CN104448156B - A kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer - Google Patents

A kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer Download PDF

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CN104448156B
CN104448156B CN201410673602.3A CN201410673602A CN104448156B CN 104448156 B CN104448156 B CN 104448156B CN 201410673602 A CN201410673602 A CN 201410673602A CN 104448156 B CN104448156 B CN 104448156B
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solution
room temperature
water reducer
polycarboxylic acid
parts
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CN104448156A (en
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王浩雨
马丽涛
刘纪伟
杨道顺
李宁
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Anhui Xin Solid Environmental Co Ltd
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Anhui Xin Solid Environmental Co Ltd
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Abstract

The present invention relates to additive for building material technical field, more particularly, to a kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer.This method is using methyl allyl polyoxyethylene ether, acrylic acid as reaction monomers, the redox system set up by oxidants hydrogen peroxide, reducing agent rongalite, and specific synthetic method is:Using methyl allyl polyoxyethylene ether, hydrogen peroxide and deionized water as bottom liquid, the water solution A and rongalite aqueous solution B of acrylic acid and chain-transferring agent is added dropwise, Raolical polymerizable is carried out at room temperature.This method can be synthesized at room temperature, and energy consumption is small, economic and environment-friendly.Preparation technology of the present invention is simple, and the water reducer of synthesis has high water reducing rate, and fluidity, function of slump protection are good.

