CN104788629A - Polycarboxylate water-reducing agent and normal-temperature preparation method thereof - Google Patents
Polycarboxylate water-reducing agent and normal-temperature preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polycarboxylate water-reducing agent and a normal-temperature preparation method thereof. The polycarboxylate water-reducing agent is characterized by being prepared at normal temperature from the following raw materials: 27.5-31wt% of unsaturated polyoxyethylene ether, 2.6-3.0wt% of unsaturated carboxylic acid, 0.26-0.43wt% of an organosilicon monomer, 4.5-8.0wt% of lignosulfonate, 0.030-0.08wt% of a reducing agent, 0.16-0.30wt% of an oxidizing agent, 0.041-0.063wt% of a transfer agent, 1.0-1.16wt% of an alkaline regulating agent, and 60wt% of water. The prepared polycarboxylate water-reducing agent is high in water-reducing rate and good in slump performance, solves the adaptability problems of the polycarboxylate water-reducing agent and a concrete raw materialm and has high water retention cohesiveness in the application of concrete, in particular to machine-made sand concrete. Lignosulfonate, as one of the raw materials of the polycarboxylate water-reducing agent, is rich in source, reproducible, suitable for industrialized mass production and wide in product market prospect.
Description
Technical field
The present invention relates to the technical field of concrete additives in material of construction, be specifically related to a kind of polycarboxylate water-reducer and normal temperature preparation method thereof.
Background technology
High performance water reducing agent of polyocarboxy acid is the base mateiral preparing high performance concrete, prepare high performance water reducing agent of polyocarboxy acid at present raw materials used a lot of with synthesis technique, different reaction raw materials and synthesis technique have a significant impact the Structure and Properties preparing polycarboxylate water-reducer.The advantage of high performance water reducing agent of polyocarboxy acid is that its Molecular Structure Design degree of freedom is large, environmental pollution is little, function controllable, water-reducing rate advantages of higher, is widely used in concrete works in recent years.
But traditional polycarboxylate water-reducer adopts heat temperature raising method to carry out Raolical polymerizable preparation, boiler is mostly needed to heat during production, energy consumption is large, polyreaction terminates rear system also to be needed to be cooled to certain temperature and just can carry out in alkaline solution and adjust ph, whole production process length consuming time, production cost is high.Secondly, produce polycarboxylate water-reducer raw materials mainly from the Nonrenewable resources oil of worsening shortages, expensive, particularly some starting material domestic still dependence on import, therefore cost is also higher.
In addition, because the raw material types of producing the reinforcement of concrete is various, regional disparity is large, polycarboxylate water-reducer is often easily caused to occur incompatibility phenomenon with ground material etc., particularly along with the decline of natural river sand produced quantity, Machine-made Sand progressively replaces natural sand to become concrete important production starting material, and it is lack of standardization due to what produce, grating and the grain type of Machine-made Sand can have a strong impact on concrete serviceability, cause fresh concrete easily to occur the phenomenons such as segregation, bleeding, cause concrete engineering quality accident.
Summary of the invention
The object of the present invention is to provide a kind of can the polycarboxylate water-reducer containing organosilicon and xylogen prepared of normal temperature.
For achieving the above object, the invention provides a kind of normal temperature preparation method of polycarboxylate water-reducer, be prepared from by the material composition of following weight percent,
According to embodiments of the invention, described unsaturated Soxylat A 25-7 is isopentenol polyoxyethylene ether or methacrylic Soxylat A 25-7, and molecular weight is 1000 ~ 2500.
According to embodiments of the invention, described unsaturated carboxylic acid is at least one in vinylformic acid, methacrylic acid or maleic anhydride.
According to embodiments of the invention, described silicoorganic compound are γ-(methacryloxypropyl) oxypropyl trimethyl silane or vinyltrimethoxy silane.
According to embodiments of the invention, described reductive agent is L-AA or rongalite.
According to embodiments of the invention, described oxygenant is hydrogen peroxide or ammonium persulphate.
According to embodiments of the invention, described chain-transfer agent is Thiovanic acid or thiohydracrylic acid.
According to embodiments of the invention, described alkaline conditioner is sodium hydroxide or potassium hydroxide.
