CN1648099A - Method for producing water reducer of cement concrete - Google Patents

Method for producing water reducer of cement concrete Download PDF

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Publication number
CN1648099A
CN1648099A CN 200510008403 CN200510008403A CN1648099A CN 1648099 A CN1648099 A CN 1648099A CN 200510008403 CN200510008403 CN 200510008403 CN 200510008403 A CN200510008403 A CN 200510008403A CN 1648099 A CN1648099 A CN 1648099A
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water
cement
concrete
water reducer
phenol
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CN 200510008403
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CN1266070C (en
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冯乃谦
王湘才
张智峰
丁宏
李崇智
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冯乃谦
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The present invention relates to the production process of water reducer for cement and concrete, and belongs to the field of building material technology. The water reducer consists of calcium lignosulfonate, p-aminobenzenesulfonic acid, phenol, alkali and formaldehyde, and is produced into water preparation via adding water in 1-3 times. The production process includes heating water to 85-100 deg.c, adding the said materials successively via stirring, cooling to room to form water preparation, or further drying to form powder preparation. The present invention has the advantages of low temperature and normal pressure production, easy control of technological process, no environmental pollution, high function of controlling flowability loss of cement slurry and concrete and no harm to concrete durability.

Description

A kind of manufacture method of water reducer of cement concrete
Technical field
The present invention relates to a kind of manufacture method of water reducer of cement concrete, is the feedstock production high efficiency water reducing agent with Sulphanilic Acid, sulfonated lignin, phenol, alkali and formaldehyde etc., belongs to building material technical field.
Background technology
China's concrete output is about 1,300,000,000 m 3/ year.The high efficiency water reducing agent ultimate production is about 250,000 tons/year.The principal item of high efficiency water reducing agent has naphthalene system and melamine system.The former accounts for 90% of high efficiency water reducing agent consumption.In recent years, also have a small amount of poly carboxylic acid series water reducer to be used for engineering.
Concrete to the main technical requirements of water reducer is: (1) water-reducing rate height, to reduce folk prescription concrete water amount; (2), reduce water cement ratio to the cement good dispersity; (3) better function of control loss of slump; (4) good to concrete durability, do not contain or contain less Na 2SO 4Deng using pest.Naphthalene system, melamine based water reducer can not be controlled and spoil degree of falling loss, Na on the coagulation 2SO 4Content is also high.
Current production and the application that a spot of amido sulfoacid series high-efficiency water reducer is still arranged of China.But the easy bleeding of mixture on the coagulation produces segregation and layering, causes constructional difficulties, and concrete intensity and weather resistance are also influenced.Such water reducer is because phenol usage is big, thereby the cost height.The batching complexity of existing such water reducer, the production temperature surpasses 100 ℃ (actual is 110 ℃), and is also wayward.
Polycarboxylic acid series high efficiency water reducing agent cost height, expensive, the complex manufacturing technology of price.
Summary of the invention
The objective of the invention is to propose a kind of manufacture method of water reducer of cement concrete, with Sulphanilic Acid, sulfonated lignin, phenol is raw material, under 90 ℃-100 ℃, carry out condensation reaction, make a kind of new and effective water reducer,, and make production technique easy with the raising performance, easy handling reduces cost.
The manufacture method of the water reducer of cement concrete that the present invention proposes comprises following each step:
(1) weight ratio of water in the water reducer and material is: water: material=1: 1~3: 1, and wherein the weight ratio of each component is in the material:
1.0 parts of calcium lignin sulphonates
1.56~2.88 parts of Sulphanilic Acid
0.45~1.55 part of phenol
0.4~0.75 part in alkali
1.8~4.0 parts in formaldehyde
(2) heat water to 85 ℃~100 ℃, add calcium lignin sulphonate, Sulphanilic Acid, phenol and alkali according to the above ratio successively, reacted while stirring 1~2 hour;
(3) in the reactant in above-mentioned second step, add formaldehyde in proportion, continue to stir and carried out condensation reaction 8~10 hours;
(4) be cooled to room temperature, become aqua, or drying becomes pulvis.
Efficient cement water reducing agent of the present invention has aqua and 2 kinds of forms of pulvis.Mix in the concrete with aqua formation, its volume is 1.2%~3.0% of a cement weight; Also can mix in the concrete with pulvis, its volume is 0.5~1.2%.Mix in the premixing mortar with pulvis, the system of can mixing is at the scene used, and also can make gravity flowing levelling mortar etc., and its volume is the 0.5-2.0% of gelling material in the mortar.
The manufacture method of the water reducer of cement concrete that the present invention proposes has the following advantages:
(1) low temperature, normal pressure are produced down, and production unit is simple, and technology is convenient to control;
(2) discharging of no waste liquid, waste gas, waste residue etc., environmentally safe;
(3) high efficiency water reducing agent of the present invention with existing naphthalene is, the melamine series high-efficiency water-reducing agent compares, diminishing efficient height, and the better function of control grout and concrete flowability loss, can reach 2 hours does not have loss of slump substantially;
(4) contains sodium sulfate not, harmless to concrete weather resistance;
(5) compare with existing high-efficiency water-reducing agent of poly-carboxylic acid, technology is simple, easy handling, and cost is low.
(6) compare with existing amido sulfoacid series high-efficiency water reducer, cost is low, no bleeding, concrete good fluidity.
Embodiment
The present invention makes the calcium lignin sulphonate that uses in the water reducer, be China Jilin Province cut into a mountain the village paper mill byproduct (wooden calcium), the Sulphanilic Acid and the phenol of use are the commercially available prod.The alkaline conditioner that uses preferably uses NaOH or Ca (OH) 2
Embodiment one
In 85 ℃ 600 milliliters water, drop into calcium lignin sulphonate 55 grams, Sulphanilic Acid 86 grams, phenol 25 grams stirred 30 minutes, added sodium hydroxide 22 grams, the pH value of adjusting solution is 7-8, at 85 ℃, splash into formaldehyde 100 grams, reaction is 9 hours under this temperature, cool off efficient liquid water reducer (aqua), solid content is about 24%, drying again, powdery high efficiency water reducing agent (pulvis).
The flowing degree of net paste of cement measurement result
Cement (the general silicon 425 of Mitsubishi), 300 grams, w/c-0.30, aqua high efficiency water reducing agent volume 3.0%, powdery volume 0.7%, starch only degree of mobilization and through the time change as follows:
1 hour 2 hours at the beginning outward appearances
1# aqua (3.0%) 240 Mm240 Mm230 MmNo bleeding
2# aqua (0.7%) 240 Mm245 Mm235 MmNo bleeding
Embodiment two
At 90 ℃, in 1000 milliliters the water, drop into calcium lignin sulphonate 55 grams, Sulphanilic Acid 86g, phenol 55 grams stirred 30 minutes, add sodium hydroxide 23 grams, the pH value of adjusting solution is 8, at 90 ℃, splash into formaldehyde 120 grams, under this temperature the reaction 10 hours, cool off efficient liquid water reducer (aqua), solid content about 24%, drying gets the powdery high efficiency water reducing agent again.
Flowing degree of net paste of cement and through the time change
The proportioning of cement paste such as example 1
The cement of test usefulness is 425 two kinds in general silicon Mitsubishi 425 and mountain aluminium, and code name is 3#, 4#.
The water reducer volume is degree of mobilization 1 hour 2 hours at the beginning
3# aqua 2.5% 250 Mm245 Mm250 Mm
Pulvis 0.7% 250 Mm260 Mm250 Mm
4# aqua 2.5% 240 Mm230 Mm220 Mm
Pulvis 0.7% 240 Mm230 Mm230 Mm
Embodiment three
At 90 ℃, in 1000 milliliters the water, drop into calcium lignin sulphonate 90 grams, Sulphanilic Acid 260 grams, phenol 140 grams stirred 30 minutes, add sodium hydroxide 68 grams, the pH value of adjusting solution is 8,90 ℃ of temperature, splash into formaldehyde 360 grams, under this temperature the reaction 10 hours, cool off efficient liquid water reducer (aqua), solid content about 30%, drying gets the powdery high efficiency water reducing agent again.
Flowing degree of net paste of cement and through the time change
The proportioning of cement paste:
Cement be general silicon Mitsubishi 425 and, water cement ratio w/e=0.39, water: 86 grams, high efficiency water reducing agent 2.0%, 6 gram in the present embodiment, starch only the flow degree and through the time change as follows:
The water reducer volume is 1 hour 2 hours outward appearances of degree of mobilization at the beginning
Aqua 2.0% 255 Mm250 Mm240 MmNo bleeding
Pulvis 0.6% 250 Mm250 Mm245 MmNo bleeding
High efficiency water reducing agent of the present invention and the clean slurry degree of mobilization contrast of naphthalene series high-efficiency water-reducing agent now:
Test example 1: cement (the general silicon 42 of Tianshan Mountains board), 300 grams
Water cement ratio w/e=0.3 water, 90 grams
Add water reducer 2.0%, 6.0 gram of the embodiment of the invention, the FDN-20 of Sichuan factory naphthalene series high-efficiency water-reducing agent (pulvis) volume respectively is 0.75%, 1.0% and 1.5%, West China naphthalene series high-efficiency water-reducing agent pulvis volume 1.0%, 1.2%.
Test-results is as follows:
Initially 1 hour 2 hours
Aqua of the present invention mixes 2.0% 250×255 mm 250×255 mm 250×255 mm
FDN-20 pulvis 0.75% Do not flow -- --
FDN-20 pulvis 0.75% 175×180 mm -- --
FDN-20 pulvis 0.75% 220×220 mm -- --
The West China naphthalene is a pulvis 1.0% 160×16 mm -- --
The West China naphthalene is a pulvis 1.2% 197×201 mm -- --
Test example 2
Cement: Jia Xinpu silicon 425, the general silicon 425 of arrow drum, water cement ratio w/c=0.29.The pulvis high efficiency water reducing agent.The result is as follows:
The contrast water reducer Cement type ?w/c Volume Clean slurry degree of mobilization
Initially 30 minutes 60 minutes 120 minutes
Product of the present invention (pulvis) Good new 425 arrow drums 425 ?0.29 ?0.64% 260 mm270 mm ?260 mm?270 mm ?260 mm?270 mm ??260 mm??270 mm
Tianjin naphthalene system (pulvis) Good new 425 arrow drums 425 ?0.29 ?1.0% ?1.1% 180 mm190 mm ?----- ?---- ??---

