CN109912752A - A kind of water-reducing agent and preparation method thereof - Google Patents

A kind of water-reducing agent and preparation method thereof Download PDF

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CN109912752A
CN109912752A CN201711326210.XA CN201711326210A CN109912752A CN 109912752 A CN109912752 A CN 109912752A CN 201711326210 A CN201711326210 A CN 201711326210A CN 109912752 A CN109912752 A CN 109912752A
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water
reducing agent
unsaturated
polyoxyethylene ether
preparation
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孙肖武
关世发
恵蔷
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SHANXI HUANGTENG CHEMICAL CO Ltd
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SHANXI HUANGTENG CHEMICAL CO Ltd
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Abstract

The present invention relates to concrete admixture field, in particular to a kind of water-reducing agent and preparation method thereof.The water-reducing agent is formed by polymerization of unsaturated monomers, and the unsaturated monomer includes: 81~95wt% of polyoxyethylene ether containing unsaturated bond;1~6wt% of unsaturated sulfonic acid salt;4~13wt% of unsaturated carboxylic acid or derivatives thereof;The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.Water-reducing agent of the invention introduces unsaturated sulfonic acid base, plays and is impregnated with wetting action, also improves dispersion effect;Not only water reducing and strength increasing effect is significant, and after being added in concrete, concrete flowability also obtains higher holding.Preparation method of the invention simultaneously is simple, and no three industrial wastes generate, and environment-friendly type is good;Production cost is low, and economic benefit is prominent.

Description

A kind of water-reducing agent and preparation method thereof
Technical field
The present invention relates to concrete admixture field, in particular to a kind of water-reducing agent and preparation method thereof.
Background technique
Water-reducing agent is a kind of under conditions of maintaining concrete slump to be basically unchanged, and can be reduced the coagulation of mixing water amount Native additive.Belong to anionic surfactant mostly, there is lignosulfonates, naphthalene sulphonate formaldehyde polymer etc..It is added mixed There is peptizaiton to cement granules after solidifying soil mixture, its workability can be improved, reduce unit consumption of water, improve concrete mixing The mobility of object, or unit cement consumption is reduced, save cement.
It is higher to concrete quality performance requirement with the rapid growth of national basis Facilities Construction.Therefore, to additional Agent, especially water-reducing agent are put forward higher requirements.Polycarboxylate water-reducer is third generation high-performance water reducing agent, has volume low, subtracts The features such as water rate is big, little loss of slump, good with cement adaptability.The application of polycarboxylic acids series water-reducing agent, can be significantly The dosage of cement is saved, industry of exchanging work waste residue and pulverized fuel ash, miberal powder etc. are treasured, largely to reduce the hydration heat of concrete, Especially suitable for the large volumes such as high-speed railway, bridge, harbour, high intensity, high-durability concrete works.
But the kind that polycarboxylic acids subtracts serial aqua is also relatively simple, it is main to use unsaturated polyoxyethylene ether monomer in oxygen Change copolymerization in reduction system to be made.The multifunction research of water-reducing agent properties of product is really realized from polymer molecular structure also In the starting stage, mature product is seldom.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of water-reducing agent and preparation method thereof, the water-reducing agent water reducing and strength increasing And function of slump protection is significant, stability is good, after concrete is added, concrete flowability is made to obtain good holding.
The invention discloses a kind of water-reducing agents, are formed by polymerization of unsaturated monomers, and the unsaturated monomer includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
Preferably, the polyoxyethylene ether containing unsaturated bond is allyl polyethenoxy ether, methacrylic polyoxy second One or more of alkene ether and isoamyl alcohol polyoxyethylene ether.
Preferably, the unsaturated sulfonic acid salt is methylpropene sodium sulfonate or Sodium Allyl Sulfonate.
Preferably, the unsaturated carboxylic acid is acrylic acid, methacrylic acid, styrene sulfonic acid and 2- Methacrylamide- One or both of 3- propene sulfonic acid.
