CN111484591B - Preparation method of retarding water reducer - Google Patents
Preparation method of retarding water reducer Download PDFInfo
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- CN111484591B CN111484591B CN202010287924.XA CN202010287924A CN111484591B CN 111484591 B CN111484591 B CN 111484591B CN 202010287924 A CN202010287924 A CN 202010287924A CN 111484591 B CN111484591 B CN 111484591B
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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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
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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)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a preparation method of a retarding water reducer, and mainly relates to the field of concrete admixtures. Adding metered water, sulfanilic acid or sodium sulfanilate, salicylic acid or sodium salicylate and glucose in formula amount into a four-neck flask, adjusting to be alkaline by using sodium hydroxide, heating to 90 ℃, dropwise adding a formaldehyde solution, and reacting at constant temperature until the reaction is finished. The invention has the beneficial effects that: the condensation reaction is carried out by using materials with different functional groups, and the condensation reaction has the characteristics of high water reduction, controllable slow setting time, good adaptability to sandstone materials and the like.
Description
Technical Field
The invention relates to the field of concrete admixtures, in particular to a preparation method of a retarding water reducer.
Background
The water reducing agents widely used at home and abroad at present mainly comprise polycarboxylic acid, naphthalene sulfonate, melamine, sulfamic acid and aliphatic water reducing agents, the polycarboxylic acid water reducing agent is prepared by free radical polymerization reaction of unsaturated monomers, and the other four water reducing agents are high-molecular formaldehyde polycondensates of sulfonic acids. In order to meet the actual engineering requirements, various water reducing agents are usually compounded with retarders when used. Commonly used retarders include saccharides, hydroxycarboxylic acids, etc., all of which have hydroxyl groups or both of hydroxyl and carboxyl functional groups. Although the compound retarder can solve the problem of short setting time of concrete under most conditions, the conditions of mismatching of retarder type and cement, poor adaptability and concrete bleeding segregation are common reports even for engineering accidents without setting for days.
The polycarboxylate superplasticizer has the characteristics of adjustable and controllable molecular structure and capability of polymerizing according to a pre-designed structure, so that in recent years, a scholars introduces a retarding group into the polycarboxylate superplasticizer to synthesize a retarding polycarboxylate superplasticizer, but the slow-setting polycarboxylate superplasticizer is not suitable for sand and stone materials with high mud content. The sulfonic acid water reducing agent does not contain polyether long side chain, so that the adaptability to sand and mud containing is better than that of the polycarboxylic acid water reducing agent.
The retarding group is introduced into the molecular structure of the sulfonic acid water reducing agent, so that the polymer has the retarding function, and has the advantages of good adaptability, adjustable setting time and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a retarding water reducer, which utilizes materials with different functional groups to carry out condensation reaction and has the characteristics of high water reduction, controllable retarding time, good adaptability to sandstone materials and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a retarding water reducer comprises the following steps:
adding 450-600g of water, 150-180g of sulfanilic acid or 210-230g of sulfanilic acid sodium salt, 140-160g of salicylic acid or 160-180g of sodium salicylate and 15-35g of glucose into a reaction container, and uniformly stirring;
adjusting the pH of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dripping 170-190g of formaldehyde solution for 3-5 hours;
after the formaldehyde solution is dripped, reacting for 3-5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
Preferably, the method comprises the following steps:
471g of water, 163 g of sulfanilic acid, 150 g of salicylic acid and 20 g of glucose are added into a reaction container and stirred uniformly;
adjusting the pH of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dropwise adding 180g of formaldehyde solution for 4 hours;
after the formaldehyde solution is dripped, reacting for 5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
Preferably, the method comprises the following steps:
adding 575 g of water, 220 g of sodium sulfanilate, 171 g of sodium salicylate and 30g of glucose into a reaction container;
adjusting the pH of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dropwise adding 180g of formaldehyde solution for 4 hours;
after the formaldehyde solution is dripped, reacting for 5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
The reaction vessel is a four-neck flask provided with a reflux condenser, a stirrer and a thermometer.
Compared with the prior art, the invention has the beneficial effects that:
the invention is prepared by condensing sulfanilic acid or sulfanilic acid sodium sulfanilate and salicylic acid or sodium salicylate through formaldehyde and glucose under the alkaline condition. The sulfanilic acid provides strong hydrophilicity through sulfonic acid groups, the benzene ring of the salicylic acid contains adjacent hydroxyl and carboxyl, the slow-setting function is strong, the glucose has the characteristic of aldehyde, the condensation reaction can be carried out by partially or completely replacing formaldehyde under the alkaline condition, meanwhile, the glucose contains a large number of hydroxyl, and the slow-setting function is also strong, SO that the molecular chain containing-SO is prepared under the proper reaction condition 3 H, -OH, -COOH and other functional groups. The water reducing agent has the characteristics of high water reducing rate, controllable retardation time, good adaptability to sandstone materials and the like, and has a good development prospect.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example 1: preparation method of retarding water reducer
471g of water, 163 g of sulfanilic acid, 150 g of salicylic acid and 20 g of glucose are added into a four-neck flask provided with a reflux condenser, a stirrer and a thermometer, the mixture is neutralized by sodium hydroxide until the pH value is 10, the temperature is raised to 90 ℃, 180g of formaldehyde solution is dropwise added, the dropwise addition time is 4 hours, and the constant temperature reaction is carried out for 5 hours.
