CN105293981A - Slump retention agent and preparation method thereof - Google Patents

Slump retention agent and preparation method thereof Download PDF

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CN105293981A
CN105293981A CN201510724872.7A CN201510724872A CN105293981A CN 105293981 A CN105293981 A CN 105293981A CN 201510724872 A CN201510724872 A CN 201510724872A CN 105293981 A CN105293981 A CN 105293981A
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reactant
retention agent
slump retention
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CN105293981B (en
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白杰
蔡阳
王博
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China Building Materials Academy CBMA
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China Building Materials Academy CBMA
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Abstract

The invention discloses a slump retention agent and a preparation method thereof, relating to the field of concrete admixtures and solving the problem that the sources of raw materials of slump retention agents are limited. The slump retention agent comprises the following raw materials by mass percent: 30-39% of polyether, 0.2-0.4% of initiator, 0.24-0.35% of chain transfer agent, 0.01-0.1% of reducing agent, 5-15% of small monomers and 45.15-64.55% of water, wherein polyether is methyl allyl ethylene glycol polyoxyethylene ether or a mixture of methyl allyl ethylene glycol polyoxyethylene ether and methyl allyl polyoxyethylene ether and/or methyl butenyl polyoxyethylene ether. The slump retention agent has a wide range of selectable raw materials and excellent properties.

Description

Slump retention agent and preparation method thereof
Technical field
The present invention relates to concrete admixture field, particularly relate to a kind of slump retention agent and preparation method thereof.
Background technology
Concrete is widely used in various fields as a kind of material of construction, the technology also promoting concrete admixture along with concrete development develops rapidly, concrete admixture is requisite a kind of component in concrete, in concrete production technology, play central role, decide concrete quality.Wherein, water reducer can effectively improve concrete workability as a kind of important concrete admixture, improves concrete intensity.In numerous water reducer, polycarboxylate water-reducer is as third generation water reducer, there is water-reducing rate high, volume is few, the ability of environmental protection and maintenance concrete slump, along with the fast development of China's economy and the raising at full speed of building level, high performance water reducing agent of polyocarboxy acid relies on its a series of outstanding properties to become the maximum admixture of usage quantity.But in the face of factors such as sand silt content is higher, content of stone powder is higher, cement constituent change, temperature variation, high performance water reducing agent of polyocarboxy acid still inevitably occurs that function of slump protection is not enough, lose too fast phenomenon in actual applications, and this phenomenon is the technical bottleneck of the construction of restriction new concrete and long-distance transportation.In recent years, slump retention agent became domestic new study hotspot and was widely used in concrete.
Along with the widespread use of slump retention agent, its usage quantity increases day by day, the synthesis material of existing slump retention agent generally comprises polyethers, initiator, chain-transfer agent, reductive agent, minor comonomer and water, wherein, polyethers often select in poly glycol monomethyl ether, allyl polyethenoxy ether, methacrylic Soxylat A 25-7 and methyl butene base Soxylat A 25-7 one or both and more than; Existing slump retention agent raw material sources are limited, and because of the difference of concrete composition, preparation technology and construction environment, and slump retention agent is very different and then have impact on concrete workability to concrete function of slump protection; Existing slump retention agent can not meet actual user demand, is therefore ensureing need develop more slump retention agent raw material while slump retention agent has excellent properties.
Summary of the invention
In view of this, embodiments provide a kind of slump retention agent and preparation method thereof, main purpose is the raw material sources expanding slump retention agent.
For achieving the above object, invention broadly provides following technical scheme:
On the one hand, the invention provides a kind of slump retention agent, its raw material is made up of the component of following mass percentage:
Wherein, described polyethers is methacrylic ethylene polyethenoxy ether, or described polyethers is the mixture of methacrylic ethylene polyethenoxy ether and methacrylic Soxylat A 25-7 and/or methyl butene base Soxylat A 25-7.
