CN1557766A - Production process of low-air-entraining high-performance anthracene sulfonate concrete water reducer - Google Patents
Production process of low-air-entraining high-performance anthracene sulfonate concrete water reducer Download PDFInfo
- Publication number
- CN1557766A CN1557766A CNA2004100139735A CN200410013973A CN1557766A CN 1557766 A CN1557766 A CN 1557766A CN A2004100139735 A CNA2004100139735 A CN A2004100139735A CN 200410013973 A CN200410013973 A CN 200410013973A CN 1557766 A CN1557766 A CN 1557766A
- Authority
- CN
- China
- Prior art keywords
- anthracene
- reducing agent
- concrete
- performance
- water reducing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- ILFFFKFZHRGICY-UHFFFAOYSA-N anthracene-1-sulfonic acid Chemical compound C1=CC=C2C=C3C(S(=O)(=O)O)=CC=CC3=CC2=C1 ILFFFKFZHRGICY-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000004567 concrete Substances 0.000 title abstract description 24
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 8
- 230000005494 condensation Effects 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000005194 fractionation Methods 0.000 claims abstract description 4
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 4
- 239000004568 cement Substances 0.000 claims description 19
- 238000005516 engineering process Methods 0.000 claims description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 25
- LILBTUIVFDYIDP-UHFFFAOYSA-N anthracene;hydrate Chemical compound O.C1=CC=CC2=CC3=CC=CC=C3C=C21 LILBTUIVFDYIDP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 abstract 1
- 239000012264 purified product Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000001035 drying Methods 0.000 description 10
- 239000012263 liquid product Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- MYKQKWIPLZEVOW-UHFFFAOYSA-N 11h-benzo[a]carbazole Chemical compound C1=CC2=CC=CC=C2C2=C1C1=CC=CC=C1N2 MYKQKWIPLZEVOW-UHFFFAOYSA-N 0.000 description 2
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 2
- 150000001454 anthracenes Chemical class 0.000 description 2
- WZJYKHNJTSNBHV-UHFFFAOYSA-N benzo[h]quinoline Chemical compound C1=CN=C2C3=CC=CC=C3C=CC2=C1 WZJYKHNJTSNBHV-UHFFFAOYSA-N 0.000 description 2
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthene Chemical compound C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 2
- FTMRMQALUDDFQO-UHFFFAOYSA-N beta-brazan Natural products C1=CC=C2C=C3C4=CC=CC=C4OC3=CC2=C1 FTMRMQALUDDFQO-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000011372 high-strength concrete Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000005002 naphthylamines Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for preparing concrete water-reducing agent by using polycyclic aromatic hydrocarbon, and is characterized by that it uses anthracene oil, and makes it undergo the processes of fractionation to obtain purified product or crude anthracene or their mixture as raw material, and makes them undergo the processes of sulfonation, hydrolysis, condensation and neutralization so as to obtain the invented anthracene sulfonate concrete water-reducing agent with low air-entraining property and high performance. The invention avoids the poor index of the air entraining of the water reducing agent caused by the organic matter doped in the original production process, is easy to control the air entraining and water reducing performance of concrete engineering and products, realizes that the homogeneity index and the concrete performance index of the anthracene water reducing agent exceed all indexes of products prepared by the original process, and has low production cost and easy control of the process.
Description
Technical field
The present invention relates to make the manufacture method of cement water reducing agent with polynuclear aromatics.
Background technology
The production method of traditional anthracene sulfonic acid salt cement water reducing agent: carbolineum obtains the anthracene sulfonic acid salt cement water reducing agent through sulfonation, hydrolysis, condensation, neutralization, drying, and also drying does not manufacture liquid product.Its technology weak point: owing to mainly contain in the carbolineum: anthracene, luxuriant and rich with fragrance, fluoranthene, carbazole, naphthylamines, benzoquinoline, brazan, the benzo carbazole, the organism that different benzo carbazole etc. are relatively more complicated, use carbolineum to have the bleed feature as the resulting anthracene sulfonic acid salt cement water reducing agent of raw material production, the size of amount of air entrainment also changes along with the variation of organism composition, concrete uses such water reducer can cause the fluctuation of concrete strength, limit to its volume scope in concrete works and goods use, especially in the engineering and goods application of high-strength concrete, though can adopt suitable modification preparation to be improved, but still be difficult to control preferably the bleed situation, the relation allotment of water-reducing property and concrete strength loss makes the range of application of this product be subjected to serious restriction.
Summary of the invention
The object of the invention is to invent a kind of production technique that can improve the low bleed high-performance anthracene sulfonic acid salt cement water reducing agent of concrete performance index and homogeneity index.
