CN109705283A - A kind of slow-setting polycarboxylic acid water reducing agent and preparation method thereof - Google Patents

A kind of slow-setting polycarboxylic acid water reducing agent and preparation method thereof Download PDF

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Publication number
CN109705283A
CN109705283A CN201910031929.3A CN201910031929A CN109705283A CN 109705283 A CN109705283 A CN 109705283A CN 201910031929 A CN201910031929 A CN 201910031929A CN 109705283 A CN109705283 A CN 109705283A
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reducing agent
slow
polycarboxylic acid
water reducing
acid water
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CN109705283B (en
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李芳�
杨秀芳
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Xiamen R & B Sunstone Building Materials Technology Co Ltd
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Xiamen R & B Sunstone Building Materials Technology Co Ltd
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Abstract

The invention belongs to water-reducing agent field, a kind of slow-setting polycarboxylic acid water reducing agent and preparation method thereof is specifically disclosed.The slow-setting polycarboxylic acid water reducing agent is prepared by following components in percentage by weight: unsaturated polyether 20%~45%, unsaturated acids 2%~6%, sodium p styrene sulfonate 0.9%~10%, organic phosphoric acid 0.5%~2%, oxidant 0.2%~1%, reducing agent 0.05%~0.2%, chain-transferring agent 0.1%~0.5%, surplus are water.The slow-setting polycarboxylic acid water reducing agent has water-reducing rate high, and retarding effect is good, and all has well adapting to property with the cement of different cultivars, will not generate side effect because of the kind of cement difference.In addition, the slow-setting polycarboxylic acid water reducing agent has preferable anti-corrosion effect, summer polycarboxylate water-reducer phenomena such as corruption, be layered, be smelly will not occur because standing time is too long.

