CN102249589A - Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves - Google Patents
Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves Download PDFInfo
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- CN102249589A CN102249589A CN2011100880582A CN201110088058A CN102249589A CN 102249589 A CN102249589 A CN 102249589A CN 2011100880582 A CN2011100880582 A CN 2011100880582A CN 201110088058 A CN201110088058 A CN 201110088058A CN 102249589 A CN102249589 A CN 102249589A
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- Prior art keywords
- reducing agent
- water reducing
- efficiency water
- lignosulfonate
- high efficiency
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a method for preparing a lignosulfonate high-efficiency water reducing agent by mixing ordinary lignosulfonate with chemical modifiers such as aniline sulfonic acid, phenol, formaldehyde and the like under the promoting action of ultrasonic waves. The method comprises the following specific steps of: adding lignosulfonate, sulfanilic acid, phenol and water in sequence according to a certain proportion under the action of ultrasonic radiation at the power of 600-1,200W; uniformly stirring and adding a proper amount of alkali; adjusting a mixed liquor to a weakly alkaline state; heating to 80-95 DEG C and adding formaldehyde according to a certain proportion; continuously reacting for 2.0-3.0 hours; cooling to room temperature; and adding a proper amount of rosin serving as an air entraining agent for performing physical modification to obtain the lignosulfonate high-efficiency water reducing agent. The product has the advantages of abundant raw material source, simple synthesis process, short production period, high water reducing rate and capability of serving as a mixture of concrete and improving the workability and compression strength of concrete.
Description
Technical field
The invention belongs to the concrete additives in building materials field, more specifically relate to the method that a kind of ultrasonic wave promotes to prepare the sulfonated lignin high efficiency water reducing agent.
Background technology
Cement water reducing agent claims super contracting agent again, is a kind of anion surfactant, itself not with cement generation chemical reaction, but by tensio-active agent be used for improving concrete performance, concrete is had diminishing enhanced effect significantly.Concrete to the main technical requirements of water reducer is: (1) water-reducing rate height, to reduce water consumption; (2), reduce water cement ratio to the cement good dispersity; (3) better function of control slump loss; (4) good to concrete durability, do not contain or contain less Na
2SO
4Deng nuisance.Available coagulation soil high efficiency water reducing agent mainly contain naphthene sulfonic acid system (US 2,141,569; JP5078157), trimeric cyanamide system (US 3,985,696; US6214965), (US4479826 of sulfamate system; US5245001; JP04275926), polycarboxylic acid series (US6136950; US6211317), aliphatic water reducing agent (CN101508536A; CN101234865A), modified lignin mahogany sulfonate (CN1208027A; CN1648099A; CN101357831A).
At present, both at home and abroad the high efficiency water reducing agent of producing is generally based on naphthalene sulfonic salt, and its water-reducing rate is higher, but makes concrete workability relatively poor, and the slump loss is also bigger, easily produces bleeding and segregation layering, and it is higher to have certain toxicity and cost simultaneously; Trimeric cyanamide is that efficient water-reducing property and naphthalene are close, but because of its liquid product concentration is low, storage period is short, and the slump loss is also big, is further promoted; Sulfamate series high-efficiency water-reducing agent advantage is that volume is little, the water-reducing rate height, and the slump loss is little.Shortcoming is that volume causes concrete water bleeding when high easily, emanates and hardens, and cost is higher; Though the polycarboxylic acid series high efficiency water reducing agent better performances, the cost height, price is expensive, complex manufacturing technology; Aliphatic high-efficiency water reducing agent is good to the adaptability of cement, and dispersive ability is strong, and good water-retaining property does not have corrosive nature to reinforcing bar.But exist water-reducing rate low than naphthalene system and polycarboxylic acid series, slump is lost problems such as bigger.
Along with the shortage of world resource and the raising day by day of people's environmental consciousness, more and more come into one's own with application for the research that with biomass is the concrete admixture of raw material.Product of the present invention is a raw material with papermaking wastewater regenerant sulfonated lignin, and preparation sulfonated lignin high efficiency water reducing agent can economize on resources under ultrasonic wave promotes, turns waste into wealth, and helps protecting environment, benefits the society and the mankind.
Summary of the invention
Purpose of the present invention is intended to propose the method that a kind of ultrasonic wave promotes to prepare the sulfonated lignin high efficiency water reducing agent, to improve its serviceability, comprises water-reducing rate, concrete flowability, workability, water-retentivity and ultimate compression strength etc., shortens its production cycle simultaneously.
A kind of ultrasonic wave that the present invention proposes promotes to prepare the method for sulfonated lignin high efficiency water reducing agent, may further comprise the steps:
(1) the shared per-cent of the weight of each component is (%) in the water reducer:
(2) be under the ultrasonic wave radiation of 600W～1200W at power, in reactor, add sulfonated lignin, Sulphanilic Acid, phenol, alkaline conditioner and water successively according to the above ratio, stir heat temperature raising to 60 ℃～90 ℃ of reaction 20min～30min;
(3) in above-mentioned reaction mixture, add formaldehyde in proportion in batches, behind continuation stirring reaction 2.0h～3.0h, stopped reaction.
(4) the question response mixture is cooled to room temperature, adds an amount of air entrapment agent rosin in proportion and stirs, and makes the sulfonated lignin high efficiency water reducing agent.
A kind of ultrasonic wave that the present invention proposes promotes to prepare the method for modified lignosulfonate high-efficiency water reducing agent, has the following advantages:
(1) aqua solid content height (25%～45%), liquid volume little (be cement weight 1%～1.5%);
(2) be raw material with papermaking wastewater regenerant sulfonated lignin, can economize on resources that turn waste into wealth, preparation process does not have the discharging of waste liquid, waste gas, waste residue, helps protecting environment.
(3) do not contain Na
2SO
4, good to concrete durability, reinforcing bar there is not corrosive nature;
(4) technology is simple, easy handling, cost is low and the one-tenth product cycle is short (2.5h～3.0h);
(5) concrete serviceability is improved a lot, water-reducing rate is big, good fluidity, workability, water-retentivity and ultimate compression strength all have greatly improved, no bleeding, segregation phenomenon, the better function of control grout and concrete flowability loss, the loss of 1h slump is less.
Embodiment
The plain sulfonate of the raw material wood that uses in the product of the present invention is the papermaking byproduct of Tianhong Paper Co Ltd, Xinjiang, and the Sulphanilic Acid of use, phenol, formaldehyde and rosin are the commercially available prod.The alkaline conditioner that uses is sodium hydroxide or potassium hydroxide or yellow soda ash, and the sodium hydroxide effect is best.The cement that uses is Tianshan Mountains board ordinary Portland cement P.O 42.5R.
Embodiment one
Adding calcium lignin sulphonate 84g, Sulphanilic Acid 84g, phenol 54g, sodium hydroxide 26g and water 250mL in the 1000mL three-necked flask, is under the ultrasonic wave radiation of 600W at power, and the post-heating that stirs is warming up to 85 ℃～90 ℃, reaction 30min.In above-mentioned reaction mixture, add formaldehyde 145mL in proportion in batches, behind the continuation stirring reaction 3.0h, stopped reaction.The question response mixture is cooled to room temperature, adds an amount of air entrapment agent rosin and stirs, and obtains calcium lignin sulphonate high efficiency water reducing agent YP-1.
Embodiment two
Adding sodium lignosulfonate 45g, Sulphanilic Acid 90g, phenol 60g, sodium hydroxide 24g and water 300mL in the 1000mL three-necked flask, is under the ultrasonic wave radiation of 800W at power, and the post-heating that stirs is warming up to 85 ℃～90 ℃, reaction 25min.In above-mentioned reaction mixture, add formaldehyde 140mL in proportion in batches, behind the continuation stirring reaction 2.5h, stopped reaction.The question response mixture is cooled to room temperature, adds an amount of air entrapment agent rosin and stirs, and obtains sodium lignosulfonate high efficiency water reducing agent YP-2.
Embodiment three
Adding calcium lignin sulphonate 33g, Sulphanilic Acid 56g, phenol 33g, sodium hydroxide 14g and water 250mL in the 1000mL three-necked flask, is that the ultrasonic wave radiation of 1000W is following at power, and the post-heating that stirs is warming up to 85 ℃～90 ℃, reacts 20min.In above-mentioned reaction mixture, add formaldehyde 145mL in proportion in batches, behind the continuation stirring reaction 2.0h, stopped reaction.The question response mixture is cooled to room temperature, adds an amount of air entrapment agent rosin and stirs, and obtains calcium lignin sulphonate high efficiency water reducing agent YP-3.
The mensuration of flowing degree of net paste of cement
Table 1. flowing degree of net paste of cement measurement result
The measurement of concrete crushing strength
The measurement of concrete crushing strength adopts the method for GB175-92 regulation to carry out.Liquid volume at the calcium lignin sulphonate high efficiency water reducing agent is under the condition of cement consumption 1.3%, has measured concrete respectively at 3 days, 7 days, and the ultimate compression strength in the time of 16 days.
