CN111484589B - Preparation method of modified melamine water reducer - Google Patents
Preparation method of modified melamine water reducer Download PDFInfo
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- CN111484589B CN111484589B CN202010287923.5A CN202010287923A CN111484589B CN 111484589 B CN111484589 B CN 111484589B CN 202010287923 A CN202010287923 A CN 202010287923A CN 111484589 B CN111484589 B CN 111484589B
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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
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
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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
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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
- 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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a simple preparation method of a modified melamine water reducer, and mainly relates to the field of water reducers. Adding a proper amount of water into a sealing device, adding quantitative sodium sulfanilate, melamine and formaldehyde under the drive of a circulating pump, respectively adjusting the pH value of the system by using sodium hydroxide and sulfuric acid at different stages according to the reaction conditions of the process requirements, and carrying out constant-temperature circulating reaction. The invention has the beneficial effects that: the preparation process has low energy consumption, safety and simple process, ensures that the performance of the melamine water reducing agent is better, and improves various problems in the prior art.
Description
Technical Field
The invention relates to the field of water reducing agents, in particular to a preparation method of a modified melamine water reducing agent.
Background
The melamine water reducing agent is successfully developed in Germany in 1963, and is also successfully developed and industrially produced in 70 years in the last century in China. The whole synthesis reaction has four courses: methylolation, sulfonation, polycondensation, neutralization of melamine. The temperature range of the reaction process is 70-90 degrees, steam or electric heating is usually adopted in industrial production, and the energy consumption is very large.
Patent CN 103254380B reports a method for preparing a melamine high-efficiency water reducing agent, wherein a sulfonating agent in production adopts an acidic component, then alkali is added for neutralization, and the heat release of neutralization reaction is utilized to realize the production without an external heat source. Although the method can realize non-heat source production, the process control has a violent exothermic reaction stage, the pressure in the reaction kettle rises instantly, the control is not easy, accidents such as material spraying and the like are easy to cause, and potential safety production hazards exist.
The production of the melamine water reducing agent generally adopts an enamel reaction kettle or a stainless steel reaction kettle, an inner coil or a jacket is arranged to be filled with cooling water for cooling, and a motor, a speed reducer and a corresponding standard stirring paddle are arranged, so that the defects of large investment, complex production process and the like exist.
In conclusion, it is necessary to provide a method for preparing the melamine water reducing agent, which is energy-saving, safe and simple.
Disclosure of Invention
The invention aims to provide a preparation method of a modified melamine water reducer, which has the advantages of low energy consumption, safety and simple process in the preparation process, enables the performance of the melamine water reducer to be better and solves various problems in the prior art.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a modified melamine water reducer comprises the following steps:
150-250 g of sodium sulfanilate, 110-130 g of melamine and 350-450 g of formaldehyde are put into 400-700 g of water for closed reaction;
regulating the pH value of a pH system to 6-6.4 by using sulfuric acid, and carrying out constant-temperature circulating reaction for 5.5-6.5 hours;
adjusting the pH value of the system to 6.8-7.0, and carrying out constant-temperature circulating reaction for 6.5-7.5 hours;
adjusting the pH value of the system to 11-11.2, and carrying out constant-temperature circulating reaction for 7.5-8.5 hours.
Further, the method comprises the following steps:
adding 208 g of sodium sulfanilate, 126 g of melamine and 380 g of formaldehyde into 487g of water, and carrying out a closed reaction;
regulating the pH value of a pH system to be 6 by using sulfuric acid, and carrying out constant-temperature circulating reaction for 6 hours;
adjusting the pH value of the system to 6.8, and carrying out constant-temperature circulating reaction for 7 hours;
the pH of the system is adjusted to be 11, and the reaction is carried out for 8 hours in a constant temperature circulating manner.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention only uses the sodium sulfanilate as the sulfonating agent, and the water reducing agent has higher water reducing rate and slump retaining performance because the product can form a more three-dimensional adsorption layer on the surface of cement particles and has larger steric hindrance compared with the water reducing agent synthesized by common sulfonating agents such as sodium sulfite and the like.
2) The whole reaction process is mild and exothermic, and has no potential safety production hazards such as material spraying and the like.
3) The whole reaction material homogenizing process is driven by only one circulating pump, and no external heat source is needed for heating reaction in production, so that the energy consumption is lower.
4) The reaction equipment is shown in figure 1, only one storage tank with good sealing condition and one set of circulating device are used for meeting the production requirement, and equipment such as a boiler, a reaction kettle, a condenser, cooling water circulation and the like is not required to be equipped.
