CN105293981B - Slump retention agent and preparation method thereof - Google Patents
Slump retention agent and preparation method thereof Download PDFInfo
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- CN105293981B CN105293981B CN201510724872.7A CN201510724872A CN105293981B CN 105293981 B CN105293981 B CN 105293981B CN 201510724872 A CN201510724872 A CN 201510724872A CN 105293981 B CN105293981 B CN 105293981B
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Abstract
The invention discloses a kind of slump retention agent and preparation method thereof, is related to concrete admixture field, solves the problems, such as that slump retention agent raw material sources are limited.The raw material of the slump retention agent of the present invention is made of the component of following mass percentage：Polyethers 30% 39%, initiator 0.2% 0.4%, chain-transferring agent 0.24% 0.35%, reducing agent 0.01% 0.1%, minor comonomer 5% 15%, water 45.15% 64.55%；Wherein, the polyethers is methacrylic ethylene polyethenoxy ether, or the polyethers is methacrylic ethylene polyethenoxy ether and methyl allyl polyoxyethylene ether and/or the mixture of methyl butene base polyoxyethylene ether.The optional scope of slump retention agent raw material of the present invention is more and excellent performance.
Description
Technical field
The present invention relates to concrete admixture field, more particularly to a kind of slump retention agent and preparation method thereof.
Background technology
Concrete is widely used in various fields as a kind of construction material, with the development of concrete also promote it is mixed
The technology of solidifying soil additive develops rapidly, and concrete admixture is essential a kind of component in concrete, autochthonal in coagulation
Central role is played in production technology, decides the quality of concrete.Wherein, water-reducing agent is as a kind of important concrete admixture
The workability of concrete can be effectively improved, improves the intensity of concrete.In numerous water-reducing agents, polycarboxylate water-reducer is as
Three generations's water-reducing agent, has that water-reducing rate is high, and volume is few, environmental protection and the ability for keeping concrete slump, fast with China's economy
Speed development and the raising at full speed of building level, high performance water reducing agent of polyocarboxy acid have become use by a series of its outstanding properties
Measure maximum additive.But in face of factors such as sand clay content is higher, content of stone powder is higher, cement constituent change, temperature changes, gather
Still inevitably there is function of slump protection deficiency, loses too fast phenomenon in practical applications in carboxylic acid high-performance water reducing agent, this
Phenomenon is to restrict the technical bottleneck of new concrete construction and long-distance transportation.In recent years, slump retention agent became domestic new
Research hotspot and be widely used in concrete.
With the extensive use of slump retention agent, its usage amount increasingly increases, and the synthesis of existing slump retention agent is former
Material generally comprises polyethers, initiator, chain-transferring agent, reducing agent, minor comonomer and water, wherein, polyethers often selects polyethyleneglycol
Methyl ether, allyl polyethenoxy ether, methyl allyl polyoxyethylene ether and one kind in methyl butene base polyoxyethylene ether or
Two kinds and more than；Existing slump retention agent raw material sources are limited, and the component because of concrete, preparation process and construction ring
The difference in border, slump retention agent is very different to the function of slump protection of concrete and then have impact on the workability of concrete；It is existing
Some slump retention agents have been unable to meet actual use demand, therefore are ensureing that slump retention agent is same with excellent properties
When need to develop more slump retention agent raw materials.
The content of the invention
In view of this, an embodiment of the present invention provides a kind of slump retention agent and preparation method thereof, main purpose is to expand
The raw material sources of high slump retention agent.
To reach above-mentioned purpose, invention broadly provides following technical solution：
On the one hand, the present invention provides a kind of slump retention agent, its raw material by following mass percentage component group
Into：
Wherein, the polyethers is methacrylic ethylene polyethenoxy ether, or the polyethers is methacrylic second two
Alcohol polyoxyethylene ether and methyl allyl polyoxyethylene ether and/or the mixture of methyl butene base polyoxyethylene ether.
Preferably, the polyethers is methacrylic ethylene polyethenoxy ether and methyl allyl polyoxyethylene ether
And/or methyl butene base polyoxyethylene ether mixture when, the methacrylic ethylene polyethenoxy ether accounts for the mixing
The mass percent of thing is 1%-90%.
Preferably, the initiator is ammonium persulfate, sodium peroxydisulfate or hydrogen peroxide；The chain-transferring agent is sulfydryl second
Acid or mercaptopropionic acid；The reducing agent is ascorbic acid, sodium sulfite or sodium hydrogensulfite.
