CN103183486A - Amino-sulfonic acid and naphthalene compound water reducing agent and preparation method thereof - Google Patents
Amino-sulfonic acid and naphthalene compound water reducing agent and preparation method thereof Download PDFInfo
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- CN103183486A CN103183486A CN2013100663791A CN201310066379A CN103183486A CN 103183486 A CN103183486 A CN 103183486A CN 2013100663791 A CN2013100663791 A CN 2013100663791A CN 201310066379 A CN201310066379 A CN 201310066379A CN 103183486 A CN103183486 A CN 103183486A
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Abstract
The invention relates to an amino-sulfonic acid and naphthalene compound water reducing agent and a preparation method thereof. The water reducing agent comprises the following components in percentage by weight: 23 percent to 29 percent of amino-sulfonic acid water reducing agent, 29 percent to 35 percent of naphthalene water reducing agent and 36 percent to 48 percent of water. The preparation method comprises the following steps: heating naphthalene to a molten state; adding concentrated sulfuric acid to sulfonation reaction; then adding water to carry out hydrolysis; adding phenol into sodium hydroxide solution; after uniformly stirring, adding sodium anilinesulfonate to carry out condensation; mixing and stirring two products; and firstly adding formaldehyde, then adding urea and finally adding sodium hydroxide solution to regulate pH to obtain the amino-sulfonic acid and naphthalene compound water reducing agent. The amino-sulfonic acid and naphthalene compound water reducing agent improves performances of high loss speed of the used slump, poor cement adaptability and the like by adding the amino-sulfonic acid water reducing agent into the naphthalene water reducing agent and reaches an effect of improving water reducing rate.
Description
Technical field
The present invention relates to a kind of water reducer and preparation method thereof, relating in particular to a kind of amido sulfoacid series and naphthalene is composite water reducer and preparation method thereof, belongs to concrete and uses the admixture field.
Background technology
Water reducer refers under concrete workability and cement consumption permanence condition, can reduce the mixing water amount, improve concrete strength; Or under workability and intensity permanence condition, save the admixture of cement consumption.
Naphthalene water reducer is that China uses the earliest, is that naphthalene passes through sulfuric acid sulfonation, carries out the product of condensation again with formaldehyde, belongs to aniorfic surfactant.The difference that such water reducer outward appearance is looked product can be light yellow to auburn powder, and soluble in water, good to many powder body material disseminations such as cement, water-reducing rate reaches 25%.But naphthalene series high-efficiency water-reducing agent exists slump-loss fast in production and use, and cohesiveness is poor, with the bad deficiency that waits of cement adaptability.
Amido sulfoacid series high-efficiency water reducer belongs to novel third generation high efficiency water reducing agent, many technical feature characteristics such as have that water-reducing rate height, slump retention excellence, alkalinity are low, good with the adaptability of various cement, the non-crystallizable precipitation of low temperature, synthesis technique are simpler, environmental.But the concrete water-retentivity is bad in the thionamic acid based water reducer application process, the bleeding segregation phenomenon is serious, has restricted the application of thionamic acid based water reducer in concrete.
Summary of the invention
Technical problem to be solved by this invention provides a kind of novel water reducer, adopt the composite of thionamic acid based water reducer and naphthalene water reducer, overcome deficiency of the prior art, namely solve the common naphthalene water reducer of knowing clearly and mix the big deficiency of concrete slump loss behind the concrete, can also further improve water-reducing rate.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of amido sulfoacid series and naphthalene are composite water reducer, formed by following compositions in weight percentage: thionamic acid based water reducer 23%～29%, naphthalene water reducer 29%～35% and water 36%～48%, be preferably thionamic acid based water reducer 27%, naphthalene water reducer 32% and water 41%
Wherein, described thionamic acid based water reducer comprises that structural formula is the compound of formula I,
The formula I:
Wherein, x is 18～110, y is 15～110, z is 19～37, and the molecular weight of compound is about 6000.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described thionamic acid based water reducer is made up of following compositions in weight percentage: sodium sulfanilate 10%～12%, phenol 8%～21%, formaldehyde 28%～31%, urea 1%～3%, sodium hydroxide 9%～10% and water 23%～44%.
The beneficial effect that adopts above-mentioned further scheme is to add urea [CO (NH in building-up process
2)
2], can save cost so on the one hand, the more important thing is add urea after, can reduce the free formaldehyde content in the finished product effectively.
Further, described naphthalene water reducer is made up of following compositions in weight percentage: naphthalene 20%～25%, massfraction are 96% the vitriol oil 20%～25%, formaldehyde 13%～19%, sodium hydroxide 19%～24% and water 7%～28%.
Another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of amido sulfoacid series and naphthalene are the preparation method of composite water reducer, it is characterized in that, may further comprise the steps:
(1) naphthalene is heated to 175 ℃～185 ℃, makes it reach molten state, add massfraction and be 96% the vitriol oil and carry out sulfonation reaction, add the water reaction that is hydrolyzed in the sulfonated products that obtains, obtain hydrolysate;
(2) phenol is joined in the sodium hydroxide solution, the back that stirs adds sodium sulfanilate, carries out condensation reaction, obtains condensation product;
(3) hydrolysate that obtains in the described step (1) is mixed and fully stirring with the condensation product that step (2) obtains, obtain mixing solutions;
(4) temperature of described mixing solutions is controlled at 90～95 ℃, added formaldehyde and fully react 3～5h, be preferably 4h, add urea again and fully react 3～5h, be preferably 4h;
(5) adding sodium hydroxide solution adjusting pH value at last is 9～11, and obtaining amido sulfoacid series and naphthalene is composite water reducer.
The invention has the beneficial effects as follows: improve performances such as its use slump-loss is fast, inferior suitability by in naphthalene water reducer, adding the thionamic acid based water reducer, and reach the effect that improves water-reducing rate.By the composite research to naphthalene water reducer and thionamic acid based water reducer, with the high product of acquired price ratio, thereby determine the best in quality per-cent that the two and water are shared.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explaining the present invention, is not for restriction scope of the present invention.
Embodiment 1
Preparation amido sulfoacid series and naphthalene are composite water reducer, may further comprise the steps:
(1) the 1600g naphthalene is heated to 180 ℃, makes it reach molten state, add the 1600g massfraction and be 96% the vitriol oil and carry out sulfonation reaction 3h, add the reaction that is hydrolyzed of 1000g water in the sulfonated products that obtains, obtain hydrolysate;
(2) 1500g phenol being joined the 2000g massfraction is in 50% the sodium hydroxide solution, and the back that stirs adds the 1200g sodium sulfanilate, carries out condensation reaction, obtains condensation product;
(3) hydrolysate that obtains in the described step (1) is mixed according to certain ratio and fully stirring with the condensation product that step (2) obtains, obtain mixing solutions;
(4) with the control of the temperature of described mixing solutions at 90 ℃, add 1700g formaldehyde and fully react 4h, add 200g urea again and fully react and be 4h;
(5) adding proper amount of sodium hydroxide solution adjusting pH value at last is 10, and obtaining amido sulfoacid series and naphthalene is composite water reducer.
Product is tested, be the results are shown in Table 1.
Comparison example 1
Prepare 100% naphthalene water reducer, may further comprise the steps:
The 1600g naphthalene is heated to 180 ℃, make it reach molten state, add the 1600g massfraction and be 96% the vitriol oil and carry out sulfonation reaction 3.5h, add the reaction that is hydrolyzed of 1000g water in the sulfonated products that obtains, when the acidity of reaction system proceeds to 28% left and right sides, add 1000g formaldehyde and carry out condensation reaction 4h, temperature is controlled at 90 ℃.Adding the 1600g massfraction again is that 50% sodium hydroxide solution neutralizes, and making pH value is 8～10, obtains naphthalene water reducer.
Product is tested, be the results are shown in Table 2.
Comparison example 2
Prepare 100% thionamic acid based water reducer, may further comprise the steps:
It is in 50% the sodium hydroxide solution that 1500g phenol is joined the 2000g massfraction, stir the back adding to the 1200g sodium sulfanilate, stir after 40 minutes, add 700g formaldehyde and fully react 4h, add 200g urea again and fully react and be 4h, obtain % thionamic acid based water reducer.Through measuring, wherein, the molecular weight of products therefrom is about 6000.
Product is tested, be the results are shown in Table 3.
The test method that the water reducer product is adopted is GBT8077-2000 concrete admixture uniformity test method.
A certain amount of cement additive of adding and water stir in the cement paste stirrer, and the clean slurry that stirs is injected in the truncated cone circle mould, mention truncated cone circle mould, measure the maximum diameter that cement paste freely trickles on glass planar.Sheet glass is placed on level attitude, with wet cloth erasing sheet glass, truncated cone circle mould, agitator and agitator kettle make its surface wet and be not with water stainly, and truncated cone circle mould is placed on the central authorities of sheet glass and covers stand-by with wet cloth.Take by weighing 300g cement, pour in the agitator kettle, add admixture and 87g or the 105g water of recommending volume, stir 3min.The clean slurry of mixing is injected rapidly in the truncated cone circle mould, use doctor blade, truncated cone circle mould is mentioned by vertical direction, open manual time-keeping simultaneously, appoint cement paste to flow at sheet glass, measure the maximum diameter of trickling part orthogonal both direction to 30s with ruler, average as flowing degree of net paste of cement.
The admixture water-reducing rate is slump when basic identical, normal concrete and examined the difference of concrete unit consumption of water and the ratio of normal concrete unit consumption of water.And degree of mobilization represents that a kind of of cement mortar flowability measures.Under certain amount of water, degree of mobilization depends on the need water-based of cement.The mean diameter that degree of mobilization is expanded at flowing table with cement mortar is represented.So degree of mobilization is more big, water-reducing rate is more high, and the water reducer effect is more good.
Table 1 amido sulfoacid series and naphthalene are composite water reducer
| Cement/g | Water/g | Water reducer solid/g | Degree of mobilization/mm |
| 300.0 | 105.0 | 1.5 | 172 |
| 300.0 | 105.0 | 1.7 | 189 |
| 300.0 | 105.0 | 1.8 | 211 |
| 300.0 | 105.0 | 2.0 | 228 |
| 300.0 | 105.0 | 2.1 | 248 |
Table 2100% naphthalene water reducer (solid)
Table 3 sulfamate water reducer (solution)
Table 2 shows along with the every increase of naphthalene water reducer 0.2g, starches degree of mobilization only and changes more than about 15mm, and unusual effect is arranged, and starches degree of mobilization only and alters a great deal.Table 3 shows the thionamic acid based water reducer of every variation 0.03g, starches degree of mobilization only and changes 20mm.By table 1, as can be seen, along with the increase of thionamic acid based water reducer content, flowing degree of net paste of cement significantly improves.Cement has good adaptability to these two kinds of water reducers, so synergy is obviously effective.Because the solid total content of two kinds of water reducers only is 1.2g, far below single consumption with naphthalene sulfonic salt water reducer, we can say that composite effect is very desirable.Although the selling price of thionamic acid based water reducer exceeds much than naphthalene water reducer, the adding of thionamic acid based water reducer significantly reduces total water reducer consumption.Take all factors into consideration from aspects such as material costs, the compound use of two kinds of water reducers has tangible actual application value.
Can also draw amido sulfoacid series and naphthalene is in the composite water reducer through overtesting, the best proportioning of thionamic acid based water reducer and naphthalene water reducer, i.e. naphthalene water reducer 32%, sulfamate water reducer 27% remain and are water.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. an amido sulfoacid series and naphthalene are composite water reducer, it is characterized in that, are made up of following compositions in weight percentage: thionamic acid based water reducer 23%～29%, naphthalene water reducer 29%～35% and water 36%～48%,
Wherein, described thionamic acid based water reducer comprises that structural formula is the compound of formula I,
The formula I:
Wherein, x is 18～110, y is 15～110, z is 19～37.
2. be composite water reducer according to the described amido sulfoacid series of claim 1 and naphthalene, it is characterized in that described thionamic acid based water reducer is made up of following compositions in weight percentage: sodium sulfanilate 10%～12%, phenol 8%～21%, formaldehyde 28%～31%, urea 1%～3%, sodium hydroxide 9%～10% and water 23%～44%.
3. be composite water reducer according to the described amido sulfoacid series of claim 1 and naphthalene, it is characterized in that described naphthalene water reducer is made up of following compositions in weight percentage: naphthalene 20%～25%, massfraction are 96% the vitriol oil 20%～25%, formaldehyde 13%～19%, sodium hydroxide 19%～24% and water 7%～28%.
4. an amido sulfoacid series and naphthalene are the preparation method of composite water reducer, it is characterized in that, may further comprise the steps:
(1) naphthalene is heated to 175 ℃～185 ℃, makes it reach molten state, add massfraction and be 96% the vitriol oil and carry out sulfonation reaction, add the water reaction that is hydrolyzed in the sulfonated products that obtains, obtain hydrolysate;
(2) phenol being joined massfraction is in 50% sodium hydroxide solution, and the back that stirs adds sodium sulfanilate, carries out condensation reaction, obtains condensation product;
(3) hydrolysate that obtains in the described step (1) is mixed and fully stirring with the condensation product that step (2) obtains, obtain mixing solutions;
(4) temperature of described mixing solutions is controlled at 90～95 ℃, added formaldehyde and fully react 3～5h, add urea again and fully react 3～5h;
(5) adding sodium hydroxide solution adjusting pH value at last is 9～11, and obtaining amido sulfoacid series and naphthalene is composite water reducer.
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Cited By (5)
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| CN103524385A (en) * | 2013-10-15 | 2014-01-22 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN106117482A (en) * | 2016-06-29 | 2016-11-16 | 南京瑞迪高新技术有限公司 | A kind of modified high-thin arch dam naphthalene water reducer and preparation method thereof |
| CN110079284A (en) * | 2018-01-26 | 2019-08-02 | 中国电力科学研究院有限公司 | A kind of mud and drilling construction method for drilling construction |
| CN110452346A (en) * | 2019-07-16 | 2019-11-15 | 江苏博思通新材料有限公司 | A kind of water reducing agent for rare earth concrete for building |
| CN115819012A (en) * | 2023-02-15 | 2023-03-21 | 山东大元实业股份有限公司 | High-performance concrete water reducing agent and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524385A (en) * | 2013-10-15 | 2014-01-22 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN103524385B (en) * | 2013-10-15 | 2015-04-29 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN106117482A (en) * | 2016-06-29 | 2016-11-16 | 南京瑞迪高新技术有限公司 | A kind of modified high-thin arch dam naphthalene water reducer and preparation method thereof |
| CN106117482B (en) * | 2016-06-29 | 2018-05-18 | 南京瑞迪高新技术有限公司 | A kind of modified high-thin arch dam naphthalene water reducer and preparation method thereof |
| CN110079284A (en) * | 2018-01-26 | 2019-08-02 | 中国电力科学研究院有限公司 | A kind of mud and drilling construction method for drilling construction |
| CN110452346A (en) * | 2019-07-16 | 2019-11-15 | 江苏博思通新材料有限公司 | A kind of water reducing agent for rare earth concrete for building |
| CN115819012A (en) * | 2023-02-15 | 2023-03-21 | 山东大元实业股份有限公司 | High-performance concrete water reducing agent and preparation method thereof |
| CN115819012B (en) * | 2023-02-15 | 2023-04-28 | 山东大元实业股份有限公司 | High-performance concrete water reducer and preparation method thereof |
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Application publication date: 20130703 |