Example 2: preparation method of retarding water reducer
575 g of water, 220 g of sodium sulfanilate, 171 g of sodium salicylate and 30g of glucose are added into a four-neck flask provided with a reflux condenser, a stirrer and a thermometer, neutralized by sodium hydroxide until the pH value is 10, heated to 90 ℃, 180g of formaldehyde solution is dropwise added for 4 hours, and the constant temperature reaction is carried out for 5 hours.
Example 3: performance testing
1. Determination of cement paste fluidity and cement paste setting time: the samples synthesized in the above examples were tested according to GB/T8077-2012 "method for testing homogeneity of concrete admixtures" and "method for testing water consumption, setting time, and stability at standard consistency of cement", and the mixing amount of the set-retarding water reducer prepared by the present invention was 1.8%, and the results are shown in table 1.
TABLE 1
Note: in the table "- -" represents no net slurry fluidity.
As can be seen from the test data, the retarding water reducer synthesized by the invention has good retarding effect.
2. Testing the performance of the concrete: the test is carried out according to GB8076-2008 'concrete admixture', and the result is shown in Table 2.
TABLE 2
As can be seen from the test data, the retarding water reducer synthesized by the invention has good water reducing and slump retaining effects.
Claims (4)
1. The preparation method of the retarding water reducer is characterized by comprising the following steps:
adding 450-600g of water, 150-180g of sulfanilic acid or 210-230g of sulfanilic acid sodium salt, 140-160g of salicylic acid or 160-180g of sodium salicylate and 15-35g of glucose into a reaction container, and uniformly stirring;
adjusting the PH of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dripping 170-190g of formaldehyde solution for 3-5 hours;
after the formaldehyde solution is dripped, reacting for 3-5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
2. The preparation method of the set-retarding water reducer according to claim 1, characterized by comprising the following steps:
471g of water, 163 g of sulfanilic acid, 150 g of salicylic acid and 20 g of glucose are added into a reaction container and stirred uniformly;
adjusting the Ph of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dropwise adding 180g of formaldehyde solution for 4 hours;
after the formaldehyde solution is dripped, reacting for 5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
3. The preparation method of the set-retarding water reducer according to claim 1, characterized by comprising the following steps:
adding 575 g of water, 220 g of sodium sulfanilate, 171 g of sodium salicylate and 30g of glucose into a reaction container;
adjusting the PH of the system to 10 by using sodium hydroxide, and heating to 90 ℃;
dropwise adding 180g of formaldehyde solution for 4 hours;
after the formaldehyde solution is dripped, reacting for 5 hours at the constant temperature of 90 ℃;
cooling to 50 deg.C, and discharging.
4. The method for preparing the water reducing agent of claim 1, 2 or 3, wherein the reaction vessel is a four-neck flask equipped with a reflux condenser, a stirrer and a thermometer.
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| CN202010287924.XA CN111484591B (en) | 2020-04-14 | 2020-04-14 | Preparation method of retarding water reducer |
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| CN111484591B true CN111484591B (en) | 2023-03-31 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000351661A (en) * | 1999-04-08 | 2000-12-19 | Nissan Chem Ind Ltd | Cement composition containing sulfanilic acid-modified melamine-formaldehyde resin |
| CN1621383A (en) * | 2003-11-26 | 2005-06-01 | 杜云青 | Modified melamine high efficiency water reducing agent |
| CN104119013A (en) * | 2014-07-21 | 2014-10-29 | 广西科技大学 | Preparation method of glucose-base setting-retarding water reducer |
| CN104496248A (en) * | 2014-11-03 | 2015-04-08 | 广西南宁至简至凡科技咨询有限公司 | Preparation method of water reducer for concrete |
| CN105017517A (en) * | 2015-07-08 | 2015-11-04 | 广西科技大学 | Preparation method for green, environment-friendly and highly-efficient retardation type water reducer |
-
2020
- 2020-04-14 CN CN202010287924.XA patent/CN111484591B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000351661A (en) * | 1999-04-08 | 2000-12-19 | Nissan Chem Ind Ltd | Cement composition containing sulfanilic acid-modified melamine-formaldehyde resin |
| CN1621383A (en) * | 2003-11-26 | 2005-06-01 | 杜云青 | Modified melamine high efficiency water reducing agent |
| CN104119013A (en) * | 2014-07-21 | 2014-10-29 | 广西科技大学 | Preparation method of glucose-base setting-retarding water reducer |
| CN104496248A (en) * | 2014-11-03 | 2015-04-08 | 广西南宁至简至凡科技咨询有限公司 | Preparation method of water reducer for concrete |
| CN105017517A (en) * | 2015-07-08 | 2015-11-04 | 广西科技大学 | Preparation method for green, environment-friendly and highly-efficient retardation type water reducer |
Non-Patent Citations (1)
| Title |
|---|
| 羟基氨基羧基磺酸系高效减水剂的应用性能研究;赵晖等;《新型建筑材料》;20081031(第10期);摘要，1.1AH高效减水剂的合成，3.2AH高效减水剂掺量对混凝土凝结时间的影响 * |
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Effective date of registration: 20230308 Address after: 251600 Shahe Industrial Park, Shahe Town, Shanghe County, Jinan City, Shandong Province Applicant after: Shandong Hengfeng Tianli New Material Technology Co.,Ltd. Address before: 250105 Dong Jia Zhen Dong Jia Zhuang Cun East, Licheng District, Jinan City, Shandong Province Applicant before: JINAN RONGQI BUILDING MATERIAL Co.,Ltd. |
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