CN103819622A - Polycarboxylate superplasticizer masterbatch capable of prolonging coagulating time of concrete and preparation method thereof - Google Patents
Polycarboxylate superplasticizer masterbatch capable of prolonging coagulating time of concrete and preparation method thereof Download PDFInfo
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- CN103819622A CN103819622A CN201410024129.6A CN201410024129A CN103819622A CN 103819622 A CN103819622 A CN 103819622A CN 201410024129 A CN201410024129 A CN 201410024129A CN 103819622 A CN103819622 A CN 103819622A
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Abstract
The invention relates to a water-reducing agent for concrete and a preparation method thereof, in particular to a polycarboxylate superplasticizer masterbatch capable of prolonging the coagulating time of concrete and a preparation method thereof. The polycarboxylate superplasticizer masterbatch capable of prolonging the coagulating time of concrete is formed by polymerizing isoamyl alcohol polyoxyethylene ether, maleic anhydride, 2-acrylamide-2-methyl sodium propanesulfonate, acrylic acid, methyl methacrylate, an initiator, a chain transfer agent and water. The prepared polycarboxylate superplasticizer masterbatch adopts a comb-type structure of the conventional polycarboxylate superplasticizer, an isoamyl alcohol polyoxyethylene ether macromonomer is used as a side chain, a calcium ion chelating structure which is copolymerized from acrylic acid, maleic anhydride, methyl methacrylate and 2-acrylamide-2-methyl sodium propanesulfonate is used as a main chain, the polycarboxylate superplasticizer masterbatch has water-reducing and coagulation-slowing effects, can obviously prolong the coagulating time of polycarboxylic acid concrete, and is applicable to preparation of a pumping agent for concrete in summer.
Description
Technical field
The present invention relates to the reinforcement of concrete water reducer and preparation method, specifically, relate to a kind of polycarboxylate water-reducer masterbatch that can extend concrete coagulating time and preparation method thereof.
Background technology
Polycarboxylate water-reducer starts to occur from eighties of last century in China the nineties, and experienced up till now the development of more than 20 year, its performance is constantly improved, and Application Areas is constantly expanded, and becomes from laboratory product originally the main flow water reducer kind that occupies 50% above market.
The kind of polycarboxylate water-reducer: divide by use properties, have water reducing type, standard type, collapse protection type, early-strength type etc.; Keyed jointing mode according to polyoxyethylene and main chain is different, can be divided into again ester class, ethers and amine.Polycarboxylate water-reducer is comb-type structure, its side chain is polyoxyethylene structure, the raw material that this structure can be provided is the large monomer of double bond containing polyoxyethylene, as: (methyl) acrylic acid polyoxyethylene monomethyl ether ester, (methyl) allyl polyethenoxy ether, isopentene group Soxylat A 25-7 etc.; Its main chain is containing carboxyl, double bond containing material, as: (methyl) acrylic acid, MALEIC ANHYDRIDE, fumaric acid, furoate clothing etc.
Mainly there are four kinds of theories in the understanding that is delayed coagulation mechanism to prolongation concrete coagulating time at present:
1, adsorption theory.Having surface-active retardant can be adsorbed in the solid-liquid interface of cement granules, form interfacial layer, thereby change the hydrophilic/lipophilic of cement particle surface, stop water molecules to enter cement particle surface, suppress hydrated cementitious, thereby cause the prolongation of concrete coagulating time.
2, complex compound generative theory.The Ca that retardant molecule can generate with hydrated cementitious
2+form complex compound, controlled liquid phase at the hydrated cementitious initial stage in Ca
2+ionic concn, hinders the formation of hydrated product Aft, suppresses the crystalline growth of hydrated product CH, has delayed C
3s and C
3the aquation of A, produces delayed coagulation.
3, sedimentation theory.Organic or inorganic retardant is by forming the insoluble thin layer of one deck at cement particle surface, and prevention cement granules contacts with water, thereby delays the aquation of cement, plays delayed coagulation.
4, Ca(OH)
2crystallization theory.Retardant is by being adsorbed on Ca(OH)
2nucleus on, suppress Ca(OH)
2crystallization continued growth and produce delayed coagulation.