Description

A kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer
Technical field
The present invention relates to additive for building material technical field, more particularly, to a kind of room temperature of high-efficiency polycarboxylic acid water reducer Preparation method.
Background technology
With the development of building trade, the requirement in engineer applied to water reducer is stepped up.Grew up in recent years Poly carboxylic acid series water reducer is known as after the first generation water reducer using calcium lignosulfonate as representative and using naphthalene system as the second of representative both at home and abroad For the third generation high-performance water reducing agent grown up after water reducer.Polycarboxylate water-reducer because its water-reducing rate is high, adaptability compared with Good the advantages of, great popularization and application are obtained.
Chinese patent(CN103275280A)A kind of normal temperature synthesis method of polyocarboxy acid type high-thin arch dam water reducer is disclosed, is led to Unsaturated polyether, unsaturated carboxylic acid are crossed for raw material, by the foundation of redox system, polyocarboxy acid type diminishing has been synthesized at room temperature Agent, but the conversion ratio of this method product is low, and the reaction time is long.Therefore, seek it is a kind of at room temperature can synthesize, technique is simple Controllable and efficiently high-efficiency polycarboxylic acid water reducer preparation method is extremely urgent.
The content of the invention
In view of the above-mentioned problems, the invention provides a kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer, this water reducer It can synthesize at room temperature, short the time required to reaction, products obtained therefrom water-reducing rate is high, function of slump protection is good, properties of product are stable.
The technical scheme is that:
The invention provides a kind of room temperature preparation method of high-efficiency polycarboxylic acid water reducer, reaction monomers pass through radical polymerization Carry out according to the following steps:
A. monomer methyl allyl polyoxyethylene ether, the hydrogen peroxide of oxidant 30% and deionized water are put into as bed material In reactor, stirring is to being completely dissolved;
B. configured in advance good solution A and solution B are added dropwise simultaneously after bed material dissolving, solution A was added dropwise to complete through 1 hour, molten Liquid B was added dropwise to complete through 1.5 hours, after solution B completion of dropwise addition, continued stirring reaction 30 minutes;
C. it is 6-7 the liquid caustic soda that above-mentioned mixed solution is 32% with mass concentration to be adjusted into pH value, rear to continue to stir 20 minutes, Produce described high-efficiency polycarboxylic acid water reducer;
Described solution A is monomeric acrylic, the thin base propionic acid of chain-transferring agent and deionized water;
Described solution B is reducing agent rongalite and deionized water.
Described radical polymerization system is composed of the following raw materials by weight:Methyl allyl polyoxyethylene ether 280-330, 30% hydrogen peroxide(30%H2O2)2.5-4.5 part, acrylic acid(AA)40-52 parts, dredge base propionic acid 1.2-2.0, rongalite 1.2-2;
The deionized water quality is 1.5-2.5 times of each raw material gross mass.
The molecular weight of described methyl allyl polyoxyethylene ether is 2000-2400.
Described liquid caustic soda is sodium hydrate aqueous solution.
30% described hydrogen peroxide is the aqueous hydrogen peroxide solution that mass concentration is 30%.
The present invention triggers radical polymerization, reaction is carried out at room temperature, formaldehyde by using redox system Sodium bisulphite has strong reducing property, can prevent hydroxyl excessive in water reducer from causing cement to be adsorbed by moment, improves coagulation The slump holding capacity of soil, by adjusting proportion relation of the oxidant with reducing agent, determines each monomer consumption, improves conversion Rate, prevents the waste of raw material and is effectively controlled the generation of high temperature side reaction.The water reducer has high water reducing rate, function of slump protection It is good, it is applied widely, it is adapted to industrialization large-scale production.
Advantages of the present invention and beneficial effect:
1. the present invention is by the foundation of redox system, strong reducing property rongalite is added, is at room temperature It can be synthesized, energy consumption is small, it is economic and environment-friendly.
2. preparation technology of the present invention is simple, the water reducer of synthesis has high water reducing rate, and fluidity, function of slump protection are good.
Embodiment
Below by embodiment, the present invention will be further elaborated, and the description below is only for explaining the present invention, not Its content is defined.
Embodiment 1
A kind of high-efficiency polycarboxylic acid water reducer, is made up of the raw material of following parts by weight:
Bed material:Methyl allyl polyoxyethylene ether:280、30%H2O2:2.6th, deionized water:280;
Solution A:AA:40th, base propionic acid is dredged:1.2nd, deionized water:65;
Solution B:Rongalite:1.25, deionized water:165.
A kind of preparation method of high-efficiency polycarboxylic acid water reducer:Under room temperature condition, solution A, time for adding are added dropwise into bottom liquid For 1 hour, while solution B is added dropwise into bottom liquid, time for adding was 1.5 hours;After being added dropwise to complete, insulation continues to react 30 points Clock, the sodium hydrate aqueous solution regulation pH value that the mass concentration for then adding 22-30 parts by weight is 32% is 6-7, continues to stir 20 Minute, both the heavy duty detergent polycarboxylate water-reducer.
Embodiment 2
A kind of high-efficiency polycarboxylic acid water reducer, is made up of the raw material of following parts by weight:
Bed material:Methyl allyl polyoxyethylene ether:293、30%H2O2:3.0th, deionized water:300;
Solution A:AA:43.5th, base propionic acid is dredged:1.45, deionized water:75;
Solution B:Rongalite:1.5th, deionized water:170.
A kind of preparation method of high-efficiency polycarboxylic acid water reducer:Under room temperature condition, solution A, time for adding are added dropwise into bottom liquid For 1 hour, while solution B is added dropwise into bottom liquid, time for adding was 1.5 hours;After being added dropwise to complete, insulation continues to react 30 points Clock, the sodium hydrate aqueous solution regulation pH value that the mass concentration for then adding 22-30 parts by weight is 32% is 6-7, continues to stir 20 Minute, both the heavy duty detergent polycarboxylate water-reducer.
Embodiment 3
A kind of high-efficiency polycarboxylic acid water reducer, is made up of the raw material of following parts by weight:
Bed material:Methyl allyl polyoxyethylene ether:306、30%H2O2:3.56, deionized water:315;
Solution A:AA:46.8th, base propionic acid is dredged:1.7th, deionized water:88;
Solution B:Rongalite:1.63, deionized water:182.
A kind of preparation method of high-efficiency polycarboxylic acid water reducer:Under room temperature condition, solution A, time for adding are added dropwise into bottom liquid For 1 hour, while solution B is added dropwise into bottom liquid, time for adding was 1.5 hours;After being added dropwise to complete, insulation continues to react 30 points Clock, the sodium hydrate aqueous solution regulation pH value that the mass concentration for then adding 22-30 parts by weight is 32% is 6-7, continues to stir 20 Minute, both the heavy duty detergent polycarboxylate water-reducer.
Embodiment 4
A kind of high-efficiency polycarboxylic acid water reducer, is made up of the raw material of following parts by weight:
Bed material:Methyl allyl polyoxyethylene ether:319、30%H2O2:4.2nd, deionized water:335;
Solution A:AA:49.2nd, base propionic acid is dredged:1.85, deionized water:95;
Solution B:Rongalite:1.79, deionized water:200.
A kind of preparation method of high-efficiency polycarboxylic acid water reducer:Under room temperature condition, solution A, time for adding are added dropwise into bottom liquid For 1 hour, while solution B is added dropwise into bottom liquid, time for adding was 1.5 hours;After being added dropwise to complete, insulation continues to react 30 points Clock, the sodium hydrate aqueous solution regulation pH value that the mass concentration for then adding 22-30 parts by weight is 32% is 6-7, continues to stir 20 Minute, both the heavy duty detergent polycarboxylate water-reducer.
Embodiment 5
A kind of high-efficiency polycarboxylic acid water reducer, is made up of the raw material of following parts by weight:
Bed material:Methyl allyl polyoxyethylene ether:330、30%H2O2:4.45, deionized water:350;
Solution A:AA:52nd, base propionic acid is dredged:1.9th, deionized water:110;
Solution B:Rongalite:2.0th, deionized water:210.
A kind of preparation method of high-efficiency polycarboxylic acid water reducer:Under room temperature condition, solution A, time for adding are added dropwise into bottom liquid For 1 hour, while solution B is added dropwise into bottom liquid, time for adding was 1.5 hours;After being added dropwise to complete, insulation continues to react 30 points Clock, it is 6-7 then to add the sodium hydrate aqueous solution regulation pH value that mass concentration is 32%, continues to stir 20 minutes, had both obtained described Heavy duty detergent polycarboxylate water-reducer.
Comparative example 1:The polycarboxylate water-reducer is using ferrous sulfate as reducing agent, and other step be the same as Examples 3 are identical.
Comparative example 2:Contrast product is commercially available polycarboxylate water-reducer
Found through Experimental Comparison, the reaction time needed for comparative example 1 than the present invention long 3 hours or so, product income rate is low.
Application Example
Using reference cement, according to《Concrete admixture》(GB8076-2008)In test request, compare the present invention The high-efficiency polycarboxylic acid water reducer of preparation(Embodiment 1-5)With comparative example 1, the water-reducing rate of comparative example 2, fluidity, the slump, as a result It is shown in Table 1.
Table 1
As can be seen from the table, the high-efficiency polycarboxylic acid water reducer for preparing of the present invention has that fluidity is big, water-reducing rate is high, and guarantor is collapsed The excellent feature of performance.
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by embodiment System, other any Spirit Essences and the change made under principle, modifications without departing from the present invention, combines, substitutes, simplifying and should be Equivalence replacement mode, is included within protection scope of the present invention.

