CN108409182A - High-effective concrete air entraining agent, preparation method and applications - Google Patents
High-effective concrete air entraining agent, preparation method and applications Download PDFInfo
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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
- C04B24/10—Carbohydrates or derivatives thereof
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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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/304—Air-entrainers
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- Health & Medical Sciences (AREA)
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- Molecular Biology (AREA)
- Materials Engineering (AREA)
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Abstract
The invention discloses a kind of high-effective concrete air entraining agent, preparation method and applications.The preparation method of the high-effective concrete air entraining agent, includes the following steps：Quinoa wheat bran is added to the water, cellulase, pectase, neutral proteinase is added, is uniformly mixed, EtOH Sonicate extraction is added, is sieved, is concentrated by evaporation, is dried under reduced pressure.The bubble that the concrete composite air entraining agent of the present invention introduces is fine and smooth, uniform in size, and foam stabilizing effect is good, and air content keeps high, moreover it is possible to improve the intensity and endurance quality of concrete.
Description
Technical field
The present invention relates to a kind of concrete air-entrainer, preparation method and applications, and in particular to a kind of high-effective concrete draws
Gas agent, preparation method and applications.
Background technology
Air entraining agent is that concrete is instigated to introduce a large amount of uniform, stable, closed micro-bubbles in whipping process, to improve
The additive of concrete mix workability and maturing frost-proof test.Air entraining agent is to improve concrete durability,
Especially one of the most effective measure of frost resistance and Deicer-scaling resistance.In the flourishing state such as the U.S., Canada, Japan and Europe
Family, since they attach great importance to the durability of engineering, air entraining agent is most common additive, and the concrete for mixing air entraining agent accounts for coagulation
The 70-80% of native total amount, it is even more.
In China, except the related standard of hydro-structure provides that concrete must add outside bleed extremely, Other Engineering is such as public
Road, road, bridge, building, underground structure, the Important Projects such as airfield runway, which are all not specified by, must mix air entraining agent, therefore, practical
On in addition to water conservancy project and northern harbour engineering, other Important Projects rarely mix air entraining agent.
Most of air entraining agents are petrochemical industries, paper pulp processed, the byproduct of papermaking and some other industry.Air entraining agent is most at present
Common chemical constituent has five classes：1. the sodium salt compound of rosin tree lipid；2. fatty acid salt compound；3. sulfonation hydrocarbonization
Close object；4. alkyl-benzyl Sulfonates compound；5. triterpenoid saponin natural products.
As one of the concrete admixture kind used earliest, what air entraining agent played in terms of improving concrete durability
Important function is widely paid attention to by people.However, after the air entraining agents such as traditional rosin, saponin, it is newly developed go out bleed
Agent kind is very few, and most of for petrochemical industry, the oceangoing ship of the byproduct of paper industry and other industry or other industry
Carry out product.With the increasingly raising that building requires concrete performance, existing air entraining agent kind cannot increasingly meet engineer application
Demand, expose various deficiencies in bleed, foam stabilizing, intensity and compatibility etc..
Invention content
Patent of the present invention is insufficient mainly for bleed existing for existing concrete air entraining agent, and the problems such as influence intensity, carries
There are new and effective concrete air-entrainer, preparation method and applications for one kind.
The present invention adopts the following technical scheme that：
A kind of preparation method of high-effective concrete air entraining agent, includes the following steps：
300-900g quinoa wheat brans are added in 1000-3000g water, 0.05-0.5g cellulases, 0.05- is added
0.5g pectases, 0.01-0.1g neutral proteinases, are warming up to 35-45 DEG C after mixing, and 1-5 hours are kept the temperature at 35-45 DEG C,
1000-3000g ethyl alcohol is added, is warming up to 50-70 DEG C after mixing, in 50-70 DEG C of ultrasonic extraction 20-60 minutes, ultrasonic wave
Frequency is 20-60KHz, power 200-500W, then crosses 100-300 mesh sieve, filtrate is crossed 300-1000g macroporous absorption trees
Fat, filtrate flow velocity are 0.5-2BV/h, and the ethanol water for being then 20%-40% with mass fraction elutes macroporous absorbent resin,
Flow velocity is 0.5-2BV/h, abandons this eluent, then the ethanol water elution macropore for being 60%-85% with mass fraction is inhaled
Attached resin, flow velocity 0.5-2BV/h collect eluent, and it is 1.15- that eluent, which is concentrated by evaporation, and measures relative density to 60 DEG C
Medicinal extract is dried under reduced pressure to obtain quinoa wheat bran saponin extract by 1.35 medicinal extract, and mass fraction used is the ethyl alcohol of 20%-40%
The volume of aqueous solution is 2-5BV, and the volume for the ethanol water that mass fraction used is 60%-85% is 3-6BV.
