CN108084383A - A kind of high efficiency water reducing agent and preparation method thereof - Google Patents
A kind of high efficiency water reducing agent and preparation method thereof Download PDFInfo
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- CN108084383A CN108084383A CN201711375560.5A CN201711375560A CN108084383A CN 108084383 A CN108084383 A CN 108084383A CN 201711375560 A CN201711375560 A CN 201711375560A CN 108084383 A CN108084383 A CN 108084383A
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- reducing agent
- water
- high efficiency
- sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/0212—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds
- C08G16/0218—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen
- C08G16/0237—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen containing sulfur
-
- 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)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The present invention relates to water-reducing agent fields, and in particular to a kind of high efficiency water reducing agent and preparation method thereof, the water-reducing agent are made of following raw material:10 15 parts of naphtalene oil, 49 parts of liquid caustic soda, 15 20 parts of acetone, 5 11 parts of formaldehyde, 7 12 parts of potassium permanganate, 49 parts of sodium nitrite, 13 21 parts of the concentrated sulfuric acid, appropriate amount of water;The defects of water-reducing agent provided by the present invention effectively compensates for a certain extent easily to go mouldy existing for existing water-reducing agent, low production efficiency.
Description
Technical field
The present invention relates to water-reducing agent fields, and in particular to a kind of high efficiency water reducing agent and preparation method thereof.
Background technology
Water-reducing agent is outside a kind of concrete that under conditions of maintaining concrete slump constant, can reduce mixing water amount
Add agent.Belong to anion surfactant mostly, there is lignosulfonates, naphthalene sulphonate formaldehyde polymer etc..Add in concrete
There is peptizaiton to cement granules after mixture, its workability can be improved, reduce unit consumption of water, improve concrete mix
Mobility;Or unit cement consumption is reduced, save cement.
For a kind of high efficiency water reducing agent is obtained in patent application CN104119021B disclosed in China, by following weight
The raw material of part mixes:Beta-naphthalenesulfonic-acid salt formaldehyde condensation products 50-60, polyethylene glycol monomethyl ethermethacrylic acid esters 20-30,
Calcium lignosulfonate 15-25, ethylene oxide-propylene oxide copolymer 10-15, trehalose 2-4, silicone powder 1.5-2.5, shale ashes
4-8, sodium hydrogensulfite 2.5-4.5, polyethylene glycol oxide 5-10, aluminium triphosphate 8-14, cocounut oil acyl diethanol amine 2-3, dinonyl
Naphthalene sulfonate barium 1-2, methenamine 2-3, auxiliary agent 3-5.Water-reducing agent water-reducing rate of the present invention is high, good fluidity, can obviously improve coagulation
Native mobility and workability, early strong effect is notable after final set, the intensity of concrete each age can be increased substantially, suitable for all kinds of
Concrete;For a kind of high efficiency water reducing agent is obtained in patent application CN101948265A disclosed in China, by a species of orchid oil and calcium lignosulfonate
It is formulated, which is powdery.It is an advantage of the invention that the water-reducing rate of water-reducing agent is high, more than 15% is reached, to mixed
Solidifying soil, which is shunk, to have no adverse effects, and reinforcing bar non-corroding is endangered.
Although what currently available technology was provided prepares water-reducing agent with water-reducing rate height, good fluidity, can obviously improve mixed
The defects of the advantages that solidifying soil mobility and workability, but also exist and easily go mouldy, low production efficiency.
The content of the invention
In view of the above problems, the present invention proposes a kind of high efficiency water reducing agent and preparation method thereof.The present invention provides
Technical solution can make up easily going mouldy present in existing water-reducing agent to a certain extent, the defects of low production efficiency.
In order to realize above-mentioned purpose, the present invention uses following technical solution:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:10-15 parts of naphtalene oil, 4-9 parts of liquid caustic soda, third
15-20 parts of ketone, 5-11 parts of formaldehyde, 7-12 parts of potassium permanganate, 4-9 parts of sodium nitrite, 13-21 parts of the concentrated sulfuric acid, appropriate amount of water.
Preferably, which is made of following raw material:11-13 parts of naphtalene oil, 5-8 parts of liquid caustic soda, acetone 16-18
Part, 7-10 parts of formaldehyde, 8-11 parts of potassium permanganate, 6-8 parts of sodium nitrite, 10-19 parts of the concentrated sulfuric acid, appropriate amount of water.
Preferably, the addition of the naphtalene oil and the concentrated sulfuric acid is 1:1.3-1.4.
Preferably, the preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 130-140 DEG C, in churned mechanically condition
The lower dropwise addition concentrated sulfuric acid, sulfonation 2h;
(2) step (1) products therefrom is cooled to certain temperature, adds in the water equal with naphtalene oil quality, stir 30min,
Obtain hydrolyzate;
(3) hydrolyzate is added in reaction kettle, is cooled to 80-90 DEG C, adjusting pressure is 2-2.5MPa, in the item of stirring
Formaldehyde and acetone are added dropwise under part, condensation reaction occurs, obtains condensation liquid;
(4) condensation liquid pH value is adjusted to 7-9, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain and efficiently subtract
Aqua.
Preferably, mechanical agitation speed is 100-200r/min in the step (1).
Preferably, temperature is 120-125 DEG C after cooling in the step (2).
Using above-mentioned technical solution, beneficial effects of the present invention are as follows:The concentrated sulfuric acid is added in naphtalene oil and is easy to cause office
Portion overheats, so the concentrated sulfuric acid must be added dropwise, is added dropwise while stirring so that between temperature maintains 160-165 DEG C, ensure its sulfonation
Reaction is smoothed out;Sulfonation time section, sulfonation is insufficient, and sulfonation time is long, influences yield, increases production cost;Naphtalene oil with
The concentrated sulfuric acid generates naphthalene sulfonic acids after sulfonating reaction occurs, and naphthalene sulfonic acids hydrolysis generates a part of α-naphthalenesulfonicacid and β naphthalene sulfonic acids, for water
α-naphthalenesulfonicacid is solved, is conducive to later polycondensation reaction, by greenhouse cooling is 120-125 DEG C during hydrolysis, β naphthalene sulfonic acids is stablized at this time,
And α-naphthalenesulfonicacid hydrolyzes;Sodium nitrite is added in water-reducing agent, has certain inhibitory action, and nitrous to the increment of microorganism
Sour sodium decomposes the nitroso generated can also be reacted with the metabolite to go mouldy, so as to play a role.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical solution in the embodiment of the present invention is clearly and completely described.Based on the embodiment of the present invention, the common skill in this field
Art personnel all other embodiments obtained without creative efforts belong to the model that the present invention protects
It encloses.
Embodiment 1:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:10 parts of naphtalene oil, 4 parts of liquid caustic soda, acetone 15
Part, 5 parts of formaldehyde, 7 parts of potassium permanganate, 4 parts of sodium nitrite, 13 parts of the concentrated sulfuric acid, appropriate amount of water.
The preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 130 DEG C, is 100r/ in mechanical agitation speed
The concentrated sulfuric acid, sulfonation 2h are added dropwise under conditions of min;
(2) step (1) products therefrom is cooled to 120 DEG C, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 80 DEG C, adjusting pressure is 2MPa, is added dropwise under conditions of stirring
Formaldehyde and acetone occur condensation reaction, obtain condensation liquid;
(4) condensation liquid pH value is adjusted to 7, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
Embodiment 2:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:15 parts of naphtalene oil, 9 parts of liquid caustic soda, acetone 20
Part, 11 parts of formaldehyde, 12 parts of potassium permanganate, 9 parts of sodium nitrite, 21 parts of the concentrated sulfuric acid, appropriate amount of water.
The preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 140 DEG C, is 200r/ in mechanical agitation speed
The concentrated sulfuric acid, sulfonation 2h are added dropwise under conditions of min;
(2) step (1) products therefrom is cooled to 125 DEG C, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 90 DEG C, adjusting pressure is 2.5MPa, is dripped under conditions of stirring
Add formaldehyde and acetone, condensation reaction occurs, obtains condensation liquid;
(4) condensation liquid pH value is adjusted to 9, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
Embodiment 3:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:11 parts of naphtalene oil, 5 parts of liquid caustic soda, acetone 16
Part, 7 parts of formaldehyde, 8 parts of potassium permanganate, 6 parts of sodium nitrite, 10 parts of the concentrated sulfuric acid, appropriate amount of water.
The preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 135 DEG C, is 120r/ in mechanical agitation speed
The concentrated sulfuric acid, sulfonation 2h are added dropwise under conditions of min;
(2) step (1) products therefrom is cooled to 120 DEG C, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 85 DEG C, adjusting pressure is 2MPa, is added dropwise under conditions of stirring
Formaldehyde and acetone occur condensation reaction, obtain condensation liquid;
(4) condensation liquid pH value is adjusted to 8, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
Embodiment 4:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:13 parts of naphtalene oil, 8 parts of liquid caustic soda, acetone 18
Part, 10 parts of formaldehyde, 11 parts of potassium permanganate, 8 parts of sodium nitrite, 19 parts of the concentrated sulfuric acid, appropriate amount of water.
The preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 135 DEG C, is 120r/ in mechanical agitation speed
The concentrated sulfuric acid, sulfonation 2h are added dropwise under conditions of min;
(2) step (1) products therefrom is cooled to 120 DEG C, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 85 DEG C, adjusting pressure is 2.5MPa, is dripped under conditions of stirring
Add formaldehyde and acetone, condensation reaction occurs, obtains condensation liquid;
(4) condensation liquid pH value is adjusted to 7, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
Embodiment 5:
A kind of high efficiency water reducing agent, the water-reducing agent are made of following raw material:13 parts of naphtalene oil, 7 parts of liquid caustic soda, acetone 17
Part, 8 parts of formaldehyde, 9 parts of potassium permanganate, 7 parts of sodium nitrite, 14 parts of the concentrated sulfuric acid, appropriate amount of water.
