CN102718426A - Modified carboxylic acid water-reducing agent and preparation method thereof - Google Patents
Modified carboxylic acid water-reducing agent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a modified carboxylic acid water-reducing agent, which comprises the following raw materials: allyl alcohol polyoxyethylene ether or methyl allyl alcohol polyoxyethylene ether, crylic acid, sodium methylacrylsulfonate, an initiating agent, a chain transfer agent, an antalkali and water. The water-reducing agent has the advantages of environment protection, small slump loss, high water reducing rate, simplicity in preparation and low cost. The invention further discloses a preparation method of the modified carboxylic acid water-reducing agent.
Description
Technical field
The present invention relates to a kind of concrete with admixture and preparation method thereof, relate in particular to a kind of modified carboxylic acid class water reducer and preparation method thereof.
Background technology
Along with developing rapidly of concrete technology; Utilize concrete admixture to improve the attention that concrete performance more and more obtains people; And polycarboxylic acids dehydragent has lot of advantages, such as making when the low-dosage concrete have good flowability, with cement good relatively flexibility is arranged; When low water-cement ratio, have LV and good relatively slump retentivity etc., thereby in the concrete preparation, be widely used in recent years.
External this type water reducer commonly used is main with maleic anhydride series mainly.With Japan is example, and the product compound method is mainly: the first step, under the nitrogen protection condition, methyl alcohol and oxyethane react under certain temperature and pressure, in reaction vessel, add NaOH, elevated temperature decompression dehydration again.Subsequently, in mixture, add a certain amount of chlorallylene, when mixture basicity is reduced to a stationary value, use the HCl neutralise mixt, separate obtaining allyl ethers.Second step: as solvent, under nitrogen protection, the allyl ethers and the maleic anhydride that obtain with the first step reaction carry out polyreaction, steam and remove toluene solvant, obtain maleic anhydride series high performance concrete water reducer with toluene.
The domestic relevant report that polycarboxylic acid series high efficiency water reducing agent is also arranged in recent years.It uses raw material unsaturated carboxylic acid class (vinylformic acid, methylacrylic acid, maleic anhydride), polyoxy alkene (T 46155, polyoxyethylene glycol etc.), unsaturated carboxylate type generally to be arranged, contain the unsaturated monomer of sulfonic acid group etc.; Its synthesis step generally be divided into two the step carry out.Make catalyzer, Resorcinol like the polycarboxylic acid series water reducing agents for efficient aerocrote reported among the CN1316398A at tosic acid and make stopper, BPO and do under the initiator condition and the methylacrylic acid polymerization reaction take place, remove to desolvate after question response is accomplished basically and obtain bleed type high efficiency water reducing agent.The water reducer that this method obtains is only soluble in alkali lye and is insoluble in water, brings very big inconvenience to use.CN1800076A also discloses a kind of acrylic acid series multiple copolymer analog high efficiency water reducing agent; The shared umber of its each raw material is: 100 parts of vinylformic acid or derivatives thereofs, 150～450 parts of polyoxy alkenes, sulfonic acid are 10～80 parts in verivate, 450～800 parts of deionized water solvents, 0.5～6 part of catalyzer, 0.1～5 part of stopper, 5～30 parts of Virahol chain-transfer agents, 0.5～5 part of initiator, and the add-on of NaOH solution is to make the pH value of product reach 6～8.But the method reaction process that this patent provided is difficult to control, and water-reducing rate and slump retention value still are not very desirable yet.
In addition, also all disclose a kind of poly carboxylic acid series water reducer among CN101955333A and the CN102268121A, still wherein said method temperature of reaction is than higher, and reaction process is difficult with control, needs vacuum or nitrogen protection.
Though the raw material commonly used of this type water reducer is limited; Such as commonly used acrylic compounds, unsaturated organic acid such as maleic anhydride, allyl alcohol polyethenoxy ether, initiator such as ammonium persulphate, chain-transfer agent such as Virahol etc. are arranged; But, to form and consumption based on different order of addition(of ingredients), different raw materials, the performance of this type water reducer has very big difference again; And so far, any rule can not sought.
Summary of the invention
Contriver of the present invention finds unexpectedly, through the order of addition(of ingredients) of reasonable control raw material and the amount ratio of raw material, can access environmental protection, slump-loss is little, water-reducing rate is high novel water reducer, and the preparation technology of this water reducer is simple, and is with low cost.Especially, the present invention is surprised to find that, adopts and forms the water reducer that the feedstock production in limited range of the present invention obtains; Use the less conventional raw material of kind in its preparation process; Need not to adopt the condition of pyroreaction, also need not nitrogen protection or vacuumize, just can obtain comparing with water reducer of the prior art; Have and be equal to or the water reducer of more excellent water-reducing property, and reaction yield is than higher.