The conditional parameter that is dried under reduced pressure is：Pressure is 0.03-0.07MPa, temperature is 45-75 DEG C, the time is 3-12 small
When.
The macroporous absorbent resin is one kind in D101 types, HP100 types, X-5 types, and the macroporous absorbent resin is further
Preferably D101 types.
The present invention also provides a kind of high-effective concrete air entraining agents, are prepared using the above method.
The present invention also provides a kind of application of high-effective concrete air entraining agent, the addition of the concrete air-entrainer with
The mass ratio 1 of cement addition in concrete：(2500-300000), preferred mass ratio are 1：(20000-80000).
The bubble that the concrete composite air entraining agent of the present invention introduces is fine and smooth, uniform in size, and foam stabilizing effect is good, and air content is kept
It is high, moreover it is possible to improve the intensity and endurance quality of concrete.
Specific implementation mode
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
Product specification selects.
In following embodiments, primary raw material and instrument used are as follows：
Portland cement, intensity：P.O.42.5 executes standard GB175-2007, Gaungzhou Yuebao Cement Co., Ltd.'s life
Production.
Flyash meets GB/T 1596-2005《For the flyash in cement and concrete》In F classes, II grade mark
It is accurate.
Rubble, grain size are the limestone gravel of 5-7mm.
Calcium stearate, No. CAS：1592-23-0.
Oleic acid, CAS：112-80-1.
Quinoa wheat bran, the wheat bran of quinoa (Classification system Chenopodium quinoawilld), the white quinoa of kind, purchase
From Shanxi Jingle quinoa planting base.
Cellulase, enzyme activity 7000U/g, by trichoderma reesei (Classification system：Trichodermareesei it) ferments
It arrives, model full constituent type 7000, is purchased from Ningxia Sunson Industrial Group Co., Ltd..
Pectase, enzyme activity 10,000 U/g, model SAC-015 are purchased from Ningxia Sunson Industrial Group Co., Ltd..
Neutral proteinase, No. CAS：9068-59-1,150,000 U/g of enzyme activity are bought from the limited public affairs of Nanning Pang Bo bioengineering
Department.
Ethyl alcohol, No. CAS：64-17-5.
D101 type macroporous absorbent resins are bought from Anhui Samsung resin Science and Technology Ltd., comply with standard Q/GSX022-
2015。
Isobutyl hydramine, No. CAS：124-68-5.
Two butanolamines, No. CAS：79448-06-9.
3- amino -1- propyl alcohol, No. CAS：156-87-6.
Methylpropene sodium sulfonate, No. CAS：1561-92-8.
Sodium lignin sulfonate, No. CAS：8061-51-6.Mw=52000Da, Mn=7000Da.Producer：
SigmaAldrich。
In following embodiments, used test method is as follows：
Intensity test：The freeze proof pervious concrete of high intensity is made into the examination that size is 150mm × 150mm × 150mm
Block uses covered rearing with plastic film surface after test block forming, is placed in the environment that temperature is 20 ± 2 DEG C, relative humidity is 95% immediately
Lower maintenance 28d ages.According to GB/T50081-2002《Normal concrete mechanical test method》Test 28 days compression strength.
Anti-freezing property is tested：By the freeze proof pervious concrete of high intensity according to GB/T 50082-2009《Normal concrete is long-term
Performance and endurance quality test method standard》In fast jelly method carry out product and test, measure Frozen-thawed cycled grade F.
Coefficient of permeability is tested：The freeze proof pervious concrete of high intensity is made into a diameter of 100mm, is highly the cylinder of 50mm
Test block uses covered rearing with plastic film surface after test block forming, is placed in the environment that temperature is 20 ± 2 DEG C, relative humidity is 95%
Lower maintenance 28d ages, then according to Xinan Science and Technology Univ.'s master thesis《It is influenced based on orthogonal method pervious concrete performance
Factorial experiments are studied》(author：Pay Dongshan) 2.4.1 section coefficient of permeability assay method tested.