Claims (3)

1. the room temperature preparation method of a kind of high-efficiency polycarboxylic acid water reducer, it is characterised in that by radical polymerization according to the following steps Carry out:
A. monomer methyl allyl polyoxyethylene ether, the hydrogen peroxide of oxidant 30% and deionized water are put into as bed material and reacted In kettle, stirring is to being completely dissolved;
B. configured in advance good solution A and solution B are added dropwise simultaneously after bed material dissolving, solution A was added dropwise to complete through 1 hour, solution B warp It is added dropwise to complete within 1.5 hours, after solution B completion of dropwise addition, continues stirring reaction 30 minutes;
C. it is 6-7 the liquid caustic soda that above-mentioned mixed solution is 32% with mass concentration to be adjusted into pH value, rear to continue to stir 20 minutes, is produced Described high-efficiency polycarboxylic acid water reducer;
Described solution A is monomeric acrylic, the thin base propionic acid of chain-transferring agent and deionized water;
Described solution B is reducing agent rongalite and deionized water;
Described radical polymerization system is made up of the raw material of following parts by weight:280-330 parts of methyl allyl polyoxyethylene ether, 30% 2.5-4.5 parts of hydrogen peroxide, 40-52 parts of acrylic acid, thin 1.2-2.0 parts of base propionic acid, 1.2-2 parts of rongalite;
The deionized water quality is 1.5-2.5 times of each raw material gross mass.
2. the room temperature preparation method of high-efficiency polycarboxylic acid water reducer according to claim 1, it is characterised in that:Described methyl The molecular weight of allyl polyethenoxy ether is 2000-2400.
3. the room temperature preparation method of high-efficiency polycarboxylic acid water reducer according to claim 1, it is characterised in that:Described liquid caustic soda For sodium hydrate aqueous solution.
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CN105037648B (en) * 2015-08-25 2019-01-15 科之杰新材料集团有限公司 It is a kind of to protect collapse water reducing type polycarboxylate water-reducer and its low-temperature rapid preparation method
CN105330193B (en) * 2015-11-24 2017-12-26 同济大学 Nuclear power ultra dense real concrete polycarboxylate water-reducer and preparation method thereof
CN105542091B (en) * 2015-12-16 2019-02-01 广东复特新型材料科技有限公司 A kind of anti-mud polycarboxylate high performance water-reducing agent of sustained release cationic and preparation method thereof
CN105418856B (en) * 2015-12-18 2017-10-24 中建商品混凝土有限公司 A kind of wide temperature range of normal temperature synthesizes the preparation method of polycarboxylate water-reducer
CN105524230B (en) * 2015-12-24 2018-07-06 湖南铭煌科技发展有限公司 A kind of preparation method of high-efficiency water-reducing agent of poly-carboxylic acid
CN105622862A (en) * 2015-12-28 2016-06-01 沈阳华盈环保材料有限公司 Concrete polycarboxylate water reducing agent and preparing method thereof
CN106380552A (en) * 2016-09-29 2017-02-08 湖北工业大学 High-adaptability polycarboxylic acid water reducing agent master batch
CN106632742A (en) * 2016-12-30 2017-05-10 长沙加美乐素化工有限公司 Composite activator system and method for preparing concrete water-reducing admixture from same
CN108586674A (en) * 2018-05-18 2018-09-28 萧县沃德化工科技有限公司 A method of preparing polycarboxylate water-reducer using itaconic acid waste liquid
CN108585595A (en) * 2018-06-26 2018-09-28 云南圣比奥建材有限公司 High performance water reducing agent of polyocarboxy acid and preparation method thereof
CN109336448B (en) * 2018-12-07 2021-07-13 临沂海螺新材料科技有限公司 Liquid cement chromium-removing grinding aid and preparation method thereof
CN113072317A (en) * 2021-02-24 2021-07-06 山西佳维新材料股份有限公司 Polycarboxylate superplasticizer and preparation method and application thereof

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