The measurement of table 2. concrete crushing strength
Annotate: this tests used cement is Tianshan Mountains board ordinary Portland cement P.O 42.5R
Claims (3)
1. the present invention is the method that a kind of ultrasonic wave promotes to prepare down the sulfonated lignin high efficiency water reducing agent.
2. press the preparation method of claims 1 described water reducer, it is characterized in that this method may further comprise the steps:
(1) the shared per-cent of the weight of each component is (%) in the water reducer:
(2) under the ultrasonic wave radiation condition, in reactor, add sulfonated lignin, Sulphanilic Acid, phenol, alkaline conditioner and water successively according to the above ratio, stir heat temperature raising to 80 ℃～95 ℃, reaction 20min～30min;
(3) in above-mentioned reaction mixture, add formaldehyde in proportion in batches, behind continuation stirring reaction 2.0h～3.0h, stopped reaction.
(4) the question response mixture is cooled to room temperature, adds an amount of air entrapment agent rosin in proportion and stirs, and becomes the sulfonated lignin high efficiency water reducing agent.
3. press the preparation method of claims 1 described water reducer, it is characterized in that: adopting power is the ultrasonic wave radiation of 600W～1200W, under 80 ℃～95 ℃ temperature condition, and preparation sulfonated lignin high efficiency water reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100880582A CN102249589A (en) | 2011-04-08 | 2011-04-08 | Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves |
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|---|---|---|---|
| CN2011100880582A CN102249589A (en) | 2011-04-08 | 2011-04-08 | Method for preparing lignosulfonate high-efficiency water reducing agent under promoting action of ultrasonic waves |
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| CN102249589A true CN102249589A (en) | 2011-11-23 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633460A (en) * | 2012-03-31 | 2012-08-15 | 安徽省建筑工程质量第二监督检测站 | Method for preparing concrete liquid admixture by utilizing waste water from production of alcohol from molasses |
| CN102924735A (en) * | 2012-10-29 | 2013-02-13 | 江门职业技术学院 | Method for preparing modified lignosulfonate high-performance water reducing agent |
| CN103755972A (en) * | 2013-12-24 | 2014-04-30 | 中科院广州化学有限公司 | Method for preparing ultrasonic alkylated lignosulfonate bio-based surfactant |
| CN108623768A (en) * | 2018-05-18 | 2018-10-09 | 萧县沃德化工科技有限公司 | A kind of useless rosin in adhesive production process is used for amido sulfoacid series high-efficiency water reducer |
| CN112526115A (en) * | 2020-12-14 | 2021-03-19 | 中建西部建设西南有限公司 | Device and method for rapidly measuring solid content of concrete waste slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648099A (en) * | 2005-02-18 | 2005-08-03 | 冯乃谦 | Method for producing water reducer of cement concrete |
| CN101514217A (en) * | 2009-03-26 | 2009-08-26 | 江南大学 | Ultrasonic synthetic method of sucrose caprylic acid ester |
-
2011
- 2011-04-08 CN CN2011100880582A patent/CN102249589A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648099A (en) * | 2005-02-18 | 2005-08-03 | 冯乃谦 | Method for producing water reducer of cement concrete |
| CN101514217A (en) * | 2009-03-26 | 2009-08-26 | 江南大学 | Ultrasonic synthetic method of sucrose caprylic acid ester |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633460A (en) * | 2012-03-31 | 2012-08-15 | 安徽省建筑工程质量第二监督检测站 | Method for preparing concrete liquid admixture by utilizing waste water from production of alcohol from molasses |
| CN102924735A (en) * | 2012-10-29 | 2013-02-13 | 江门职业技术学院 | Method for preparing modified lignosulfonate high-performance water reducing agent |
| CN102924735B (en) * | 2012-10-29 | 2014-08-27 | 江门职业技术学院 | Method for preparing modified lignosulfonate high-performance water reducing agent |
| CN103755972A (en) * | 2013-12-24 | 2014-04-30 | 中科院广州化学有限公司 | Method for preparing ultrasonic alkylated lignosulfonate bio-based surfactant |
| CN108623768A (en) * | 2018-05-18 | 2018-10-09 | 萧县沃德化工科技有限公司 | A kind of useless rosin in adhesive production process is used for amido sulfoacid series high-efficiency water reducer |
| CN112526115A (en) * | 2020-12-14 | 2021-03-19 | 中建西部建设西南有限公司 | Device and method for rapidly measuring solid content of concrete waste slurry |
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Application publication date: 20111123 |