CN104356315A - Antisludge polycarboxylate superplasticizer and preparation method thereof - Google Patents
Antisludge polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN104356315A CN104356315A CN201410673599.5A CN201410673599A CN104356315A CN 104356315 A CN104356315 A CN 104356315A CN 201410673599 A CN201410673599 A CN 201410673599A CN 104356315 A CN104356315 A CN 104356315A
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- reducer
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Abstract
The invention relates to the technical field of the concrete admixtures and specifically relates to an antisludge polycarboxylate superplasticizer and a preparation method thereof. The antisludge polycarboxylate superplasticizer is synthesized through copolymerization of monomers isopentenyl alcohol polyoxyethylene ether, acrylic acid, sodium acrylsulfonate and hydroxyethyl acrylate. According to the antisludge polycarboxylate superplasticizer, the addition of the raw materials during time periods in the reaction process is controlled, and meanwhile, sodium acrylsulfonate and hydroxyethyl acrylate are introduced, and therefore, the copolymerization rate of the monomers is increased and the self-polymerization reaction of the acrylic acid high in activity is reduced; and due to the introduction of sulfonic acid groups, the dispersibility and peaceability of concrete are improved. The preparation method of the antisludge polycarboxylate superplasticizer is simple and controllable in process, short in reaction time and obvious in economic benefit.
Description
Technical field
The invention belongs to technical field of concrete additives, be specifically related to a kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof.
Background technology
The development of cement concrete production and construction technology depends on that the developmental level with utilisation technology produced by water reducer to a great extent.Water-reducing rate is high, slump-loss is low, shrinking percentage is little, advantages of environment protection is known as the third generation high-performance water reducing agent grown up after wooden calcium and naphthalene system both at home and abroad because it has for polycarboxylate water-reducer.When but in aggregate, silt content is higher, high silt content affects the bond of cement and aggregate and mud powder is assembled agglomerating, have a strong impact on concrete mechanical property and workability, when poly carboxylic acid series water reducer is applied to silt content high aggregate, there is strong absorption trend, there is bad adaptability, responsive to earth, the problems such as slump retaining difference.
Mostly by the composite two kinds of methods of super blending during current solution problems, virtually add use cost, and easily cause concrete segregation when volume is excessive, have a strong impact on concrete intensity, cause potential safety hazard.
Therefore, research and develop that a kind of reaction process is simple efficient, synthesis cost is low and can the poly carboxylic acid series water reducer of effective anti-earth absorption, the development for concrete production and operating technique is significant.
Summary of the invention
The object of the invention is to the defect existed for prior art, provide that a kind of water-reducing rate is high, Slump Time losing of Large is low, the anti-chamotte mould polycarboxylate water-reducer low to cement content susceptibility.
Present invention also offers a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, this preparation method's technique is simple, and cost is low.
For achieving the above object, the present invention is achieved through the following technical solutions:
The invention provides a kind of anti-chamotte mould polycarboxylate water-reducer, adopt following raw material to carry out copolyreaction by described weight part:
Isopentenol polyoxyethylene ether 280-330, vinylformic acid sodium sulfonate 5-10, ammonium persulphate 2.5-3.5,30% hydrogen peroxide 1.2-2, vinylformic acid (AA) 30-45, Hydroxyethyl acrylate 30-60, thin base propionic acid 1.4-2.2.
The molecular weight of described isopentenol polyoxyethylene ether is 2000-2400.
Present invention also offers a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, comprise the following steps:
A. get the isopentenol polyoxyethylene ether 280-330 of weight part, vinylformic acid sodium sulfonate 5-10, ammonium persulphate 2.5-3.5,30% hydrogen peroxide 1.2-2 join in the deionized water of 286-380 weight part, be made into end liquid;
B. get vinylformic acid (AA) 30-45, the Hydroxyethyl acrylate 30-60 of weight part, thin base propionic acid 1.4-2.2 joins in the deionized water of 190-270 weight part and mixes, stir, wiring solution-forming A;
C. when end liquid temp is heated to 65 DEG C, drip the solution A in step b in end liquid, time for adding is 2 hours;
E., after being added dropwise to complete, insulation continues reaction 1 hour, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, be warming up to 70 DEG C, be incubated aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
When dripping solution A in described step c, within first 1 hour, drip 1/3 of solution A total mass.
