CN103011677A - Intermediate-acting water reducing agent with functions of plastic retaining and coagulation adjustment and preparation method - Google Patents

Intermediate-acting water reducing agent with functions of plastic retaining and coagulation adjustment and preparation method Download PDF

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CN103011677A
CN103011677A CN2012105448161A CN201210544816A CN103011677A CN 103011677 A CN103011677 A CN 103011677A CN 2012105448161 A CN2012105448161 A CN 2012105448161A CN 201210544816 A CN201210544816 A CN 201210544816A CN 103011677 A CN103011677 A CN 103011677A
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temperature
reaction
add
water
concrete
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黄靖
黎春海
张鸿毓
原衷旭
李斌
王毅
张环宇
李树志
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TIANJIN RESEARCH INSTITUTE OF BUILDING SCIENCE Co Ltd
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TIANJIN RESEARCH INSTITUTE OF BUILDING SCIENCE Co Ltd
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Abstract

The invention discloses an intermediate-acting water reducing agent with functions of plastic retaining and coagulation adjustment and a preparation method. The preparation method comprises the following steps of: (1) putting a catalyst in a container, adding water for dissolving, adding plant fiber powder to uniformly mix; raising the temperature to react for 0.5-1 hour; raising the temperature to 70-90 DEG C to react for 0.5-1.5 hours; (2) heating the mixture and instantly reducing the temperature after the color of the mixture is from brown to be transparent; (3) reducing the temperature to 80-90 DEG C to regulate a pH value to be between 11 and 12, controlling the temperature to be between 90 and 95 DEG C to preserve the temperature and react for 2-4 hours; and (4) reducing the temperature to 50-60 DEG C, adjusting a pH value to be between 9 and 10, and adding an air entraining agent to uniformly stir, react and cool. Natural raw materials are used, so that the toxicity and the pollution are avoided in the production process and the use process, corrosion of reinforcing steel bars is avoided, and the production process is simple and low in cost. For concrete, the intermediate-acting water reducing agent is high in dispersion action upon cement particles and active material particles, the water reducing ratio is up to 8-18 percent, and concrete has the effects of delayed coagulation, plastic retaining and air entraining.

Description

A kind of guarantor moulds and transfers solidifying middle effect water reducer and preparation method
Technical field
The invention belongs to technical field of concrete additives, relate to a kind of concrete admixture, be specifically related to a kind of guarantor and mould the preparation method who transfers solidifying middle effect water reducer.
Background technology
In nineteen thirty-five, the first water reducer came out time of seven more than ten years so far, water reducer was being played the part of important role always in concrete field.The main component of water reducer is exactly tensio-active agent, why it has the diminishing function is because the oriented adsorption of tensio-active agent, make on the cement particle surface electric charge with same-sign, so under the effect of electrical repulsion, make cement add the formed flocculence structure dispersion disintegration of water initial stage, free-water in the flocculence aggregate is discharged, thereby reach the purpose of diminishing.Dissimilar tensio-active agents is being of quite diverse character because molecular structure is different, common are hydroxyl, carboxylic acid and carboxylate group, sulfonic group, hydroxycarboxylate.The oh type tensio-active agent can oriented adsorption in mixture in cement particle surface, be easy to associate with the hydrogen bond form with water molecules, the reactive force of this association is far longer than the gravitation between water molecules and cement granules, after cement has adsorbed enough tensio-active agents, its surface can form the stable solvation moisture film of one deck, stop the direct contact between cement granules, played lubrication, thereby improved the workability of concrete mix.The tensio-active agent of sulfonate type is typical aniorfic surfactant.Owing at aquation initial stage cement particle surface band positive charge, be conducive to the absorption of anion surfactant, thereby cause the effect that delays hydrated reaction of cement.Simultaneously, the sorptive power of tensio-active agent reduces interfacial free energy, changes the wettability of solid, also can improve the workability of mixture.
Along with the develop rapidly of Building technology, the kind of water reducer is also in continuous increase, and high efficiency water reducing agent has naphthalene system, anthracene system and the efficient water reducer such as melamine resin type and polycarboxylic acid series, and is wherein maximum with naphthalene water reducer output; Ordinary water-reducing agent is then take calcium lignin sulphonate as main products.From last century the seventies apply water reducer to the nineties, basically it is the epoch take ordinary water-reducing agent as main body, although the output of high efficiency water reducing agent and application significantly improved in recent years, but because its price is higher, be subject to certain restriction in application, ordinary water-reducing agent still occupies the very large market share.Wherein wooden calcium is because its price is low, volume is little, and is good with the composite effect of admixture, and usage quantity is maximum.
21st century, environmental issue is extensively paid close attention to by people.Requirement for environmental protection, paper technology will progressively change, this will directly have influence on spent pulping liquor---produce the required raw-material supply problem of wooden calcium, thereby supply falls short of demand to cause market, and wooden calcium also comes with some shortcomings on some performance, in recent years, the adaptability problem of itself and cement is more and more outstanding, therefore must develop a kind of performance better in the usefulness water reducer with the needs of satisfying the market.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of employing natural matter is provided, production process is nontoxic, pollution-free, the guarantor of reinforcing bar non-corroding is moulded the preparation method of the solidifying middle effect water reducer of accent.
A kind of guarantor that provides of the second day of the present invention moulds the solidifying middle effect water reducer of accent.
Technical scheme of the present invention is summarized as follows:
A kind of guarantor moulds the preparation method who transfers solidifying middle effect water reducer, comprises the steps:
(1) catalyzer is put into reaction vessel, add water and make its dissolving, add while stirring plant fiber powder, mixing is warming up to 60 ℃~65 ℃ reaction 0.5h~1h, stops to stir and continuing to be warming up to 70 ℃~90 ℃ reaction 0.5h~1.5h;
(2) heating, when temperature rises to 95 ℃~105 ℃ reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treat that it is 11~12 that temperature is down to 80 ℃~90 ℃ adding liquid caustic soda adjust pHs, temperature is controlled at 90 ℃~95 ℃, insulation reaction 2h~4h;
(4) be cooled to 50 ℃~60 ℃, regulate pH value to 9~10 with liquid caustic soda, add that air entrapment agent stirs and at 50 ℃~60 ℃, reaction 0.5h~1.5h is cooled to 20 ℃~30 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying.
The mass ratio of described catalyzer, water, plant fiber powder and air entrapment agent is 0~3:45~55:35~45:0.1~1.0.
Described step (1) is preferably: catalyzer is put into reaction vessel, add water and make its dissolving, add while stirring plant fiber powder, mixing is warming up to 63 ℃ of reaction 0.75h, stops to stir and continuing to be warming up to 80 ℃ reaction 1h.
Described step (2) is preferably: the heating, when temperature rises to 100 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately the cooling.
Described step (3) is preferably: treat that it is 11.5 that temperature is down to 85 ℃ of adding liquid caustic soda adjust pHs, temperature is controlled at 93 ℃, insulation reaction 3h.
Described step (4) is preferably: be cooled to 55 ℃, regulate pH value to 9.5 with liquid caustic soda, add that air entrapment agent stirs and at 55 ℃, reaction 1h is cooled to 25 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying;
The mass ratio of described catalyzer, water, plant fiber powder and air entrapment agent is preferably 1:50:40:0.5.
Described catalyzer is preferably oxalic acid, hydrochloric acid or sulfuric acid.
Described plant fiber powder is preferably W-Gum, yam starch, glutinous rice starch or wheat starch.
Described air entrapment agent is preferably Witco 1298 Soft Acid sodium sulfate or Sodium dodecylbenzene sulfonate.
The guarantor of aforesaid method preparation moulds and transfers solidifying middle effect water reducer.
Advantage of the present invention:
1. the present invention adopts natural matter, and production and use procedure are all nontoxic, pollution-free, do not contain benzene, ammonia, formaldehyde and chlorine etc., to the reinforcing bar non-corroding, belongs to the environmental type product, and production technique is simple, economical rationality.
