CN102452806A - Novel melamine water reducer and preparation method - Google Patents
Novel melamine water reducer and preparation method Download PDFInfo
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- CN102452806A CN102452806A CN2010105098510A CN201010509851A CN102452806A CN 102452806 A CN102452806 A CN 102452806A CN 2010105098510 A CN2010105098510 A CN 2010105098510A CN 201010509851 A CN201010509851 A CN 201010509851A CN 102452806 A CN102452806 A CN 102452806A
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Abstract
The invention relates to a novel melamine water reducer which comprises the following raw materials by mass: 18.7-23.2% of melamine, 38-42.6% of formaldehyde, 20-27% of sodium bisulfite, 2-3% of sulfuric acid, 3-5% of liquid alkali, and 20-30% of water. The method of the invention comprises the following steps: adding water, melamine, the formaldehyde solution into a reaction vessel, stirring and heating to 50-60 DEG C for reaction for 1-3 hours, performing heat preservation and reaction at 60-75 DEG C for 1-5 hours, adjusting the pH of the solution to 8.5-9.5 by the liquid alkali solution; adding sodium bisulfite, heating, reacting at 84-90 DEG C for 1-3 hours, maintaining the pH at 10-11; finally cooling the solution to 50 DEG C, adjusting the pH value to 5-6.5 by 30% sulfuric acid, continuing the reaction for 1-2 hours, neutralizing the solution to obtain a pH of 7, discharging to obtain the finished product. The water reducer prepared by the invention has strong water retention capacity for concrete, a high water-reducing rate, high early strength of concrete, low air entraining, and less slump loss.
Description
Technical field
The present invention relates to technical field of concrete additives, particularly a kind of novel melamine water reducer and preparation method.
Background technology
Cement concrete is the maximum material of construction of consumption in the world, but cement concrete exists from great, intensity low with weakness such as fragility.Along with developing rapidly of construction industry, the performance of concrete each side is constantly proposed new requirement, as improved concrete intensity, improve loss of slump in the concrete transportation etc.Normal concrete has been difficult to satisfy new construction process requirement.The admixture admixture is effective, the easy and economic method that improves concrete strength, improves the various performances of concrete in concrete.Water reducer is the maximum admixture kind of consumption in the concrete.
Along with the development of concrete admixture industry, the research work of novel concrete high efficiency water reducing agent is also constantly being goed deep into.Just at present domestic, in order to satisfy different construction requirements, the admixture industry still generally adopts composite mode, has high-performance, multi-functional single high efficiency water reducing agent is still less.The kind of at present domestic high efficiency water reducing agent mainly contains: high-efficiency water-reducing agent of poly-carboxylic acid, sulfamate high-effective water-reducing agent, naphthalenesulfonate high efficiency water reducing agent; But above three kinds of high efficiency water reducing agents are the problem of various degrees again in use: though the high-efficiency water-reducing agent of poly-carboxylic acid water-reducing rate is high; But reaction is responsive, is difficult to control in the construction process; Sulfamate high-effective water-reducing agent is owing to molecular structure, and concrete water bleeding is serious, and construction quality is difficult to be guaranteed; The naphthalenesulfonate high efficiency water reducing agent is the most frequently used high efficiency water reducing agent, and low dense product naphthalenesulfonate high efficiency water reducing agent sodium sulphate content is very easily separated out under coldcondition and caused plugging up to 20%, all causes bigger influence for engineering construction.Therefore, a kind ofly have good flexibility, bleeding rate is low, slump-loss is little, production technique is simple, easy to use high efficiency water reducing agent becomes the direction that the admixture industry is pursued always and made great efforts.
Melamine system water reducer is a kind of anionic, strong, non-bleed type high efficiency water reducing agent early, and excellent performance, and is environmentally friendly; It can obviously improve concrete multiple performance, and comparing with general cement water reducing agent has significant diminishing, and reinforced effects is obvious; Especially sclerosis back endurance performance of concrete obviously improves; No bleed property can not form a large amount of bubbles at inside concrete, and is strong to the flexibility of cement type; Good with the consistency of other admixture, can composite together use form multi-functional compound additive.Its color is colourless or white, is suitable for clear-water concrete.