As preferably, when described polyethers is the mixture of methacrylic ethylene polyethenoxy ether and methacrylic Soxylat A 25-7 and/or methyl butene base Soxylat A 25-7, the mass percent that described methacrylic ethylene polyethenoxy ether accounts for described mixture is 1%-90%.
As preferably, described initiator is ammonium persulphate, Sodium Persulfate or hydrogen peroxide; Described chain-transfer agent is Thiovanic acid or thiohydracrylic acid; Described reductive agent is xitix, S-WAT or sodium bisulfite.
As preferably, described minor comonomer is selected from least two kinds in following vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, hydroxyethyl methylacrylate, Propylene glycol monoacrylate, Rocryl 410, hy-droxybutyl, methacrylate, methylpropene sodium sulfonate and methylene-succinic acid.
As preferably, described minor comonomer is the mixture of vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate and hy-droxybutyl, and the mass ratio of described vinylformic acid, described Hydroxyethyl acrylate, described Propylene glycol monoacrylate and described hy-droxybutyl is 15-20:75-80:0.1-5:0.1-5.
As preferably, the solid content of described slump retention agent is 35%-55%, and pH value is 3-5.
On the other hand, the invention provides the preparation method of above-mentioned slump retention agent, comprise the following steps:
Take raw material in proportion, initiator being joined the temperature that polyethers and water is mixed to get is in the polyether solutions of 20 DEG C-25 DEG C, obtain the first reactant, by chain-transfer agent, the mixture solution that reductive agent and water are mixed to get is added drop-wise in described first reactant, described mixture solution is added drop-wise in described first reactant needs 3.5 ± 0.25 hours, while dripping described mixture solution, minor comonomer solution minor comonomer and water are mixed to get is added drop-wise in described first reactant, described minor comonomer solution is added drop-wise in described first reactant needs 3.0 ± 0.25 hours, the second reactant is obtained after dropping terminates, controlling the temperature of described second reactant at 55 DEG C-60 DEG C, react and obtain the 3rd reactant after 1 hour, joining in described 3rd reactant by remaining water in raw material, described 3rd reactant after dilution is slump retention agent.
As preferably, the mass percentage concentration of described minor comonomer solution is more than or equal to 80% and is less than 100%, and the mass percentage concentration of described polyether solutions is 50%-60%, and the mass percentage concentration of described mixture solution is 3%-5%.
As preferably, when the temperature dripping described polyether solutions during described initiator is less than 20 DEG C, adopt calrod or solar heating to 20 DEG C-25 DEG C; When the temperature of described second reactant is less than 55 DEG C, adopt calrod or solar heating to 55 DEG C-60 DEG C.
As preferably, the described mixture solution time for adding dropped in described first reactant is 3.5 hours; The described minor comonomer solution time for adding dropped in described first reactant is 3.0 hours.
Compared with prior art, the invention has the beneficial effects as follows:
The consumption that the present invention is directed to slump retention agent increases day by day, the problem that raw material sources are limited, adopt the synthesis material using methacrylic ethylene polyethenoxy ether as slump retention agent, according to the introducing of methacrylic ethylene polyethenoxy ether and the performance requriements of slump retention agent, the proportion relation of each component materials in adjustment slump retention agent synthesis material, optimize the technique means of slump retention agent preparation technology, reach the raw material sources expanding slump retention agent, and the technical purpose of the function of slump protection excellence of slump retention agent.
Embodiment
For further setting forth the present invention for the technique means reaching predetermined goal of the invention and take and effect, below with preferred embodiment, to according to the embodiment of the present patent application, technical scheme, feature and effect thereof, be described in detail as follows.Special characteristic, structure or feature in multiple embodiments in following explanation can be combined by any suitable form.
