CN102211912B - Cement-based grouting material containing sulfamate water reducing agent and preparation method thereof - Google Patents
Cement-based grouting material containing sulfamate water reducing agent and preparation method thereof Download PDFInfo
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- CN102211912B CN102211912B CN2011100875391A CN201110087539A CN102211912B CN 102211912 B CN102211912 B CN 102211912B CN 2011100875391 A CN2011100875391 A CN 2011100875391A CN 201110087539 A CN201110087539 A CN 201110087539A CN 102211912 B CN102211912 B CN 102211912B
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- cement
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- water reducer
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- grouting material
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a cement-based grouting material containing sulfamate water reducing agent and a preparation method thereof. The cement-based grouting material comprises the following components in parts by weight: 350-500 parts of cement clinker, 80-130 parts of pulverized fuel ash, 20-30 parts of expanding agent, 80-120 parts of gypsum, 1-2 parts of pH value regulating agent, 8-15 parts of water reducing agent and 300-500 parts of quartz sand, wherein the sulfamate water reducing agent is prepared from the raw materials of phenol, sodium hydroxide, formaldehyde, sulfamic acid and para-aminobenzene sulfonic acid in the weight ratio of (15-25):(9-13):(20-3):(20-35):(10-15). The cement-based grouting material has high strength and low bleeding rate; the used water reducing agent has small slump loss, high water reducing rate, simple preparation process and low cost; and an external heating source is not required to be provided in the reaction process, so that energy is greatly saved and the environmental pollution is reduced.
Description
Technical field
The present invention relates to a kind of material of construction and preparation method thereof, relate in particular to a kind of cement-based grouting material that contains particular variety thionamic acid class water reducer and preparation method thereof.
Background technology
Concrete structure is large because of its fragility, tends to the cracking phenomenon in engineering is used, and the concrete structure watertightness descends, seepage and concrete cracking can cause, and then affects the work-ing life of engineering.Thereby in construction and operational phase, many engineerings such as water conservancy, railway, highway, bridge etc. need the injection material fracture to repair and reinforce inevitably.And the installation of many large-scale instruments also needs with high-performance grouting material perfusion wall screw and machinery bed or steel construction and basic combining site etc.
Repairing concrete crack commonly used and the injection material of reinforcing are a lot, divide from material type, mainly contain chemical grouting material and cement-based grouting material two large classes.Chemical grouting material has that particle is thin, intensity is high, viscosity is low, and flowability, stability and concrete castability are good, gelling or set time can the advantage such as regulate by requirement of engineering, but its cost is high, transport and store inconvenience, complicated construction technique, mostly has toxicity in various degree, comprise pungency, corrodibility, sensitization and the shortcoming such as inflammable and explosive, simultaneously, because test, constructing operation and discharging dead meal etc. cause environmental pollution and to groundwater pollution, the application of chemical grouting material also more and more is restricted.That the cement based cement grouting material has is easy to use, intensity is high, good endurance, pollution-free, the characteristics such as cost is low, the source is wide, thereby, more and more obtained using widely.But Portland cement base grouting material particle is thicker, the poor stability of slurries, easily precipitates bleed, and volumetric shrinkage is arranged during sclerosis.In addition, after the strengthening of foundation grouting, slurry has certain contraction, again ftractures easily.Therefore, those skilled in the art are devoted to overcome by adding the approach such as admixture the defects of cement-based grouting material in recent years.Wherein, cement additive commonly used, also be concrete admixture for example the adding of water reducer help to improve defects, but, it is that those skilled in the art want to solve again very scabrous problem that the necessity, the especially raising of winter severe cold Water Under mud base grouting material intensity that improve are still arranged again always.
Water reducer is called again dispersion agent or fluidizer, during owing to use the water consumption of fresh concrete is reduced, and therefore gains the name.In the modern concrete technical field, water reducer is one of admixture that improves rheological property of concrete, has been taken as five component of concrete except cement, sand, stone and water.Select appropriate water reducer, not only can improve concrete rheological property, and can be so that the water consumption in concrete/cement reduces, and then improve the intensity after concrete/cement solidification, reduce bleeding rate.
Common water reducer mainly contains xylogen ring phosphate-gallate series, naphthalene system, melamine series, sulfamate system and polycarboxylic acid series etc.Be the application and development period of ordinary water-reducing agent the thirties to the sixties in 20th century, the water reducer of early application is mainly the organic compound such as sodium abietate, sodium lignosulfonate, stearate, it mainly is be used to improving concrete application property, solving the endurance issues such as freeze-thaw-of concrete road surface.But along with improving constantly of construction requirement, the water-reducing effect of the water reducer that these are early stage can not satisfy the needs of modern construction.
Since at first developing naphthalene sulfonic acidformaldehyde condensation product high efficiency water reducing agent and West Germany's exploitation melamine superplasticizer in 1964 from Japan in 1962, exploitation and the application period of high efficiency water reducing agent have been entered, advantageously promoted the development of concrete technology, the outstanding feature of these two series of high efficiency water reducers is that water-reducing rate is high, the cement dispersion effect is good, its Main Function is decrease unit consumption of water or unit cement consumption, be used for preparing high-strength, superelevation is strong, high durability concrete, but its fatal shortcoming is that slump-loss is large, and formaldehyde volatilization environmental pollution is serious in the preparation process.And polycarboxylic acid series high efficiency water reducing agent blending amount is low, but to the good dispersity of concrete (cement), slump retaining is good, and easily modification so its high performance potentiality are large, is considered to the regeneration product of high efficiency water reducing agent, but its cost is higher, therefore uses and is subject to certain limitation.
Aminosulfonic water-reducing agent also is considered to an analog high efficiency water reducing agent, and its cost is low with respect to poly carboxylic acid series water reducer, therefore, also is widely used.But, need to consume a large amount of heat energy in traditional aminosulfonic water-reducing agent production process, otherwise perhaps cause easily implode, therefore the production of industrial aminosulfonic water-reducing agent has caused serious environmental pollution or has existed because the potential safety hazard that reaction raw materials generation implode causes.
Summary of the invention
The present invention is in order to overcome above-mentioned deficiency of the prior art, a kind of novel water reducer is provided, this water reducer environmental protection, little loss of slump, water-reducing rate height, and preparation technology is simple, with low cost, especially need not to provide external heat source in the reaction process, thereby greatly saved the energy, reduced environmental pollution.Further, the invention provides a kind of cement-based grouting material that contains this water reducer and preparation method thereof, this injection material intensity is high, and bleeding rate is low.
The cement-based grouting material that contains sulfamate water reducer of the present invention comprises by weight: cement clinker 350～500, flyash 80～130, swelling agent 20～30, gypsum 80～120, pH value conditioning agent 1～2, sulfamate water reducer 8～15, quartz sand 300～500, wherein said sulfamate water reducer is prepared from by following part by weight by following raw material: phenol: sodium hydroxide: formaldehyde: thionamic acid: Sulphanilic Acid is 15～25: 9～13: 20～3: 20～35: 10～15.Preferably, the parts by weight of described cement clinker are 380～420, and the parts by weight of described water reducer are 9～11.
Preferably, described cement clinker is Portland clinker.Preferably, described swelling agent comprises sulplo-aluminate, and further preferably, described swelling agent is sulplo-aluminate, more preferably calcium sulphoaluminate.Preferably, the described pH value conditioning agent mixed thing that to be boric acid and tripoly phosphate sodium STPP obtain according to 1: 2 ratio.
Preferably, described quartz sand comprises thick quartz sand, middle quartz sand and three kinds of fractions of fine quartz sand, the amount ratio of three kinds of fractions is 45～60: 35～50: 10～20, wherein the particle size range of thick quartz sand is＞3mm～5mm, the particle size range of middle quartz sand is 2～3mm, and the particle size range of fine quartz sand is＞0mm～2mm.The inventor finds unexpectedly, is used according to three kinds of quartz sands that will satisfy above-mentioned restriction and can further improves concrete intensity, reduces bleeding rate.
Preferably, sulfamate water reducer of the present invention is prepared from following ratio by following raw material: phenol: sodium hydroxide: formaldehyde: thionamic acid: Sulphanilic Acid is 18～21: 9～10: 28～31: 28～31: 10～12.
The present invention provides a kind of preparation method who contains the cement-based grouting material of sulfamate water reducer in addition, comprising the step that following raw material is mixed according to following parts by weight: cement clinker 350～500, flyash 80～130, swelling agent 20～30, gypsum 80～120, pH value conditioning agent 1～2, sulfamate water reducer 8～15, quartz sand 300～400, wherein said sulfamate water reducer is prepared from by following part by weight by following raw material: phenol: sodium hydroxide: formaldehyde: thionamic acid: Sulphanilic Acid is 15～25: 9～13: 20～3: 20～35: 10～15.
The preparation process of described sulfamate water reducer comprises: phenol is joined in the aqueous sodium hydroxide solution, rear adding thionamic acid stirs, continue to stir, add part formaldehyde after even to mixing solutions, add Sulphanilic Acid after between reacting one section, then, residual formaldehyde is added, continue reaction and obtain liquid product.Wherein need not the external heat source heat supply in the reaction process, circulation obtains initial reaction stage institute heat requirement from reaction later stage liberated heat.
Preferably, the adding of described part formaldehyde and described residual formaldehyde all adopts the mode of dropping to add.Preferably, the amount of the described part formaldehyde that adds of initial stage is add 0.25～0.4 times of the formaldehyde total amount.Preferably, the joining day of described part formaldehyde is 5～15 minutes, and the joining day of described residual formaldehyde is 2～4 hours.Preferably, gained liquid product further drying is solid, for example passes through spraying drying.
The present invention unexpectedly finds, with thionamic acid and the composite replacement of Sulphanilic Acid Sulphanilic Acid of the prior art as the heat that produces in its production process of raw material production sulfamate water reducer through reclaiming, can satisfy the required heat requirement of initial reaction stage after the circulation, and regulate addition step and feed time, can be so that the heat that reaction generates satisfies self needs, and can so that reaction process is carried out smoothly, implode and sticking still can not occur in the reaction.
In addition, the inventor further finds, use water reducer of the present invention, can be so that required discharge reduction be more than 20% in the cement-based grouting material use procedure, thereby improved the intensity after described cement-based grouting material solidifies, reduce bleeding rate, especially improved the performance after the winter construction.
Embodiment
The testing method explanation:
The testing method of the slump: with a 100mm suitable for reading, end opening 200mm, the trumpet-shaped slump bucket of high 300mm, tamping behind the penetration concrete, then pull up bucket, concrete produces the slump phenomenon because of deadweight, deduct the height of concrete vertex after the slump with bucket high (300mm), be called slump, unit is mm.
Water-reducing rate is according to the method test of stipulating among the GB8076-2008.
Ultimate compression strength is tested according to GB/T 50448-2008; Bleeding rate is according to the regulation test of GB/T 50080 the 5.1st joint.
Preparation Example 1
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, rear adding 600Kg phenol stirs, then continue to stir, add the 1050Kg thionamic acid, stirred 40 minutes, 300Kg formaldehyde is added drop-wise in the reaction system reacted about 1 hour, add the 350Kg Sulphanilic Acid, then 700Kg formaldehyde is added drop-wise in the reaction system, continues to react half an hour, obtain product liquid.Need not in the reaction process to provide to add heat, turn back to reactor by circulation line after only will reacting the heat collection that produces.Through measuring, wherein the molecular weight of gained condensation product is about 6000.
Preparation Example 2
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, rear adding 600Kg phenol stirs, then continue to stir, add the 1000Kg thionamic acid, stirred 40 minutes, 300Kg formaldehyde is added drop-wise in the reaction system reacted about 1 hour, add the 450Kg Sulphanilic Acid, then 700Kg formaldehyde is added drop-wise in the reaction system, continues to react half an hour, obtain product liquid.Need not in the reaction process to provide to add heat, turn back to reactor by circulation line after only will reacting the heat collection that produces.Through measuring, wherein the molecular weight of gained condensation product is about 6200.