In described step c, liquid caustic soda is aqueous sodium hydroxide solution.
Present invention employs unique raw material and drip mode, strict control is carried out to the dripping quantity in the time period of raw material, copolyreaction can be made fully to carry out.In raw material, vinylformic acid activity is higher, and when temperature of reaction raises, vinylformic acid very easily produces self-polymeric reaction, thus causes with active little compared with the copolymerization rate of low isopentenol polyoxyethylene ether, the water reducer poor-performing of synthesis.By introducing active moderate vinylformic acid sodium sulfonate and Hydroxyethyl acrylate in the present invention, control the dripping quantity of raw material simultaneously, effectively can control the molecular weight synthesizing water reducer, reduce the generation of acrylic acid self-polymeric reaction, introduce sulfonic acid group simultaneously, produce reversible adsorption effect, improve concrete dispersiveness, earth can not be assembled agglomerating, low to the susceptibility of earth.
Advantage of the present invention and beneficial effect are:
1. in preparation process of the present invention, control the dripping quantity of raw material within the time period, make reaction more abundant, preparation method's technique is simply controlled.
2. introduce vinylformic acid sodium sulfonate and Hydroxyethyl acrylate in water reducer, both copolyreaction rate had been improved, reduce vinylformic acid autohemagglutination, sulfonic acid group makes water reducer have stronger dispersiveness, reversible adsorption effect can be produced, reach the insensitive effect to earth, improve concrete adaptability, water-reducing rate is high, degree of mobilization and function of slump protection good.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
Embodiment 1
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 280, vinylformic acid sodium sulfonate: 8.94, ammonium persulphate: 2.5,30% hydrogen peroxide: 1.25, deionized water: 286;
Solution A: vinylformic acid (AA): 30, Hydroxyethyl acrylate: 30, dredge base propionic acid: 1.43, deionized water: 190.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Embodiment 2
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 293, vinylformic acid sodium sulfonate: 5.73, ammonium persulphate: 2.69,30% hydrogen peroxide: 1.4, deionized water: 310;
Solution A: vinylformic acid (AA): 34, Hydroxyethyl acrylate: 37.5, dredge base propionic acid: 1.65, deionized water: 215.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Embodiment 3
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 306, vinylformic acid sodium sulfonate: 8.16, ammonium persulphate: 3.0,30% hydrogen peroxide: 1.58, deionized water: 335;
Solution A: vinylformic acid (AA): 37.9, Hydroxyethyl acrylate: 45, dredge base propionic acid: 1.83, deionized water: 240.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Embodiment 4
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 320, vinylformic acid sodium sulfonate: 4.85, ammonium persulphate: 3.33,
30% hydrogen peroxide: 1.8, deionized water: 360;
Solution A: vinylformic acid (AA): 40.65, Hydroxyethyl acrylate: 54, dredge base propionic acid: 1.95, deionized water: 255.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Embodiment 5
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 330, vinylformic acid sodium sulfonate: 10.51, ammonium persulphate: 3.48,30% hydrogen peroxide: 2.0, deionized water: 380;
Solution A: vinylformic acid (AA): 45, Hydroxyethyl acrylate: 59.5, dredge base propionic acid: 2.2, deionized water: 270.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Comparative example 1
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 306, ammonium persulphate: 3.0,30% hydrogen peroxide: 1.58, deionized water: 335;
Solution A: vinylformic acid (AA): 37.9, Hydroxyethyl acrylate: 45, dredge base propionic acid: 1.83, deionized water: 240.
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Comparative example 2
A kind of anti-chamotte mould polycarboxylate water-reducer, is made up of the raw material of following weight part:
Bed material: isopentenol polyoxyethylene ether: 306, ammonium persulphate: 3.0,30% hydrogen peroxide: 1.58, deionized water: 335;
Solution A: vinylformic acid (AA): 37.9, dredge base propionic acid: 1.83, deionized water: 240
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer: when end liquid temp is 65 DEG C, solution A is dripped in end liquid, time for adding is 2 hours, front 1h drips 1/3rd of total mass,, insulation continues reaction 60 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, at 70 DEG C of temperature aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
Application Example
Adopt reference cement, according to the test request in " concrete admixture " (GB8076-2008), compare modified polycarboxylic acid water reducer (embodiment 1-3) prepared by the present invention with comparative example 1, the water-reducing rate of comparative example 2, degree of mobilization, the slump, the results are shown in Table 1.
High cement content concrete proportioning is as follows:
Table 1
As can be seen from the table: in comparative example 1, do not add vinylformic acid sodium sulfonate, in comparative example 2, vinylformic acid sodium sulfonate and Hydroxyethyl acrylate all do not add, water reducer prepared by the present invention that compares, concrete function of slump protection is good, sulfonic introducing, there is well dispersed and retentivity, and in comparative example building-up process, in product, have the vinylformic acid macrobead of autohemagglutination.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not by the restriction of embodiment; other is any do not deviate from spirit of the present invention and principle under make change, modification, combination, substitute, simplify and all should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (5)
1. an anti-chamotte mould polycarboxylate water-reducer, is characterized in that, adopts following raw material to carry out copolyreaction by described weight part:
Isopentenol polyoxyethylene ether 280-330, vinylformic acid sodium sulfonate 5-10, ammonium persulphate 2.5-3.5,30% hydrogen peroxide 1.2-2, vinylformic acid (AA) 30-45, Hydroxyethyl acrylate 30-60, thin base propionic acid 1.4-2.2.
2. the anti-chamotte mould polycarboxylate water-reducer of one according to claim 1, is characterized in that: the molecular weight of described isopentenol polyoxyethylene ether is 2000-2400.
3. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1, is characterized in that, comprise the following steps:
A. get the isopentenol polyoxyethylene ether 280-330 of weight part, vinylformic acid sodium sulfonate 5-10, ammonium persulphate 2.5-3.5,30% hydrogen peroxide 1.2-2 join in the deionized water of 286-380 weight part, be made into end liquid;
B. get vinylformic acid (AA) 30-45, the Hydroxyethyl acrylate 30-60 of weight part, thin base propionic acid 1.4-2.2 joins in the deionized water of 190-270 weight part and mixes, stir, wiring solution-forming A;
C. when end liquid temp is heated to 65 DEG C, in end liquid, drip solution A, time for adding is 2 hours;
E., after being added dropwise to complete, insulation continues reaction 1 hour, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, be warming up to 70 DEG C, be incubated aging 30 minutes, both described anti-chamotte mould polycarboxylate water-reducer.
4. the preparation method of anti-chamotte mould polycarboxylate water-reducer according to claim 3, is characterized in that: when dripping solution A in described step c, within first 1 hour, drips 1/3 of solution A total mass.
5. the preparation method of anti-chamotte mould polycarboxylate water-reducer according to claim 3, is characterized in that: described liquid caustic soda is aqueous sodium hydroxide solution.