Claims (1)

1, a kind of manufacture method of cement water reducing agent is characterized in that this method comprises following each step:
(1) weight ratio of water in the water reducer and material is: water: material=1~3: 1, and wherein the weight ratio of each component is in the material:
1.0 parts of calcium lignin sulphonates
1.56~2.88 parts of Sulphanilic Acid
0.45~1.55 part of phenol
0.4~0.75 part in alkali
1.8~4.0 parts in formaldehyde
(2) heat water to 85 ℃~100 ℃, add calcium lignin sulphonate, Sulphanilic Acid, phenol and alkali according to the above ratio successively, reacted while stirring 1~2 hour;
(3) in the reactant in above-mentioned second step, add formaldehyde in proportion, continue to stir and carried out condensation reaction 8~10 hours;
(4) be cooled to room temperature, become aqua, or drying becomes pulvis.
CN 200510008403 2005-02-18 2005-02-18 Method for producing water reducer of cement concrete Expired - Fee Related CN1266070C (en)

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Application Number Priority Date Filing Date Title
CN 200510008403 CN1266070C (en) 2005-02-18 2005-02-18 Method for producing water reducer of cement concrete

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Application Number Priority Date Filing Date Title
CN 200510008403 CN1266070C (en) 2005-02-18 2005-02-18 Method for producing water reducer of cement concrete

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CN1648099A true CN1648099A (en) 2005-08-03
CN1266070C CN1266070C (en) 2006-07-26

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157531B (en) * 2007-09-13 2010-11-24 华南理工大学 Alkali lignin modified sulfamate high-effective water reducer and preparation method thereof
CN101975789A (en) * 2010-10-14 2011-02-16 同济大学 Method for testing plastification property of water reducing agent by adopting nuclear magnetic resonance technology
CN102249589A (en) * 2011-04-08 2011-11-23 新疆大学 Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves
CN102249588A (en) * 2011-04-08 2011-11-23 新疆大学 Method for preparing lignosulfonate superplasticizer by microwave promotion
CN102503224A (en) * 2011-10-19 2012-06-20 山东宏艺科技股份有限公司 Water reducing agent and preparation method thereof
CN103965417A (en) * 2013-12-28 2014-08-06 福清市永春混凝土外加剂有限公司 Lignin sulfonate modified aminosulfonic acid series efficient water reducer and preparation method thereof
CN107759121A (en) * 2017-09-29 2018-03-06 镇江泽枫霖建筑材料有限公司 A kind of water reducer for being used to prepare portland cement
CN111978002A (en) * 2020-09-03 2020-11-24 傅春英 Efficient environment-friendly concrete water reducing agent and preparation method thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103351108B (en) * 2013-07-12 2015-02-18 武陟县智辉科技有限公司 Process for synthesizing concrete water reducer by emissions and secondary products during production of bibenzyl

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157531B (en) * 2007-09-13 2010-11-24 华南理工大学 Alkali lignin modified sulfamate high-effective water reducer and preparation method thereof
CN101975789A (en) * 2010-10-14 2011-02-16 同济大学 Method for testing plastification property of water reducing agent by adopting nuclear magnetic resonance technology
CN102249589A (en) * 2011-04-08 2011-11-23 新疆大学 Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves
CN102249588A (en) * 2011-04-08 2011-11-23 新疆大学 Method for preparing lignosulfonate superplasticizer by microwave promotion
CN102503224A (en) * 2011-10-19 2012-06-20 山东宏艺科技股份有限公司 Water reducing agent and preparation method thereof
CN102503224B (en) * 2011-10-19 2015-04-15 临沂大学 Water reducing agent and preparation method thereof
CN103965417A (en) * 2013-12-28 2014-08-06 福清市永春混凝土外加剂有限公司 Lignin sulfonate modified aminosulfonic acid series efficient water reducer and preparation method thereof
CN103965417B (en) * 2013-12-28 2016-03-30 福清市永春混凝土外加剂有限公司 Lignin sulfonate modified amido sulfoacid series high-efficiency water reducer and preparation method thereof
CN107759121A (en) * 2017-09-29 2018-03-06 镇江泽枫霖建筑材料有限公司 A kind of water reducer for being used to prepare portland cement
CN111978002A (en) * 2020-09-03 2020-11-24 傅春英 Efficient environment-friendly concrete water reducing agent and preparation method thereof

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