CN101734877A - Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene - Google Patents
Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene Download PDFInfo
- Publication number
- CN101734877A CN101734877A CN200910263278A CN200910263278A CN101734877A CN 101734877 A CN101734877 A CN 101734877A CN 200910263278 A CN200910263278 A CN 200910263278A CN 200910263278 A CN200910263278 A CN 200910263278A CN 101734877 A CN101734877 A CN 101734877A
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- China
- Prior art keywords
- phenanthrene
- dilution
- water reducing
- reducing agent
- alkali
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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
- C04B24/226—Sulfonated naphtalene-formaldehyde condensation products
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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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 discloses a method for preparing a concrete high-efficiency water reducing agent by utilizing phenanthrene, comprising the following steps of: (1) sulfonation reaction: adding concentrated sulfuric acid with a weight ratio of 2:3 with the phenanthrene to the phenanthrene, and keeping the temperature for 1 to 5 hours at the temperature of 80 to 140 DEG C; (2) dilution: diluting sulfonated bodies after sulfonation reaction by adding water, wherein the acidity after dilution is 20 to 30%; (3) condensation reaction: adding paraformaldehyde with a mol ratio of 0.75 to 1.1 with the phenanthrene and 30 to 40% of formaldehyde or acetaldehyde aqueous solution to the materials after dilution under the condition of 80 to 120 DEG C, and keeping the temperature for 2 to 5 hours; and (4) neutralization reaction: adding alkali, and adjusting the pH value to 7 to 9, wherein the alkali is the alkali of kalium, natrium, calcium and quaternary ammonium salt ions. The water reducing rate is 26% when 0.75% of doping amount of solid is singly used according to the concrete high efficiency water reducing agent prepared by the invention, and the later strength of concrete is increased to 140%.
Description
Technical field
The present invention relates to a kind of preparation method of novel concrete water reducing agent, particularly use the luxuriant and rich with fragrance method for preparing concrete high efficiency water reducing agent.
Background technology
When the cement mixture operation, for making rapid operation effective, and the early stage demoulding reduction of erection time, require cement mixture to have high workability, effectively suppress the loss of slump, and there is sufficient early strength at the sclerosis initial stage, need to add cement water reducing agent, at present China's cement water reducing agent with how be with melamine be that product is a main flow.The cement mixture workability of this series products is bad, has the problem that water-reducing rate is not high, loss of slump is big.And the ionic efficient cement water reducing agent mainly contains naphthalene sulfonic acidformaldehyde condensation product, phenol/para-anilinesulfonic acid yuban, anthracene sulfonic acid formaldehyde condensation products, and the methylolated trimeric cyanamide of sulfonation or the like, such product application is extensive, but can not with the compound use of most of pectination poly carboxylic acid kind.Studies show that at naphthalene sulfonic acidformaldehyde condensation product, phenol/para-anilinesulfonic acid yuban, anthracene sulfonic acid formaldehyde condensation products, and in the product such as the methylolated trimeric cyanamide of sulfonation, add the efficient cement water reducing agent of a spot of luxuriant and rich with fragrance preparation, can solve naphthalene sulfonic acidformaldehyde condensation product, phenol/para-anilinesulfonic acid yuban, anthracene sulfonic acid formaldehyde condensation products, and product such as the methylolated trimeric cyanamide of sulfonation can not with the problem of the compound use of pectination poly carboxylic acid kind.
Summary of the invention
Purpose of the present invention provides a kind of luxuriant and rich with fragrance method for preparing efficient cement water reducing agent of utilizing in order to overcome above-mentioned deficiency of the prior art,
For realizing above-mentioned requirements, technical scheme of the present invention may further comprise the steps successively:
(1) sulfonation reaction: will be 2 with luxuriant and rich with fragrance mass ratio: the vitriol oil of 2.4-3 adds in the phenanthrene, 80-140 ℃ of insulation 1-5 hour;
(2) dilution: with the sulfonated bodies of sulfonation reaction, add the entry dilution at 80-110 ℃, the acidity after the dilution is 20-30%;
(3) condensation reaction: through the material after the dilution, under 80-120 ℃ of condition, adding is Paraformaldehyde 96,30～40% formalins of 0.75-1.1 with luxuriant and rich with fragrance mol ratio, and is incubated 2-5 hour under this temperature; Wherein said Paraformaldehyde 96 is the formaldehyde low-molecular(weight)polymer, molecular formula (CH
2O)
n, molecular weight: (30)
nPolymerization degree n=8-100, product are the white solid powder.Specification is commercially available top grade Industrial products.
(4) neutralization reaction: add alkali, adjust the pH value at 7-9, wherein said alkali is potassium, sodium, calcium, quaternary ammonium salt ionic alkali, as sodium hydroxide, potassium hydroxide, calcium hydroxide etc.