Preferably, the minor comonomer is selected from following acrylic acid, methacrylic acid, hydroxy-ethyl acrylate, methacrylic acid
Hydroxyl ethyl ester, hydroxypropyl acrylate, hydroxy propyl methacrylate, hy-droxybutyl, methacrylate, metering system sulphur
At least two in sour sodium and itaconic acid.
Preferably, the minor comonomer is acrylic acid, hydroxy-ethyl acrylate, hydroxypropyl acrylate and hy-droxybutyl
Mixture, the acrylic acid, the hydroxy-ethyl acrylate, the mass ratio of the hydroxypropyl acrylate and the hy-droxybutyl
For 15-20:75-80:0.1-5:0.1-5.
Preferably, the solid content of the slump retention agent is 35%-55%, pH value 3-5.
On the other hand, the present invention provides the preparation method of above-mentioned slump retention agent, comprise the following steps：
Raw material is weighed in proportion, and initiator is added to the polyethers that polyethers is 20 DEG C -25 DEG C with the temperature that water is mixed to get
In solution, the first reactant is obtained, the mixing agent solution that chain-transferring agent, reducing agent and water are mixed to get is added drop-wise to described first
In reactant, it is described mixing agent solution be added drop-wise in first reactant need 3.5 ± 0.25 it is small when, the intermixture is added dropwise
While solution, the minor comonomer solution that minor comonomer and water are mixed to get is added drop-wise in first reactant, the minor comonomer
Solution be added drop-wise in first reactant need 3.0 ± 0.25 it is small when, the second reactant is obtained after completion of dropwise addition；Described in control
The temperature of second reactant at 55 DEG C -60 DEG C, when reaction 1 is small after obtain the 3rd reactant, remaining water in raw material is added to institute
State in the 3rd reactant, the 3rd reactant after dilution is slump retention agent.
Preferably, the mass percentage concentration of the minor comonomer solution, which is more than or equal to 80%, is less than 100%, the polyethers is molten
The mass percentage concentration of liquid is 50%-60%, and the mass percentage concentration of the mixing agent solution is 3%-5%.
Preferably, when the temperature of the polyether solutions is less than 20 DEG C when the initiator is added dropwise, using electrical bar or too
Sun can be heated to 20 DEG C -25 DEG C；When the temperature of second reactant is less than 55 DEG C, using electrical bar or solar energy heating to 55
℃-60℃。
Preferably, when the time for adding that the mixing agent solution is added dropwise in first reactant is 3.5 small；It is described
When the time for adding that minor comonomer solution is added dropwise in first reactant is 3.0 small.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention increasingly increases for the problem that the dosage of slump retention agent, and raw material sources are limited, use with methyl alkene
Synthesis material of the propyl glycol polyoxyethylene ether as slump retention agent, according to methacrylic ethylene polyethenoxy ether
Introducing and slump retention agent performance requirement, adjust slump retention agent synthesis material in each component material proportioning close
System, optimizes the technological means of slump retention agent preparation process, has reached the raw material sources for expanding slump retention agent, and collapse
The excellent technical purpose of the function of slump protection of degree of falling retention agent.
Embodiment
Be further illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below with compared with
Good embodiment, to embodiment, technical solution, feature and its effect according to the present patent application, describes in detail as after.Under
State it is bright in multiple embodiments in special characteristic, structure or feature can be combined by any suitable form.