2. be used for concrete, addition is 0.6%~1.2% of gelling material, and cement particle and active material particles are had stronger dissemination, and water-reducing rate can reach 8%~18%; Can make concrete have slow setting, protect and mould and the bleed effect, can obviously improve mortar and concrete workability, can make that concrete retarding 4h is above, the initial stage slump is more than the 180mm, slump-loss 5-10mm behind 1h, it is fast through time loss effectively to solve concrete slump, obviously improve mortar and concrete workability, improve mortar and concrete protect plasticity; And do not affect the later strength development, 28d ultimate compression strength is more than 110%.Have good slow setting and model retention effect after compound with naphthalene series high-efficiency water-reducing agent, be applicable to prepare high-strength and high performance concrete and mass concrete, can effectively reduce the hydrated cementitious thermal peak, postpone the time that thermal peak occurs, can prevent well or reduce the generation of thermal cracking.
Embodiment
Contain many assorted bases without utility value in the molecular structure of starch, molecular weight is also excessive, by chemical reaction its molecular chain is shortened, and removes useless group, again by in and can generate behind the graft copolymerization protect mould transfer solidifying in the effect water reducer.Contain carboxyl, hydroxyl, free thionyl and various carbohydrate in the water reducer molecule of the present invention, its these functional group active effects are between cement granules and cause powerful water-reducing effect just.
The present invention is further illustrated below in conjunction with specific embodiment, and following each embodiment only is used for explanation the present invention but not limitation of the present invention.
Embodiment 1
A kind of guarantor moulds the preparation method who transfers solidifying middle effect water reducer, comprises the steps:
(1) 1g sulfuric acid is put into reaction vessel, add 50g water and make its dissolving, add while stirring the 40g W-Gum, mixing is warming up to 63 ℃ of reaction 0.75h, stops to stir and continuing to be warming up to 80 ℃ reaction 1h;
(2) heating, when temperature rises to 100 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treating temperature to be down to 85 ℃, to add mass concentrations be that 40% aqueous sodium hydroxide solution adjust pH is 11.5, and temperature is controlled at 93 ℃, insulation reaction 3h;
(4) being cooled to 55 ℃, is that 40% aqueous sodium hydroxide solution is regulated pH value to 9.5 with mass concentration, adds that 0.5g Witco 1298 Soft Acid sodium sulfate stirs and at 55 ℃, and reaction 1h is cooled to 25 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying;
Table 1 is protected to mould and is transferred solidifying middle effect water reducer on the impact of concrete mixture characteristic
Figure BDA00002584641000031
Annotate: positive water flowing mud is adopted in test.
Table 2 is protected to mould and is transferred solidifying middle effect water reducer on the impact of concrete crushing strength
Figure BDA00002584641000041
Annotate: positive water flowing mud is adopted in test.
After tested, the guarantor is moulded the solidifying middle effect water reducer of accent add in the concrete, volume is 1.0% of gelling material quality, making the concrete initial stage slump is 215mm, the slump is 210mm behind 1h, can obviously improve mortar and concrete workability, improves mortar and concrete protect plasticity.
Embodiment 2
A kind of guarantor moulds the preparation method who transfers solidifying middle effect water reducer, comprises the steps:
(1) 50g water is put into reaction vessel, add while stirring the 35g yam starch, mixing is warming up to 65 ℃ of reaction 1h, stops to stir and continuing to be warming up to 90 ℃ reaction 0.5h;
(2) heating, when temperature rises to 95 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treating temperature to be down to 90 ℃, to add mass concentrations be that 40% aqueous sodium hydroxide solution adjust pH is 11, and temperature is controlled at 95 ℃, insulation reaction 2h;
(4) being cooled to 60 ℃, is that 40% aqueous sodium hydroxide solution is regulated pH value to 9 with mass concentration, adds that 0.5g Witco 1298 Soft Acid sodium sulfate stirs and at 60 ℃, and reaction 0.5h is cooled to 30 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying.
After tested, the guarantor that embodiment 2 is obtained moulds in the solidifying middle effect water reducer adding concrete of accent, volume is 1.0% of gelling material quality, concrete water-reducing ratio reaches 14%, can make concrete retarding 5h, the initial stage slump is 190mm, the slump is 180mm behind 1h, can obviously improve mortar and concrete workability, improves mortar and concrete protect plasticity.
Embodiment 3
A kind of guarantor moulds the preparation method who transfers solidifying middle effect water reducer, comprises the steps:
(1) 1g hydrochloric acid is put into reaction vessel, add 45g water and make its dissolving, add while stirring the 45g glutinous rice starch, mixing is warming up to 60 ℃ of reaction 0.75h, stops to stir and continuing to be warming up to 70 ℃ reaction 1.5h;
(2) heating, when temperature rises to 98 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treating temperature to be down to 80 ℃, to add mass concentrations be that 40% aqueous sodium hydroxide solution adjust pH is 12, and temperature is controlled at 90 ℃, insulation reaction 4h;
(4) being cooled to 55 ℃, is that 40% aqueous sodium hydroxide solution is regulated pH value to 9.5 with mass concentration, adds that the 1.0g Sodium dodecylbenzene sulfonate stirs and at 55 ℃, and reaction 1h is cooled to 25 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying.
After tested, the guarantor that embodiment 3 is obtained moulds in the solidifying middle effect water reducer adding concrete of accent, volume is 1.0% of gelling material quality, concrete water-reducing ratio reaches 16%, can make concrete retarding 4h, the initial stage slump is 210mm, the slump is 205mm behind 1h, can obviously improve mortar and concrete workability, improves mortar and concrete protect plasticity.
Embodiment 4
A kind of guarantor moulds the preparation method who transfers solidifying middle effect water reducer, comprises the steps:
(1) 3g oxalic acid is put into reaction vessel, add 55g water and make its dissolving, add while stirring the 40g wheat starch, mixing is warming up to 65 ℃ of reaction 0.5h, stops to stir and continuing to be warming up to 80 ℃ reaction 1h;
(2) heating, when temperature rises to 105 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treating temperature to be down to 85 ℃, to add mass concentrations be that 40% aqueous sodium hydroxide solution adjust pH is 12, and temperature is controlled at 93 ℃, insulation reaction 3h;
(4) being cooled to 50 ℃, is that 40% aqueous sodium hydroxide solution is regulated pH value to 10 with mass concentration, adds that the 0.1g Sodium dodecylbenzene sulfonate stirs and at 50 ℃, and reaction 1.5h is cooled to 20 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying.
After tested, the guarantor that embodiment 4 is obtained moulds in the solidifying middle effect water reducer adding concrete of accent, volume is 1.0% of gelling material quality, concrete water-reducing ratio reaches 18%, can make concrete retarding 4.5h, the initial stage slump is 205mm, the slump is 200mm behind 1h, can obviously improve mortar and concrete workability, improves mortar and concrete protect plasticity.

Claims (9)

1. a guarantor moulds the preparation method who transfers solidifying middle effect water reducer, it is characterized in that comprising the steps:
(1) catalyzer is put into reaction vessel, add water and make its dissolving, add while stirring plant fiber powder, mixing is warming up to 60 ℃~65 ℃ reaction 0.5h~1h, stops to stir and continuing to be warming up to 70 ℃~90 ℃ reaction 0.5h~1.5h;
(2) heating, when temperature rises to 95 ℃~105 ℃ reactions, carry out colorimetric test, color to brown transparent after immediately the cooling;
(3) treat that it is 11~12 that temperature is down to 80 ℃~90 ℃ adding liquid caustic soda adjust pHs, temperature is controlled at 90 ℃~95 ℃, insulation reaction 2h~4h;
(4) be cooled to 50 ℃~60 ℃, regulate pH value to 9~10 with liquid caustic soda, add that air entrapment agent stirs and at 50 ℃~60 ℃, reaction 0.5h~1.5h is cooled to 20 ℃~30 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying.
The mass ratio of described catalyzer, water, plant fiber powder and air entrapment agent is 0~3:45~55:35~45:0.1~1.0.
2. method according to claim 1 is characterized in that described step (1) is: catalyzer is put into reaction vessel, add water and make its dissolving, add while stirring plant fiber powder, mixing is warming up to 63 ℃ of reaction 0.75h, stop to stir and continuing to be warming up to 80 ℃ reaction 1h.
3. method according to claim 1 is characterized in that described step (2) is: heating, when temperature rises to 100 ℃ of reactions, carry out colorimetric test, color to brown transparent after immediately cooling.
4. method according to claim 1 is characterized in that described step (3) is: treating temperature to be down to 85 ℃, to add the liquid caustic soda adjust pHs be 11.5, and temperature is controlled at 93 ℃, insulation reaction 3h.
5. method according to claim 1 is characterized in that described step (4) is: be cooled to 55 ℃, regulate pH value to 9.5 with liquid caustic soda, add that air entrapment agent stirs and at 55 ℃, reaction 1h is cooled to 25 ℃ and namely obtains protecting moulding to transfer and imitate water reducer in solidifying;
The mass ratio of described catalyzer, water, plant fiber powder and air entrapment agent is 1:50:40:0.5.
6. method according to claim 1 and 2 is characterized in that described catalyzer is oxalic acid, hydrochloric acid or sulfuric acid.
7. method according to claim 1 and 2 is characterized in that described plant fiber powder is W-Gum, yam starch, glutinous rice starch or wheat starch.
8. method according to claim 1 or 5 is characterized in that described air entrapment agent is Witco 1298 Soft Acid sodium sulfate or Sodium dodecylbenzene sulfonate.
9. the guarantor of the method for one of claim 1-8 preparation moulds and transfers solidifying middle effect water reducer.
CN2012105448161A 2012-12-14 2012-12-14 Intermediate-acting water reducing agent with functions of plastic retaining and coagulation adjustment and preparation method Pending CN103011677A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85108156A (en) * 1985-11-05 1987-05-13 内蒙古农牧学院 Cement water reducing agent
CN101538351A (en) * 2009-04-10 2009-09-23 陕西科技大学 Method for preparing thickening and water holding agent for polycarboxylate type concrete water reducing agent
CN101906167A (en) * 2010-06-07 2010-12-08 新疆大学 Method for preparing concrete water reducing agent by utilizing waste cellulose deposited in pulping black liquor
CN102372460A (en) * 2010-08-24 2012-03-14 上海台界化工有限公司 Concrete composite water reducer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85108156A (en) * 1985-11-05 1987-05-13 内蒙古农牧学院 Cement water reducing agent
CN101538351A (en) * 2009-04-10 2009-09-23 陕西科技大学 Method for preparing thickening and water holding agent for polycarboxylate type concrete water reducing agent
CN101906167A (en) * 2010-06-07 2010-12-08 新疆大学 Method for preparing concrete water reducing agent by utilizing waste cellulose deposited in pulping black liquor
CN102372460A (en) * 2010-08-24 2012-03-14 上海台界化工有限公司 Concrete composite water reducer

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Application publication date: 20130403