According to embodiments of the invention, the normal temperature preparation method of polycarboxylate water-reducer, comprises the following steps:
(1) unsaturated Soxylat A 25-7 is taken and water adds reactor, be stirred under normal temperature and dissolve completely, add oxygenant, stir 5-10 minute, then respectively to the mixing solutions dripping the mixing solutions of unsaturated carboxylic acid and organosilane monomer, lignin liquor, chain-transfer agent and reductive agent in reactor, time for adding is 3-5 hour, drips off rear continuation reaction 1-2 hour;
(2) after having reacted, being neutralized to pH with alkaline conditioner is 6-7, obtains the polycarboxylate water-reducer solution that concentration is 40%.
The polycarboxylate water-reducer that the present invention also protects the preparation method of described polycarboxylate water-reducer to prepare.
For solving the technical barrier of the aspects such as the high and water-retentivity of polycarboxylate water-reducer cost is not enough, the present invention proposes and a kind ofly contain polycarboxylate water-reducer of organosilicon and xylogen and preparation method thereof.The polycarboxylate water-reducer synthesized in this way has larger advantage in cost and water conservation cohesiveness.
Silane bond structure in organosilicon is similar to the raw-material silicate sturcture of concrete parts, and both can form strong chemical bond, good bonding strength, thus improves the water conservation cohesiveness of concrete entirety.And sulfonated lignin are a kind of natural reproducible resources, cost is low, and itself also has certain thickening power, can improve concrete water conservation cohesiveness.In polycarboxylate water-reducer, introduce organosilicon and sulfonated lignin, both have certain synergy simultaneously, can improve concrete workability, improve the adaptability of product, reduce the susceptibility of product.
Beneficial effect:
A kind of normal temperature preparation method containing the polycarboxylate water-reducer of organosilicon and xylogen provided by the invention, this preparation technology is simple, and reaction is carried out at normal temperatures, whole production process temperature is without the need to controlling, and the reaction times is short, and energy consumption is low, cost is low, and safety coefficient is high, is easy to suitability for industrialized production.
A kind of normal temperature preparation method containing the polycarboxylate water-reducer of organosilicon and xylogen provided by the invention, according to design theory of molecular structure, in polycarboxylate water-reducer building-up process, directly introducing organosilicon and lignin molecule carry out graft copolymerization, the micro molecule of product is made to introduce functional group, not only water-reducing rate is high, function of slump protection is good, and solve the adaptability problem of polycarboxylate water-reducer and concrete raw material, in concrete particularly machine-made sand concrete application, there is good water conservation cohesiveness.
Raw material wood element of the present invention (being also sulfonated lignin) is a kind of renewable resources of abundance, and environmental protection and economy, can reduce production cost, and be applicable to industrialization scale operation, produce market has a extensive future.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
Embodiment 1:
The each embodiment of table 1 component list (gram) used
Preparation method:
(1) each starting material are taken according to the data in table 1.
(2) unsaturated Soxylat A 25-7 and water are added reactor, be stirred under normal temperature and dissolve completely, add oxygenant, stir 5-10 minute, then respectively to the mixing solutions dripping the mixing solutions of unsaturated carboxylic acid and organosilane monomer, sulfonated lignin, chain-transfer agent and reductive agent in reactor, time for adding is 3-5 hour, drips off rear continuation reaction 1-2 hour;
(2) after having reacted, being neutralized to pH with alkaline conditioner is 6-7, obtains the polycarboxylate water-reducer solution that concentration is 40%.
Embodiment 2:
Starting material: in table 1.
Preparation method is shown in embodiment 1.
Embodiment 3:
Starting material: in table 1.
Preparation method is shown in embodiment 1.
Embodiment 4:
Starting material: in table 1.
Preparation method is shown in embodiment 1.
Embodiment 5:
Starting material: in table 1.
Preparation method is shown in embodiment 1.
Embodiment 6: compliance test result is tested
Comparative example:
Unsaturated for 347.8g Soxylat A 25-7 and 278.4g water are added reactor, be heated with stirring to 60 DEG C, 1.5g ammonium persulphate is added after unsaturated Soxylat A 25-7 all dissolves, start after stirring to drip 104.4g acrylic acid solution (being mixed by 34.8g vinylformic acid and 69.6g water) and 105.2g mercaptoacetic acid solution (being mixed by 0.8g Thiovanic acid and 104.4g water) simultaneously, time for adding controls at 3 hours, after dropping terminates, 1 hour is incubated at 60 DEG C, make polyreaction complete, after insulation terminates, cool to less than 45 DEG C, add the NaOH solution adjust ph of 38.5g30 % by weight to 6-7, moisturizing 124.2g obtains the polycarboxylate water-reducer that concentration is 40%.
