CN109705282A - A kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer - Google Patents
A kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer, comprising the following steps: S1: polyether macromonomer and deionized water being added in reaction kettle, stirring dissolves it at normal temperature, obtains liquid on earth, spare；A liquid is obtained after unsaturated acids or anhydride minor comonomer are mixed in water, it is spare；B liquid is obtained after reducing agent, chain-transferring agent and water are sufficiently mixed, it is spare；S2: being added a certain amount of A liquid into polymeric monomer aqueous solution obtained by step S1, stir evenly, and obtains mixture；S3: being added oxidant into mixture obtained by step S2 in advance, and A liquid and B liquid then is added dropwise simultaneously, keeps the temperature 0.5h after being added dropwise；S4: lye is added after reaction and neutralizes, product is poured out to get superelevation water reducing type polycarboxylate water-reducer is arrived.The present invention has superelevation diminishing, Self-leveling, adaptable strong, high-durability feature.
Description
Technical field
The present invention relates to technical field of concrete additives more particularly to a kind of novel polyether to synthesize the poly- carboxylic of superelevation water reducing type
The preparation method of sour water-reducing agent.
Background technique
Polycarboxylate water-reducer is as third generation concrete admixture, because water-reducing rate with higher, preferable cement adapt to
Property, and the features such as production process is environmentally friendly and popularization energetically has been obtained, so that the polyether macromonomer industry in China also obtains
Significant progress.The yield and production capacity of national polyether macromonomer are all continuing to increase, and 2017 are to have reached all-time high.
The synthesis common polyethers of polycarboxylate water-reducer is mostly HPEG and TPEG at present, and product structure is relatively single, and its initiator exists
Supply side still has partial dependency import, especially 5 carbon alcohol initiators.Compared with existing 4 carbon, 5 carbon polymeric monomers, firstly, making
The time for adding of acrylic acid can not only be shortened with EPEG polymeric monomer, but also reaction process is easier to control, it can be to its reaction process
Carry out adjustment preferably；Secondly, requirement of the EPEG monomer to reaction temperature is very low, when polymerization reaction, it is being higher than 5 DEG C of room temperature
Under the conditions of reaction can be completed, without being heated.Therefore, polycarboxylic acids diminishing is synthesized using the polyethers that EPEG polymeric monomer is representative
Agent will become the development trend of polycarboxylic acids industry in following a period of time.
Patent CN105601827A describes a kind of preparation method of the cement water reducing agent of superelevation water-reducing property, by insatiable hunger
With carboxylic acid monomer A, unsaturated phosphorus acid monomer B, the particular monomers C of UV active and help cause monomer D used in toluene solution
Initiator E obtains active macromolecular F using thermal-initiated polymerization, and polymerization temperature is 60-70 DEG C, polymerization time 7-10h,
Toluene is removed after the completion of polymerization, macromolecular F is obtained, F is add to deionized water dissolution, under the irradiation of ultraviolet light, is added
N-vinyl pyrrolidone (N-DP) and monomer A graft reaction obtain diminishing agent molecule, although this water-reducing agent water-reducing property is big
It is big to be promoted, but its polymerization temperature demand is higher, polymerization time is long, and toluene is used in reaction process, causes process of producing product
Complexity, energy consumption is high, not environmentally.
Patent CN103467671A describes a kind of preparation method of high water reduction polycarboxylate water-reducer, and unsaturated polyether is big
Monomer and unsaturated sulfonic acid class minor comonomer by azo initiator, peroxide initiator and cause promotor as component 1 is added dropwise,
As component 2 is added dropwise, using acrylic acid as component 3 is added dropwise, using molecular weight regulator as dropwise addition component 4.Unsaturated polyether
Polymeric monomer and unsaturated sulfonic acid class minor comonomer and deionized water, put into reactor, stirring heating, when temperature is raised to drop
When heating is spent, component 1-4 is sequentially added drop-wise in reactor, be added dropwise 3-4h, after keep the temperature 0.5-1h, add alkali neutralization, the hair
Bright products obtained therefrom water-reducing rate is high, and guarantor is collapsed, and sustained release performance is good, and reaction process is simple, but the reaction time is long, and reaction temperature is high, energy consumption
Greatly, reaction process is not easy to control.
Patent CN107056993A discloses a kind of environmentally protective high-performance polycarboxylic acids water reducing agent, and synthetic method is that will gather
Ether polymeric monomer A1, unsaturated carboxylic acid or acid anhydrides A2, unsaturated sulfonic acid A3, under the action of reducing agent and molecular weight regulator,
To get high-performance polycarboxylic acids water reducing agent is arrived after pH value, the invention synthetic method is simple, and required temperature is low, and synthetic method letter
Single, required temperature is low, but time for adding is too long, still there is improved space.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of novel polyether synthesis proposed is super
The preparation method of high water reduction type polycarboxylate water-reducer.
To achieve the goals above, present invention employs following technical solutions:
A kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer, comprising the following steps:
S1: polyether macromonomer and deionized water are added in reaction kettle, and stirring dissolves it at normal temperature, are obtained on earth
Liquid, it is spare；A liquid is obtained after unsaturated acids or anhydride minor comonomer are mixed in water, it is spare；By reducing agent, chain-transferring agent with
Water obtains B liquid after being sufficiently mixed, spare；
S2: being added a certain amount of A liquid into polymeric monomer aqueous solution obtained by step S1, stir evenly, and obtains mixture；
S3: being added oxidant into mixture obtained by step S2 in advance, A liquid and B liquid then is added dropwise simultaneously, after being added dropwise
Keep the temperature 0.5h；
S4: lye is added after reaction and neutralizes, product is poured out to get superelevation water reducing type polycarboxylate water-reducer is arrived.
Preferably, novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer is made of following parts by weight material: poly-
250-300 parts of ether polymeric monomer, 200-240 parts of deionized water；1.8-2.8 parts of initiator；50-95 parts of A liquid, 30-45 parts of B liquid；Alkali
10-15 parts of liquid.
Preferably, the reaction in the S1-S4 carries out at normal temperature.
Preferably, the polyether macromonomer in the step S1 is ethylene glycol mono-vinyl polyglycol ether (EPEG, C4 (2+
2) type), structural formula are as follows: CH2=CH-O-R-O- (C2H4O) n-H, molecular weight 1200-4000.
Preferably, A liquid described in S1 is comprised the following components in parts by weight: 30-65 parts of unsaturated acids or anhydride minor comonomer,
20-30 parts of water；The B liquid comprises the following components in parts by weight: 0.6-2 parts of chain-transferring agent, 0.5-2 parts of reducing agent, water 30-40
Part.
Preferably, the minor comonomer of unsaturation acids described in S1 is acrylic acid, methacrylic acid, methylpropene sodium sulfonate, horse
Come acid anhydrides, itaconic acid, styrene sulfonic acid, p styrene sulfonic acid, sodium allylsulfonate, hydroxy-ethyl acrylate, acrylamide, 2- propylene
One of amide -2- methyl propane sulfonic acid, 2- acrylamido myristyl sulfonic acid are a variety of.
Preferably, reducing agent described in S1 be L-AA, sodium bisulphite formaldehyde, sodium sulfite, Sodium Thiosulfate,
One of sodium thiosulfate, sodium hypophosphite, sodium phosphite and frerrous chloride are a variety of；The chain-transferring agent is sulfydryl second
One of acid, mercaptopropionic acid, mercaptobutyric acid are a variety of.
Preferably, the oxidant being added in advance described in S3 is hydrogen peroxide, dibenzoyl peroxide, the tertiary fourth of peroxidating
One of alcohol, tert-butyl hydroperoxide, isopropyl benzene hydroperoxide are a variety of, and the oxidant parts by weight are 3-6 parts.
Preferably, the time for adding of A liquid described in S3 is 30min, and the time for adding of B liquid is 30-50min.
Preferably, lye described in S4 be potassium hydroxide or its aqueous solution, sodium hydroxide or its aqueous solution, sodium carbonate or its
One of aqueous solution is a variety of.
The present invention has the products characteristics such as superelevation diminishing, Self-leveling, adaptable, high-durability；The present invention is using novel poly-
Carboxylic acid water reducer polymeric monomer ethylene glycol mono-vinyl polyglycol ether (EPEG) is as reaction polymeric monomer, with reactivity
Height, synthesized polycarboxylate water-reducer have higher adaptability；Short the time required to reaction, reaction process is easily controllable；Reaction
Required temperature is low, is being higher than 5 DEG C the advantages that can reacting at room temperature.Institute's spent glycol mono-vinyl polyglycol ether (EPEG)
The initiator of polymeric monomer directly reacts generation with ethylene glycol by acetylene, does not generate by-product, and unreacted acetylene is recyclable to be recycled,
With environmental protection, the advantages that low-carbon, sustainable development.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
Embodiment 1
300g ethylene glycol mono-vinyl polyglycol ether polymeric monomer, 220g deionized water, room temperature are added in four-hole boiling flask
Stirring is dissolved to whole, spare.Acrylic acid 49g, methylpropene sodium sulfonate 27g, water 20g are uniformly mixed, A liquid is made, it is spare；
Chain-transferring agent 0.7g, reducing agent 1g, water 32g are uniformly mixed, B liquid is made.A liquid is added into polyether macromonomer solution in advance
24g is added 4g30% content hydrogen peroxide, stirs evenly.A liquid and B liquid are then added dropwise simultaneously, time for adding 30min is added dropwise
30min is kept the temperature after the completion, the sodium hydroxide solution of 12g30% concentration is added, and adjusts PH to 6-7 to get a kind of novel super-high is arrived
Water reducing type water-reducing agent.