In conclusion, the method has the advantages of better performance of the melamine water reducing agent, safe production process, low energy consumption and simpler process and equipment through technical optimization.
Drawings
FIG. 1 is a schematic diagram of an apparatus used in the present invention.
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 modified melamine water reducer
Adding 557g of metered water into the equipment shown in the figure 1, starting a circulating pump, adding 162 g of sodium sulfanilate and 126 g of melamine, adding 5g of sodium hydroxide and adding 400 g of formaldehyde; adding sulfuric acid to adjust the pH value to 6, carrying out constant temperature circulating reaction for 6 hours, adjusting the pH value to 6.8, carrying out constant temperature circulating reaction for 7 hours, finally adjusting the pH value to 11, carrying out constant temperature circulating reaction for 8 hours, and discharging.
The structure of the device is as follows:
a sealed heat-preservation reaction tank can be a vertical tank or a horizontal tank, a material pipeline shown in the attached drawing 1 is arranged on the reaction tank, and specifically comprises a water inlet pipe, a circulating pipe and a material beating pipe, wherein the water inlet pipe is used for inputting water into the reaction tank in a one-way mode, the water inlet pipe is connected to the reaction tank and provided with a water inlet valve, one end of the circulating pipe is connected to the water inlet pipe, the other end of the circulating pipe is connected to the bottom of the reaction tank and provided with a circulating pump, the circulating pipe is provided with a valve 2 and a valve 5, the valve 5 is in front of incoming materials of the circulating pump, the valve 2 is behind the circulating pump, the circulating pipe is connected with a material mixing pipe, one end of the material mixing pipe is connected between the valve 5 and the circulating pump, the other end of the material mixing pipe is connected between the valve 2 and the circulating pump, the material feeding pipe with a valve is arranged on the material mixing pipe and used for feeding materials, acid-base regulators, sampling and the like, and the valves are arranged in front and back of a material feeding port and are respectively provided with the valve 3 and the valve 4. The circulating pipe is connected with a material beating pipe, and the material beating pipe is provided with a valve 1 for controlling discharging.
The material flow is shown in figure 1.
The reaction scheme of the equipment is as follows:
adding water from a water inlet according to the formula amount, opening a valve 3, a valve 4 and a valve 5, starting a circulating pump, feeding powder according to the formula amount from a feeding port, closing the valve 3 and the valve 4 after the feeding is finished, opening the valve 2, and carrying out material circulating reaction until the reaction is finished.
And opening the valve 1 to perform material beating.
Example 2: preparation method of modified melamine water reducer
Adding 666 g of metered water into the equipment shown in the figure 1, starting a circulating pump, adding 185 g of sodium sulfanilate and 126 g of melamine, adding 5g of sodium hydroxide, and adding 370 g of formaldehyde; adding sulfuric acid to adjust the pH value to 6, carrying out constant temperature circulating reaction for 6 hours, adjusting the pH value to 6.8, carrying out constant temperature circulating reaction for 7 hours, finally adjusting the pH value to 11, carrying out constant temperature circulating reaction for 8 hours, and discharging.
The reaction equipment and the flow are the same as in example 1.
Example 3: preparation method of modified melamine water reducer
Adding 487g of metered water into the equipment shown in the figure 1, starting a circulating pump, adding 208 g of sodium sulfanilate and 126 g of melamine, adding 5g of sodium hydroxide and adding 380 g of formaldehyde; adding sulfuric acid to adjust the pH value to 6, carrying out constant temperature circulating reaction for 6 hours, adjusting the pH value to 6.8, carrying out constant temperature circulating reaction for 7 hours, finally adjusting the pH value to 11, carrying out constant temperature circulating reaction for 8 hours, and discharging.
The reaction equipment and the flow are the same as in example 1.
Example 4: performance testing
The samples synthesized in the above examples were tested according to the test method for the fluidity of the cement paste in GB/T8077-2012 "the homogeneity test method for concrete admixtures", and the test method for the determination of the water reduction rate in GB8076-2008 "the concrete admixtures", and the water reducing agent prepared by the conventional synthesis method for melamine water reducing agents was used as a comparative sample, and the results are shown in table 1.
TABLE 1
As can be seen from the above clear paste and concrete test data, the performance of the melamine water reducer synthesized by the invention is superior to that of the melamine water reducer synthesized by the conventional method.