Embodiment 1
Each feed composition is as follows by mass parts: 132 parts of methacrylic ethylene polyethenoxy ethers, 1188 parts of methacrylic Soxylat A 25-7s, 8.8 parts of ammonium persulphates, 10.6 part Thiovanic acid, 0.44 part of xitix, 40 parts of vinylformic acid, 170 parts of Hydroxyethyl acrylates, 10 parts of hy-droxybutyl, 2840.16 parts of water;
By above-mentioned 132 parts of methacrylic ethylene polyethenoxy ethers, above-mentioned 1188 parts of methacrylic Soxylat A 25-7s and 1320 parts of water drop in reaction unit, open and stir material, the polyether solutions that mass percentage concentration is 50% is obtained after abundant dissolving, the temperature of polyether solutions is 20 DEG C, by above-mentioned 10.6 parts of Thiovanic acids, above-mentioned 0.44 part of xitix and 356.96 parts of water mixing, stir, obtain the mixture solution that mass percentage concentration is 3%, by above-mentioned 40 parts of vinylformic acid, 170 parts of Hydroxyethyl acrylates, 10 parts of hy-droxybutyl and 55 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%,
It is in the polyether solutions of 50% that above-mentioned 8.8 parts of ammonium persulphates are joined above-mentioned mass percentage concentration, stir, obtain the first reactant, by above-mentioned mass percentage concentration be 3% mixture solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the mixture solution of 3% is 3.25 hours, while the above-mentioned mass percentage concentration of dropping is the mixture solution of 3%, by above-mentioned mass percentage concentration be 80% minor comonomer solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the minor comonomer solution of 80% is 2.75 hours, the second reactant is obtained after dropping terminates, wherein, in order to make reaction more abundant, reaction product performance is better, and above-mentioned mass percentage concentration is that the dropping process that the dropping process of the minor comonomer solution of 80% must be the mixture solution of 3% than above-mentioned mass percentage concentration is fulfiled ahead of schedule,
Reaction heat is utilized to provide heat for reactant, temperature of reaction is 50 DEG C, adopt calrod to above-mentioned second reactant heating, control reactant 55 DEG C of isothermal reactions 1 hour, obtaining the 3rd reactant, adding above-mentioned 3rd reactant by remaining water in raw material, after above-mentioned 3rd reactant dilution, be slump retention agent, the solid content obtaining above-mentioned slump retention agent according to the detection method of GB8077-2012 is 35%, and the pH value obtaining above-mentioned slump retention agent is 3.5.
Embodiment 2
Each feed composition is as follows by mass parts: 345 parts of methacrylic ethylene polyethenoxy ethers, 1371 parts of methyl butene base Soxylat A 25-7s, 17.6 parts of Sodium Persulfates, 15.4 parts of thiohydracrylic acids, 4.4 parts of S-WATs, 130 parts of vinylformic acid, 530 parts of hydroxyethyl methylacrylates, 1986.6 parts of water;
By above-mentioned 345 parts of methacrylic ethylene polyethenoxy ethers, above-mentioned 1371 parts of methyl butene base Soxylat A 25-7s and 1144 parts of water drop in reaction unit, open and stir material, the polyether solutions that mass percentage concentration is 60% is obtained after abundant dissolving, the temperature of polyether solutions is 22 DEG C, by above-mentioned 15.4 parts of thiohydracrylic acids, above-mentioned 4.4 parts of S-WATs and 376.2 parts of water mixing, stir, obtain the mixture solution that mass percentage concentration is 5%, by above-mentioned 130 parts of vinylformic acid, 530 parts of hydroxyethyl methylacrylates and 73.3 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 90%,
It is in the polyether solutions of 60% that above-mentioned 17.6 parts of Sodium Persulfates are joined above-mentioned mass percentage concentration, stir, obtain the first reactant, by above-mentioned mass percentage concentration be 5% mixture solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the mixture solution of 5% is 3.75 hours, while the above-mentioned mass percentage concentration of dropping is the mixture solution of 5%, by above-mentioned mass percentage concentration be 90% minor comonomer solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the minor comonomer solution of 90% is 3.25 hours, the second reactant is obtained after dropping terminates, wherein, in order to make reaction more abundant, reaction product performance is better, and above-mentioned mass percentage concentration is that the dropping process that the dropping process of the minor comonomer solution of 90% must be the mixture solution of 5% than above-mentioned mass percentage concentration is fulfiled ahead of schedule,
Reaction heat is utilized to provide heat for reactant, when temperature of reaction is 60 DEG C, control reactant 60 DEG C of isothermal reactions 1 hour, obtain the 3rd reactant, above-mentioned 3rd reactant is added by remaining water in raw material, be slump retention agent after above-mentioned 3rd reactant dilution, the solid content obtaining above-mentioned slump retention agent according to the detection method of GB8077-2012 is 54%, and the pH value obtaining above-mentioned slump retention agent is 5.0.