Along with the continuous development of melamine high-efficiency water-reducing agent, to the further investigation of the modification work of molecular structure, melamine high-efficiency water-reducing agent has obtained increasing application.Like patent publication No. CN1621383A; Open day is on June 1st, 2005; Disclosed modified melamine high-efficiency water-reducing agent is that melamine high-efficiency water-reducing agent is in the past carried out modification; Improved concrete time of coagulation, made concrete big problem of slump-loss in transportation, construction process obtain solution.But it is compared with melamine high-efficiency water-reducing agent in the past, and its diminishing, water conservation effect improve not obviously.
Summary of the invention
In order to overcome above defective, the technical problem that the present invention will solve is: a kind of novel melamine water reducer and preparation method are provided, and the water reducer product that makes is strong to the concrete water retention property; Water-reducing rate is high; Characteristics such as early age strength of concrete is high, hangs down bleed, and slump-loss is little.
The technical scheme that the present invention adopted is: a kind of novel melamine water reducer, and according to the mass fraction, composition of raw materials is:
Trimeric cyanamide 18.7-23.2%;
Formaldehyde 38-42.6%;
Sodium sulfite anhy 96 20-27%;
Sulfuric acid 2-3%;
Liquid caustic soda 3-5%;
Water 20-30%.
According to another preferred embodiment, a kind of novel melamine water reducer comprises that further described formaldehyde is a kind of in Paraformaldehyde 96 or the 20-37% formalin.
According to another preferred embodiment, a kind of novel melamine water reducer comprises that further described liquid caustic soda is a kind of in sodium hydroxide, Pottasium Hydroxide or the calcium hydroxide.
According to another preferred embodiment, a kind of novel melamine water reducer comprises that further described sulfuric acid is 30% sulphuric acid soln.
The invention also discloses a kind of preparation method of novel melamine water reducer, it is characterized in that may further comprise the steps:
1) in the reaction kettle that TM, condensing surface, whisking appliance are housed, adds entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 1-3 hour; 60-75 ℃ insulation reaction 1-5 hour, after hydroxymethylation finishes, the solution pH value is transferred to 8.5-9.5 with 32% liquid caustic soda solution;
(2) sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 1-3 hour;
(3) after sulfonation reaction finishes, solution temperature is reduced to 50 ℃, to 5-6.5, continues reaction 1-2 hour with the pH value of sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
The invention has the beneficial effects as follows:
1, have extremely strong flexibility, various concrete and admixture are all had fabulous intermiscibility, can be with other admixtures (like air entrapment agent, retardant, swelling agent, hardening accelerator etc.) use or composite.
2, water-reducing rate is high, can reach 14-30%, and concrete is not emanated, and slump-loss is little, more helps concrete transportation, cast.
3, air content is little, and concrete strength is high, and chloride ion-containing not is to the effect of reinforcing bar non-corroding.Can be widely used in Highrise buildings, road engineering, hydroelectric project, large scale prefabricated member and the cement products.
4, early age strength of concrete is high, and strong to the flexibility of temperature, can not produce very big variation because of the difference of temperature.
Embodiment
In conjunction with the preferred embodiments the present invention is done further detailed explanation now.
Embodiment 1
A kind of novel melamine water reducer, raw materials quality per-cent is:
Trimeric cyanamide 19%;
Paraformaldehyde 96 38%;
Sodium sulfite anhy 96 20%;
30% sulfuric acid 2%;
Sodium hydroxide solution 3%;
Water 20%.
In the reaction kettle that TM, condensing surface, whisking appliance are housed, add entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 1 hour; 60-75 ℃ of insulation reaction 1 hour, hydroxymethylation transfers to 8.5-9.5 with sodium hydroxide solution with the solution pH value after finishing; Sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 1 hour; After sulfonation reaction finishes, solution temperature is reduced to 50 ℃,, continues to react 1 hour to 5-6.5 with the pH value of 30% sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
Embodiment 2
A kind of novel melamine water reducer, raw materials quality per-cent is:
Trimeric cyanamide 20%;
Paraformaldehyde 96 39%;
Sodium sulfite anhy 96 22%;
30% sulfuric acid 2.4%;
Sodium hydroxide solution 3%;
Water 25%.
In the reaction kettle that TM, condensing surface, whisking appliance are housed, add entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 1 hour; 60-75 ℃ of insulation reaction 2 hours, hydroxymethylation transfers to 8.5-9.5 with sodium hydroxide solution with the solution pH value after finishing; Sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 1 hour; After sulfonation reaction finishes, solution temperature is reduced to 50 ℃,, continues to react 1.5 hours to 5-6.5 with the pH value of 30% sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
Embodiment 3
A kind of novel melamine water reducer, raw materials quality per-cent is:
Trimeric cyanamide 21%;
20-28% formalin 40%;
Sodium sulfite anhy 96 25%;
30% sulfuric acid 2.5%;
Potassium hydroxide solution 4%;
Water 28%.
In the reaction kettle that TM, condensing surface, whisking appliance are housed, add entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 2 hours; 60-75 ℃ of insulation reaction 3 hours, hydroxymethylation transfers to 8.5-9.5 with potassium hydroxide solution with the solution pH value after finishing; Sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 2 hours; After sulfonation reaction finishes, solution temperature is reduced to 50 ℃,, continues to react 2 hours to 5-6.5 with the pH value of 30% sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
Embodiment 4
A kind of novel melamine water reducer, raw materials quality per-cent is:
Trimeric cyanamide 22%;
20-28% formalin 42%;
Sodium sulfite anhy 96 25%;
30% sulfuric acid 3%;
Potassium hydroxide solution 4.5%;
Water 30%.
In the reaction kettle that TM, condensing surface, whisking appliance are housed, add entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 3 hours; 60-75 ℃ of insulation reaction 4 hours, hydroxymethylation transfers to 8.5-9.5 with potassium hydroxide solution with the solution pH value after finishing; Sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 2.5 hours; After sulfonation reaction finishes, solution temperature is reduced to 50 ℃,, continues to react 1.8 hours to 5-6.5 with the pH value of 30% sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
Embodiment 5
A kind of novel melamine water reducer, raw materials quality per-cent is:
Trimeric cyanamide 23.2%;
20-28% formalin 42.6%;
Sodium sulfite anhy 96 27%;
30% sulfuric acid 3%;
Aqua calcis 5%;
Water 30%.
In the reaction kettle that TM, condensing surface, whisking appliance are housed, add entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 3 hours; 60-75 ℃ of insulation reaction 5 hours, hydroxymethylation transfers to 8.5-9.5 with aqua calcis with the solution pH value after finishing; Sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 3 hours; After sulfonation reaction finishes, solution temperature is reduced to 50 ℃,, continues to react 5 hours to 5-6.5 with the pH value of 30% sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
Water reducer of the present invention is made an experiment according to national standard and relevant cement and concrete testing method, and product performance index is following:
Table 1 product performance index
Table 1 is the product index of novel melamine water reducer, can find out, water-reducing rate of the present invention is high, can reach 14-30%, and concrete is not emanated, and slump-loss is little, more helps concrete transportation, cast; Air content is little, and concrete strength is high; The present invention makes early age strength of concrete high, and strong to the flexibility of temperature, can not produce very big variation because of the difference of temperature.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must confirm its technical scope according to the claim scope.
Claims (5)
1. a novel melamine water reducer is characterized in that according to the mass fraction, and raw materials quality per-cent is:
Trimeric cyanamide 18.7-23.2%;
Formaldehyde 38-42.6%;
Sodium sulfite anhy 96 20-27%;
Sulfuric acid 2-3%;
Liquid caustic soda 3-5%;
Water 20-30%.
2. a kind of novel melamine water reducer according to claim 1 is characterized in that described formaldehyde is a kind of in Paraformaldehyde 96 or the 20-37% formalin.
3. a kind of novel melamine water reducer according to claim 1 is characterized in that described liquid caustic soda is a kind of in sodium hydroxide, Pottasium Hydroxide or the calcium hydroxide.
4. a kind of novel melamine water reducer according to claim 1 is characterized in that described sulfuric acid is 30% sulphuric acid soln.