Embodiment 2
300g ethylene glycol mono-vinyl polyglycol ether polymeric monomer, 220g deionized water, room temperature are added in four-hole boiling flask
Stirring is dissolved to whole, spare.Acrylic acid 49g, hydroxy-ethyl acrylate 12.3g, water 20g are uniformly mixed, A liquid is made, it is spare；
Reducing agent 0.9g, chain-transferring agent 0.6g, water 32g are uniformly mixed, B liquid is made.A liquid is added into polyether macromonomer solution in advance
12g is added the hydrogen peroxide of 3g30% concentration, stirs evenly.Remaining A liquid and B liquid is added dropwise simultaneously after mixing evenly, A drop adds
Time is 30min, and B liquid time for adding is 40min, and 30min is kept the temperature after being added dropwise to complete, the sodium hydroxide of 12g30% concentration is added
Solution adjusts PH to 6-7 to get a kind of novel super-high water reducing type water-reducing agent is arrived.
Embodiment 3
300g ethylene glycol mono-vinyl polyglycol ether polymeric monomer, 220g deionized water, room temperature are added in four-hole boiling flask
Stirring is dissolved to whole, spare.By acrylic acid 49g, 13.7g acrylamide, 20g water is uniformly mixed, and A liquid is made, spare；It will be also
Former agent 0.8g, chain-transferring agent 0.7g, water 32g are uniformly mixed, and B liquid is made.A liquid is added into polyether macromonomer mixed solution in advance
12.5g is added the hydrogen peroxide of 3g30% concentration, stirs evenly.Remaining A liquid and B liquid are added dropwise simultaneously after mixing evenly, when dropwise addition
Between be 30min, keep the temperature 30min after being added dropwise to complete, the sodium hydroxide solution of 12g30% concentration be added, adjust PH to 6-7 to get
To a kind of novel super-high water reducing type water-reducing agent.
Commercially available room temperature synthetic fluid superelevation water reducing type polycarboxylate water-reducer.
Performance test
1. flowing degree of net paste of cement
According to GB/T8077-2000 " concrete admixture homogeneity test method ", its net slurry is measured using reference cement
Fluidity, test condition W/C=0.29, it is 0.14% that water-reducing agent, which rolls over solid volume, and concrete performance test is according to GB 8076-
2008 " concrete admixtures " carry out.Select Beijing Jinyu cement (P.O42.5) detection concrete slump/divergence measurement knot
Fruit is as shown in Table 1:
Table one: the cement paste fluidity measuring result of embodiment 1-3 and comparative example
As can be seen from Table I, the water-reducing agent for the superelevation water reducing type polycarboxylate water-reducer that the present invention is synthesized using novel polyether
It is dispersed and slump-retaining equally matched with commercially available liquid superelevation water reducing type polycarboxylate water-reducer in addition it is excellent with it is commercially available
Superelevation water reducing type polycarboxylate water-reducer.And on raw material, the present invention is poly- using novel polyether polymeric monomer ethylene glycol mono-vinyl
Glycol ether, EPEG novel polyether not only have reactivity high, and reaction required time is short, can synthesize under higher than 5 DEG C environment
The advantages that, and the initiator of EPEG type polyethers directly reacts generation by acetylene gas and ethylene glycol, without extra by-product,
After completion of the reaction, extra acetylene can be recycled and be utilized again, not will cause environmental pollution, significant excellent with sustainable development
Point.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer, which is characterized in that including following step
It is rapid:
S1: polyether macromonomer and deionized water are added in reaction kettle, and stirring dissolves it at normal temperature, obtains liquid on earth, standby
With；A liquid is obtained after unsaturated acids or anhydride minor comonomer are mixed in water, it is spare；Reducing agent, chain-transferring agent and water is abundant
B liquid is obtained after mixing, it is spare；
S2: being added a certain amount of A liquid into polymeric monomer aqueous solution obtained by step S1, stir evenly, and obtains mixture；
S3: being added oxidant into mixture obtained by step S2 in advance, and A liquid and B liquid then is added dropwise simultaneously, keeps the temperature after being added dropwise
0.5h；
S4: lye is added after reaction and neutralizes, product is poured out to get superelevation water reducing type polycarboxylate water-reducer is arrived.
2. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer is made of following parts by weight material: the big list of polyethers
250-300 parts of body, 200-240 parts of deionized water, 1.8-2.8 parts of initiator, 50-95 parts of A liquid, 30-45 parts of B liquid, lye 10-15
Part.
3. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: the reaction in the S1-S4 carries out at normal temperature.
4. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: the polyether macromonomer in the step S1 is ethylene glycol mono-vinyl polyglycol ether, structural formula are as follows: CH2=CH-
O-R-O- (C2H4O) n-H, molecular weight 1200-4000.
5. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: A liquid described in S1 is comprised the following components in parts by weight: unsaturated acids or 30-65 parts of anhydride minor comonomer, water 20-
30 parts；The B liquid comprises the following components in parts by weight: 0.6-2 parts of chain-transferring agent, 0.5-2 parts of reducing agent, 30-40 parts of water.
6. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: the minor comonomer of unsaturation acids described in S1 be acrylic acid, methacrylic acid, methylpropene sodium sulfonate, maleic anhydride,
Itaconic acid, styrene sulfonic acid, p styrene sulfonic acid, sodium allylsulfonate, hydroxy-ethyl acrylate, acrylamide, 2- acrylamide -2-
One of methyl propane sulfonic acid, 2- acrylamido myristyl sulfonic acid are a variety of.
7. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: reducing agent described in S1 is L-AA, sodium bisulphite formaldehyde, sodium sulfite, Sodium Thiosulfate, thio sulphur
One of sour sodium, sodium hypophosphite, sodium phosphite and frerrous chloride are a variety of；The chain-transferring agent is thioacetic acid, sulfydryl
One of propionic acid, mercaptobutyric acid are a variety of.
8. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: the oxidant being added in advance described in S3 is hydrogen peroxide, dibenzoyl peroxide, tertbutanol peroxide, tertiary fourth
One of base hydrogen peroxide, isopropyl benzene hydroperoxide are a variety of, and the oxidant parts by weight are 3-6 parts.
9. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: the time for adding of A liquid described in S3 is 30min, and the time for adding of B liquid is 30-50min.
10. a kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer according to claim 1,
Be characterized in that: lye described in S4 is potassium hydroxide or its aqueous solution, sodium hydroxide or its aqueous solution, sodium carbonate or its aqueous solution
One of or it is a variety of.
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| CN110591015A (en) * | 2019-09-29 | 2019-12-20 | 贵州石博士科技有限公司 | Polycarboxylate superplasticizer and method for rapidly synthesizing same at normal temperature |
| CN111393584A (en) * | 2020-03-26 | 2020-07-10 | 山西佳维新材料股份有限公司 | Polycarboxylate superplasticizer and preparation method and application thereof |
| CN111704413A (en) * | 2020-06-24 | 2020-09-25 | 南宁市嘉大混凝土有限公司 | Concrete prepared from waste slurry of concrete mixing plant |
| CN111777725A (en) * | 2020-08-05 | 2020-10-16 | 四川鸿鹏新材料有限公司 | Synthesis method of diethylene glycol monovinyl polyether water reducer |
| CN111909323A (en) * | 2019-05-10 | 2020-11-10 | 亚泰集团沈阳现代建筑工业有限公司 | Normal-temperature synthesis method of polycarboxylate superplasticizer |
| CN111995717A (en) * | 2020-08-20 | 2020-11-27 | 安徽海螺新材料科技有限公司 | High-performance polycarboxylate superplasticizer, preparation method thereof and concrete |
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| CN112708063A (en) * | 2020-12-08 | 2021-04-27 | 科之杰新材料集团有限公司 | Reducing agent for improving monomer conversion rate, preparation method thereof and redox method for preparing polycarboxylic acid with high monomer conversion rate |
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| CN114716621A (en) * | 2022-03-09 | 2022-07-08 | 陕西友邦新材料科技有限公司 | Normal-temperature six-carbon comprehensive polycarboxylate superplasticizer mother liquor and preparation method thereof |
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| CN115260406A (en) * | 2022-07-22 | 2022-11-01 | 佛山市华轩新材料有限公司 | Method for synthesizing polycarboxylate superplasticizer at normal temperature by compositely dropwise adding multiple chain transfer agents |
| CN116333231A (en) * | 2023-05-25 | 2023-06-27 | 中建材中岩科技有限公司 | Ultra-high dispersion type water reducer and preparation method thereof |
| CN116333231B (en) * | 2023-05-25 | 2023-08-18 | 中建材中岩科技有限公司 | Ultra-high dispersion type water reducer and preparation method thereof |
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Application publication date: 20190503 |