Embodiment 3
Each feed composition is as follows by mass parts: 700 parts of methacrylic ethylene polyethenoxy ethers, 350 parts of methacrylic Soxylat A 25-7s, 350 parts of methyl butene base Soxylat A 25-7s, 11 parts of hydrogen peroxide, 11 parts of thiohydracrylic acids, 2.64 part S-WAT, 64 parts of vinylformic acid, 330 parts of Hydroxyethyl acrylates, 3 parts of Propylene glycol monoacrylates, 3 parts of hy-droxybutyl, 2575.36 parts of water;
By above-mentioned 700 parts of methacrylic ethylene polyethenoxy ethers, 350 parts of methacrylic Soxylat A 25-7s, 350 parts of methyl butene base Soxylat A 25-7s and 1400 parts of water drop in reaction unit, open and stir material, the polyether solutions that mass percentage concentration is 50% is obtained after abundant dissolving, the temperature of polyether solutions is 25 DEG C, by above-mentioned 11 parts of thiohydracrylic acids, above-mentioned 2.64 parts of S-WATs and 327.36 parts of water mixing, stir, obtain the mixture solution that mass percentage concentration is 4%, by above-mentioned 64 parts of vinylformic acid, above-mentioned 330 parts of Hydroxyethyl acrylates, above-mentioned 3 parts of Propylene glycol monoacrylates, above-mentioned 3 parts of hy-droxybutyl and 100 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%,
It is in the polyether solutions of 50% that above-mentioned 11 parts of hydrogen peroxide are joined above-mentioned mass percentage concentration, stir, obtain the first reactant, by above-mentioned mass percentage concentration be 4% mixture solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the mixture solution of 4% is 3.5 hours, while the above-mentioned mass percentage concentration of dropping is the mixture solution of 4%, by above-mentioned mass percentage concentration be 80% minor comonomer solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the minor comonomer solution of 80% is 3 hours, the second reactant is obtained after dropping terminates, wherein, in order to make reaction more abundant, reaction product performance is better, and above-mentioned mass percentage concentration is that the dropping process that the dropping process of the minor comonomer solution of 80% must be the mixture solution of 4% than above-mentioned mass percentage concentration is fulfiled ahead of schedule,
Reaction heat is utilized to provide heat for reactant, temperature of reaction is 53 DEG C, adopt calrod to above-mentioned second reactant heating, control reactant 55 DEG C of isothermal reactions 1 hour, obtaining the 3rd reactant, adding above-mentioned 3rd reactant by remaining water in raw material, after above-mentioned 3rd reactant dilution, be slump retention agent, the solid content obtaining above-mentioned slump retention agent according to the detection method of GB8077-2012 is 41%, and the pH value obtaining above-mentioned slump retention agent is 4.3.