It is further illustrated the present invention below by the mode of embodiment, unless otherwise specified, used number is attached most importance to
Measure number.
Embodiment 1
A kind of freeze proof pervious concrete of high intensity, including following components in parts by weight are prepared：30 parts of portland cement,
3.5 parts of flyash, 95 parts of rubble, 0.005 part of calcium stearate, 0.0002 part of oleic acid, 0.4 part of water-reducing agent, saponins air entraining agent
0.0006 part, 8 parts of water.
The saponins air entraining agent is quinoa wheat bran saponin(e, and the preparation method of the quinoa wheat bran saponin(e is：By 500g lamb's-quarters
Wheat bran skin is added in 1600g water, 0.1g cellulases, 0.1g pectases, 0.05g neutral proteinases is added, after mixing
40 DEG C are warming up to, 3 hours are kept the temperature at 40 DEG C, 1500g ethyl alcohol is added, 60 DEG C are warming up to after mixing, in 60 DEG C of ultrasonic extractions
Then it sieves with 100 mesh sieve within 40 minutes, ultrasonic frequency 20KHz, power 350W, filtrate is crossed into 500g D101 type macroporous absorptions
Resin, filtrate flow velocity are 1BV/h, and the ethanol water that mass fraction is 30% is then used to elute D101 type macroporous absorbent resins,
Flow velocity is 1BV/h, abandons this eluent, then the ethanol water for being 70% with mass fraction elutes D101 type macroporous absorption trees
Fat, flow velocity 1BV/h collect eluent, and eluent is concentrated by evaporation to 60 DEG C and measures the medicinal extract that relative density is 1.25, will be soaked
Cream is dried under reduced pressure to obtain quinoa wheat bran saponin extract.The volume for the ethanol water that mass fraction used is 30% is 3BV, institute
The volume for the ethanol water for being 70% with mass fraction is 5BV.Being dried under reduced pressure conditional parameter is：Pressure is 0.05MPa, temperature
It it is 6 hours for 50 DEG C, time.
The water-reducing agent is that modified sodium lignosulfonate and methylpropene sodium sulfonate are 1 in mass ratio:1 mixture.
The preparation method of the modified sodium lignosulfonate is：100g sodium lignin sulfonates are added in 250g water,
40 DEG C, stirred 60 minutes with 200 revs/min of rotating speed, 150g alcamines modifying agent is added, at 40 DEG C, with 200 revs/min
Rotating speed stirs 60 minutes, is warming up to 65 DEG C, the formalin that 120g mass fractions are 37% is added, in 70 DEG C of back flow reactions 12
Hour, aqueous solvent is removed through distillation, obtained product is added in 200g ethyl alcohol, at 30 DEG C, with 200 revs/min of rotating speed
Then stirring 10 minutes is centrifuged 40 minutes with 8000 revs/min of rotating speed, by centrifugation gained sediment, at 50 DEG C, drying 24 is small
When, obtain modified sodium lignosulfonate.The alcamines modifying agent is two butanolamines.
The preparation method of the freeze proof pervious concrete of high intensity is：Water-reducing agent is added to the water to be uniformly mixed and obtains mixed liquor,
Mixed liquor is added after portland cement, flyash, rubble, calcium stearate, oleic acid, saponins air entraining agent are uniformly mixed,
It is stirred 300 seconds with 35 revs/min of rotating speed, obtains the freeze proof pervious concrete of high intensity.
Embodiment 2
It is substantially the same manner as Example 1, it differs only in, in the present embodiment 2：The preparation method of modified sodium lignosulfonate
For：100g sodium lignin sulfonates are added in 250g water, stirs 60 minutes, is added at 40 DEG C, with 200 revs/min of rotating speed
150g alcamines modifying agent is stirred 60 minutes at 40 DEG C, with 200 revs/min of rotating speed, is warming up to 65 DEG C, 120g mass is added
The formalin that score is 37% removed aqueous solvent through distillation, obtained product is added in 70 DEG C of back flow reactions 12 hours
Into 200g ethyl alcohol, stirs 10 minutes at 30 DEG C, with 200 revs/min of rotating speed, then centrifuged with 8000 revs/min of rotating speed
It is 40 minutes, centrifugation gained sediment is 24 hours dry at 50 DEG C, obtain modified sodium lignosulfonate.The alcamines modifying agent
For 3- amino -1- propyl alcohol.