Embodiment 1
Each raw material components are as follows in parts by mass：132 parts of methacrylic ethylene polyethenoxy ethers, 1188 parts of methyl alkene
Propyl group polyoxyethylene ether, 8.8 parts of ammonium persulfates, 10.6 parts of thioacetic acid, 0.44 part of ascorbic acid, 40 parts of acrylic acid, 170 part third
Olefin(e) acid hydroxyl ethyl ester, 10 parts of hy-droxybutyls, 2840.16 parts of water；
By above-mentioned 132 parts of methacrylic ethylene polyethenoxy ethers, above-mentioned 1188 parts of methyl allyl polyoxyethylene ethers
Put into 1320 parts of water in reaction unit, open stirring material, the polyethers that mass percentage concentration is 50% is fully obtained after dissolving
Solution, the temperature of polyether solutions is 20 DEG C, by above-mentioned 10.6 parts of thioacetic acid, above-mentioned 0.44 part of ascorbic acid and 356.96 parts of water
Mixing, stirs evenly, and the mixing agent solution that mass percentage concentration is 3% is obtained, by above-mentioned 40 parts of acrylic acid, 170 parts of acrylic acid
Hydroxyl ethyl ester, 10 parts of hy-droxybutyls and 55 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%；
Above-mentioned 8.8 parts of ammonium persulfates are added in the polyether solutions that above-mentioned mass percentage concentration is 50%, stirred evenly,
The first reactant is obtained, the mixing agent solution that above-mentioned mass percentage concentration is 3% is added dropwise in above-mentioned first reactant, it is above-mentioned
The time for adding for the mixing agent solution that mass percentage concentration is 3% is 3.25 hours, is above-mentioned mass percentage concentration is added dropwise
While 3% mixing agent solution, the minor comonomer solution that above-mentioned mass percentage concentration is 80% is added dropwise to above-mentioned first reaction
In thing, the time for adding for the minor comonomer solution that above-mentioned mass percentage concentration is 80% is 2.75 hours, is obtained after completion of dropwise addition
Second reactant；Wherein, in order to make reaction more abundant, reaction product performance is more preferable, above-mentioned mass percentage concentration be 80% it is small
The dropwise addition process of monomer solution must be fulfiled ahead of schedule than the dropwise addition process for the mixing agent solution that above-mentioned mass percentage concentration is 3%；
Heat is provided for reactant using reaction heat, reaction temperature is 50 DEG C, using electrical bar to above-mentioned second reactant
Heating, control reactant obtain the 3rd reactant when 55 DEG C of isothermal reactions 1 are small, and remaining water in raw material is added the above-mentioned 3rd
Reactant, is slump retention agent after above-mentioned 3rd reactant dilution, is obtained according to the detection method of GB8077-2012 above-mentioned
The solid content of slump retention agent is 35%, and the pH value for obtaining above-mentioned slump retention agent is 3.5.
Embodiment 2
Each raw material components are as follows in parts by mass：345 parts of methacrylic ethylene polyethenoxy ethers, 1371 parts of methyl fourths
Alkenyl polyoxyethylene ether, 17.6 parts of sodium peroxydisulfates, 15.4 parts of mercaptopropionic acids, 4.4 parts of sodium sulfites, 130 parts of acrylic acid, 530 parts
Hydroxyethyl methacrylate, 1986.6 parts of water；
By above-mentioned 345 parts of methacrylic ethylene polyethenoxy ethers, above-mentioned 1371 parts of methyl butenes base polyoxyethylene ether
Put into 1144 parts of water in reaction unit, open stirring material, the polyethers that mass percentage concentration is 60% is fully obtained after dissolving
Solution, the temperature of polyether solutions is 22 DEG C, and above-mentioned 15.4 parts of mercaptopropionic acids, above-mentioned 4.4 parts of sodium sulfites and 376.2 parts of water are mixed
Close, stir evenly, the mixing agent solution that mass percentage concentration is 5% is obtained, by above-mentioned 130 parts of acrylic acid, 530 parts of metering systems
Sour hydroxyl ethyl ester and 73.3 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 90%；
Above-mentioned 17.6 parts of sodium peroxydisulfates are added in the polyether solutions that above-mentioned mass percentage concentration is 60%, stirring is equal
It is even, the first reactant is obtained, the mixing agent solution that above-mentioned mass percentage concentration is 5% is added dropwise in above-mentioned first reactant,
The time for adding for the mixing agent solution that above-mentioned mass percentage concentration is 5% is 3.75 hours, and being added dropwise, above-mentioned quality percentage is dense
While spending the mixing agent solution for 5%, the minor comonomer solution that above-mentioned mass percentage concentration is 90% is added dropwise to above-mentioned first
In reactant, the time for adding for the minor comonomer solution that above-mentioned mass percentage concentration is 90% is 3.25 hours, after completion of dropwise addition
Obtain the second reactant；Wherein, in order to make reaction more abundant, reaction product performance is more preferable, and above-mentioned mass percentage concentration is 90%
Minor comonomer solution dropwise addition process must than above-mentioned mass percentage concentration be 5% mixing agent solution dropwise addition process it is complete in advance
Into；
Heat is provided for reactant using reaction heat, when reaction temperature is 60 DEG C, control reactant is in 60 DEG C of isothermal reactions 1
Hour, the 3rd reactant is obtained, remaining water in raw material is added into above-mentioned 3rd reactant, is after above-mentioned 3rd reactant dilution
Slump retention agent, the solid content that above-mentioned slump retention agent is obtained according to the detection method of GB8077-2012 is 54%, is obtained
The pH value of above-mentioned slump retention agent is 5.0.