Under normal circumstances, depend on the side chain length of polycarboxylate water-reducer the time of coagulation of polycarboxylate water-reducer, ester class polycarboxylate water-reducer side chain is shorter, and the polymerization degree is in 25 left and right, and time of coagulation is slightly long, generally at 8～12 hours; Ethers poly carboxylic acid side chain is longer, and the polymerization degree is in 50 left and right, and time of coagulation is shorter, generally at 6～8 hours; Because all amines have early strength function, so amine polycarboxylate water-reducer is shorter time of coagulation.In summer along with the rising of temperature declines rapidly time of coagulation, sometimes be subject to construction infection, can cause concrete waste, at this moment just need to regulate time of coagulation, conventionally way is to add a large amount of gluconic acid sodium salt (polycarboxylate water-reducer feature: when high temperature, a small amount of interpolation changes not obvious time of coagulation), and the composite cost of pumping agent rises larger.
Summary of the invention
The object of the invention is to, a kind of polycarboxylate water-reducer masterbatch that can extend concrete coagulating time and preparation method thereof is provided, to solve above-mentioned technical problem.
The present invention is achieved through the following technical solutions:
A kind of polycarboxylate water-reducer masterbatch that can extend concrete coagulating time, it is characterized in that: this polycarboxylate water-reducer masterbatch that can extend concrete coagulating time is polymerized by prenol Soxylat A 25-7, MALEIC ANHYDRIDE, 2-acrylamide-2-methyl propane sulfonic sodium, vinylformic acid, methyl methacrylate, initiator, chain-transfer agent, water, and its repeating unit and molecular formula can be represented by following general formula:
Wherein: m=25～30, n=2～4, k=5～8, p=8～10, q=4～5, h=50～60.
The preparation method of the described polycarboxylate water-reducer masterbatch that can extend concrete coagulating time, comprises the steps:
1, get the raw materials ready: 300 parts of prenol Soxylat A 25-7s, 10 parts of MALEIC ANHYDRIDE, 8.5 parts, 2-acrylamide-2-methyl propane sulfonic sodium, 34 parts, vinylformic acid, 6.8 parts of methyl methacrylates, 4～6 parts of initiators, 5 parts of chain-transfer agents, 550 parts, water;
2, batching:
2A, in conversion unit, add prenol Soxylat A 25-7, MALEIC ANHYDRIDE and 400 parts of water, open and stir, it is fully dissolved, and be warming up to 65 ℃-85 ℃, stand-by;
2B, in a dropping equipment, add initiator, 2-acrylamide-2-methyl propane sulfonic sodium and 150 parts of water, be uniformly mixed, it is fully dissolved, stand-by;
2C, in No. two dropping equipment, add chain-transfer agent, vinylformic acid and methyl methacrylate, be uniformly mixed, it is fully dissolved, stand-by;
3, drip polymerization: the solution in the solution in a dropping equipment and No. two dropping equipment is at the uniform velocity added drop-wise in conversion unit simultaneously, time for adding is 4.5 hours, guarantee that, after 4.5 hours, the material in the material in a dropping equipment and No. two dropping equipment is all added drop-wise in conversion unit; In dropping process, temperature maintains 65 ℃-85 ℃;
4, insulation slaking: after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
5, be cooled to 45 ℃, discharging.
say further:
Described initiator is ammonium persulphate, Sodium Persulfate or Potassium Persulphate.
Described chain-transfer agent is Virahol.
beneficial effect:the polycarboxylate water-reducer masterbatch that adopts the present invention to prepare, there is the comb-type structure of traditional polycarboxylate water-reducer, its side chain is the large monomer of prenol Soxylat A 25-7, the polymerization degree is more than 50, effective guarantee water-reducing property and the function of slump protection of this masterbatch, main chain is vinylformic acid, cis-butenedioic anhydride, methyl methacrylate, the quarternary copolymerized calcium ion chelate structure of 2-acrylamide-2-methyl propane sulfonic sodium, energy and calcium ion, aluminum ion, zine ion form complex compound, stop the generation of calcium carbonate, and then affect hydrated cementitious process, extend concrete coagulating time.Therefore, the polycarboxylate water-reducer masterbatch that can extend concrete coagulating time of the present invention has diminishing and delayed coagulation simultaneously, can significantly extend the time of coagulation of polycarboxylic acid concrete, suitable configuration pumping agent for concrete in summer.
embodiment
Below with reference to specific embodiment, the present invention is described further.
embodiment 1
1, in the there-necked flask that is 1000ml at capacity, add 300g prenol Soxylat A 25-7,10g MALEIC ANHYDRIDE, 400g water, open and stir, it is fully dissolved, and be warming up to 65 ℃, stand-by;
A expects configuration: in a 250ml beaker, adds 4g ammonium persulphate, 8.5g2-acrylamide-2-methyl propane sulfonic sodium and 150g water, is uniformly mixed, it is fully dissolved, and stand-by;
B expects configuration: in a 50ml beaker, adds 34g vinylformic acid, 5g Virahol, 6.8g methyl methacrylate, is uniformly mixed, it is fully dissolved, and stand-by;
2, in there-necked flask, drip A material and B material simultaneously, within 4.5 hours, drip off, in dropping process, holding temperature is constant;
3, after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
4, be cooled to 45 ℃, discharging.
embodiment 2
1, in the there-necked flask that is 1000ml at capacity, add 300g prenol Soxylat A 25-7,10g MALEIC ANHYDRIDE, 400g water, open and stir, it is fully dissolved, and be warming up to 75 ℃, stand-by;
A expects configuration: in a 250ml beaker, adds 5g Sodium Persulfate, 8.5g2-acrylamide-2-methyl propane sulfonic sodium and 150g water, is uniformly mixed, it is fully dissolved, and stand-by;
B expects configuration: in a 50ml beaker, adds 34g vinylformic acid, 5g Virahol, 6.8g methyl methacrylate, is uniformly mixed, it is fully dissolved, and stand-by;
2, in there-necked flask, drip A material and B material simultaneously, within 4.5 hours, drip off, in dropping process, holding temperature is constant;
3, after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
4, be cooled to 45 ℃, discharging.
embodiment 3
1, in the there-necked flask that is 1000ml at capacity, add 300g prenol Soxylat A 25-7,10g MALEIC ANHYDRIDE, 400g water, open and stir, it is fully dissolved, and be warming up to 85 ℃, stand-by;
A expects configuration: in a 250ml beaker, adds 6g Potassium Persulphate, 8.5g2-acrylamide-2-methyl propane sulfonic sodium and 150g water, is uniformly mixed, it is fully dissolved, and stand-by;
B expects configuration: in a 50ml beaker, adds 34g vinylformic acid, 5g Virahol, 6.8g methyl methacrylate, is uniformly mixed, it is fully dissolved, and stand-by;
2, in there-necked flask, drip A material and B material simultaneously, within 4.5 hours, drip off, in dropping process, holding temperature is constant;
3, after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
4, be cooled to 45 ℃, discharging.
comparative example
1, in the there-necked flask that is 1000ml at capacity, add isopentene group Soxylat A 25-7 (molecular weight 2400) and water 310g, open and stir, dissolve, be warming up to 60～65 ℃;
A expects configuration: in a 250ml beaker, add 2.8g ammonium persulphate and 170g water, stirring and dissolving;
B expects configuration: in another 250ml beaker, add 2.4g thiohydracrylic acid, 40g vinylformic acid and 170g water, stirring and dissolving;
2, in there-necked flask, drip A material and B material simultaneously, within 3 hours, drip off, in dropping process, holding temperature is constant;
3, after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
4, be cooled to 45 ℃, discharging.
[concrete coagulating time experiment]
Experimental technique: it is 10% solution that the product of embodiment 1～3 product and comparative example configuration is become respectively to concentration, and volume is by 2% of gelling material, and proportioning press GB8076-2008 and detected proportioning, does concrete coagulating time test according to GB8076-2008 method.
Cement: standard cement
Sand, stone: meet GB8076-2008 requirement.