Embodiment 4
Each feed composition is as follows by mass parts: 1120 parts of methacrylic ethylene polyethenoxy ethers, 200 parts of methacrylic Soxylat A 25-7s, 80 parts of methyl butene base Soxylat A 25-7s, 11 parts of hydrogen peroxide, 11 parts of thiohydracrylic acids, 2.64 part S-WAT, 72 parts of vinylformic acid, 288 parts of Hydroxyethyl acrylates, 20 parts of Propylene glycol monoacrylates, 20 parts of hy-droxybutyl, 2575.36 parts of water;
By above-mentioned 1120 parts of methacrylic ethylene polyethenoxy ethers, 200 parts of methacrylic Soxylat A 25-7s, 80 parts of methyl butene base Soxylat A 25-7s and 1400 parts of water drop in reaction unit, open and stir material, the polyether solutions that mass percentage concentration is 50% is obtained after abundant dissolving, the temperature of polyether solutions is 25 DEG C, by above-mentioned 11 parts of thiohydracrylic acids, above-mentioned 2.64 parts of S-WATs and 327.36 parts of water mixing, stir, obtain the mixture solution that mass percentage concentration is 4%, by above-mentioned 72 parts of vinylformic acid, above-mentioned 288 parts of Hydroxyethyl acrylates, above-mentioned 20 parts of Propylene glycol monoacrylates, above-mentioned 20 parts of hy-droxybutyl and 100 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%,
It is in the polyether solutions of 50% that above-mentioned 11 parts of hydrogen peroxide are joined above-mentioned mass percentage concentration, stir, obtain the first reactant, by above-mentioned mass percentage concentration be 4% mixture solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the mixture solution of 4% is 3.5 hours, while the above-mentioned mass percentage concentration of dropping is the mixture solution of 4%, by above-mentioned mass percentage concentration be 80% minor comonomer solution drop in above-mentioned first reactant, the time for adding of above-mentioned mixing minor comonomer solution is 3 hours, the second reactant is obtained after dropping terminates, wherein, in order to make reaction more abundant, reaction product performance is better, and above-mentioned mass percentage concentration is that the dropping process that the dropping process of the minor comonomer solution of 80% must be the mixture solution of 4% than above-mentioned mass percentage concentration is fulfiled ahead of schedule,
Reaction heat is utilized to provide heat for reactant, temperature of reaction 54 DEG C, adopt calrod to above-mentioned second reactant heating, control reactant 55 DEG C of isothermal reactions 1 hour, obtaining the 3rd reactant, adding above-mentioned 3rd reactant by remaining water in raw material, after above-mentioned 3rd reactant dilution, be slump retention agent, the solid content obtaining above-mentioned slump retention agent according to the detection method of GB8077-2012 is 41%, and the pH value obtaining above-mentioned slump retention agent is 4.4.
Embodiment 5
Each feed composition is as follows by mass parts: 1400 parts of methacrylic ethylene polyethenoxy ethers, 11 parts of hydrogen peroxide, 11 parts of thiohydracrylic acids, 2.64 parts of S-WATs, 72 parts of vinylformic acid, 288 parts of Hydroxyethyl acrylates, 20 parts of Propylene glycol monoacrylates, 20 parts of hy-droxybutyl, 2575.36 parts of water;
Above-mentioned 1400 parts of methacrylic ethylene polyethenoxy ethers and 1400 parts of water are dropped in reaction unit, open and stir material, the polyether solutions that mass percentage concentration is 50% is obtained after abundant dissolving, the temperature of polyether solutions is 25 DEG C, by above-mentioned 11 parts of thiohydracrylic acids, above-mentioned 2.64 parts of S-WATs and 327.36 parts of water mixing, stir, obtain the mixture solution that mass percentage concentration is 4%, by above-mentioned 66 parts of vinylformic acid, above-mentioned 290 parts of Hydroxyethyl acrylates, above-mentioned 22 parts of Propylene glycol monoacrylates, above-mentioned 22 parts of hy-droxybutyl and 100 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%,