Preparation Example 3
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, rear adding 600Kg phenol stirs, then continue to stir, add the 1050Kg thionamic acid, stirred 40 minutes, 350Kg formaldehyde is added drop-wise in the reaction system reacted about 1 hour, add the 350Kg Sulphanilic Acid, then 600Kg formaldehyde is added drop-wise in the reaction system, continues to react half an hour, obtain product liquid.Need not in the reaction process to provide to add heat, turn back to reactor by circulation line after only will reacting the heat collection that produces.Through measuring, wherein the molecular weight of gained condensation product is about 6100.
Preparation Comparative Examples 1
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, and then the rear adding 600Kg phenol that stirs continue to stir, add the 1400Kg Sulphanilic Acid, stirred 40 minutes, and 1000Kg formaldehyde was added drop-wise in the reaction system reacted about 2 hours, obtain product liquid.Need provide in the reaction process and add heat, could be so that react smooth.Through measuring, wherein the molecular weight of gained condensation product is about 6000.
Preparation Comparative Examples 2
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, rear adding 600Kg phenol stirs, then continue to stir, add 1050Kg thionamic acid and 350Kg Sulphanilic Acid, stirred about 1 hour, 1000Kg formaldehyde is added drop-wise in the reaction system reaction about 2 hours, obtains product liquid.Need not in the reaction process to provide to add heat, turn back to reactor by circulation line after only will reacting the heat collection that produces.Through measuring, wherein the molecular weight of gained condensation product is about 8000.
Preparation Comparative Examples 3
The sodium hydroxide of 3000kg water and about 300Kg is joined in the reactor, rear adding 600Kg phenol stirs, then continue to stir, add 1050Kg thionamic acid and 350Kg Sulphanilic Acid, stirred about 1 hour, join in the reaction system very fast generation implode with 1000Kg formaldehyde is disposable.
Application Example about water reducer of the present invention
For the effect of water reducer of the present invention is described, following table provides adds respectively in the Lafarge cement water reducer of the present invention and the described water reducer of Comparative Examples the contrast table of cement performance to.
Table 1:
Performance Ratio after adding to respectively water reducer of the present invention and the described water reducer of Comparative Examples in the Lafarge cement
Embodiment 1
A kind of preparation method of cement-based grouting material is provided, and the method makes by following component is mixed according to following weight part, wherein:
Cement clinker 380, flyash 90, calcium sulphoaluminate 25, gypsum 80, boric acid 0.5, tripoly phosphate sodium STPP 1, the water reducer 10 of Preparation Example 1, average particle size particle size is the middle quartz sand 450 about 2.5mm.
Embodiment 2
Other is identical with embodiment 1, and difference is to replace with the water reducer of Preparation Example 2 water reducer of Preparation Example 1.
Embodiment 3
Other is identical with embodiment 1, and difference is to replace with the water reducer of Preparation Example 3 water reducer of Preparation Example 1.
Embodiment 4
Other is identical with embodiment 1, and it is that to replace average particle size particle size among the embodiment 1 be quartz sand in 450 weight parts about 2.5mm for fine quartz sand 70 weight parts, middle quartz sand 200 weight parts about 2.5mm and thick quartz sand 180 weight parts about 4mm about 1mm that difference is with average particle size particle size.
Comparative Examples 1
Other is identical with embodiment 1, and difference is that the water reducer with preparation Comparative Examples 1 replaces the water reducer of Preparation Example 1.
Comparative Examples 2
Other is identical with embodiment 1, and difference is that the water reducer with preparation Comparative Examples 2 replaces the water reducer of Preparation Example 1.
Comparative Examples 3
In the Lafarge cement of 1026 commercially available weight parts, add the water reducer that makes in the Preparation Example 1 of 10 weight parts.
The Performance Ratio of table 2 embodiment 1-4 and the described cement-based grouting material of Comparative Examples 1-3
Annotate 1:R
-7The ratio of expression 7 days test specimen compression strength value of negative temperature conservation and 28 days test specimen compression strength value of normal curing.
Claims (7)
1. cement-based grouting material that contains sulfamate water reducer, it comprises following component by weight: cement clinker 350～500, flyash 80～130, swelling agent 20～30, gypsum 80～120, pH value conditioning agent 1～2, sulfamate water reducer 8～15, quartz sand 300～500, wherein said sulfamate water reducer is prepared from by following part by weight by following raw material: phenol: sodium hydroxide: formaldehyde: thionamic acid: Sulphanilic Acid is 18～21: 9～10: 28～31: 28～31: 10～12.