Embodiment 3
It is substantially the same manner as Example 1, it differs only in, in the present embodiment 3：The preparation method of modified sodium lignosulfonate
For：100g sodium lignin sulfonates are added in 250g water, stirs 60 minutes, is added at 40 DEG C, with 200 revs/min of rotating speed
150g alcamines modifying agent is stirred 60 minutes at 40 DEG C, with 200 revs/min of rotating speed, is warming up to 65 DEG C, 120g mass is added
The formalin that score is 37% removed aqueous solvent through distillation, obtained product is added in 70 DEG C of back flow reactions 12 hours
Into 200g ethyl alcohol, stirs 10 minutes at 30 DEG C, with 200 revs/min of rotating speed, then centrifuged with 8000 revs/min of rotating speed
It is 40 minutes, centrifugation gained sediment is 24 hours dry at 50 DEG C, obtain modified sodium lignosulfonate.The alcamines modifying agent
For isobutyl hydramine.
Embodiment 4
It is substantially the same manner as Example 1, it differs only in, in the present embodiment 4, the water-reducing agent is modified lignin resin sulfonic acid
Sodium.The preparation method is the same as that of Example 1 for modified sodium lignosulfonate described in the present embodiment 4.
Embodiment 5
It is substantially the same manner as Example 1, it differs only in, in the present embodiment 5, the water-reducing agent is methacrylic sulfonic acid
Sodium.
Comparative example 1
It is substantially the same manner as Example 1, it differs only in, in this comparative example 1, the preparation method of the quinoa wheat bran saponin(e
For：500g quinoa wheat brans are added in 1600g water, 0.1g cellulases, 0.1g pectases, 0.05g neutral proteinases is added,
It is warming up to 40 DEG C after mixing, 3 hours are kept the temperature at 40 DEG C, 1500g ethyl alcohol is added, sieves with 100 mesh sieve after mixing, by filtrate
500g D101 type macroporous absorbent resins are crossed, filtrate flow velocity is 1BV/h, and it is 30% ethanol aqueous wash then to use mass fraction
De- D101 type macroporous absorbent resins, flow velocity 1BV/h abandon this eluent, then water-soluble with the ethyl alcohol that mass fraction is 70%
Liquid elutes D101 type macroporous absorbent resins, and flow velocity 1BV/h collects eluent, and eluent is concentrated by evaporation to 60 DEG C of measurement phases
The medicinal extract for being 1.25 to density, medicinal extract is dried under reduced pressure to obtain quinoa wheat bran saponin extract.Mass fraction used is 30%
The volume of ethanol water is 3BV, and the volume for the ethanol water that mass fraction used is 70% is 5BV.It is dried under reduced pressure condition
Parameter is：Pressure is 0.05MPa, temperature is 50 DEG C, the time is 6 hours.
Comparative example 2
It is substantially the same manner as Example 1, it differs only in, in this comparative example 2, the preparation method of the quinoa wheat bran saponin(e
For：500g quinoa wheat brans are added in 1600g water, are warming up to 40 DEG C after mixing, 3 hours are kept the temperature at 40 DEG C, are added
1500g ethyl alcohol is warming up to 60 DEG C after mixing, and in 60 DEG C of ultrasonic extractions 40 minutes, ultrasonic frequency 20KHz, power is
Then 350W is sieved with 100 mesh sieve, filtrate is crossed 500g D101 type macroporous absorbent resins, filtrate flow velocity is 1BV/h, then uses quality
The ethanol water that score is 30% elutes D101 type macroporous absorbent resins, and flow velocity 1BV/h abandons this eluent, then uses
The ethanol water that mass fraction is 70% elutes D101 type macroporous absorbent resins, and flow velocity 1BV/h collects eluent, will wash
De- liquid is concentrated by evaporation to 60 DEG C and measures the medicinal extract that relative density is 1.25, and medicinal extract is dried under reduced pressure to obtain quinoa wheat bran saponin extraction
Object.The volume for the ethanol water that mass fraction used is 30% is 3BV, the ethanol water that mass fraction used is 70%
Volume is 5BV.Being dried under reduced pressure conditional parameter is：Pressure is 0.05MPa, temperature is 50 DEG C, the time is 6 hours.
