speed is 79.65rpm, adds 1- amino -4- nitro -2- anthraquinone formic acid
59.169 parts, make the hydrophobic-hydrophilic balance threshold value of its reaction solution be 11.09755, and cause that pH is adjusted to 8.9379, be incubated quiet
Put 98.437 minutes；
5th step：Start with the mixer in stirring heated type reactor, setting speed is 98.386rpm, is stirred to band while stirring
Mix addition N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-β-ammonia in heated type reactor
74.290 parts of base methyl propionate, starts with the drum heater in stirring heated type reactor, and setting band stirring heated type is anti-
It is 9.870 × 10 to answer the temperature in device2DEG C, after being incubated 98.437 minutes, add 2- [[4- (dimethylamino) phenyl] azo] -6-
85.612 parts of methoxyl group -3- methylbenzothiazoles chloride, carries out Esterification catalytic reaction 36.399 minutes；Add afterwards
118.421 parts of cetyl acid -1, the 2- ethylidene ester of 298.698ppm, starts with the rotary drum in stirring heated type reactor
Heater, it is 165.870 DEG C to set with the temperature in stirring heated type reactor, and pH is adjusted to 8.9622, and pressure is
0.32550MPa, the reaction time is 0.949 hour；0MPa is depressurized to afterwards, 59.31190 DEG C of dischargings are cooled to, that is, obtain one kind
Air entrained concrete activity excitant.
The particle diameter of wherein described chromium nanoparticle is 49.716 μm.
In the application, a kind of air entrained concrete activity excitant needs to be used cooperatively with double spike, a kind of aerating
Concrete active exciting agent is 1 with double spike fit quality ratio:900.892；The double spike is：Two [5- chloros -3-
[(4,5- dihydro -3- methyl -5- oxo -1- phenyl -1H- pyrazoles -4- bases) azo] -2- hydroxy benzene sulfonic acids base]-chromic acid base ethanol
Amine the sodium salt, [5- chloros -3- [(4,5- dihydro -3- methyl -5- oxo -1- phenyl -1H- pyrazoles -4- bases) of the double spike two
Azo] -2- hydroxy benzene sulfonic acids base]-chromic acid ethylethanolamine sodium salt be common commercial goods.
Embodiment 3
A kind of air entrained concrete activity excitant of the present invention is prepared according to following steps, and is counted by weight：
1st step：In band stirring heated type reactor, 240.9106 parts of purified water is added, 32.9482 parts of bodied ferric sulfate is opened
Mixer in the dynamic heated type reactor with stirring, setting speed is 33.9113rpm, is started with stirring heated type reactor
Drum heater, temperature is risen to 48.9101 DEG C, add 35.9969 parts of hydroxy succinic acid to stir, carry out esterification and urge
Change reaction 25.9810 minutes, add 31.9237 parts of Disodium Sulfosuccinate AEO-9 Ester, be passed through flow for 24.9726m3/
The oxygen of min 0.933 hour；Afterwards N, N- bis- (polyoxyethylene)-P- toluenesulfonic acids are added in band stirring heated type reactor
34.9856 parts of acid amides, is again started up, with the drum heater in stirring heated type reactor, making temperature rise to 65.9101 DEG C,
Insulation 25.9726 minutes, adds 37.9133 parts of high-strength alpha-half hydrated gypsum, pH of the adjustment with solution in stirring heated type reactor
It is 4.8918 to be worth, and is incubated 25.9726 minutes；
2nd step：Separately take 39.9184 parts of chromium nanoparticle, by chromium nanoparticle power be 5.659138KW under ultrasonication
0.931 hour, attrition grinding, and by 420.9361 eye mesh screens；Chromium nanoparticle is added to another band stirring heated type
In reactor, it is 32.9184 parts of the 1- amino-2-methyls anthraquinone of 35.9252ppm to add mass concentration, disperses chromium nanoparticle,
Start with the drum heater in stirring heated type reactor, make solution temperature at 4.89726 × 10 DEG C, start band stirring and receive
Mixer in hot type reactor, and with 4.89101 × 102The speed stirring of rpm, adjustment pH value is in 4.89138, insulated and stirred
5.659×10-1Hour；Stop reaction afterwards and stand 5.659 × 10 minutes, go the removal of impurity；Suspension is added into N- ethyls-N-