It is in the polyether solutions of 50% that above-mentioned 11 parts of hydrogen peroxide are joined above-mentioned mass percentage concentration, stir, obtain the first reactant, by above-mentioned mass percentage concentration be 4% mixture solution drop in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the mixture solution of 4% is 3.5 hours, while the above-mentioned mass percentage concentration of dropping is the mixture solution of 4%, the minor comonomer solution being first 80% by 350 parts of above-mentioned mass percentage concentration drops in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the minor comonomer solution of 80% is 1.5 hours, the minor comonomer solution being 80% by 150 parts of above-mentioned mass percentage concentration again drops in above-mentioned first reactant, above-mentioned mass percentage concentration is the time for adding of the minor comonomer solution of 80% is 1.5 hours, the second reactant is obtained after dropping terminates, wherein, in order to make reaction more abundant, reaction product performance is better, and above-mentioned mass percentage concentration is that the dropping process that the dropping process of the minor comonomer solution of 80% must be the mixture solution of 4% than above-mentioned mass percentage concentration is fulfiled ahead of schedule,
Reaction heat is utilized to provide heat for reactant, temperature of reaction 56 DEG C, control reactant 56 DEG C of isothermal reactions 1 hour, obtain the 3rd reactant, adding above-mentioned 3rd reactant by remaining water in raw material, being slump retention agent after above-mentioned 3rd reactant dilution, detecting through acidity, the solid content obtaining above-mentioned slump retention agent according to the detection method of GB8077-2012 is 41%, and the pH value obtaining above-mentioned slump retention agent is 4.4.
Comparative example 1
Comparative example 1 is with the difference of embodiment 3, by mass parts, polyethers in comparative example 1 is the mixture of 700 parts of methacrylic Soxylat A 25-7s and 700 parts of methyl butene base Soxylat A 25-7s, obtains slump retention agent by the preparation method of above-described embodiment.
Embodiment 1-5 and comparative example have prepared 6 kinds of slump retention agent, mix in concrete by above-mentioned 6 kinds of products with the mass ratio of gelling material (gelling material refers to the mixture of cement, flyash and breeze) total mass 0.16%, incorporation calculates by folding solid content; Embodiment 1-5 correspondence obtained concrete 1, concrete 2, concrete 3, concrete 4 and concrete 5, the obtained concrete 6 of comparative example 1 correspondence, wherein, above-mentioned concrete quality proportioning is, m1 (cement): m2 (flyash): m3 (breeze): m4 (sand): m5 (stone): m6 (water)=225:80:75:861:971:162, the test method specified according to GB8076-2008 detects above-mentioned 6 kinds of concrete slumps, divergence and ultimate compression strength, and measuring result is in table 1.
Table 1 six kinds of testing concrete performance results
Can find out that above-mentioned six kinds of concrete over-all propertieies are good by the measuring result of embodiment 1-5 and comparative example 1, all meet service requirements, illustrate that slump retention agent prepared by the embodiment of the present invention can be used as concrete admixture and in actual production; Further illustrating the embodiment of the present invention adopts methacrylic ethylene polyethenoxy ether can prepare as the synthesis material of slump retention agent the slump retention agent met the demands; Wherein, the mass percentage of methacrylic ethylene polyethenoxy ether in polyethers can carry out adjusting to obtain the good slump retention agent of over-all properties according to actual needs.
Concrete, by the slump retention agent selecting suitable minor comonomer and adjustment minor comonomer ratio in the feed can prepare slump retaining excellence, minor comonomer in the embodiment of the present invention is preferably following vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, hydroxyethyl methylacrylate, Propylene glycol monoacrylate, Rocryl 410, hy-droxybutyl, methacrylate, at least two kinds in methylpropene sodium sulfonate and methylene-succinic acid, more excellent, the minor comonomer of the embodiment of the present invention is vinylformic acid, Hydroxyethyl acrylate, the mixture of Propylene glycol monoacrylate and hy-droxybutyl, aforesaid propylene acid, aforesaid propylene acid hydroxyl ethyl ester, the mass ratio of aforesaid propylene acid hydroxypropyl acrylate and aforesaid propylene acid hydroxy butyl ester is 15-20:75-80:0.1-5:0.1-5.