Priority Applications (1)
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| CN201410673599.5A CN104356315A (en) | 2014-11-21 | 2014-11-21 | Antisludge polycarboxylate superplasticizer and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861127A (en) * | 2015-04-10 | 2015-08-26 | 广州市建筑科学研究院有限公司 | Preparation method for anti-mud-type polycarboxylic-acid water-reducing agent and application thereof |
| CN105199054A (en) * | 2015-09-17 | 2015-12-30 | 河北三楷深发科技股份有限公司 | Synthetic technology of slump-retaining polycarboxylic type water reducer |
| CN105621930A (en) * | 2015-12-24 | 2016-06-01 | 湖南中岩建材科技有限公司 | Mud-resistant and low-sensitive water reducer |
| CN106977129A (en) * | 2017-04-10 | 2017-07-25 | 河北润砼新材料科技有限公司 | Anti- mud collapse protective poly-carboxylic acid high efficiency water reducing agent and preparation method thereof |
| CN107344988A (en) * | 2017-08-24 | 2017-11-14 | 重庆三圣实业股份有限公司 | A kind of high-adaptability protects the water reducer polycarboxylate water-reducer and preparation method thereof that collapses |
| CN107556439A (en) * | 2017-09-16 | 2018-01-09 | 芜湖市立泰建筑新材料有限公司 | A kind of high-slump-retentionpolycarboxylate polycarboxylate water reducer and preparation method thereof |
| CN107827388A (en) * | 2017-11-15 | 2018-03-23 | 河北合众建材有限公司 | A kind of high-performance compounds polycarboxylate water-reducer |
| CN109467329A (en) * | 2018-09-04 | 2019-03-15 | 江苏兆佳建材科技有限公司 | A kind of corrosion resistance polycarboxylate water-reducer formula |
| CN113955967A (en) * | 2021-12-03 | 2022-01-21 | 山西科腾环保新材料股份有限公司 | Nano tackifying additive and preparation method thereof |
-
2014
- 2014-11-21 CN CN201410673599.5A patent/CN104356315A/en active Pending
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| 逄建军 等: ""保坍型醚类聚羧酸减水剂的合成及应用性能研究"", 《商品混凝土》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861127A (en) * | 2015-04-10 | 2015-08-26 | 广州市建筑科学研究院有限公司 | Preparation method for anti-mud-type polycarboxylic-acid water-reducing agent and application thereof |
| CN104861127B (en) * | 2015-04-10 | 2017-06-27 | 广州市建筑科学研究院有限公司 | A kind of preparation method and applications of anti-chamotte mould polycarboxylate water-reducer |
| CN105199054A (en) * | 2015-09-17 | 2015-12-30 | 河北三楷深发科技股份有限公司 | Synthetic technology of slump-retaining polycarboxylic type water reducer |
| CN105621930A (en) * | 2015-12-24 | 2016-06-01 | 湖南中岩建材科技有限公司 | Mud-resistant and low-sensitive water reducer |
| CN106977129A (en) * | 2017-04-10 | 2017-07-25 | 河北润砼新材料科技有限公司 | Anti- mud collapse protective poly-carboxylic acid high efficiency water reducing agent and preparation method thereof |
| CN107344988A (en) * | 2017-08-24 | 2017-11-14 | 重庆三圣实业股份有限公司 | A kind of high-adaptability protects the water reducer polycarboxylate water-reducer and preparation method thereof that collapses |
| CN107556439A (en) * | 2017-09-16 | 2018-01-09 | 芜湖市立泰建筑新材料有限公司 | A kind of high-slump-retentionpolycarboxylate polycarboxylate water reducer and preparation method thereof |
| CN107827388A (en) * | 2017-11-15 | 2018-03-23 | 河北合众建材有限公司 | A kind of high-performance compounds polycarboxylate water-reducer |
| CN107827388B (en) * | 2017-11-15 | 2020-03-24 | 河北合众建材有限公司 | High-performance compound polycarboxylate superplasticizer |
| CN109467329A (en) * | 2018-09-04 | 2019-03-15 | 江苏兆佳建材科技有限公司 | A kind of corrosion resistance polycarboxylate water-reducer formula |
| CN113955967A (en) * | 2021-12-03 | 2022-01-21 | 山西科腾环保新材料股份有限公司 | Nano tackifying additive and preparation method thereof |
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