[4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl] 34.9768 parts of-Beta-alanine methyl esters, adjustment pH value exists
1.9726, sediment purifying water elution is formed, by centrifuge in rotating speed 4.9361 × 103Solid content is obtained under rpm,
2.9190×102Dried at a temperature of DEG C, 8.9361 × 10 are crossed after grinding3Mesh sieve, it is standby；
3rd step：It is another to take the treatment of 34.9921 parts of 1- amino anthraquinones -2- sulfonic acid, 31.9962 parts of 3,5- syringol and the 2nd step
39.9184 parts of chromium nanoparticle, are irradiated after being well mixed using 60Co- gamma Rays afterwards, the irradiation of 60Co- gamma Rays
Energy is 22.9430MeV, dosage is 70.941kGy, irradiation time is 34.9670 minutes, obtains the 1- amino anthracenes of proterties change
Quinone -2- sulfonic acid, 3,5- syringol and chromium nanoparticle mixture；By 1- amino anthraquinones -2- sulfonic acid, 3,5- dimethoxys
Phenol and chromium nanoparticle mixture are placed in another band stirring heated type reactor, are started with stirring heated type reactor
Drum heater, 33.918 DEG C of design temperature starts with the mixer in stirring heated type reactor, and rotating speed is
25.9726rpm, pH are adjusted to 4.89430, are dehydrated 34.9844 minutes, standby；
4th step：1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the chromium nanometer that the proterties that 3rd step is obtained changes are micro-
Grain is well mixed, adds in 32.9184 parts of the 1- amino-2-methyls anthraquinone that mass concentration is 35.9252ppm, and cocurrent adds to the 1st
In the band stirring heated type reactor of step, flow acceleration is 170.9176mL/min；Start band stirring heated type reactor stirring
Machine, setting speed is 39.9553rpm；Stirring 4.89113 minutes；Add 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4-
Ethoxyl phenenyl) 22.9856 parts of -3- oxos butyramide, start with the drum heater in stirring heated type reactor, heat up
To 69.9751 DEG C, pH is adjusted to 4.89252, is passed through oxygen ventilation amount for 24.9113m3/ min, insulation stands 59.9749 points
Clock；Band stirring heated type reaction mechanical stirrer is again started up, rotating speed is 34.9867rpm, adds 1- amino -4- nitro -2- anthraquinones
23.9351 parts of formic acid, makes the hydrophobic-hydrophilic balance threshold value of its reaction solution be 5.659138, and causes that pH is adjusted to 4.89751,
Insulation stands 58.9188 minutes；
5th step：Start with the mixer in stirring heated type reactor, setting speed is 31.9454rpm, while stirring to band
Stirring heated type reactor in add N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-β -
34.9768 parts of aminopropanoate, starts with the drum heater in stirring heated type reactor, setting band stirring heated type
Temperature in reactor is 4.9122 × 102DEG C, after being incubated 58.9188 minutes, [[4- (dimethylamino) phenyl] is even to add 2-
Nitrogen] 41.9377 parts of -6- methoxyl group -3- methylbenzothiazoles chloride, carry out Esterification catalytic reaction 25.9810 minutes；Afterwards
64.9686 parts of cetyl acid -1, the 2- ethylidene ester of 31.9226ppm is added, turning in starting with stirring heated type reactor
Drum heater, it is 109.9122 DEG C to set with the temperature in stirring heated type reactor, and pH is adjusted to 4.89113, and pressure is
0.319607MPa, the reaction time is 0.4924 hour；0MPa is depressurized to afterwards, 54.319751 DEG C of dischargings are cooled to, that is, obtain
A kind of air entrained concrete activity excitant.
The particle diameter of wherein described chromium nanoparticle is 39.9940 μm.
In the application, a kind of air entrained concrete activity excitant needs to be used cooperatively with double spike, a kind of aerating
Concrete active exciting agent is 1 with double spike fit quality ratio:460.9300；The double spike is：4- (5- amino -3-
Methyl isophthalic acid-phenyl -1H- pyrazoles -4- bases azo) -2,5- dichloro-s-benzene sulfonic acid list lithium salts, the double spike 4- (5- amino -
3- methyl isophthalic acids-phenyl -1H- pyrazoles -4- bases azo) -2,5- dichloro-s-benzene sulfonic acid list lithium salts be common commercial goods.