Embodiment 3
Each raw material components are as follows in parts by mass：700 parts of methacrylic ethylene polyethenoxy ethers, 350 parts of methyl alkene
Propyl group polyoxyethylene ether, 350 parts of methyl butene base polyoxyethylene ether, 11 parts of hydrogen peroxide, 11 parts of mercaptopropionic acids, 2.64 parts of sulfurous
Sour sodium, 64 parts of acrylic acid, 330 parts of hydroxy-ethyl acrylates, 3 parts of hydroxypropyl acrylates, 3 parts of hy-droxybutyls, 2575.36 parts
Water；
By above-mentioned 700 parts of methacrylic ethylene polyethenoxy ethers, 350 parts of methyl allyl polyoxyethylene ethers, 350 parts
In methyl butene base polyoxyethylene ether and 1400 parts of water input reaction units, stirring material is opened, fully obtains quality after dissolving
Percentage concentration is 50% polyether solutions, and the temperature of polyether solutions is 25 DEG C, by above-mentioned 11 parts of mercaptopropionic acids, above-mentioned 2.64 parts of Asias
Sodium sulphate and 327.36 parts of water mixing, stir evenly, the mixing agent solution that mass percentage concentration is 4% are obtained, by above-mentioned 64 parts
Acrylic acid, above-mentioned 330 parts of hydroxy-ethyl acrylates, above-mentioned 3 parts of hydroxypropyl acrylates, above-mentioned 3 parts of hy-droxybutyls and 100 parts of water
It is mixed to get the minor comonomer solution that mass percentage concentration is 80%；
Above-mentioned 11 parts of hydrogen peroxide are added in the polyether solutions that above-mentioned mass percentage concentration is 50%, stirred evenly,
The first reactant is obtained, the mixing agent solution that above-mentioned mass percentage concentration is 4% is added dropwise in above-mentioned first reactant, it is above-mentioned
The time for adding for the mixing agent solution that mass percentage concentration is 4% is 3.5 hours, is above-mentioned mass percentage concentration is added dropwise
While 4% mixing agent solution, the minor comonomer solution that above-mentioned mass percentage concentration is 80% is added dropwise to above-mentioned first reaction
It is anti-that second is obtained in thing, when the time for adding for the minor comonomer solution that above-mentioned mass percentage concentration is 80% is 3 small, after completion of dropwise addition
Answer thing；Wherein, in order to make reaction more abundant, reaction product performance is more preferable, and the minor comonomer that above-mentioned mass percentage concentration is 80% is molten
The dropwise addition process of liquid must be fulfiled ahead of schedule than the dropwise addition process for the mixing agent solution that above-mentioned mass percentage concentration is 4%；
Heat is provided for reactant using reaction heat, reaction temperature is 53 DEG C, using electrical bar to above-mentioned second reactant
Heating, control reactant obtain the 3rd reactant when 55 DEG C of isothermal reactions 1 are small, and remaining water in raw material is added the above-mentioned 3rd
Reactant, is slump retention agent after above-mentioned 3rd reactant dilution, is obtained according to the detection method of GB8077-2012 above-mentioned
The solid content of slump retention agent is 41%, and the pH value for obtaining above-mentioned slump retention agent is 4.3.