The invention discloses the preparation methods of the water-reducing agent described in above-mentioned technical proposal, comprising the following steps:
Unsaturated monomer carries out polymerization reaction in the redox system added with chain-transferring agent, obtains water-reducing agent;
The unsaturated monomer includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
Preferably, the preparation method specifically:
Polyoxyethylene ether, unsaturated sulfonic acid salt, oxidant and water containing unsaturated bond are mixed, mixed liquor is obtained;It is described The additive amount of oxidant is the 0.1~5% of the unsaturated monomer gross mass;
Unsaturated carboxylic acid monomer or derivatives thereof is soluble in water, obtain combination liquid A;
Reducing agent, chain-transferring agent and water are mixed, combination liquid B is obtained;The additive amount of the reducing agent is unsaturated monomer The 0.1~6% of gross mass;The additive amount of the chain-transferring agent is the 0.1~5% of unsaturated monomer gross mass;
Combination liquid A and combination liquid B are added drop-wise in mixed liquor, polymerization reaction is carried out, obtains water-reducing agent.
Preferably, it after the polymerization reaction, adds alkali or aqueous slkali carries out neutralization reaction, the alkali is sodium hydroxide, hydrogen Potassium oxide or triethanolamine;The temperature when neutralization reaction is 50 DEG C or less.
Preferably, after the neutralization reaction, the water-reducing agent that solid content is 30~70% is obtained.
Preferably, the time that the combination liquid A and combination liquid B are added dropwise is 1~4 hour, and the polymerization time is 1~3 small When, the temperature of the polymerization reaction is 30~60 DEG C.
Preferably, the hydrogen peroxide that the oxidant is ammonium persulfate or mass concentration is 30%, the reducing agent are anti-bad Hematic acid or sodium hypophosphite;The chain-transferring agent is one or more of mercaptopropionic acid, thioacetic acid and mercaptoethanol.
Compared with prior art, water-reducing agent of the invention introduces unsaturated sulfonic acid base, plays and is impregnated with wetting action, Dispersion effect is improved, by adjusting relative scale, main polymer chain and the graft side chain of functional group each on main polymer chain Length with graft side chain number, can be water-reducing agent molecular structure rationalization, better adaptability.Therefore, of the present invention Water-reducing agent not only water reducing and strength increasing effect is significant, after being added in concrete, concrete flowability also obtains higher holding.Together When preparation method of the invention it is simple, no three industrial wastes generate, and environment-friendly type is good;Production cost is low, and economic benefit is prominent.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention Limitation.
Embodiment of the invention discloses a kind of water-reducing agents, are formed by polymerization of unsaturated monomers, the unsaturated monomer packet It includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
In the present invention, the water-reducing agent is polymerize under the effect of oxidant, reducing agent and chain-transferring agent by unsaturated monomer It forms.By MOLECULE DESIGN, introducing is a certain amount of containing the sulfonic unsaturated monomer of functional group, plays and is impregnated with wetting work With, also improve dispersion effect, by adjusting the relative scale of main polymer chain Shang Ge functional group, main polymer chain and grafting side The length of chain and graft side chain number, rationalize its molecular structure, better adaptability.
In the present invention, the polyoxyethylene ether containing unsaturated bond is preferably allyl polyethenoxy ether, methallyl One or more of base polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether, the polyoxyethylene ether molecule containing unsaturated bond Amount is 1500~3500, preferably 2000~3000.The content of the polyoxyethylene ether molecular weight containing unsaturated bond accounts for insatiable hunger With 81~95wt% of monomer gross mass, preferably 85~90%.
The unsaturated sulfonic acid salt is preferably methylpropene sodium sulfonate or Sodium Allyl Sulfonate.The unsaturated sulfonic acid salt Content accounts for 1~6wt% of unsaturated monomer gross mass, preferably 1.5~3wt%.
The unsaturated carboxylic acid is preferably acrylic acid, methacrylic acid, styrene sulfonic acid, 2- Methacrylamide -3- third The one or two of alkene sulfonic acid.The content of the unsaturated carboxylic acid monomer or derivatives thereof account for unsaturated monomer gross mass 4~ 13wt%, preferably 5~20wt%.