Reference examples
Reference examples carry out construction material bonding provocative test using the desulfurization flyash activity excitant of commercially available certain brand.
Embodiment 4
The air entrained concrete activity excitant that embodiment 1~3 and reference examples are obtained carries out construction material bonding provocative test,
Wherein air entrained concrete activity excitant is used cooperatively with double spike, the matter of air entrained concrete activity excitant and double spike
Amount is than being 1:460.300, the double spike in embodiment 1 for 2- [[1- (2,5- bis- chloro- 4- sulfophenyls) -4,5- dihydros -
3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] -1-naphthalene sulfonic aicd sodium salt (9CL), in example 2 be two [5- chloros -3-
[(4,5- dihydro -3- methyl -5- oxo -1- phenyl -1H- pyrazoles -4- bases) azo] -2- hydroxy benzene sulfonic acids base]-chromic acid base ethanol
Amine sodium salt, in embodiment 3 be 4- (5- amino -3- methyl isophthalic acids-phenyl -1H- pyrazoles -4- bases azo) -2,5- dichloro-s-benzene sulphur
Sour list lithium salts；Treatment is analyzed after terminating to parameters such as tensile strength, viscosity, solids content rate, curing rates.Data analysis
As shown in table 1.
As seen from Table 1, a kind of air entrained concrete activity excitant of the present invention, its tensile strength, viscosity, solid contain
Dose rate, curing rate are above the product of prior art production.
Additionally, being that a kind of air entrained concrete activity excitant of the present invention is entered with reference examples as shown in Figures 1 to 3
Capable, counted with use time change test data.Find out in figure, embodiment 1~3 is cut in shearing impact intensity, socket compression
Shearing stress, peel strength technical indicator, significantly better than the product of prior art production.
Claims (7)
1. a kind of air entrained concrete activity excitant, it is characterised in that matched by weight by following components and constituted：
240.106~465.940 parts of purified water, 32.482~74.716 parts of bodied ferric sulfate, hydroxy succinic acid 35.969~
144.300 parts, 31.237~48.892 parts of Disodium Sulfosuccinate AEO-9 Ester, N, N- bis- (polyoxyethylene)-P- toluene sulphurs
34.856~91.609 parts of sour acid amides, 37.133~98.620 parts of high-strength alpha-half hydrated gypsum, 1- amino anthraquinones -2- sulfonic acid 34.921
~57.852 parts, 3,5- 31.962~76.643 parts of syringol, 39.184~94.777 parts of chromium nanoparticle, 1- ammonia
32.184~74.694 parts of base -2-methylanthraquinone, 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- ethoxyl phenenyls) -3- oxygen
For 22.856~65.839 parts of butyramide, 23.351~59.169 parts of 1- amino -4- nitro -2- anthraquinones formic acid, N- ethyls-N-
[4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl] 34.768~74.290 parts of-Beta-alanine methyl esters, 2-
[[4- (dimethylamino) phenyl] azo] 41.377~85.612 parts of -6- methoxyl group -3- methylbenzothiazoles chloride, quality
Concentration is 64.686~118.421 parts of the cetyl acid -1,2- ethylidene ester of 31.226ppm~298.698ppm.
2. a kind of air entrained concrete activity excitant according to claim 1, it is characterised in that by following components by weight
Number proportioning composition：
241.106~464.940 parts of purified water, 33.482~73.716 parts of bodied ferric sulfate, hydroxy succinic acid 36.969~
143.300 parts, 32.237~47.892 parts of Disodium Sulfosuccinate AEO-9 Ester, N, N- bis- (polyoxyethylene)-P- toluene sulphurs
35.856~90.609 parts of sour acid amides, 38.133~97.620 parts of high-strength alpha-half hydrated gypsum, 1- amino anthraquinones -2- sulfonic acid 35.921
~56.852 parts, 3,5- 32.962~75.643 parts of syringol, 40.184~93.777 parts of chromium nanoparticle, 1- ammonia
33.184~73.694 parts of base -2-methylanthraquinone, 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- ethoxyl phenenyls) -3- oxygen
For 23.856~64.839 parts of butyramide, 24.351~58.169 parts of 1- amino -4- nitro -2- anthraquinones formic acid, N- ethyls-N-
[4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl] 35.768~73.290 parts of-Beta-alanine methyl esters, 2-
[[4- (dimethylamino) phenyl] azo] 42.377~84.612 parts of -6- methoxyl group -3- methylbenzothiazoles chloride, quality
Concentration is 65.686~117.421 parts of the cetyl acid -1,2- ethylidene ester of 32.226ppm~297.698ppm.