Embodiment 4
Each raw material components are as follows in parts by mass：1120 parts of methacrylic ethylene polyethenoxy ethers, 200 parts of methyl alkene
Propyl group polyoxyethylene ether, 80 parts of methyl butene base polyoxyethylene ether, 11 parts of hydrogen peroxide, 11 parts of mercaptopropionic acids, 2.64 parts of sulfurous
Sour sodium, 72 parts of acrylic acid, 288 parts of hydroxy-ethyl acrylates, 20 parts of hydroxypropyl acrylates, 20 parts of hy-droxybutyls, 2575.36 parts
Water；
By above-mentioned 1120 parts of methacrylic ethylene polyethenoxy ethers, 200 parts of methyl allyl polyoxyethylene ethers, 80 parts
In methyl butene base polyoxyethylene ether and 1400 parts of water input reaction units, stirring material is opened, fully obtains quality after dissolving
Percentage concentration is 50% polyether solutions, and the temperature of polyether solutions is 25 DEG C, by above-mentioned 11 parts of mercaptopropionic acids, above-mentioned 2.64 parts of Asias
Sodium sulphate and 327.36 parts of water mixing, stir evenly, the mixing agent solution that mass percentage concentration is 4% are obtained, by above-mentioned 72 parts
Acrylic acid, above-mentioned 288 parts of hydroxy-ethyl acrylates, above-mentioned 20 parts of hydroxypropyl acrylates, above-mentioned 20 parts of hy-droxybutyls and 100 parts
Water is mixed to get the minor comonomer solution that mass percentage concentration is 80%；
Above-mentioned 11 parts of hydrogen peroxide are added in the polyether solutions that above-mentioned mass percentage concentration is 50%, stirred evenly,
The first reactant is obtained, the mixing agent solution that above-mentioned mass percentage concentration is 4% is added dropwise in above-mentioned first reactant, it is above-mentioned
The time for adding for the mixing agent solution that mass percentage concentration is 4% is 3.5 hours, is above-mentioned mass percentage concentration is added dropwise
While 4% mixing agent solution, the minor comonomer solution that above-mentioned mass percentage concentration is 80% is added dropwise to above-mentioned first reaction
In thing, when the time for adding of above-mentioned mixing minor comonomer solution is 3 small, the second reactant is obtained after completion of dropwise addition；Wherein, in order to make
Reaction is more abundant, and reaction product performance is more preferable, and above-mentioned mass percentage concentration is that the dropwise addition process of 80% minor comonomer solution is necessary
Dropwise addition process than the mixing agent solution that above-mentioned mass percentage concentration is 4% is fulfiled ahead of schedule；
Heat is provided for reactant using reaction heat, 54 DEG C of reaction temperature, adds above-mentioned second reactant using electrical bar
Heat, control reactant obtain the 3rd reactant when 55 DEG C of isothermal reactions 1 are small, and it is anti-that remaining water in raw material is added the above-mentioned 3rd
Thing is answered, is slump retention agent after above-mentioned 3rd reactant dilution, above-mentioned collapse is obtained according to the detection method of GB8077-2012
The solid content of degree of falling retention agent is 41%, and the pH value for obtaining above-mentioned slump retention agent is 4.4.
Embodiment 5
Each raw material components are as follows in parts by mass：1400 parts of methacrylic ethylene polyethenoxy ethers, 11 parts of peroxidating
Hydrogen, 11 parts of mercaptopropionic acids, 2.64 parts of sodium sulfites, 72 parts of acrylic acid, 288 parts of hydroxy-ethyl acrylates, 20 parts of hydroxypropyl acrylates,
20 parts of hy-droxybutyls, 2575.36 parts of water；
By in above-mentioned 1400 parts of methacrylic ethylene polyethenoxy ethers and 1400 parts of water input reaction units, unlatching is stirred
Material is mixed, the polyether solutions that mass percentage concentration is 50% are fully obtained after dissolving, the temperature of polyether solutions is 25 DEG C, will be above-mentioned
11 parts of mercaptopropionic acids, above-mentioned 2.64 parts of sodium sulfites and 327.36 parts of water mixing, stir evenly, obtaining mass percentage concentration is
4% mixing agent solution, by above-mentioned 66 parts of acrylic acid, above-mentioned 290 parts of hydroxy-ethyl acrylates, above-mentioned 22 parts of hydroxypropyl acrylates,
Above-mentioned 22 parts of hy-droxybutyls and 100 parts of water are mixed to get the minor comonomer solution that mass percentage concentration is 80%；
Above-mentioned 11 parts of hydrogen peroxide are added in the polyether solutions that above-mentioned mass percentage concentration is 50%, stirred evenly,
The first reactant is obtained, the mixing agent solution that above-mentioned mass percentage concentration is 4% is added dropwise in above-mentioned first reactant, it is above-mentioned
The time for adding for the mixing agent solution that mass percentage concentration is 4% is 3.5 hours, is above-mentioned mass percentage concentration is added dropwise
While 4% mixing agent solution, the minor comonomer solution that 350 parts of above-mentioned mass percentage concentrations are 80% is first added dropwise to above-mentioned the
In one reactant, when the time for adding for the minor comonomer solution that above-mentioned mass percentage concentration is 80% is 1.5 small, then by 150 parts
State the minor comonomer solution that mass percentage concentration is 80% to be added dropwise in above-mentioned first reactant, above-mentioned mass percentage concentration is 80%
Minor comonomer solution time for adding for 1.5 it is small when, the second reactant is obtained after completion of dropwise addition；Wherein, in order to make reaction more fill
Point, reaction product performance is more preferable, and above-mentioned mass percentage concentration is that the dropwise addition process of 80% minor comonomer solution must be than above-mentioned matter
The dropwise addition process for the mixing agent solution that amount percentage concentration is 4% is fulfiled ahead of schedule；
Heat is provided for reactant using reaction heat, 56 DEG C of reaction temperature, controls reactant small in 56 DEG C of isothermal reactions 1
When, the 3rd reactant is obtained, remaining water in raw material is added into above-mentioned 3rd reactant, is to collapse after above-mentioned 3rd reactant dilution
Degree of falling retention agent, is detected by acidity, and the solid content of above-mentioned slump retention agent is obtained according to the detection method of GB8077-2012
For 41%, the pH value for obtaining above-mentioned slump retention agent is 4.4.