The slump: 200mm.
Envrionment temperature: 25 ℃.
| Water reducer | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Time of coagulation/h | 16.5 | 17.0 | 16 | 8.5 |
Claims (4)
1. one kind can extend the polycarboxylate water-reducer masterbatch of concrete coagulating time, it is characterized in that: this polycarboxylate water-reducer masterbatch that can extend concrete coagulating time is polymerized by prenol Soxylat A 25-7, MALEIC ANHYDRIDE, 2-acrylamide-2-methyl propane sulfonic sodium, vinylformic acid, methyl methacrylate, initiator, chain-transfer agent, water, and its repeating unit and molecular formula can be represented by following general formula:
Wherein: m=25～30, n=2～4, k=5～8, p=8～10, q=4～5, h=50～60.
2. the preparation method that can extend as claimed in claim 1 the polycarboxylate water-reducer masterbatch of concrete coagulating time, is characterized in that: comprise the steps:
(1) get the raw materials ready: 300 parts of prenol Soxylat A 25-7s, 10 parts of MALEIC ANHYDRIDE, 8.5 parts, 2-acrylamide-2-methyl propane sulfonic sodium, 34 parts, vinylformic acid, 6.8 parts of methyl methacrylates, 4～6 parts of initiators, 5 parts of chain-transfer agents, 550 parts, water;
(2) batching:
(2A) in conversion unit, add prenol Soxylat A 25-7, MALEIC ANHYDRIDE and 400 parts of water, open and stir, it is fully dissolved, and be warming up to 65 ℃-85 ℃, stand-by;
(2B) in a dropping equipment, add initiator, 2-acrylamide-2-methyl propane sulfonic sodium and 150 parts of water, be uniformly mixed, it is fully dissolved, stand-by;
(2C) in No. two dropping equipment, add chain-transfer agent, vinylformic acid and methyl methacrylate, be uniformly mixed, it is fully dissolved, stand-by;
(3) drip polymerization: the solution in the solution in a dropping equipment and No. two dropping equipment is at the uniform velocity added drop-wise in conversion unit simultaneously, time for adding is 4.5 hours, guarantee that, after 4.5 hours, the material in the material in a dropping equipment and No. two dropping equipment is all added drop-wise in conversion unit; In dropping process, temperature maintains 65 ℃-85 ℃;
(4) insulation slaking: after being added dropwise to complete, holding temperature is constant, insulation slaking 1 hour;
(5) be cooled to 45 ℃, discharging.
3. the preparation method that can extend according to claim 2 the polycarboxylate water-reducer masterbatch of concrete coagulating time, is characterized in that: described initiator is ammonium persulphate, Sodium Persulfate or Potassium Persulphate.
4. the preparation method that can extend according to claim 2 the polycarboxylate water-reducer masterbatch of concrete coagulating time, is characterized in that: described chain-transfer agent is Virahol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104446093A (en) * | 2014-12-04 | 2015-03-25 | 河北铁园科技发展有限公司 | Polycarboxylate-based water reducing agent with integrated functions of water reduction and slump retaining |
| CN109053967A (en) * | 2018-05-25 | 2018-12-21 | 湖北工业大学 | A kind of stepwise hydrolysis release type polycarboxylic acid slump retaining agent and preparation method |
| CN114085333A (en) * | 2021-10-29 | 2022-02-25 | 张家港市德宝化工有限公司 | Alkali-resistant phosphorus-free chelating agent for pretreatment of cotton knitted fabric and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446093A (en) * | 2014-12-04 | 2015-03-25 | 河北铁园科技发展有限公司 | Polycarboxylate-based water reducing agent with integrated functions of water reduction and slump retaining |
| CN109053967A (en) * | 2018-05-25 | 2018-12-21 | 湖北工业大学 | A kind of stepwise hydrolysis release type polycarboxylic acid slump retaining agent and preparation method |
| CN114085333A (en) * | 2021-10-29 | 2022-02-25 | 张家港市德宝化工有限公司 | Alkali-resistant phosphorus-free chelating agent for pretreatment of cotton knitted fabric and preparation method thereof |
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