The preparation method of the water-reducing agent includes the following steps:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 135 DEG C, is 150r/ in mechanical agitation speed
The concentrated sulfuric acid, sulfonation 2h are added dropwise under conditions of min;
(2) step (1) products therefrom is cooled to 125 DEG C, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 90 DEG C, adjusting pressure is 2-2.5MPa, under conditions of stirring
Formaldehyde and acetone is added dropwise, condensation reaction occurs, obtains condensation liquid;
(4) condensation liquid pH value is adjusted to 9, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
The parameter of the water-reducing agent such as following table:
Product common in product provided by the present invention and market is done into performance comparison test, test result is as follows:
To sum up, the embodiment of the present invention has the advantages that:The water-reducing agent of the present invention is simple and easy to control with production process,
Cement granules are had peptizaiton by the characteristics of yield is high, and anti-mildew effect is good, can improve its workability, reduce unit consumption of water,
Improve the mobility of concrete mix.
Above example is only to illustrate the technical solution of type of the present invention, rather than its limitations;Although with reference to foregoing implementation
Type of the present invention is described in detail in example, it will be understood by those of ordinary skill in the art that:It still can be to foregoing each
Technical solution recorded in embodiment modifies or carries out equivalent substitution to which part technical characteristic;And these are changed
Or replace, the essence of appropriate technical solution is not made to depart from the spirit and scope of each embodiment technical solution of type of the present invention.
Claims (6)
1. a kind of high efficiency water reducing agent, which is made of following raw material:10-15 parts of naphtalene oil, 4-9 parts of liquid caustic soda, acetone
15-20 parts, 5-11 parts of formaldehyde, 7-12 parts of potassium permanganate, 4-9 parts of sodium nitrite, 13-21 parts of the concentrated sulfuric acid, appropriate amount of water.
2. high efficiency water reducing agent according to claim 1, which is characterized in that the water-reducing agent is made of following raw material:
It is 11-13 parts of naphtalene oil, 5-8 parts of liquid caustic soda, 16-18 parts of acetone, 7-10 parts of formaldehyde, 8-11 parts of potassium permanganate, 6-8 parts of sodium nitrite, dense
10-19 parts of sulfuric acid, appropriate amount of water.
3. high efficiency water reducing agent according to claim 1, which is characterized in that the addition of the naphtalene oil and the concentrated sulfuric acid is
1:1.3-1.4。
4. high efficiency water reducing agent according to claim 1, which is characterized in that the preparation method of the water-reducing agent includes following several
Step:
(1) naphtalene oil and potassium permanganate are added in reaction pot, heating is melted to 130-140 DEG C, is dripped under conditions of mechanical agitation
Enriching sulfuric acid, sulfonation 2h;
(2) step (1) products therefrom is cooled to certain temperature, adds in the water equal with naphtalene oil quality, stirred 30min, obtain water
Solve liquid;
(3) hydrolyzate is added in reaction kettle, is cooled to 80-90 DEG C, adjusting pressure is 2-2.5MPa, is dripped under conditions of stirring
Add formaldehyde and acetone, condensation reaction occurs, obtains condensation liquid;
(4) condensation liquid pH value is adjusted to 7-9, then adds liquid caustic soda and sodium nitrite thereto, stir evenly, obtain efficient diminishing
Agent.
5. high efficiency water reducing agent according to claim 4, which is characterized in that mechanical agitation speed is in the step (1)
100-200r/min。
6. high efficiency water reducing agent according to claim 4, which is characterized in that temperature is 120- after cooling in the step (2)
125℃。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108047403A (en) * | 2017-12-19 | 2018-05-18 | 萧县沃德化工科技有限公司 | A kind of aliphatic water reducing agent and preparation method thereof |
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CN108047403A (en) * | 2017-12-19 | 2018-05-18 | 萧县沃德化工科技有限公司 | A kind of aliphatic water reducing agent and preparation method thereof |
CN108101402A (en) * | 2017-12-19 | 2018-06-01 | 萧县沃德化工科技有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof |
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2017
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US20030217847A1 (en) * | 1999-07-15 | 2003-11-27 | Reddy B. Raghava | Methods of cementing |
CN102464464A (en) * | 2010-11-09 | 2012-05-23 | 浙江龙盛集团股份有限公司 | Preparation method of naphthalene series water reducer |
CN102491671A (en) * | 2011-11-18 | 2012-06-13 | 大连科诺科技发展有限公司 | Concrete nano water-reducing super high-early-strength agent |
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Application publication date: 20180529 |