Comparative example 1
Comparative example 1 and the difference of embodiment 3 are that in parts by mass, the polyethers in comparative example 1 is 700 parts of methyl
The mixture of allyl polyethenoxy ether and 700 parts of methyl butene base polyoxyethylene ether, passes through the preparation method of above-described embodiment
Slump retention agent is made.
Embodiment 1-5 and comparative example are prepared for 6 kinds of slump retention agents, by above-mentioned 6 kinds of products with cementitious material (gelling material
Material refers to the mixture of cement, flyash and miberal powder) in the mass ratio incorporation concrete of gross mass 0.16%, incorporation is solid by folding
Content calculation；Embodiment 1-5, which is corresponded to, is made concrete 1, concrete 2, concrete 3, concrete 4 and concrete 5, and comparative example 1 is right
Concrete 6 should be made, wherein, the quality proportioning of above-mentioned concrete is m1 (cement)：M2 (flyash)：M3 (miberal powder)：m4
(sand)：M5 (stone)：M6 (water)=225:80:75:861:971:162, on test method detects as defined in GB8076-2008
The slump, divergence and compression strength of 6 kinds of concrete are stated, measurement result is shown in Table 1.
1 six kinds of testing concrete performance results of table
It can be seen that the comprehensive performance of above-mentioned six kinds of concrete is good by the measurement result of embodiment 1-5 and comparative example 1,
Meet requirement, illustrate that slump retention agent prepared by the embodiment of the present invention can be used for reality as the additive of concrete
In production；Further illustrate the embodiment of the present invention using methacrylic ethylene polyethenoxy ether as slump retention agent
Synthesis material can prepare the slump retention agent met the requirements；Wherein, methacrylic ethylene polyethenoxy ether is poly-
Mass percentage in ether can be adjusted to obtain the good slump retention agent of comprehensive performance according to being actually needed.
Specifically, slump retaining can be prepared by selecting suitable minor comonomer and adjusting the ratio of minor comonomer in the feed
Excellent slump retention agent, the minor comonomer in the embodiment of the present invention is preferably following acrylic acid, methacrylic acid, acrylic acid hydroxyl
Ethyl ester, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate, hy-droxybutyl, hydroxyethyl methacrylate
At least two in butyl ester, methylpropene sodium sulfonate and itaconic acid, more preferably, the minor comonomer of the embodiment of the present invention is acrylic acid,
The mixture of hydroxy-ethyl acrylate, hydroxypropyl acrylate 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.
The embodiment of the present invention described above is using methacrylic ethylene polyethenoxy ether as slump retention agent
Synthesis material, a kind of novel substance is developed for its raw material, expands the raw material range of choice of slump retention agent, and prepare
Slump retention agent has excellent function of slump protection.
It the process of minor comonomer is added dropwise in the embodiment of the present invention can also be divided into two stages and carry out, segmentation, which is added dropwise, can allow generation
Product molecular weight distribution is wider, makes the product comprehensive performance of preparation more preferable.
In preparation process, the temperature of the polyether solutions of preparation before initiator is added is the slump retention agent of the present invention
20 DEG C -25 DEG C, temperature of charge is set to reach 55 DEG C or so using exothermic heat of reaction during the reaction, substantially without a large amount of external heats
Amount, electrical bar or the small-scale auxiliary additional heat of solar energy can be used when temperature of charge is less than 55 DEG C.And existing process
Reactant is first heated to the reaction temperature needed using external heat source, and is worked as in reaction process since exothermic heat of reaction makes reactant
When temperature raises, further through cooling controlling reaction temperature, so as to cause whole technique to occur first heating the problem of afterwards cooling down, both consumed
The expense energy increases equipment cost again.The preparation process of the present invention takes full advantage of the exothermic heat of reaction of itself, saves boiler, steam etc.