The present invention at first provides a kind of modified carboxylic acid class water reducer, and its preparation raw material comprises: allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, vinylformic acid, methylpropene sodium sulfonate, initiator, chain-transfer agent, alkaline neutraliser, water.Preferably, said initiator is ammonium persulphate and ydrogen peroxide 50.Preferably, said chain-transfer agent is a thiohydracrylic acid.Preferably, said alkaline neutraliser is a sodium hydroxide.
Preferably; Above-mentioned modified carboxylic acid class water reducer, it is got by the feedstock production of following weight parts: allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7 4000-4500, vinylformic acid 500-550, methylpropene sodium sulfonate 60-80, initiator 45-65, chain-transfer agent (preferred thiohydracrylic acid) 10-15, alkaline neutraliser 100-200, water 4000-6000.Preferably, said initiator is made up of the ammonium persulphate of 30-45 weight part and the ydrogen peroxide 50 of 15-20 weight part.
Above-mentioned modified carboxylic acid class water reducer, preferably, the consumption of said methylpropene sodium sulfonate is 70-80.
Preferably, above-mentioned modified carboxylic acid class water reducer, preferably, said initiator is an ammonium persulphate, more preferably, said alkaline neutraliser is a sodium hydroxide.
Preferably, above-mentioned modified carboxylic acid class water reducer, its preparation method comprises:
(1) preparation of A material, B material and C material
(A) in end water, add big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, ydrogen peroxide 50, mix, make the C material;
(B) vinylformic acid is dissolved in makes B material in the water;
(C) methylpropene sodium sulfonate, ammonium persulphate and thiohydracrylic acid are dissolved in make A material in the water;
(2) polycarboxylate water-reducer is synthetic
In the C material, add A material and B material simultaneously, at 60-70 ℃ of isothermal reaction 2-5 hour, cool to then below 50 ℃, hydro-oxidation sodium is diluted to the pH value and is 7-9, continues reaction 1-2 hour.
Preferably; The preparation of said C material comprises: Jiang Dishui is warmed up to 30-40 ℃, to wherein adding big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, continues to be warmed up to 50-60 ℃ then; Add ydrogen peroxide 50; And then add a certain amount of water, and continue to be warmed up to 75-80 ℃, cool to 60-70 ℃ after 10-40 minute.
Preferably; The preparation of said C material comprises: the end water of 2000-2500 weight part is warmed up to 30-40 ℃, to the big monomer allyl alcohol polyethenoxy ether or the methallyl alcohol Soxylat A 25-7 that wherein add the 4000-4500 weight part, continues to be warmed up to 50-60 ℃ then; The ydrogen peroxide 50 that adds the 15-20 weight part; And then the water of adding 200-300 weight part, continue to be warmed up to 75-80 ℃, cool to 60-70 ℃ after 10-40 minute.
Preferably, the preparation of said A material comprises that thiohydracrylic acid with the ammonium persulphate of the methylpropene sodium sulfonate of 60-80 weight part, 30-45 weight part, 10-15 weight part joins in the deionized water of 1400-1600 weight part and mixes.
Preferably, above-mentioned modified carboxylic acid class water reducer, wherein A material and B expect that the mode of taking to drip at the uniform velocity joins in the bed material, the dropping time of the dropping time ratio B material II of A material is long.
In addition, the present invention also provides a kind of preparation method of modified carboxylic acid class water reducer, comprising:
(1) preparation of A material, B material and C material
(A) big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, ydrogen peroxide 50 are added to the water, mix, make the C material;
(B) vinylformic acid is dissolved in makes B material in the water;
(C) methylpropene sodium sulfonate, ammonium persulphate and thiohydracrylic acid are dissolved in make A material in the water;
(2) polycarboxylate water-reducer is synthetic
In the C material, add A material and B material simultaneously, at 60-70 ℃ of isothermal reaction 2-5 hour, cool to then below 50 ℃, hydro-oxidation sodium is diluted to the pH value and is 7-9, continues reaction 1-2 hour.
Preferably, the mode that A material and B material are taked to drip at the uniform velocity joins in the bed material, and the dropping time of the dropping time ratio B material of A material is long.Preferably, aforesaid method adds at A material and B gob wherein that temperature remains between 55-65 ℃ in the process.