More than illustrate that the embodiment of the present invention adopts methacrylic ethylene polyethenoxy ether as the synthesis material of slump retention agent, for its development of raw materials goes out a class novel substance, expand the material choice scope of slump retention agent, and the slump retention agent of preparation has excellent function of slump protection.
The process dripping minor comonomer in the embodiment of the present invention also can be divided into two stages to carry out, and segmentation drips and the product molecular weight distribution of generation can be allowed wider, makes the product over-all properties of preparation better.
Slump retention agent of the present invention is in preparation process, the temperature of polyether solutions before adding initiator of preparation is 20 DEG C-25 DEG C, in reaction process, utilize exothermic heat of reaction to make temperature of charge reach about 55 DEG C, basic without the need to a large amount of additional heat, calrod or sun power auxiliary additional heat among a small circle can be adopted when temperature of charge is less than 55 DEG C.And existing technique adopts external heat source first reactant to be heated to the temperature of reaction needed, and when making temperature of charge raise due to exothermic heat of reaction in reaction process, temperature of reaction is controlled again by cooling, thus cause whole technique to occur first heating the problem of rear cooling, not only expend the energy but also increase equipment cost.Preparation technology of the present invention takes full advantage of self exothermic heat of reaction, saves the cooling systems such as the heating installation such as boiler, steam and cooling tower, the object reaching Simplified flowsheet, energy-saving and emission-reduction and reduce costs.
The specific embodiment of the present invention is only above; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of the claims.

Claims (10)

1. slump retention agent, is characterized in that, its raw material is made up of the component of following mass percentage:
Wherein, described polyethers is methacrylic ethylene polyethenoxy ether, or described polyethers is the mixture of methacrylic ethylene polyethenoxy ether and methacrylic Soxylat A 25-7 and/or methyl butene base Soxylat A 25-7.
2. slump retention agent according to claim 1, it is characterized in that, when described polyethers is the mixture of methacrylic ethylene polyethenoxy ether and methacrylic Soxylat A 25-7 and/or methyl butene base Soxylat A 25-7, the mass percent that described methacrylic ethylene polyethenoxy ether accounts for described mixture is 1%-90%.
3. slump retention agent according to claim 1, is characterized in that, described initiator is ammonium persulphate, Sodium Persulfate or hydrogen peroxide; Described chain-transfer agent is Thiovanic acid or thiohydracrylic acid; Described reductive agent is xitix, S-WAT or sodium bisulfite.
4. slump retention agent according to claim 1, it is characterized in that, described minor comonomer is selected from least two kinds in following vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, hydroxyethyl methylacrylate, Propylene glycol monoacrylate, Rocryl 410, hy-droxybutyl, methacrylate, methylpropene sodium sulfonate and methylene-succinic acid.
5. slump retention agent according to claim 1, it is characterized in that, described minor comonomer is the mixture of vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate and hy-droxybutyl, and the mass ratio of described vinylformic acid, described Hydroxyethyl acrylate, described Propylene glycol monoacrylate and described hy-droxybutyl is 15-20:75-80:0.1-5:0.1-5.
6. slump retention agent according to claim 1, is characterized in that, the solid content of described slump retention agent is 35%-55%, and pH value is 3-5.