The cooling system such as heating equipment and cooling tower, achievees the purpose that simplified technique, energy-saving and emission-reduction and reduces cost.
Disclosed above is only the embodiment of the present invention, but protection scope of the present invention is not limited thereto, and is appointed
What those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should using above-mentioned scope of the claims as
It is accurate.
Claims (8)
1. slump retention agent, it is characterised in that its raw material is made of the component of following mass percentage：
Wherein, the polyethers is methacrylic ethylene polyethenoxy ether, or the polyethers is that methallyl ethyl glycol gathers
Ethylene oxide ether and methyl allyl polyoxyethylene ether and/or the mixture of methyl butene base polyoxyethylene ether；
The preparation method of the slump retention agent is：
Raw material is weighed in proportion, and initiator is added to the polyether solutions that polyethers is 20 DEG C -25 DEG C with the temperature that water is mixed to get
In, the first reactant is obtained, the mixing agent solution that chain-transferring agent, reducing agent and water are mixed to get is added drop-wise to first reaction
In thing, it is described mixing agent solution be added drop-wise in first reactant need 3.5 ± 0.25 it is small when, the mixing agent solution is added dropwise
While, the minor comonomer solution that minor comonomer and water are mixed to get is added drop-wise in first reactant, the minor comonomer solution
Time for adding for 3.0 ± 0.25 it is small when, the second reactant is obtained after completion of dropwise addition；The temperature of second reactant is controlled to exist
55 DEG C -60 DEG C, when reaction 1 is small after obtain the 3rd reactant, remaining water in raw material is added in the 3rd reactant, through dilute
The 3rd reactant after releasing is slump retention agent；
When adding the temperature of the polyether solutions during initiator and being less than 20 DEG C, using electrical bar or solar energy heating to 20
℃-25℃；Heat is provided for second reactant using exothermic heat of reaction, the temperature of second reactant is less than 55 DEG C
When, using electrical bar or solar energy heating to 55 DEG C -60 DEG C.
2. slump retention agent according to claim 1, it is characterised in that the polyethers gathers for methallyl ethyl glycol
When ethylene oxide ether is with methyl allyl polyoxyethylene ether and/or the mixture of methyl butene base polyoxyethylene ether, the methyl alkene
The mass percent that propyl glycol polyoxyethylene ether accounts for the mixture is 1%-90%.
3. slump retention agent according to claim 1, it is characterised in that the initiator is ammonium persulfate, persulfuric acid
Sodium or hydrogen peroxide；The chain-transferring agent is thioacetic acid or mercaptopropionic acid；The reducing agent for ascorbic acid, sodium sulfite or
Sodium hydrogensulfite.
4. slump retention agent according to claim 1, it is characterised in that the minor comonomer is selected from following acrylic acid, first
Base acrylic acid, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate, acrylic acid hydroxyl
At least two in butyl ester, methacrylate, methylpropene sodium sulfonate and itaconic acid.
5. slump retention agent according to claim 1, it is characterised in that the minor comonomer is acrylic acid, acrylic acid hydroxyl
The mixture of ethyl ester, hydroxypropyl acrylate and hy-droxybutyl, the acrylic acid, the hydroxy-ethyl acrylate, the propylene
The mass ratio of sour hydroxypropyl acrylate and the hy-droxybutyl is 15-20:75-80:0.1-5:0.1-5.
6. slump retention agent according to claim 1, it is characterised in that the solid content of the slump retention agent is
35%-55%, pH value 3-5.
7. slump retention agent according to claim 1, it is characterised in that the mass percentage concentration of the minor comonomer solution
It is less than 100% more than or equal to 80%, the mass percentage concentration of the polyether solutions is 50%-60%, the mixing agent solution
Mass percentage concentration is 3%-5%.
8. slump retention agent according to claim 1, it is characterised in that the mixing agent solution is added dropwise to described first
When time for adding in reactant is 3.5 small；The time for adding that the minor comonomer solution is added dropwise in first reactant is
3.0 it is small when.
Priority Applications (1)
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