Claims (4)
1. The preparation method of the modified melamine water reducer is characterized by comprising the following steps:
adding 208 g of sodium sulfanilate, 126 g of melamine, 5g of sodium hydroxide and 380 g of formaldehyde into 487g of water, and carrying out closed reaction;
adjusting the pH value of a pH system to 6 by using sulfuric acid, and carrying out constant-temperature circulating reaction for 6 hours;
adjusting the pH value of the system to 6.8, and carrying out constant-temperature circulating reaction for 7 hours;
adjusting the pH value of the system to 11, and carrying out constant-temperature circulating reaction for 8 hours;
the whole production process does not need an external heat source for heating.
2. A preparation method of a modified melamine water reducer is characterized by comprising the following steps: adding 557g of metered water, starting a circulating pump, adding 162 g of sodium sulfanilate and 126 g of melamine, adding 5g of sodium hydroxide and adding 400 g of formaldehyde; adding sulfuric acid to adjust the pH value to 6, carrying out constant temperature circulating reaction for 6 hours, adjusting the pH value to 6.8, carrying out constant temperature circulating reaction for 7 hours, finally adjusting the pH value to 11, and carrying out constant temperature circulating reaction for 8 hours;
the whole production process does not need an external heat source for heating.
3. A preparation method of a modified melamine water reducer is characterized by comprising the following steps:
adding 666 g of metered water, starting a circulating pump, adding 185 g of sulfanilic acid and 126 g of melamine, adding 5g of sodium hydroxide, and adding 370 g of formaldehyde; adding sulfuric acid to adjust the pH value to 6, carrying out constant temperature circulating reaction for 6 hours, adjusting the pH value to 6.8, carrying out constant temperature circulating reaction for 7 hours, finally adjusting the pH value to 11, and carrying out constant temperature circulating reaction for 8 hours;
the whole production process does not need an external heat source for heating.
4. The preparation method of the modified melamine water reducer according to claim 1, characterized in that: the method comprises the following steps of carrying out reaction through a constant-temperature sealed reaction tank, wherein the top of the reaction tank is connected with a water inlet pipe, the water inlet pipe is provided with a water inlet valve, a circulating pipe is connected between the water inlet pipe and the reaction tank, the circulating pipe is provided with a circulating pump, the circulating pump is connected with a material mixing pipe, the material mixing pipe is provided with a feeding port, and the circulating pipe is connected with a material beating pipe for discharging;
the circulating pipe is used for carrying out circulating reaction on the materials;
and the feed inlet is used for feeding materials and acid-base balancing agents.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09302057A (en) * | 1996-05-09 | 1997-11-25 | Nissan Chem Ind Ltd | Production of aqueous solution of water-reducing agent |
| JP2000191739A (en) * | 1998-10-23 | 2000-07-11 | Nissan Chem Ind Ltd | Production of aqueous solution of sulfanilic acid-modified melamine formaldehyde resin |
| CN101717480A (en) * | 2009-11-13 | 2010-06-02 | 济南京科工贸有限公司 | Preparing method of heating-free aliphatic superplasticizer admixture |
| CA2793584A1 (en) * | 2010-07-27 | 2012-02-02 | Shanghai Taijie Chemical Co., Ltd. | Synthesis method of polycarboxylic acid water-reducing agent |
| CN103254380A (en) * | 2013-05-10 | 2013-08-21 | 济南融祺建材有限公司 | Production method of melamine high-efficiency water reducer |
| CN103539380A (en) * | 2013-10-08 | 2014-01-29 | 济南融祺建材有限公司 | Energy-saving and integrated production method of efficient water reducing agent |
-
2020
- 2020-04-14 CN CN202010287923.5A patent/CN111484589B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09302057A (en) * | 1996-05-09 | 1997-11-25 | Nissan Chem Ind Ltd | Production of aqueous solution of water-reducing agent |
| JP2000191739A (en) * | 1998-10-23 | 2000-07-11 | Nissan Chem Ind Ltd | Production of aqueous solution of sulfanilic acid-modified melamine formaldehyde resin |
| CN101717480A (en) * | 2009-11-13 | 2010-06-02 | 济南京科工贸有限公司 | Preparing method of heating-free aliphatic superplasticizer admixture |
| CA2793584A1 (en) * | 2010-07-27 | 2012-02-02 | Shanghai Taijie Chemical Co., Ltd. | Synthesis method of polycarboxylic acid water-reducing agent |
| CN103254380A (en) * | 2013-05-10 | 2013-08-21 | 济南融祺建材有限公司 | Production method of melamine high-efficiency water reducer |
| CN103539380A (en) * | 2013-10-08 | 2014-01-29 | 济南融祺建材有限公司 | Energy-saving and integrated production method of efficient water reducing agent |
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Effective date of registration: 20221110 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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