Advantage of the present invention: according to the characteristics of the high-efficiency concrete additive of method for preparing, with the phenanthrene is that main raw material prepares concrete high efficiency water reducing agent, when solid 0.75% incorporation uses separately, water-reducing rate is 26%, late strength of concrete is increased to 140%, by 20---after 50% amount and naphthalene sulfonic acidformaldehyde condensation product, phenol/para-anilinesulfonic acid yuban, anthracene sulfonic acid formaldehyde condensation products are compound, can with the compound use of pectination poly carboxylic acid.
Embodiment
Be embodiments of the invention below, present embodiment is used to explain the present invention, but does not limit the present invention.
Embodiment 1
Drop into the 1200KG phenanthrene at reactor, add the dense 1900KG of sulfuric acid,, start and stir, adjust 123-127 ℃ of sulfonation temperature, be incubated 3 hours when temperature rises to the temperature of regulation.Detecting acidity should be in the scope of control.After confirming that the sulfonation endpoint parameter is normal, enter hydrolyzing process.Under stirring condition, add dilution water 1800L, stirred 20 minutes, detect acidity, should be in the 27-29% scope of regulation.Sulfonation material after the dilution is controlled at 75-80 ℃, adds 30% formaldehyde solution 430L, slowly be warming up to 95 ℃, be incubated 3 hours.Add 1500KG water, the dilution back adds the sodium hydroxide neutralization, and accent pH is 7-9.
Products obtained therefrom high-efficiency cement water reducer is carried out performance test:
(1) flowing degree of net paste of cement test
Flowing degree of net paste of cement reference " concrete admixture uniformity test method " (GB8077-2000) standard detects.
The resulting cement of dry product 0.75% incorporation according to this product records flowing degree of net paste of cement 235MM.
The 20% solid content product that is re-dubbed according to the ratio of 20% naphthalene water reducer (FDN)+20% product+60%PC.
The resulting cement of dry product 0.8% incorporation according to above-mentioned composite product records flowing degree of net paste of cement 270MM.
(wherein PC is the trade mark of a kind of concrete high efficiency water reducing agent of producing of applicant, belongs to the polycarboxylic acid series product)
(2) concrete performance test
Admixture water-reducing rate, ultimate compression strength detect with reference to " concrete admixture " relevant regulations (GB8076-1997).
The resulting cement of dry product 0.75% incorporation according to this product records the cement water-reducing rate: 26.8%
The concrete crushing strength that makes: 3 days 160% 7 days 140% 28 days 140%.
Embodiment 2
Drop into the 1200KG phenanthrene at reactor, add sulfuric acid 1400KG,, start and stir, adjust 145 ℃ of sulfonation temperatures, be incubated 3 hours when temperature rises to the temperature of regulation.Detecting acidity should be in the scope of control.After confirming that the sulfonation endpoint parameter is normal, enter hydrolyzing process.Under stirring condition, add dilution water 1300L, stirred 20 minutes, detect acidity, should be in the 20-22% scope of regulation.To dilute back back sulfonation material and be controlled at 75-80 ℃, add 40% formaldehyde solution formaldehyde 420L, slowly be warming up to 95 ℃, be incubated 3 hours.Add 1300KG water, the dilution back adds the potassium hydroxide neutralization, and accent pH is 7-9.
Products obtained therefrom high-efficiency cement water reducer is carried out performance test:
(1) flowing degree of net paste of cement test
Flowing degree of net paste of cement reference " concrete admixture uniformity test method " (GB8077-2000) standard detects.
The resulting cement of dry product 0.75% incorporation according to this product records flowing degree of net paste of cement 235MM.
The 20% solid content product that is re-dubbed according to the ratio of 20% naphthalene water reducer (FDN)+30% goods+50%PC.
The resulting cement of dry product 0.8% incorporation according to above-mentioned composite product records flowing degree of net paste of cement 255MM.
(wherein PC is the trade mark of a kind of concrete high efficiency water reducing agent of producing of applicant, belongs to the polycarboxylic acid series product)
(2) concrete performance test
Admixture water-reducing rate, ultimate compression strength detect with reference to " concrete admixture " relevant regulations (GB8076-1997).
The resulting cement of dry product 0.75% incorporation according to this product records the cement water-reducing rate: 26.8%
The concrete crushing strength that makes: 3 days 155% 7 days 150% 28 days 140%.