In the present invention, the unsaturated monomer is completed freely in redox system under the action of chain-transferring agent Base polymerization reaction generates polymer.By adjusting the additive amount of different types of unsaturated monomer, adjustable main polymer chain The number of the relative scale of Shang Ge functional group, the length of main polymer chain and graft side chain and graft side chain, to ensure that The performance of water-reducing agent.
The embodiment of the invention also discloses the preparation methods of water-reducing agent, comprising the following steps:
Unsaturated monomer carries out polymerization reaction in the redox system added with chain-transferring agent, obtains water-reducing agent;
The unsaturated monomer includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
Preferably, the redox system is preferably hydrogen peroxide-ascorbic acid system, hydrogen peroxide-sodium hypophosphite system Or ammonium persulfate-ascorbic acid system.
The chain-transferring agent is preferably one or more of mercaptopropionic acid, thioacetic acid and mercaptoethanol.
As preferred embodiment, the preparation method specifically:
Polyoxyethylene ether, unsaturated sulfonic acid salt, oxidant and water containing unsaturated bond are mixed, mixed liquor is obtained;It is described The additive amount of oxidant is the 0.1~5% of the unsaturated monomer gross mass;
Unsaturated carboxylic acid monomer or derivatives thereof is soluble in water, obtain combination liquid A;
Reducing agent, chain-transferring agent and water are mixed, combination liquid B is obtained;The additive amount of the reducing agent is unsaturated monomer The 0.1~6% of gross mass;The additive amount of the chain-transferring agent is the 0.1~5% of unsaturated monomer gross mass;
Combination liquid A and combination liquid B are added drop-wise in mixed liquor, polymerization reaction is carried out, obtains water-reducing agent.
In the preferred embodiment, firstly, by the polyoxyethylene ether containing unsaturated bond, unsaturated sulfonic acid salt, oxidation Agent and water mixing, obtain mixed liquor;The additive amount of the oxidant is the 0.1~5% of the unsaturated monomer gross mass.
The hydrogen peroxide that the oxidant is preferably ammonium persulfate or mass concentration is 30%.
Then, preparation combination liquid A and combination liquid B.Unsaturated carboxylic acid monomer and its derivative is soluble in water, it is combined Liquid A;
Reducing agent, chain-transferring agent and water are mixed, combination liquid B is obtained;The additive amount of the reducing agent is unsaturated monomer The 0.1~6% of gross mass, the reducing agent are preferably ascorbic acid or sodium hypophosphite;The additive amount of the chain-transferring agent is not It is saturated the 0.1~5% of monomer gross mass.
Finally, combination liquid A and combination liquid B are added drop-wise in mixed liquor, polymerization reaction is carried out, water-reducing agent is obtained.Described group The time closed liquid A and combine liquid B dropwise addition is preferably 1~4 hour, and the polymerization time is preferably 1~3 hour, and the polymerization is anti- The temperature answered is preferably 30~60 DEG C.
Preferably, it after the polymerization reaction, adds alkali or aqueous slkali carries out neutralization reaction;After the neutralization reaction, Obtain the water-reducing agent that solid content is 30~70%.The alkali is preferably sodium hydroxide, potassium hydroxide or triethanolamine;The neutralization Temperature when reaction is preferably 50 DEG C or less.By the neutralization reaction, pH value is adjusted to 3~7.
For a further understanding of the present invention, below with reference to embodiment to water-reducing agent provided by the invention and preparation method thereof into Row is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 55.8g molecular weight is added After 1500 methyl allyl polyoxyethylene ether and the methyl allyl polyoxyethylene ether of 300g molecular weight 2400 start stirring, then Methylpropene sodium sulfonate 5.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 4.2g mass concentration is 30% is added, obtains To mixed liquor.
34.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.7g ascorbic acid, 1.1g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 2.5h.Reactant It is that temperature is maintained at 43 DEG C~47 DEG C, continues to stir 1h later, the sodium hydroxide of 19.7g30%, adjustment system pH to 5 is added ± 2, the Mobyneb polycarboxylate water-reducer PCEs-1 that solid content is 40% is made.
Embodiment 2
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 55.8g molecular weight is added After 1800 methyl allyl polyoxyethylene ether and the methyl allyl polyoxyethylene ether of 300g molecular weight 2400 start stirring, then Methylpropene sodium sulfonate 6.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains To mixed liquor.
32.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.6g ascorbic acid, 1.0g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 2.5h.Reactant It is that temperature is maintained at 43 DEG C~47 DEG C, continues to stir 1h later, the sodium hydroxide of 19.7g30%, adjustment system pH to 5 is added ± 2, the Mobyneb polycarboxylate water-reducer PCEs-2 that solid content is 40% is made.
Embodiment 3
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 55.8g molecular weight is added After 1600 methyl allyl polyoxyethylene ether and the methyl allyl polyoxyethylene ether of 300g molecular weight 2400 start stirring, then Methylpropene sodium sulfonate 7.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains To mixed liquor.
30.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.7g ascorbic acid, 1.1g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 2h.Reaction system Temperature is maintained at 43 DEG C~47 DEG C, continues to stir 1h later, is added the sodium hydroxide of 19.7g30%, and adjustment system pH to 5 ± 2, the Mobyneb polycarboxylate water-reducer PCEs-3 that solid content is 40% is made.
Embodiment 4
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 55.8g molecular weight is added After 2400 methyl allyl polyoxyethylene ether and the methyl allyl polyoxyethylene ether of 300g molecular weight 3000 start stirring, then Methylpropene sodium sulfonate 8.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains To mixed liquor.
32.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.7g ascorbic acid, 1.1g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 3h.Reaction system Temperature is maintained at 43 DEG C~47 DEG C, continues to stir 2h later, is added the sodium hydroxide of 19.7g30%, and adjustment system pH to 5 ± 2, the Mobyneb polycarboxylate water-reducer PCEs-4 that solid content is 40% is made.
Embodiment 5
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 355.8g molecular weight is added After 2400 methyl allyl polyoxyethylene ether starts stirring, methylpropene sodium sulfonate 5.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains mixed liquor.
34.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.7g ascorbic acid, 1.1g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 3h.Reaction system Temperature is maintained at 43 DEG C~47 DEG C, continues to stir 2h later, is added the sodium hydroxide of 19.7g30%, and adjustment system pH to 5 ± 2, the Mobyneb polycarboxylate water-reducer PCEs-5 that solid content is 40% is made.
Embodiment 6
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 355.8g molecular weight is added After 2400 isoamyl alcohol polyoxyethylene ether starts stirring, methylpropene sodium sulfonate 8.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains mixed liquor.
34.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.7g ascorbic acid, 1.1g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 3h.Reaction system Temperature is maintained at 43 DEG C~47 DEG C, continues to stir 2h later, is added the sodium hydroxide of 19.7g30%, and adjustment system pH to 5 ± 2, the Mobyneb polycarboxylate water-reducer PCEs-6 that solid content is 40% is made.
Comparative example 1
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 355.8g molecular weight is added After 500 methyl allyl polyoxyethylene ether starts stirring, 45 DEG C are warming up to, the dioxygen that 3.2g mass concentration is 30% is added Water obtains mixed liquor.
32.6g acrylic acid is dissolved in 138.3g deionized water, obtains combination liquid A;
The mercaptopropionic acid of 0.6g ascorbic acid, 1.0g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid A and combination liquid B are added dropwise respectively, drop evenly and finish in 2.5h.Reactant It is that temperature is maintained at 43 DEG C~47 DEG C, continues to stir 1h later, the sodium hydroxide of 19.7g30%, adjustment system pH to 5 is added ± 2, the water-reducing agent PCEb-1 that solid content is 20% is made.