2. cement-based grouting material claimed in claim 1, the wherein said pH value conditioning agent mixed thing that to be boric acid and tripoly phosphate sodium STPP obtain according to 1: 2 ratio.
3. preparation method who contains the cement-based grouting material of sulfamate water reducer, comprising the step that following raw material is mixed according to following parts by weight: cement clinker 350～500, flyash 80～130, swelling agent 20～30, gypsum 80～120, pH value conditioning agent 1～2, sulfamate water reducer 8～15, quartz sand 300～400, wherein said sulfamate water reducer is prepared from by following part by weight by following raw material: phenol: sodium hydroxide: formaldehyde: thionamic acid: Sulphanilic Acid is 18～21: 9～10: 28～31: 28～31: 10～12.
4. the preparation method of cement-based grouting material claimed in claim 3, the preparation process of wherein said sulfamate water reducer comprises: 1) phenol is joined in the aqueous sodium hydroxide solution; 2) add thionamic acid; 3) add the part formaldehyde reaction; 4) add Sulphanilic Acid, then, will add residual formaldehyde, continue reaction and obtain liquid product, the adding of wherein said part formaldehyde and described residual formaldehyde all adopts the mode of dropping to add.
5. method claimed in claim 4, the preparation process of wherein said sulfamate water reducer specifically comprises: phenol is joined in the aqueous sodium hydroxide solution, rear adding thionamic acid stirs, continue to stir, add part formaldehyde after even to mixing solutions, add Sulphanilic Acid after between reacting one section, then, residual formaldehyde is added, continue reaction and obtain liquid product, wherein need not the external heat source heat supply in the reaction process, circulation obtains initial reaction stage institute heat requirement from reaction later stage liberated heat.
6. each described method of claim 4～5, wherein the amount of the described part formaldehyde that adds of initial stage is add 0.25～0.4 times of the formaldehyde total amount.
7. each described method of claim 4～5, the joining day of wherein said part formaldehyde is 5～15 minutes, the joining day of described residual formaldehyde is 2～4 hours.
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| CN2011100875391A CN102211912B (en) | 2011-04-08 | 2011-04-08 | Cement-based grouting material containing sulfamate water reducing agent and preparation method thereof |
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| CN102211912B true CN102211912B (en) | 2013-01-30 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104631262B (en) * | 2014-12-19 | 2018-10-02 | 大元建业集团股份有限公司 | A kind of construction method reducing live Cement Cold Regeneration Technology mixture basic crack |
| CN106188455B (en) * | 2016-07-25 | 2018-01-30 | 抚顺东科精细化工有限公司 | A kind of synthetic method of bisphenol A polyethenoxy ether modified sulfamate water reducer |
| CN107759756B (en) * | 2017-10-17 | 2020-08-11 | 江苏苏博特新材料股份有限公司 | Sulfamate water reducer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121084A (en) * | 1994-10-21 | 1996-04-24 | 遵化市钟馗实业公司 | Low-poison synthetic urea-formaldehyde resin glue and its production method |
| CN1559963A (en) * | 2004-02-26 | 2005-01-05 | 同济大学 | Sulfamate as high performance reducing water agent for building and preparing proces thereof |
| CN101602589A (en) * | 2009-06-30 | 2009-12-16 | 中国地质大学（武汉） | Post-tensioned prestressing pipeline vacuum grouting or mud jacking preformed material and preparation method thereof |
-
2011
- 2011-04-08 CN CN2011100875391A patent/CN102211912B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121084A (en) * | 1994-10-21 | 1996-04-24 | 遵化市钟馗实业公司 | Low-poison synthetic urea-formaldehyde resin glue and its production method |
| CN1559963A (en) * | 2004-02-26 | 2005-01-05 | 同济大学 | Sulfamate as high performance reducing water agent for building and preparing proces thereof |
| CN101602589A (en) * | 2009-06-30 | 2009-12-16 | 中国地质大学（武汉） | Post-tensioned prestressing pipeline vacuum grouting or mud jacking preformed material and preparation method thereof |
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