Description

A kind of slow-setting polycarboxylic acid water reducing agent and preparation method thereof
Technical field
The invention belongs to water-reducing agent field, a kind of slow-setting polycarboxylic acid water reducing agent and preparation method thereof is specifically disclosed.
Background technique
Retarding water reducer is a kind of additive being of wide application in concrete admixture, it is to have slow setting and big concurrently The additive of amplitude reduction mixing water amount.As capital construction development proposes more to the performance of concrete and higher wants It asks, to concrete admixture, higher requirements are also raised.
High-performance polycarboxylic acids water reducing agent has water-reducing rate high, and to the good dispersion of cement, concrete slump loss is small Advantage.But the retarding effect of polycarboxylate water-reducer itself is weaker, it is necessary to by reaching with compounding for retarder State effect.Although compounded technology can solve subproblem, but by the limitation solved the problems, such as is compounded, but also water-reducing agent Original water-reducing property is made that sacrifice, and the retarder being additionally added also increases cost.In addition, the water-reducing agent of compounding retarder Solution be also possible that layering, precipitating, corruption, it is smelly phenomena such as, the stability of properties of product makes people worried.Therefore, it is badly in need of out Sending out a kind of, water-reducing rate is high, retarding effect is obvious, properties of product are stable and also very ideal to the late-enhancement effect of concrete High-performance water reducing agent.
Summary of the invention
The purpose of the invention is to overcome existing polycarboxylate water-reducer presence that cannot take into account two aspect of diminishing and slow setting And the defect that will affect the performance of water-reducing agent is compounded with existing retarder, and diminishing and slow setting can be combined by providing one kind Polycarboxylate water-reducer and preparation method thereof.
Specifically, the present invention provides a kind of slow-setting polycarboxylic acid water reducing agents, wherein by following components in percentage by weight It is prepared:
Preferably, the slow-setting polycarboxylic acid water reducing agent is prepared by following components in percentage by weight:
Preferably, the unsaturated polyether is isobutenyl polyoxyethylene ether.
Preferably, the number-average molecular weight of the unsaturated polyether is 600-3000, more preferably 2400-3000.
Preferably, the unsaturated acids is acrylic acid and/or methacrylic acid.
Preferably, the organic phospho acid is 1-hydroxy ethylidene-1,1-diphosphonic acid and/or aminotrimethylenephosphonic acid.
Preferably, the oxidant is potassium peroxydisulfate and/or ammonium persulfate.
Preferably, the reducing agent is ascorbic acid and/or tartaric acid.
Preferably, the chain-transferring agent is thioacetic acid and/or mercaptopropionic acid.
The present invention also provides the preparation methods of the slow-setting polycarboxylic acid water reducing agent, method includes the following steps:
(1) sodium p styrene sulfonate and unsaturated acids are configured to the aqueous solution that concentration is 45~55wt%, are denoted as First solution, and the reducing agent and chain-transferring agent are configured to the aqueous solution that concentration is 3~10wt%, it is denoted as the second solution;
(2) unsaturated polyether is configured to the aqueous solution that concentration is 35~45wt%, the oxidant is added, later First solution and the second solution is added dropwise simultaneously again, the organic phosphoric acid is added after completion of dropwise addition, the reaction was continued 0.5~2h, A certain amount of water is supplemented after reaction obtains the slow-setting polycarboxylic acid water reducing agent solution that concentration is 40wt%.
Preferably, the total time that first solution and the second solution is added dropwise controls in 2~3h.
In addition, the present invention also provides slow-setting polycarboxylic acid water reducing agents prepared by the above method.
Key point of the invention is by unsaturated polyether, unsaturated acids, sodium p styrene sulfonate and organic phosphoric acid with specific Dosage be used cooperatively, in particular improve the dosage of sodium p styrene sulfonate, have the beneficial effect that:
(1) slow-setting polycarboxylic acid water reducing agent has water-reducing rate high, and retarding effect is good, and equal with the cement of different cultivars With well adapting to property, side effect will not be generated because of the kind of cement difference;
(2) slow-setting polycarboxylic acid water reducing agent has preferable anti-corrosion effect, and summer polycarboxylate water-reducer will not be because putting It sets overlong time and phenomena such as corruption, be layered, be smelly occurs.
(3) preparation process of the slow-setting polycarboxylic acid water reducing agent is simple, and reaction carries out at normal temperature, whole process temperature Without control, the reaction time is short, and low energy consumption, and safety coefficient is high, pollution-free, easy to industrialized production.
Specific embodiment
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to Cross the conventional products of commercially available acquisition.
Embodiment 1
Raw material: it is shown in Table 1.
Preparation process is as follows:
(1) sodium p styrene sulfonate and unsaturated acids are configured to the aqueous solution that concentration is 50wt%, are denoted as the first solution, And reducing agent and chain-transferring agent are configured to the aqueous solution that concentration is 5.5wt%, it is denoted as the second solution;
(2) unsaturated polyether is configured to the aqueous solution that concentration is 40wt%, oxidant is added, be added dropwise the simultaneously again later One solution and the second solution will simultaneously be added dropwise total time control and organic phosphoric acid is added after 2~3h, completion of dropwise addition, the reaction was continued 1h. A certain amount of water is supplemented after reaction obtains the slow-setting polycarboxylic acid water reducing agent solution that concentration is 40wt%.
Embodiment 2
Raw material: it is shown in Table 1.
Preparation method is same as Example 1.
Embodiment 3
Raw material: it is shown in Table 1.
Preparation method is same as Example 1.
Embodiment 4
Raw material: it is shown in Table 1.
Preparation method is same as Example 1.
Embodiment 5
Raw material: it is shown in Table 1.
Preparation method is same as Example 1.
Comparative example 1
Raw material: the difference from example 2 is that the dosage of sodium p styrene sulfonate is reduced to 0.5wt%, specifically it is shown in Table 1.
Preparation method is same as Example 1.
Comparative example 2
Raw material: the difference from example 2 is that organic phosphoric acid is not added, specifically it is shown in Table 1.
Preparation method is same as Example 1.
Component list (unit: parts by weight) used in each embodiment of table 1
Compliance test result
(1) it uses conch P.O42.5 cement, build II 42.5 cement of good fortune P.O42.5 cement and Fujian good fortune P., test determines same The paste flowing degree of each embodiment and comparative example under volume.According to GB/T8077-2012, " concrete admixture is homogeneous for test Property test method " carry out, W/C=2.9, cement 300g, water 87g, admixture dosage is to roll over solid volume.Test result is shown in Table 2.
The paste flowing degree results of property of the different water-reducing agent types of table 2
From table 2 it can be seen that in different cement, the cement paste of the 1h of the slow-setting polycarboxylic acid water reducing agent in embodiment Fluidity loss is small compared with comparative example.
(2) concrete test
Using first, the whole setting time of Fujian good fortune cement and conch cement test concrete, test according to GB/T50080- 2002 " concrete mixture characteristic test method standards " carry out.Concrete design class is C30, and concrete mix is water Mud: water: sand: stone: flyash: miberal powder=258:170:815:996:41:41 (weight ratio), water-reducing agent volume are that folding is mixed admittedly Amount, in terms of glue material (concrete and coal ash+miberal powder) quality.Test result is shown in Table 3.
3 concrete coagulating time of table and compression strength table (20 DEG C of test temperature)
Upper table data show, retarding water reducer provided by the invention not only water-reducing rate with higher, but also can be with Extend the setting time of concrete, and its concrete seven day, 28 days compression strength can satisfy construction requirement.
(4) anti-corrosion effect:
It is 1 that 2 three kinds of embodiment 4, comparative example 1 and comparative example samples, which are individually positioned in number,#、2#、3#Three tools fill in examination It in pipe and is stored in laboratory (30 DEG C of room temperature), finds 2 after one month#There is a slight flocculent deposit, 1#、3#It is unchanged.Two months Afterwards it has been observed that 2#There is stink, have an apparent flocculent deposit, and 1#With 3#Sample in the two test tubes is unchanged.Thus may be used Know, organic phosphoric acid, which is added, can slow down or prevent the corruption of water-reducing agent, go bad.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (10)