5. the preparation method of a kind of novel melamine water reducer according to claim 1 is characterized in that may further comprise the steps:
(1) in the reaction kettle that TM, condensing surface, whisking appliance are housed, adds entry, trimeric cyanamide, formaldehyde solution successively; Stirring is warming up to 50-60 ℃ of reaction 1-3 hour; 60-75 ℃ insulation reaction 1-5 hour; Hydroxymethylation transfers to 8.5-9.5 with 32% liquid caustic soda solution with the solution pH value after finishing;
(2) sodium sulfite anhy 96 is dropped in the reaction kettle behind the methylolation, be warmed up to 84 ℃,, keep solution PH at 10-11 84-90 ℃ of reaction 1-3 hour;
(3) after sulfonation reaction finishes, solution temperature is reduced to 50 ℃, to 5-6.5, continues reaction 1-2 hour with the pH value of sulfuric acid adjustment system, being neutralized to pH value then is discharging in 7 o'clock, promptly gets the water reducer finished product.
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| CN2010105098510A CN102452806A (en) | 2010-10-18 | 2010-10-18 | Novel melamine water reducer and preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693882A (en) * | 2013-12-02 | 2014-04-02 | 苏州市建筑科学研究院有限公司 | Slump-retaining melamine water reducing agent and preparation method thereof |
| CN103819116A (en) * | 2013-12-17 | 2014-05-28 | 山东沾化奥仕化学有限公司 | Sulfonated melamine formaldehyde resin water reducing agent and preparation method thereof |
| CN104788038A (en) * | 2015-04-02 | 2015-07-22 | 苏州市兴邦化学建材有限公司 | Modified melamine water reducer and preparation method thereof |
| CN105820300A (en) * | 2016-03-15 | 2016-08-03 | 苏州市兴邦化学建材有限公司 | Synthesis method of melamine water reducer for desulfurized gypsum |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621383A (en) * | 2003-11-26 | 2005-06-01 | 杜云青 | Modified melamine high efficiency water reducing agent |
| CN101386488A (en) * | 2008-10-23 | 2009-03-18 | 长春建工集团有限公司 | Carboxyl acid modified melamine high-efficiency water-reducing agent |
| CN101845132A (en) * | 2010-05-06 | 2010-09-29 | 山东宏艺科技股份有限公司 | Modified melamine high-efficiency water reducing agent with low cost |
-
2010
- 2010-10-18 CN CN2010105098510A patent/CN102452806A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621383A (en) * | 2003-11-26 | 2005-06-01 | 杜云青 | Modified melamine high efficiency water reducing agent |
| CN101386488A (en) * | 2008-10-23 | 2009-03-18 | 长春建工集团有限公司 | Carboxyl acid modified melamine high-efficiency water-reducing agent |
| CN101845132A (en) * | 2010-05-06 | 2010-09-29 | 山东宏艺科技股份有限公司 | Modified melamine high-efficiency water reducing agent with low cost |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693882A (en) * | 2013-12-02 | 2014-04-02 | 苏州市建筑科学研究院有限公司 | Slump-retaining melamine water reducing agent and preparation method thereof |
| CN103693882B (en) * | 2013-12-02 | 2015-10-07 | 苏州市建筑科学研究院有限公司 | A kind of collapse protection type melamine water reducer and preparation method thereof |
| CN103819116A (en) * | 2013-12-17 | 2014-05-28 | 山东沾化奥仕化学有限公司 | Sulfonated melamine formaldehyde resin water reducing agent and preparation method thereof |
| CN103819116B (en) * | 2013-12-17 | 2016-02-03 | 山东沾化奥仕化学有限公司 | A kind of sulfonated melamine compound resin water reducer and preparation method thereof |
| CN104788038A (en) * | 2015-04-02 | 2015-07-22 | 苏州市兴邦化学建材有限公司 | Modified melamine water reducer and preparation method thereof |
| CN105820300A (en) * | 2016-03-15 | 2016-08-03 | 苏州市兴邦化学建材有限公司 | Synthesis method of melamine water reducer for desulfurized gypsum |
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Application publication date: 20120516 |