Embodiment
Embodiment 1
(1) preparation of A material, B material and C material
(A) Jiang Dishui is warming up to 35 ℃, adds the big monomer methallyl alcohol Soxylat A 25-7 (molecular weight is 1200-1800) of 4300 grams, is warming up to 55 ℃; Add ydrogen peroxide 50 18 grams, continue to add the deionized water dilution of 250 grams, be warmed up to 76 ℃; Naturally cool to 63 ℃ then, make the C material;
(B) 510 gram vinylformic acid are dissolved in 770 grams and make the B material in the water;
(C) 76 gram methylpropene sodium sulfonates, 38 gram ammonium persulphates and 13 gram thiohydracrylic acids are dissolved in 1550 grams and make the A material in the water;
(2) polycarboxylate water-reducer is synthetic
In the C material, drip A material and B material simultaneously, the A gob adds 3.5 hours, and the B material was submitted 3 hours, and submitting temperature is 63 ℃, and isothermal reaction 3 hours cools to 50 ℃ then, and it is 8 that hydro-oxidation sodium is diluted to the pH value, continues reaction 1-2 hour.
Productive rate is 93% (wherein the calculating of productive rate is that benchmark calculates with big monomeric consumption, and the calculating benchmark in following examples and the Comparative Examples all is to be benchmark calculating with big monomeric consumption too).The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Embodiment 2
Other step is identical with embodiment 1, and difference is that the Thiovanic acid that adds 13g replaces thiohydracrylic acid.Productive rate is 94%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Embodiment 3
Other step is identical with embodiment 1, and difference is to add the big monomer allyl alcohol polyethenoxy ether (molecular weight is 1200-1800) of 4300 grams, rather than the methallyl alcohol Soxylat A 25-7.Productive rate is 90%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Embodiment 4
Other step is identical with embodiment 1, and difference is to replace with the ammonium persulphate of 30 grams the ammonium persulphate of 38 grams.Productive rate is 93%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Embodiment 5
Other step is identical with embodiment 1, and difference is to replace ammonium persulphate with Lucidol.Productive rate is 85%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Comparative Examples 1
Other step is identical with embodiment 1, and difference is 76 gram methylpropene sodium sulfonates are dissolved in the 770 gram water with 510 gram vinylformic acid and forms the B material, rather than forms C with 38 gram ammonium persulphates and 13 gram thiohydracrylic acids and expect.Productive rate is 90%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Comparative Examples 2
Other step is identical with embodiment 1, and difference is to replace with 300g vinylformic acid and 210g methylene-succinic acid the vinylformic acid of 510g among the embodiment 1.Productive rate is 90%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Comparative Examples 3
Other step is identical with embodiment 1, and difference is to be dissolved in the 770 gram water with 510 gram vinylformic acid among the 510 gram methacrylic acid substitution embodiment 1 and makes the B material.Productive rate is 70%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Comparative Examples 4
Other step is identical with embodiment 1, and difference is that said acrylic acid consumption is 200 grams, rather than 510 grams.Productive rate is 70%.The slump retention value and the water-reducing rate value of products obtained therefrom are seen table 1.
Table 1:
Performance after adding to water reducer of the present invention and the said water reducer of Comparative Examples in the Lafarge cement respectively relatively
Explain: " * " representative reaction is carried out smoothly
On behalf of reaction process, "-" be difficult to control
The testing method of the slump wherein: with a 100mm suitable for reading, end opening 200mm, the trumpet-shaped slump bucket of high 300mm; Tamping behind the penetration concrete; Pull up bucket then, concrete produces the slump phenomenon because of deadweight, deducts 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.
Claims (10)
1. modified carboxylic acid class water reducer, its preparation raw material comprises: allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, vinylformic acid, methylpropene sodium sulfonate, initiator, chain-transfer agent, alkaline neutraliser, water.
2. the described modified carboxylic acid class of claim 1 water reducer, it is got by the feedstock production of following weight parts: it is got by the feedstock production of following weight parts: allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7 4000-4500, vinylformic acid 500-550, methylpropene sodium sulfonate 60-80, thiohydracrylic acid 10-15, initiator 45-65, alkaline neutraliser 100-200, water 4000-6000.
3. the described modified carboxylic acid class of claim 1 water reducer, wherein said initiator is made up of the ammonium persulphate of 30-45 weight part and the ydrogen peroxide 50 of 15-20 weight part.
4. the described modified carboxylic acid class of claim 1 water reducer, wherein said initiator is made up of ammonium persulphate and ydrogen peroxide 50, and preferably, said alkaline neutraliser is a sodium hydroxide, and said chain-transfer agent is a thiohydracrylic acid.