Comparative example 2
It is added dropwise in the four-hole boiling flask of pump equipped with thermometer, blender, constant current, 246.8g water, 55.8g molecular weight is added After 500 methyl allyl polyoxyethylene ether and the methyl allyl polyoxyethylene ether of 300g molecular weight 4000 start stirring, then Methylpropene sodium sulfonate 6.9g is added, is uniformly mixed, is warming up to 45 DEG C, the hydrogen peroxide that 3.2g mass concentration is 30% is added, obtains To mixed liquor.
The mercaptopropionic acid of 0.6g ascorbic acid, 1.0g is dissolved in the deionized water of 197.6g, is uniformly mixed, and obtains combination liquid B;
In the mixed liquor, starts that combination liquid B is added dropwise, drop evenly and finish in 2.5h.Temperature of reaction system is maintained at 43 DEG C~47 DEG C, continue to stir 1h later, the sodium hydroxide of 19.7g30% is added, adjustment system pH to 5 ± 2 is made and contains admittedly The water-reducing agent PCEb-2 that amount is 40%.
Comparative example 3
In four mouthfuls of glass flasks configured with blender, thermometer, Dropping feeder, reflux condenser, nitrogen protection device The interior methylpropenyl cetomacrogol 1000 that 160 parts by weight weight average molecular weight 1000 are added, the methacrylic of 180 parts by weight are poly- The deionized water of ethylene glycol 2400,400 parts by weight, after being warming up to 35 DEG C, in 2~3 hours respectively into reaction vessel simultaneously Be added dropwise be mixed with the methacrylic acid of 20.5 parts by weight, the methyl acrylate of 17.5 parts by weight, 10.5 parts by weight metering system The monomer solution of the deionized water of sodium sulfonate, the 2- Methacrylamide -3- propene sulfonic acid of 7.5 parts by weight and 100 parts by weight, drop Add the L-AA solution of the mass concentration 2% of the thioacetic acid for being mixed with 2.5 parts by weight and 60 parts by weight, 60 weight are added dropwise The ammonium persulfate solution of the mass concentration 2.5% of part, after being added dropwise, reaction terminates, and temperature control is at 50 DEG C or less after continuation of insurance Temperature 60 minutes, completes polymerization reaction, after keeping the temperature, is added in the triethylene tetramine of the mass concentration 60% of 26 parts by weight With, and adding water to adjust to mass concentration is 40% water-reducing agent PCEb-3.
Referring to GB8076-2008 " concrete admixture ", " the normal concrete mechanical property test side GB/T50081-2002 Method standard " relevant regulations, the slump, the slump-retaining, bleeding rate, gassiness of this product are detected using concrete test The performance parameters such as amount, compression strength.Concrete mix and application effect related data are as shown in table 1,2.
1 concrete mix (kg/m of table3)
W C FA S G
165 260 100 820 1080
Note: W is tap water;C is Ji east PO42.5;FA is II grades of flyash of Yongji power plant;S is natural river sand, fineness Modulus is 2.7;G is rubble 5-31.5 continuous grading.
2 concrete application effect related data of table:
Note: 1, it is the 0.12% of cementitious material quality that additive, which rolls over solid volume, experimental enviroment: 22 DEG C of temperature, humidity 55%.
Note: 2, H-8 is Huang Teng Chemical Co., Ltd. standard type polycarboxylate water-reducer.
As above-mentioned data it is found that using Mobyneb polycarboxylate water-reducer synthesized by the present invention, production technology wiper ring It protects, properties of product are stablized, and cost performance is high, product economy considerable benefit.Product not only subtracts in volume lower (0.12~0.13%) Water reinforcing effect is significant, and has good retentivity to concrete flowability, and slump 90min does not lose substantially.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (10)

1. a kind of water-reducing agent, which is characterized in that formed by polymerization of unsaturated monomers, the unsaturated monomer includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
2. water-reducing agent according to claim 1, which is characterized in that the polyoxyethylene ether containing unsaturated bond is allyl One or more of polyoxyethylene ether, methyl allyl polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether.