1 paste flowing degree
Good fortune P.042.5 cement is built in employing, and test determination is with the paste flowing degree of each under volume embodiment and comparative example.Test is carried out according to GB/T8077-2012 " Methods for testing uniformity of concrete admixture ", W/C=0.29, and volume is the solid volume of folding, with cementaceous gauge.Test-results is in table 1:
The clean slurry flowing property result of table 1 different water reducer kind
As can be seen from Table 1, polycarboxylate water-reducer of the present invention has excellent flowing degree of net paste of cement and hold facility compared to contrast.
2 concrete tests
Employing build good fortune P.042.5 cement test concrete bleeding rate, the slump and through time slump-loss.Concrete design class is the machine-made sand concrete of C25, concrete mix is cement: water: sand (Machine-made Sand): stone: flyash: breeze=240: 176: 828: 992: 48: 32 (weight ratios), water reducer volume is the solid volume of folding, with cementaceous gauge.Test-results is in table 2:
The concrete test result table of the different water reducer kind of table 2
As can be seen from Table 2, polycarboxylate water-reducer water-reducing rate of the present invention is high, and slump retaining is good, and bleeding rate is 0, and water conservation cohesiveness is good, excellent combination property.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (10)
1. a normal temperature preparation method for polycarboxylate water-reducer, is characterized in that, is prepared from by the material composition of following weight percent,
2. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described unsaturated Soxylat A 25-7 is isopentenol polyoxyethylene ether or methacrylic Soxylat A 25-7, and molecular weight is 1000 ~ 2500.
3. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described unsaturated carboxylic acid is at least one in vinylformic acid, methacrylic acid or maleic anhydride.
4. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described silicoorganic compound are γ-(methacryloxypropyl) oxypropyl trimethyl silane or vinyltrimethoxy silane.
5. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described reductive agent is L xitix or rongalite.
6. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described oxygenant is hydrogen peroxide or ammonium persulphate.
7. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described chain-transfer agent is Thiovanic acid or thiohydracrylic acid.
8. the normal temperature preparation method of polycarboxylate water-reducer according to claim 1, is characterized in that, described alkaline conditioner is sodium hydroxide or potassium hydroxide.
9. the normal temperature preparation method of polycarboxylate water-reducer described in claim 1, is characterized in that, comprises the following steps:
(1) unsaturated Soxylat A 25-7 is taken and water adds reactor, be stirred under normal temperature and dissolve completely, add oxygenant, stir 510 minutes, then respectively to the mixing solutions dripping the mixing solutions of unsaturated carboxylic acid and organosilane monomer, lignin liquor, chain-transfer agent and reductive agent in reactor, time for adding is 35 hours, drips off rear continuation reaction 1-2 hour;
(2) after having reacted, being neutralized to pH with alkaline conditioner is 67, obtains the polycarboxylate water-reducer solution that concentration is 40%.
10. the polycarboxylate water-reducer for preparing of the preparation method of the arbitrary described polycarboxylate water-reducer of claim 1-9.
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CN105504183A (en) * | 2016-01-11 | 2016-04-20 | 中国水电十一局有限公司混凝土外加剂厂 | Method for synthesis of ether type polycarboxylic acid water reducer |
CN105504185A (en) * | 2016-01-28 | 2016-04-20 | 青海金佳源建材有限公司 | Polycarboxylate water reducing agent and preparation technology thereof |
CN105669911A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Concrete water-retention anti-segregation agent and preparation method thereof |
CN105669919A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Polycarboxylate superplasticizer with high water retention and preparation method thereof |
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CN105985047A (en) * | 2016-01-15 | 2016-10-05 | 安徽鑫润新型材料有限公司 | Modified polycarboxylate water reducer capable of improving strength of concrete |
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CN109665741A (en) * | 2017-10-14 | 2019-04-23 | 廖志琳 | A kind of room temperature cement water reducing agent that dispersion rate is high |
CN110606695A (en) * | 2019-10-17 | 2019-12-24 | 江苏兆佳建材科技有限公司 | Modified polycarboxylate superplasticizer and preparation method thereof |
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CN102241489A (en) * | 2011-04-19 | 2011-11-16 | 广东红墙新材料股份有限公司 | Super-retarding polycarboxylic acid water reducer and preparation method and using method thereof |
CN103803846A (en) * | 2014-01-22 | 2014-05-21 | 北京奥润开元环保科技研究院有限公司 | Mud-resistant and salt-resistant polycarboxylate superplasticizer and preparation method thereof |
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