5. each described polyester based carboxylic-acid water reducer of claim 1～4, the preparation method of wherein said water reducer comprises:
(1) preparation of A material, B material and C material
(A) in end water, add big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, ydrogen peroxide 50, mix, make the C material;
(B) vinylformic acid is dissolved in makes B material in the water;
(C) methylpropene sodium sulfonate, ammonium persulphate and thiohydracrylic acid are dissolved in make A material in the water;
(2) polycarboxylate water-reducer is synthetic
In the C material, add A material and B material simultaneously, at 60-70 ℃ of isothermal reaction 2-5 hour, cool to then below 50 ℃, hydro-oxidation sodium is diluted to the pH value and is 7-9, continues reaction 1-2 hour.
6. the preparation method of a modified carboxylic acid class water reducer comprises:
(1) preparation of A material, B material and C material
(A) in end water, add big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, ydrogen peroxide 50, mix, make the C material;
(B) vinylformic acid is dissolved in makes B material in the water;
(C) methylpropene sodium sulfonate, ammonium persulphate and thiohydracrylic acid are dissolved in make A material in the water;
(2) polycarboxylate water-reducer is synthetic
In the C material, add A material and B material simultaneously, at 60-70 ℃ of isothermal reaction 2-5 hour, cool to then below 50 ℃, hydro-oxidation sodium is diluted to the pH value and is 7-9, continues reaction 1-2 hour.
7. the described method of claim 6; The preparation of wherein said C material comprises: Jiang Dishui is warmed up to 30-40 ℃, to wherein adding big monomer allyl alcohol polyethenoxy ether or methallyl alcohol Soxylat A 25-7, continues to be warmed up to 50-60 ℃ then; Add ydrogen peroxide 50; And then add a certain amount of water, and continue to be warmed up to 75-80 ℃, cool to 60-70 ℃ after 10-40 minute.
8. the described method of claim 6; The preparation of wherein said C material comprises: the end water of 2000-2500 weight part is warmed up to 30-40 ℃, to the big monomer allyl alcohol polyethenoxy ether or the methallyl alcohol Soxylat A 25-7 that wherein add the 4000-4500 weight part, continues to be warmed up to 50-60 ℃ then; The ydrogen peroxide 50 that adds the 15-20 weight part; And then the water of adding 200-300 weight part, continue to be warmed up to 75-80 ℃, cool to 60-70 ℃ after 10-40 minute.
9. each described method of claim 6-8, the preparation of wherein said A material comprise that the thiohydracrylic acid with the ammonium persulphate of the methylpropene sodium sulfonate of 60-80 weight part, 30-45 weight part, 10-15 weight part joins in the deionized water of 1400-1600 weight part and mix.
10. each described method of claim 6-9, wherein A material and the B material mode taking to drip at the uniform velocity joins in the bed material, and the dropping time ratio B of A material expects that the dropping time of II is long.Preferably, aforesaid method adds at A material and B gob wherein that temperature remains between 55-65 ℃ in the process.
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| CN103864330A (en) * | 2014-03-13 | 2014-06-18 | 大连市铭源全科技开发有限公司 | Polycarboxylate superplasticizer and synthetic method of polycarboxylate superplasticizer in alkaline environment |
| CN105601843A (en) * | 2016-03-29 | 2016-05-25 | 山东卓星化工有限公司 | Early-strength ethers polycarboxylic acid water reducing agent and preparation method thereof |
| CN107446091A (en) * | 2017-09-16 | 2017-12-08 | 芜湖市立泰建筑新材料有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof |
| CN108659179A (en) * | 2018-06-15 | 2018-10-16 | 山西中铁铁诚建材科技有限公司 | A kind of polycarboxylate water-reducer and its synthetic method |
| CN108976358A (en) * | 2018-08-13 | 2018-12-11 | 山西宝路加交通科技有限公司 | A kind of polycarboxylate water-reducer synthesis technology |
| CN109437644A (en) * | 2018-12-03 | 2019-03-08 | 苏州市兴邦化学建材有限公司 | A kind of synthetic method improving polycarboxylate water-reducer cement adaptability |
| CN112794959A (en) * | 2021-01-29 | 2021-05-14 | 武汉理工大学 | Polymer for stabilizing pumped concrete and preparation method thereof |
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| CN109437644A (en) * | 2018-12-03 | 2019-03-08 | 苏州市兴邦化学建材有限公司 | A kind of synthetic method improving polycarboxylate water-reducer cement adaptability |
| CN112794959A (en) * | 2021-01-29 | 2021-05-14 | 武汉理工大学 | Polymer for stabilizing pumped concrete and preparation method thereof |
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