Test effect
Compression strength, anti-freezing property and water permeability test are carried out to the freeze proof pervious concrete of the high intensity of the present invention, surveyed
Test result is shown in Table 1.
Table 1：28 days compression strength, freeze proof grade and coefficient of permeability test result table
| 28 days compression strength, MPa | Freeze proof grade F | Coefficient of permeability, mm/s | |
| Embodiment 1 | 39.6 | 572 | 15.5 |
| Embodiment 2 | 34.2 | 519 | 13.2 |
| Embodiment 3 | 36.3 | 532 | 14.4 |
| Embodiment 4 | 29.5 | 451 | 11.3 |
| Embodiment 5 | 30.2 | 425 | 12.7 |
| Comparative example 1 | 37.0 | 552 | 14.0 |
| Comparative example 2 | 36.3 | 546 | 13.8 |
By test data it is found that the freeze proof pervious concrete of high intensity of the present invention uses saponins air entraining agent and modified wood
Quality sodium sulfonate, the concrete being prepared have good water penetration, anti-freezing property and compression strength.Saponins air entraining agent carries
It is derived from quinoa wheat bran, realizes the recycling of waste resource, the concrete being prepared has good compression strength, frost resistance
Energy and coefficient of permeability.The present invention is using quinoa wheat bran saponin(e as air entraining agent, with the use of modified sodium lignosulfonate, metering system
Sodium sulfonate effectively prevents the problem of concrete strength caused by the use of conventional air entraining agent reduces as water-reducing agent.
The bubble that the concrete composite air entraining agent of the present invention introduces is fine and smooth, uniform in size, and foam stabilizing effect is good, and air content is kept
It is high, moreover it is possible to improve the intensity and endurance quality of concrete.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical solution, all should be in the protection domain being defined in the patent claims.
Claims (4)
1. a kind of preparation method of high-effective concrete air entraining agent, includes the following steps：Quinoa wheat bran is added to the water, is added fine
The plain enzyme of dimension, pectase, neutral proteinase, are uniformly mixed, and EtOH Sonicate extraction is added, is sieved, is concentrated by evaporation, is dried under reduced pressure.
2. a kind of preparation method of high-effective concrete air entraining agent, includes the following steps：
300-900g quinoa wheat brans are added in 1000-3000g water, 0.05-0.5g cellulases, 0.05-0.5g fruits is added
Glue enzyme, 0.01-0.1g neutral proteinases, are warming up to 35-45 DEG C after mixing, and 1-5 hours are kept the temperature at 35-45 DEG C, are added
1000-3000g ethyl alcohol, is warming up to 50-70 DEG C after mixing, in 50-70 DEG C of ultrasonic extraction 20-60 minutes, ultrasonic frequency
For 20-60KHz, power 200-500W, 100-300 mesh sieve is then crossed, filtrate is crossed into 300-1000g macroporous absorbent resins, is filtered
Flow velocity is 0.5-2BV/h, and the ethanol water for being then 20%-40% with mass fraction elutes macroporous absorbent resin, flow velocity
For 0.5-2BV/h, this eluent is abandoned, then the ethanol water for being 60%-85% with mass fraction elutes macroporous absorption tree
Fat, flow velocity 0.5-2BV/h collect eluent, and it is 1.15-1.35's that eluent, which is concentrated by evaporation, and measures relative density to 60 DEG C
Medicinal extract is dried under reduced pressure to obtain the high-effective concrete air entraining agent by medicinal extract, and mass fraction used is that the ethyl alcohol of 20%-40% is water-soluble
The volume of liquid is 2-5BV, and the volume for the ethanol water that mass fraction used is 60%-85% is 3-6BV;
It is preferred that the conditional parameter that is dried under reduced pressure is：Pressure is 0.03-0.07MPa, temperature is 45-75 DEG C, the time is 3-12 small
When;
It is preferred that the macroporous absorbent resin is D101 types, HP100 types, one kind in X-5 types, the macroporous absorbent resin is into one
Step is preferably D101 types.
3. a kind of high-effective concrete air entraining agent, is prepared using claim 2 the method.
4. the application of high-effective concrete air entraining agent as claimed in claim 2, the addition of the concrete air-entrainer with it is mixed
The mass ratio 1 of cement addition in solidifying soil：(2500-300000), preferred mass ratio are 1：(20000-80000).
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Application publication date: 20180817 |