Embodiment 3
Drop into the 1200KG phenanthrene at reactor, add sulfuric acid 1900KG,, start and stir, adjust 123-127 ℃ of sulfonation temperature, be incubated 3 hours when temperature rises to the temperature of regulation.Detecting acidity should be in the scope of control.After confirming that the sulfonation endpoint parameter is normal, enter hydrolyzing process.Under stirring condition, add dilution water 2100L, stirred 20 minutes, detect acidity, should be in the 25-27% scope of regulation.To dilute back back sulfonation material and be controlled at 75-80 ℃, add Paraformaldehyde 96 162KG, slowly be warming up to 95 ℃, be incubated 3 hours.Add 1500KG water, the dilution back adds the calcium hydroxide neutralization, and accent PH is 7-9.
Products obtained therefrom high-efficiency cement water reducer is carried out performance test:
(1) flowing degree of net paste of cement test
Flowing degree of net paste of cement reference " concrete admixture uniformity test method " (GB8077-2000) standard detects.
The resulting cement of dry product 0.75% incorporation according to this product records flowing degree of net paste of cement 235MM.
The 20% solid content product that is re-dubbed according to the ratio of 30% thionamic acid based water reducer+20% goods+50%PC.
The resulting cement of dry product 0.8% incorporation according to above-mentioned composite product records flowing degree of net paste of cement 275MM.(wherein PC is the trade mark of a kind of concrete high efficiency water reducing agent of producing of applicant, belongs to the polycarboxylic acid series product)
(2) concrete performance test
Admixture water-reducing rate, ultimate compression strength detect with reference to " concrete admixture " relevant regulations (GB8076-1997).
The resulting cement of dry product 0.75% incorporation according to this product records the cement water-reducing rate: 26.8%
The concrete crushing strength that makes: 3 days 160% 7 days 155% 28 days 140%.
Claims (3)
1. utilize the luxuriant and rich with fragrance method for preparing concrete high efficiency water reducing agent, it is characterized in that, carry out according to following method:
(1) sulfonation reaction: will be 2 with luxuriant and rich with fragrance mass ratio: the vitriol oil of 2.4-3 adds in the phenanthrene, 80-140 ℃ of insulation 1-5 hour;
(2) dilution: with the sulfonated bodies of sulfonation reaction, add the entry dilution at 80-110 ℃, the acidity after the dilution is 20-30%;
(3) condensation reaction: through the material after the dilution, under 80-120 ℃ of condition, adding is Paraformaldehyde 96,30～40% formaldehyde or the acetaldehyde solution of 0.75-1.1 with luxuriant and rich with fragrance mol ratio, and is incubated 2-5 hour under this temperature;
(4) neutralization reaction: add alkali, adjust the pH value at 7-9, wherein said alkali is potassium, sodium, calcium, quaternary ammonium salt ionic alkali.
2. the method for utilizing phenanthrene to prepare concrete high efficiency water reducing agent according to claim 1 is characterized in that wherein said Paraformaldehyde 96 is the formaldehyde low-molecular(weight)polymer, molecular formula (CH
2O)
n, molecular weight: (30)
n, polymerization degree n=8-100, product are the white solid powder.
3. the method for utilizing phenanthrene to prepare concrete high efficiency water reducing agent according to claim 1 is characterized in that wherein said alkali is sodium hydroxide, potassium hydroxide or calcium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910263278A CN101734877A (en) | 2009-12-18 | 2009-12-18 | Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene |
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| CN200910263278A CN101734877A (en) | 2009-12-18 | 2009-12-18 | Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene |
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| CN101734877A true CN101734877A (en) | 2010-06-16 |
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| CN200910263278A Pending CN101734877A (en) | 2009-12-18 | 2009-12-18 | Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446097A (en) * | 2014-11-14 | 2015-03-25 | 浙江建研科之杰新材料有限公司 | Preparation method of dye dispersant and concrete naphthalene water reducer |
| CN108129054A (en) * | 2017-04-27 | 2018-06-08 | 钟建军 | A kind of natural lignin's sulfonate sodium water-reducing agent for building |
| CN113831487A (en) * | 2020-06-24 | 2021-12-24 | 江苏苏博特新材料股份有限公司 | Aromatic carboxylate intermediate, preparation method thereof and application thereof in ester type polycarboxylate superplasticizer |
-
2009
- 2009-12-18 CN CN200910263278A patent/CN101734877A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446097A (en) * | 2014-11-14 | 2015-03-25 | 浙江建研科之杰新材料有限公司 | Preparation method of dye dispersant and concrete naphthalene water reducer |
| CN108129054A (en) * | 2017-04-27 | 2018-06-08 | 钟建军 | A kind of natural lignin's sulfonate sodium water-reducing agent for building |
| CN113831487A (en) * | 2020-06-24 | 2021-12-24 | 江苏苏博特新材料股份有限公司 | Aromatic carboxylate intermediate, preparation method thereof and application thereof in ester type polycarboxylate superplasticizer |
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Open date: 20100616 |