3. water-reducing agent according to claim 1, which is characterized in that the unsaturated sulfonic acid salt be methylpropene sodium sulfonate or Sodium Allyl Sulfonate.
4. water-reducing agent according to claim 1, which is characterized in that the unsaturated carboxylic acid be acrylic acid, methacrylic acid, One or both of styrene sulfonic acid and 2- Methacrylamide -3- propene sulfonic acid.
5. a kind of preparation method of water-reducing agent described in claim 1, comprising the following steps:
Unsaturated monomer carries out polymerization reaction in the redox system added with chain-transferring agent, obtains water-reducing agent;
The unsaturated monomer includes:
81~95wt% of polyoxyethylene ether containing unsaturated bond;
1~6wt% of unsaturated sulfonic acid salt;
4~13wt% of unsaturated carboxylic acid or derivatives thereof;
The molecular weight of the polyoxyethylene ether containing unsaturated bond is 1500~3500.
6. preparation method according to claim 5, which is characterized in that the preparation method specifically:
Polyoxyethylene ether, unsaturated sulfonic acid salt, oxidant and water containing unsaturated bond are mixed, mixed liquor is obtained;The oxidation The additive amount of agent is the 0.1~5% of the unsaturated monomer gross mass;
Unsaturated carboxylic acid monomer or derivatives thereof is soluble in water, obtain combination liquid A;
Reducing agent, chain-transferring agent and water are mixed, combination liquid B is obtained;The additive amount of the reducing agent is the total matter of unsaturated monomer The 0.1~6% of amount;The additive amount of the chain-transferring agent is the 0.1~5% of unsaturated monomer gross mass;
Combination liquid A and combination liquid B are added drop-wise in mixed liquor, polymerization reaction is carried out, obtains water-reducing agent.
7. preparation method according to claim 6, which is characterized in that after the polymerization reaction, add alkali or aqueous slkali into Row neutralization reaction, the alkali are sodium hydroxide, potassium hydroxide or triethanolamine;The temperature when neutralization reaction be 50 DEG C with Under.
8. preparation method according to claim 7, which is characterized in that after the neutralization reaction, obtaining solid content is 30 ~70% water-reducing agent.
9. preparation method according to claim 6, which is characterized in that it is described combination liquid A and combine liquid B be added dropwise time be 1~4 hour, the polymerization time was 1~3 hour, and the temperature of the polymerization reaction is 30~60 DEG C.
10. preparation method according to claim 5, which is characterized in that the oxidant is ammonium persulfate or mass concentration For 30% hydrogen peroxide, the reducing agent is ascorbic acid or sodium hypophosphite;The chain-transferring agent is mercaptopropionic acid, thioacetic acid One or more of with mercaptoethanol.
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CN116284603A (en) * 2023-03-24 2023-06-23 辽宁奥克化学股份有限公司 Water reducer suitable for fly ash and slag type concrete and preparation method thereof

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CN102585115A (en) * 2011-12-26 2012-07-18 东华理工大学 Isobutylene polyether polycarboxylic water reducer and preparation method thereof
CN104692701A (en) * 2015-03-04 2015-06-10 河南新汉材料科技有限公司 Room-temperature synthetic type polycarboxylic high performance water-reducing agent and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112327953A (en) * 2020-11-05 2021-02-05 山西黄腾化工有限公司 Processing technology of polycarboxylic acid additive
CN112327953B (en) * 2020-11-05 2023-04-07 山西黄腾化工有限公司 Processing technology of polycarboxylic acid additive
CN112812238A (en) * 2020-12-30 2021-05-18 山西佳维新材料股份有限公司 Polycarboxylate superplasticizer and preparation method and application thereof
CN116284603A (en) * 2023-03-24 2023-06-23 辽宁奥克化学股份有限公司 Water reducer suitable for fly ash and slag type concrete and preparation method thereof
CN116284603B (en) * 2023-03-24 2024-01-26 辽宁奥克化学股份有限公司 Water reducer suitable for fly ash and slag type concrete and preparation method thereof

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