The present invention makes raw material through sulfonation, hydrolysis, condensation, neutralization, described raw material is that carbolineum is obtained purification thing or crude anthracene or both mixtures through fractionation.
The present invention selects for use through fractionated carbolineum or crude anthracene or both mixtures as the raw material of producing, avoid adulterated organism in the original production process to cause the bad index of water reducer bleed, be easy to control bleed, the water-reducing property of concrete works and goods, realize that anthracene water reducer homogeneity index and concrete performance index surpass every index that former technology makes product, and the products production cost is low, and technology is easy to control.
Among the present invention, NAPTHALENE FLAKES. (INDUSTRIAL GRADE can also be added in the raw material.
Simultaneously, preferred temperature is controlled to be 280～370 ℃ when distillation carbolineum.
Sulfonation temperature of the present invention is 70～150 ℃, and technology is easy to control, handled easily.
Specific embodiment
Example 1: refining carbolineum is produced the anthracene sulfonic acid salt cement water reducing agent
Carbolineum is carried out fractionation under 280～370 ℃ of conditions, it is stand-by to get the purification thing that distills out.
With 600 kilograms of the carbolineums of purifying, drop into the sulfonation reaction still, add 98% vitriol oil, under 70 ℃ of conditions, reacted 3～4 hours, after hydrolysis, added formaldehyde condensation 4～6 hours.The polymeric material neutralizes with liquid caustic soda, transfers pH value 7～8.Drying obtains cement water reducing agent again, and also drying does not manufacture liquid product, and every index is as follows:
Dry product outward appearance: brown ceramic powder pH value: 7～8
Surface tension: 68～69mN/m dry product Na
2SO
4Content: 27%
Dry product Cl
-Content :≤0.3% flowing degree of net paste of cement: 215～225mm
Dry product 0.6% volume water-reducing rate: 16%
Dry product 0.6% volume concrete strength sees the following form with blank concrete strength ratio:
| Concrete coagulates the phase | ??R3 | ??R7 | ??R28 |
| Ultimate compression strength MPa | ??29.6 | ??35.1 | ??43.1 |
| With blank strength ratio | ??155 | ??153 | ??120 |
Example 2: crude anthracene is produced the anthracene sulfonic acid salt cement water reducing agent
With 600 kilograms of crude anthracenes, drop into the sulfonation reaction still, add 98% vitriol oil, under 90 ℃ temperature, reacted 2～3.5 hours, after hydrolysis, added formaldehyde condensation 4～6 hours.The polymeric material neutralizes with liquid caustic soda, transfers pH value 7～8.Drying obtains cement water reducing agent again, and also drying does not manufacture liquid product, and every index is as follows:
Dry product outward appearance: brown ceramic powder pH value: 7～8
Surface tension: 69mN/m dry product Na
2SO
4Content: 28%
Dry product Cl
-Content :≤0.3% flowing degree of net paste of cement: 215～225mm
Dry product 0.6% volume water-reducing rate: 16%
Dry product 0.6% volume concrete strength sees the following form with blank concrete strength ratio:
| Concrete coagulates the phase | ??R3 | ??R7 | ??R28 |
| Ultimate compression strength MPa | ??30.5 | ??37.5 | ??44.5 |
| With blank strength ratio | ??160 | ??163 | ??124 |
Example 3: refining carbolineum mixes with crude anthracene produces the anthracene sulfonic acid salt cement water reducing agent
200～300 kilograms of the carbolineums and the crude anthracene of purifying are dropped into the sulfonation reaction still for 200～300 kilograms, add 98% vitriol oil, under 120 ℃ of temperature, reacted 3～4 hours, after hydrolysis, added formaldehyde condensation 4～6 hours.The polymeric material neutralizes with liquid caustic soda, transfers pH value 7～8.Drying obtains cement water reducing agent again, and also drying does not manufacture liquid product, and every index is as follows:
Dry product outward appearance: brown ceramic powder pH value: 7～8
Surface tension: 69mN/m dry product Na
2SO
4Content: 33%
Dry product Cl
-Content :≤0.3% flowing degree of net paste of cement: 220～225mm
Dry product 0.6% volume water-reducing rate: 17%
Dry product 0.6% volume concrete strength sees the following form with blank concrete strength ratio:
| Concrete coagulates the phase | ??R3 | ??R7 | ??R28 |
| Ultimate compression strength MPa | ??29.8 | ??38.2 | ??44.0 |
| With blank strength ratio | ??157 | ??166 | ??122 |
Example 4: refining carbolineum or crude anthracene mix with NAPTHALENE FLAKES. (INDUSTRIAL GRADE produces the anthracene sulfonic acid salt cement water reducing agent