3. the preparation method of a kind of air entrained concrete activity excitant according to claim 1 and 2, it is characterised in that press
Parts by weight meter, comprises the following steps：
1st step：In band stirring heated type reactor, purified water and bodied ferric sulfate are added, start band stirring heated type reaction
Mixer in device, setting speed is 33.113rpm~79.844rpm, is started with the rotary drum in stirring heated type reactor
Heater, makes temperature rise to 48.101 DEG C~49.333 DEG C, adds hydroxy succinic acid to stir, and carries out Esterification catalytic reaction
25.810~36.622 minutes, add Disodium Sulfosuccinate AEO-9 Ester, be passed through flow for 24.726m3/min~
The oxygen of 65.399m3/min 0.33~0.98 hour；Afterwards N, (the polyoxy second of N- bis- are added in band stirring heated type reactor
Alkene)-P- toluenesulfonic acid acid amides, it is again started up, with the drum heater in stirring heated type reactor, rising to temperature
65.101 DEG C~98.333 DEG C, 25.726~36.755 minutes are incubated, add high-strength alpha-half hydrated gypsum, adjustment band stirring heated type
The pH value of solution is 4.818~8.9169 in reactor, is incubated 25.726~265.755 minutes；
2nd step：Chromium nanoparticle separately is taken, by chromium nanoparticle at power is for ultrasonic wave under 5.65138KW~11.09755KW
Reason 0.31~0.98 hour, attrition grinding, and by 420.361~520.821 eye mesh screens；Chromium nanoparticle is added to another
In individual band stirring heated type reactor, it is the 1- amino-2-methyl anthraquinones of 35.252ppm~265.190ppm to add mass concentration
Dispersion chromium nanoparticle, starts with the drum heater in stirring heated type reactor, makes solution temperature 4.8726 × 10
DEG C~8.9333 × 10 DEG C between, start the mixer during band stirs heated type reactor, and with 4.8101 × 102Rpm~
8.9844×102Rpm speed stirring, adjustment pH value between 4.8138~8.9755, insulated and stirred 5.65 × 10-1~
11.09×10-1Hour；Stop reaction afterwards and stand 5.65 × 10~11.09 × 10 minutes, go the removal of impurity；Suspension is added
N- ethyls-N- [4- [(5- nitro -2,1- benzisothiazole -3- bases) azo] phenyl]-Beta-alanine methyl esters, adjustment pH value exists
Between 1.726~2.399, sediment purifying water elution is formed, by centrifuge in rotating speed 4.361 × 103Rpm~9.821
×103Solid content is obtained under rpm, 2.190 × 102DEG C~3.844 × 102Dried at a temperature of DEG C, 8.361 × 10 are crossed after grinding3
~9.821 × 103Mesh sieve, it is standby；
3rd step：It is another to take chromium nanoparticle after the treatment of 1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the 2nd step, mixing
Using the irradiation of 60Co- gamma Rays after uniform, the energy of 60Co- gamma Rays irradiation for 22.430MeV~
50.999MeV, dosage are 70.41kGy~110.781kGy, irradiation time is 34.670~59.546 minutes, obtain proterties and change
1- amino anthraquinones -2- the sulfonic acid of change, 3,5- syringol and chromium nanoparticle mixture；By 1- amino anthraquinones -2- sulfonic acid,
3,5- syringol and chromium nanoparticle mixture are placed in another band stirring heated type reactor, are started band stirring and are heated
Drum heater in formula reactor, 33.18 DEG C~79.399 DEG C of design temperature starts with stirring heated type reactor
Mixer, rotating speed is 25.726rpm~420.138rpm, and pH is adjusted between 4.8430~8.9999, dehydration 34.844~
It is 48.810 minutes, standby；
4th step：1- amino anthraquinones -2- sulfonic acid, 3,5- syringol and the chromium nanometer that the proterties that 3rd step is obtained changes are micro-
Grain is well mixed, adds in the 1- amino-2-methyl anthraquinones that mass concentration is 35.252ppm~265.190ppm, and cocurrent is added to
In the band stirring heated type reactor of the 1st step, flow acceleration is 170.176mL/min~898.185mL/min；Start band stirring
Heated type reacts mechanical stirrer, and setting speed is 39.553rpm~79.804rpm；Stirring 4.8113~8.9999 minutes；Again plus
Enter 2- ((the chloro- 2- nitrobenzophenones of 4-) azo)-N- (4- ethoxyl phenenyls) -3- oxo butyramides, start band stirring heated type anti-
The drum heater in device is answered, 69.751 DEG C~106.379 DEG C are warming up to, pH is adjusted between 4.8252~8.9190, led to
Enter oxygen ventilation amount for 24.113m3/ min~65.622m3/ min, insulation stands 59.749~89.743 minutes；It is again started up band
Stirring heated type reaction mechanical stirrer, rotating speed is 34.867rpm~79.65rpm, adds 1- amino -4- nitro -2- anthraquinone first
Acid, makes the hydrophobic-hydrophilic balance threshold value of its reaction solution be 5.65138~11.09755, and cause pH be adjusted to 4.8751~
Between 8.9379, insulation stands 58.188~98.437 minutes；
5th step：Start with the mixer in stirring heated type reactor, setting speed is 31.454rpm~98.386rpm, side
To N- ethyls-N- is added in band stirring heated type reactor, [[(5- nitro -2,1- benzisothiazole -3- bases) is even for 4- on stirring side
Nitrogen] phenyl]-Beta-alanine methyl esters, start with the drum heater in stirring heated type reactor, setting band stirring is heated
Temperature in formula reactor is 4.122 × 102DEG C~9.870 × 102DEG C, after being incubated 58.188~98.437 minutes, add 2-
[[4- (dimethylamino) phenyl] azo] -6- methoxyl group -3- methylbenzothiazole chlorides, Esterification catalytic reaction 25.810~
36.399 minutes；Cetyl acid -1,2- ethylidene esters are added afterwards, are started and are added with the rotary drum in stirring heated type reactor
Hot device, it is 109.122 DEG C~165.870 DEG C to set with the temperature in stirring heated type reactor, pH adjusted to 4.8113~
Between 8.9622, pressure is 0.31607MPa~0.32550MPa, and the reaction time is 0.424~0.949 hour；It is depressurized to afterwards
0MPa, is cooled to 54.31751 DEG C~59.31190 DEG C dischargings, that is, obtain a kind of air entrained concrete activity excitant.
4. a kind of preparation method of air entrained concrete activity excitant according to claim 3, it is characterised in that the chromium
The particle diameter of nanoparticle is 39.940 μm~49.716 μm.
5. a kind of a kind of air entrained concrete activity excitant according to claim 1, it is characterised in that aerating coagulation
Native activity excitant be mainly used in building foundation material production aerated bricks in active component excite aspect application.
6. application according to claim 5, it is characterised in that the building foundation material is the solidifying concrete in end, brick fuel, she
At least one in hair thin white silk used in ancient China stone, lime-fly-ash loess, triphase soil, high strength RC.
7. application according to claim 5, it is characterised in that a kind of air entrained concrete activity excitant and double dilutions
Agent is used cooperatively, and a kind of air entrained concrete activity excitant is 1 with double spike fit quality ratio:460.300~900.892；
The double spike is：2- [[1- (the chloro- 4- sulfophenyls of 2,5- bis-) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases]
Azo] -1-naphthalene sulfonic aicd sodium salt (9CL), 4- (5- amino -3- methyl isophthalic acids-phenyl -1H- pyrazoles -4- bases azo) -2,5- dichloro-s -
Benzene sulfonic acid list lithium salts, two [5- chloros -3- [(4,5- dihydro -3- methyl -5- oxo -1- phenyl -1H- pyrazoles -4- bases) azo] -
2- hydroxy benzene sulfonic acids base] one kind in-three kinds of chromic acid ethylethanolamine sodium salt, the double spike is common commercial goods.
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| CN102452814A (en) * | 2010-10-19 | 2012-05-16 | 上海城建物资有限公司 | High strength concrete adopting desulfurized gypsum as activator, and preparation method thereof |
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