7. the preparation method of the slump retention agent described in claim 1-6, is characterized in that, comprises the following steps:
Take raw material in proportion, initiator being joined the temperature that polyethers and water is mixed to get is in the polyether solutions of 20 DEG C-25 DEG C, obtain the first reactant, by chain-transfer agent, the mixture solution that reductive agent and water are mixed to get is added drop-wise in described first reactant, described mixture solution is added drop-wise in described first reactant needs 3.5 ± 0.25 hours, while dripping described mixture solution, minor comonomer solution minor comonomer and water are mixed to get is added drop-wise in described first reactant, the time for adding of described minor comonomer solution is 3.0 ± 0.25 hours, the second reactant is obtained after dropping terminates, controlling the temperature of described second reactant at 55 DEG C-60 DEG C, react and obtain the 3rd reactant after 1 hour, joining in described 3rd reactant by remaining water in raw material, described 3rd reactant after dilution is slump retention agent.
8. the preparation method of slump retention agent according to claim 7, it is characterized in that, the mass percentage concentration of described minor comonomer solution is more than or equal to 80% and is less than 100%, the mass percentage concentration of described polyether solutions is 50%-60%, and the mass percentage concentration of described mixture solution is 3%-5%.
9. the preparation method of slump retention agent according to claim 7, is characterized in that, when the temperature adding described polyether solutions during described initiator is less than 20 DEG C, adopts calrod or solar heating to 20 DEG C-25 DEG C; When the temperature of described second reactant is less than 55 DEG C, adopt calrod or solar heating to 55 DEG C-60 DEG C.
10. the preparation method of slump retention agent according to claim 7, is characterized in that, the described mixture solution time for adding dropped in described first reactant is 3.5 hours; The described minor comonomer solution time for adding dropped in described first reactant is 3.0 hours.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109879629A (en) * 2019-03-13 2019-06-14 兰州同邦建材有限公司 A kind of high-thin arch dam synergist and its preparation method and application
CN110668730A (en) * 2019-11-18 2020-01-10 桂林华越环保科技有限公司 Building concrete synergist
CN111205013A (en) * 2019-12-06 2020-05-29 佛山市华轩新材料有限公司 High-strength high-performance concrete polycarboxylate superplasticizer and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102286134A (en) * 2011-06-09 2011-12-21 江苏天音化工有限公司 Preparation method for high-performance water reducing agent
CN102603996A (en) * 2012-02-28 2012-07-25 武汉理工大学 Ether type polycarboxylic acid slump retaining agent and preparation method thereof
CN103881029A (en) * 2014-04-17 2014-06-25 山东卓星化工有限公司 Heat source-free short-time preparation method of controlled-release type polycarboxylic acid high-performance slump retaining agent
CN103965413A (en) * 2014-04-18 2014-08-06 上海市建筑科学研究院(集团)有限公司 Low-temperature synthesis technology of polycarboxylic acid high-performance water reducer
CN104693377A (en) * 2015-03-30 2015-06-10 安康学院 Preparation method for polycarboxylate superplasticizer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102286134A (en) * 2011-06-09 2011-12-21 江苏天音化工有限公司 Preparation method for high-performance water reducing agent
CN102603996A (en) * 2012-02-28 2012-07-25 武汉理工大学 Ether type polycarboxylic acid slump retaining agent and preparation method thereof
CN103881029A (en) * 2014-04-17 2014-06-25 山东卓星化工有限公司 Heat source-free short-time preparation method of controlled-release type polycarboxylic acid high-performance slump retaining agent
CN103965413A (en) * 2014-04-18 2014-08-06 上海市建筑科学研究院(集团)有限公司 Low-temperature synthesis technology of polycarboxylic acid high-performance water reducer
CN104693377A (en) * 2015-03-30 2015-06-10 安康学院 Preparation method for polycarboxylate superplasticizer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109879629A (en) * 2019-03-13 2019-06-14 兰州同邦建材有限公司 A kind of high-thin arch dam synergist and its preparation method and application
CN110668730A (en) * 2019-11-18 2020-01-10 桂林华越环保科技有限公司 Building concrete synergist
CN111205013A (en) * 2019-12-06 2020-05-29 佛山市华轩新材料有限公司 High-strength high-performance concrete polycarboxylate superplasticizer and preparation method thereof

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