With 400 kilograms of NAPTHALENE FLAKES. (INDUSTRIAL GRADE, drop into the sulfonation reaction still, add 98% vitriol oil, after reacting 3～4 hours under 160～165 ℃ of temperature, temperature of reaction kettle is reduced to 150 ℃, 200～300 kilograms of carbolineum that adding is purified or crude anthracenes, reacted 3～4 hours, and after hydrolysis, added formaldehyde condensation 6～8 hours.The polymeric material neutralizes with liquid caustic soda, transfers pH value 7～8.Drying obtains cement water reducing agent again, and also drying does not manufacture liquid product, and every index is as follows:
Dry product outward appearance: light brown powder pH value: 7～8
Surface tension: 69mN/m dry product Na
2SO
4Content: 18%
Dry product Cl
-Content :≤0.3% flowing degree of net paste of cement: 220～225mm
Dry product 0.5% volume water-reducing rate: 17%
Dry product 0.5% volume concrete strength sees the following form with blank concrete strength ratio:
| Concrete coagulates the phase | ??R3 | ??R7 | ??R28 |
| Ultimate compression strength MPa | ??31.0 | ??39 | ??46.4 |
| With blank strength ratio | ??158 | ??163 | ??129 |
Claims (4)
1, the production technique of low bleed high-performance anthracene sulfonic acid salt cement water reducing agent makes raw material through sulfonation, hydrolysis, condensation, neutralization, it is characterized in that described raw material is that carbolineum is obtained purification thing or crude anthracene or both mixtures through fractionation.
2,, it is characterized in that described raw material also comprises NAPTHALENE FLAKES. (INDUSTRIAL GRADE according to the described technology of claim 1.
3,, it is characterized in that the carbolineum cut point is 280～370 ℃ according to the described technology of claim 1.
4,, it is characterized in that sulfonation temperature is 70～150 ℃ according to claim 1 or 2 or 3 described technologies.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100139735A CN1557766A (en) | 2004-01-17 | 2004-01-17 | Production process of low-air-entraining high-performance anthracene sulfonate concrete water reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100139735A CN1557766A (en) | 2004-01-17 | 2004-01-17 | Production process of low-air-entraining high-performance anthracene sulfonate concrete water reducer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1557766A true CN1557766A (en) | 2004-12-29 |
Family
ID=34351222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2004100139735A Pending CN1557766A (en) | 2004-01-17 | 2004-01-17 | Production process of low-air-entraining high-performance anthracene sulfonate concrete water reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1557766A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211911A (en) * | 2011-04-08 | 2011-10-12 | 马清浩 | Cement-based grouting material containing modified naphthalene-series water reducing agent and preparation method thereof |
| CN102211910A (en) * | 2011-04-08 | 2011-10-12 | 马清浩 | Cement-based grouting material containing modified naphthalene-series water reducing agent and preparation method thereof |
| CN102515613A (en) * | 2011-12-05 | 2012-06-27 | 马鞍山中海新材料有限公司 | Method for preparing naphthalene based superplasticizer by using refined naphthalene by-product 90 naphthalene |
| CN104743954A (en) * | 2015-03-18 | 2015-07-01 | 徐兆桐 | Method for preparing water reducer from oxyanthraquinone byproduct |
-
2004
- 2004-01-17 CN CNA2004100139735A patent/CN1557766A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211911A (en) * | 2011-04-08 | 2011-10-12 | 马清浩 | Cement-based grouting material containing modified naphthalene-series water reducing agent and preparation method thereof |
| CN102211910A (en) * | 2011-04-08 | 2011-10-12 | 马清浩 | Cement-based grouting material containing modified naphthalene-series water reducing agent and preparation method thereof |
| CN102211910B (en) * | 2011-04-08 | 2012-10-24 | 马清浩 | Cement-based grouting material containing modified naphthalene-series water reducing agent and preparation method thereof |
| CN102515613A (en) * | 2011-12-05 | 2012-06-27 | 马鞍山中海新材料有限公司 | Method for preparing naphthalene based superplasticizer by using refined naphthalene by-product 90 naphthalene |
| CN102515613B (en) * | 2011-12-05 | 2013-08-07 | 马鞍山中海新材料有限公司 | Method for preparing naphthalene based superplasticizer by using refined naphthalene by-product 90 naphthalene |
| CN104743954A (en) * | 2015-03-18 | 2015-07-01 | 徐兆桐 | Method for preparing water reducer from oxyanthraquinone byproduct |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |