CN105820300A - Synthesis method of melamine water reducer for desulfurized gypsum - Google Patents
Synthesis method of melamine water reducer for desulfurized gypsum Download PDFInfo
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- CN105820300A CN105820300A CN201610145249.0A CN201610145249A CN105820300A CN 105820300 A CN105820300 A CN 105820300A CN 201610145249 A CN201610145249 A CN 201610145249A CN 105820300 A CN105820300 A CN 105820300A
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- reaction
- value
- melamine
- temperature
- liquor
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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
- C08G12/40—Chemically modified polycondensates
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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
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/166—Macromolecular compounds comprising sulfonate or sulfate groups obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
Abstract
The invention discloses a synthesis method of a melamine water reducer for desulfurized gypsum. The synthesis method comprises the following steps: (1) hydroxymethylation reactions; (2) sulfonation reactions; (3) condensation reactions; (4) stabilizing and reforming. Through chemical synthesis, various raw materials are improved; the performance of melamine water reducer on desulfurized gypsum is improved, and the application range is enlarged. The material ratio, pH value of medium, reaction temperature and reaction time of synthesis may influence the product quality.
Description
Technical field
The present invention relates to the synthetic method of a kind of water reducer, particularly relate to the synthetic method of a kind of melamine water reducing agent in desulfurated plaster.
Background technology
It is high that melamine water reducing agent has water-reducing rate, and the features such as volume is low, and usage amount is big, wide are widely used in concrete and cement-based powder mortar.But for gypsum base building material product, traditional melamine water reducing agent is difficult to meet the water-reducing effect of Gypsum Fibrosum.The reason being primarily present is:
(1) tradition high efficiency water reducing agent can not change the surface tension of water in Gypsum Fibrosum；
(2) tradition high efficiency water reducing agent can not increase the current potential of gypsum particle in Gypsum Fibrosum, and a dispersive property mainly electrostatic repulsion is main；
(3) electrostatic repulsion, sterically hindered, complexing, hydration shell wetting action can not effectively be combined in Gypsum Fibrosum by tradition high efficiency water reducing agent.
Summary of the invention
The technical problem that present invention mainly solves is to provide the synthetic method of a kind of melamine water reducing agent in desulfurated plaster, can be effectively improved melamine water reducing agent performance in desulfurated plaster.
For solving above-mentioned technical problem, the technical scheme that the present invention uses is: provide the synthetic method of a kind of melamine water reducing agent in desulfurated plaster, including step it is: (1) hydroxymethylation: in tripolycyanamide and formaldehyde, add water obtain the first reactant liquor, regulation makes the pH value of described first reactant liquor be 7-9 again, obtains melamine methylol solution after stirring reaction；(2) sulfonating reaction: sodium sulfite and tripolycyanamide are joined in described melamine methylol solution and obtain the second reactant liquor, then regulation makes the pH value of described second reactant liquor be 11-13, obtains sulfonation melamine methylol monomer mixed solution after reaction；(3) condensation reaction: described sulfonation melamine methylol monomer mixed solution is lowered the temperature, then regulation to make pH value be 4-5, stirring obtains sulfonated melamine compound resin mixed liquor；(4) stable reformation: neutralized and temperature reaction by described sulfonated melamine compound resin mixed liquor, filter afterwards, regulation pH value, to 7-9, obtains melamine water reducing agent.
In a preferred embodiment of the present invention, described in step (1), the mole ratio of tripolycyanamide and described formaldehyde is 1:4；Described in step (1), the pH value alkali liquor of the first reactant liquor regulates；The reaction temperature stirring reaction described in step (1) is 60-80 DEG C, and the response time is 40-60min；
In a preferred embodiment of the present invention, described in step (2), the mole ratio of sodium sulfite and described tripolycyanamide is 3:1；Described in step (2), the pH value alkali liquor of the second reactant liquor regulates；Described in step (2), the temperature of reaction is 80-90 DEG C, and the time of reaction is 100-120min.
In a preferred embodiment of the present invention, described in step (3), cooling is that temperature is to 69-70 DEG C；The sulphuric acid liquid of pH value described in step (3) regulates；The time stirring reaction described in step (3) is 120-150min.
In a preferred embodiment of the present invention, neutralizing described in step (4) is to add calcium oxide to be neutralized；The temperature heated up described in step (4) is to 90-100 DEG C；Response time described in step (4) is 60-80min；Filtering described in step (4) is to take advantage of heat filtering；Step (4) is with alkali liquor regulation pH value to 7-9.
The invention has the beneficial effects as follows: the synthetic method of the melamine water reducing agent in desulfurated plaster of the present invention, by chemical synthesis process, improve various raw material, improve melamine water reducing agent performance in desulfurated plaster, expand range.In synthetic method, reacting material ratio, medium acid-base condition, reaction temperature and response time are all the key factors affecting properties of product.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, all other embodiments that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Thering is provided the synthetic method of a kind of melamine water reducing agent in desulfurated plaster, synthesis technique can be divided into hydroxylating, sulfonation, be condensed and reform four-stage, including step is:
(1) hydroxymethylation
Tripolycyanamide, formaldehyde are put in reactor in the ratio that mole ratio is 1:4, adding suitable quantity of water, the pH value by alkali liquor adjustment reaction system is 7-9 simultaneously, intensification 60-80 DEG C, under stirring condition, preferably moderate-speed mixer reaction 40-60min, can obtain the melamine methylol solution of clarification.
(2) sulfonating reaction
After hydroxymethylation terminates, sodium sulfite and tripolycyanamide are put in the melamine methylol solution that step (1) obtains in the ratio that mole ratio is 3:1, then with alkali liquor, pH value is adjusted to 11-13, intensification 80-90 DEG C, reaction 100-120min, then melamine methylol can be converted into the sulfonation melamine methylol monomer of highly sulfonated, obtains sulfonation melamine methylol monomer mixed solution.
(3) condensation reaction
Reduce the temperature of reaction system of sulfonation melamine methylol monomer mixed solution to 69-70 DEG C, with sulphuric acid liquid, pH value of reaction system is adjusted to 4-5, stirring 120-150min, under the catalytic action of acid, the sulfonation melamine methylol monomer of highly sulfonated can generate high molecular polymer sulfonated melamine compound resin by intermolecular dehydration, linear condensation, obtains sulfonated melamine compound resin mixed liquor.
(4) stable reformation
Above-mentioned condensation reaction thing adds in appropriate calcium oxide and reaction system, be warming up to 90-100 DEG C, continue reaction 60-80min.Then take advantage of heat filtering, with alkali liquor regulation pH value to 7-9, obtain colourless highly sulfonated melamine resin aqueous products, be then melamine water reducing agent.
The invention has the beneficial effects as follows:
One, the present invention passes through chemical synthesis process, improves various raw material, improves melamine water reducing agent performance in desulfurated plaster, expands range；
Two, in synthetic method, reacting material ratio, medium acid-base condition, reaction temperature and response time are all the key factors affecting properties of product.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure utilizing description of the invention content to be made or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical field, the most in like manner it is included in the scope of patent protection of the present invention.
Claims (5)
1. the synthetic method of the melamine water reducing agent in desulfurated plaster, it is characterized in that, including step it is: (1) hydroxymethylation: in tripolycyanamide and formaldehyde, add water obtain the first reactant liquor, regulation makes the pH value of described first reactant liquor be 7-9 again, obtains melamine methylol solution after stirring reaction；(2) sulfonating reaction: sodium sulfite and tripolycyanamide are joined in described melamine methylol solution and obtain the second reactant liquor, then regulation makes the pH value of described second reactant liquor be 11-13, obtains sulfonation melamine methylol monomer mixed solution after reaction；(3) condensation reaction: described sulfonation melamine methylol monomer mixed solution is lowered the temperature, then regulation to make pH value be 4-5, stirring obtains sulfonated melamine compound resin mixed liquor；(4) stable reformation: neutralized and temperature reaction by described sulfonated melamine compound resin mixed liquor, filter afterwards, regulation pH value, to 7-9, obtains melamine water reducing agent.
Synthetic method the most according to claim 1, it is characterised in that described in step (1), the mole ratio of tripolycyanamide and described formaldehyde is 1:4；Described in step (1), the pH value alkali liquor of the first reactant liquor regulates；The reaction temperature stirring reaction described in step (1) is 60-80 DEG C, and the response time is 40-60min.
Synthetic method the most according to claim 1, it is characterised in that described in step (2), the mole ratio of sodium sulfite and described tripolycyanamide is 3:1；Described in step (2), the pH value alkali liquor of the second reactant liquor regulates；Described in step (2), the temperature of reaction is 80-90 DEG C, and the time of reaction is 100-120min.
Synthetic method the most according to claim 1, it is characterised in that described in step (3), cooling is that temperature is to 69-70 DEG C；The sulphuric acid liquid of pH value described in step (3) regulates；The time stirring reaction described in step (3) is 120-150min.
Synthetic method the most according to claim 1, it is characterised in that neutralizing described in step (4) is to add calcium oxide to be neutralized；The temperature heated up described in step (4) is to 90-100 DEG C；Response time described in step (4) is 60-80min；Filtering described in step (4) is to take advantage of heat filtering；Step (4) is with alkali liquor regulation pH value to 7-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610145249.0A CN105820300A (en) | 2016-03-15 | 2016-03-15 | Synthesis method of melamine water reducer for desulfurized gypsum |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610145249.0A CN105820300A (en) | 2016-03-15 | 2016-03-15 | Synthesis method of melamine water reducer for desulfurized gypsum |
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| CN105820300A true CN105820300A (en) | 2016-08-03 |
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| CN201610145249.0A Pending CN105820300A (en) | 2016-03-15 | 2016-03-15 | Synthesis method of melamine water reducer for desulfurized gypsum |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723615A (en) * | 2009-12-18 | 2010-06-09 | 江苏特密斯混凝土外加剂有限公司 | Method for preparing novel sulfamic acid high-efficiency concrete water reducing agent |
| CN102452806A (en) * | 2010-10-18 | 2012-05-16 | 江苏汇迪建材有限公司 | Novel melamine water reducer and preparation method |
| CN102898058A (en) * | 2012-11-01 | 2013-01-30 | 徐友娟 | Low-cost melamine water reducing agent and preparation method thereof |
| CN104672412A (en) * | 2013-12-02 | 2015-06-03 | 青岛惠城石化科技有限公司 | Exploration on synthesis process of melamine water reducing agent |
| 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 |
-
2016
- 2016-03-15 CN CN201610145249.0A patent/CN105820300A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723615A (en) * | 2009-12-18 | 2010-06-09 | 江苏特密斯混凝土外加剂有限公司 | Method for preparing novel sulfamic acid high-efficiency concrete water reducing agent |
| CN102452806A (en) * | 2010-10-18 | 2012-05-16 | 江苏汇迪建材有限公司 | Novel melamine water reducer and preparation method |
| CN102898058A (en) * | 2012-11-01 | 2013-01-30 | 徐友娟 | Low-cost melamine water reducing agent and preparation method thereof |
| CN104672412A (en) * | 2013-12-02 | 2015-06-03 | 青岛惠城石化科技有限公司 | Exploration on synthesis process of melamine water reducing agent |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 王子明等: "《混凝土高效减水剂》", 31 August 2011, 化学工业出版社 * |
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Application publication date: 20160803 |
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