1. a kind of slow-setting polycarboxylic acid water reducing agent, which is characterized in that be prepared by following components in percentage by weight:
2. slow-setting polycarboxylic acid water reducing agent according to claim 1, which is characterized in that by following components in percentage by weight It is prepared:
3. slow-setting polycarboxylic acid water reducing agent according to claim 1 or 2, which is characterized in that the unsaturated polyether is different Cyclobutenyl polyoxyethylene ether.
4. slow-setting polycarboxylic acid water reducing agent according to claim 1 or 2, which is characterized in that the number of the unsaturated polyether Average molecular weight is 600-3000, more preferably 2400-3000.
5. slow-setting polycarboxylic acid water reducing agent according to claim 1 or 2, which is characterized in that the unsaturated acids is propylene Acid and/or methacrylic acid.
6. slow-setting polycarboxylic acid water reducing agent according to claim 1 or 2, which is characterized in that the organic phospho acid is hydroxyl Ethylene-diphosphonic acid and/or aminotrimethylenephosphonic acid.
7. slow-setting polycarboxylic acid water reducing agent according to claim 1 or 2, which is characterized in that the oxidant is persulfuric acid Potassium and/or ammonium persulfate;The reducing agent is ascorbic acid and/or tartaric acid;The chain-transferring agent is thioacetic acid and/or mercapto Base propionic acid.
8. the preparation method of slow-setting polycarboxylic acid water reducing agent described in any one of claim 1-7, which is characterized in that the party Method the following steps are included:
(1) sodium p styrene sulfonate and unsaturated acids are configured to the aqueous solution that concentration is 45~55wt%, are denoted as first Solution, and the reducing agent and chain-transferring agent are configured to the aqueous solution that concentration is 3~10wt%, it is denoted as the second solution;
(2) unsaturated polyether is configured to the aqueous solution that concentration is 35~45wt%, the oxidant is added, it is same again later When first solution and the second solution is added dropwise, the organic phosphoric acid is added after completion of dropwise addition, the reaction was continued 0.5~2h, reaction After supplement a certain amount of water obtain concentration be 40wt% slow-setting polycarboxylic acid water reducing agent solution.
9. the preparation method of slow-setting polycarboxylic acid water reducing agent according to claim 8, which is characterized in that be added dropwise described first The total time of solution and the second solution controls in 2~3h.
10. the slow-setting polycarboxylic acid water reducing agent that the method as described in claim 8 or 9 is prepared.
CN201910031929.3A 2019-01-14 2019-01-14 Retarding polycarboxylate superplasticizer and preparation method thereof Active CN109705283B (en)

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