CN113683335A - Method for synthesizing naphthalene water reducer by residue of phthalic anhydride prepared by naphthalene method - Google Patents
Method for synthesizing naphthalene water reducer by residue of phthalic anhydride prepared by naphthalene method Download PDFInfo
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- CN113683335A CN113683335A CN202111084422.8A CN202111084422A CN113683335A CN 113683335 A CN113683335 A CN 113683335A CN 202111084422 A CN202111084422 A CN 202111084422A CN 113683335 A CN113683335 A CN 113683335A
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- naphthalene
- phthalic anhydride
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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
Abstract
The invention discloses a method for synthesizing a naphthalene water reducer by using residues of phthalic anhydride prepared by a naphthalene method, which comprises the following steps; the method comprises the following steps: crushing 30-40 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dropping 3-5 parts of sulfonating agent during stirring, and maintaining the temperature at 220-250 ℃ for 100-fold glass for 120 minutes; step two: cooling to 120-140 deg.c, adding water for hydrolysis for 90-110 min, and cooling to 90-100 deg.c. The phthalic anhydride residue of the invention contains more carbonyl, carboxyl, hydroxyl and other groups, the functions of the groups are similar to the hydroxyl in the citric acid retarder, and the groups play a certain role in hindering the hydration of cement in the hydration process of the cement, thereby effectively reducing the production cost while not being lower than the effect of the original water reducing agent.
Description
Technical Field
The invention relates to the technical field of water reducing agents, in particular to a method for synthesizing a naphthalene water reducing agent by using residues of phthalic anhydride prepared by a naphthalene method.
Background
The water reducing agent is a concrete admixture capable of reducing the mixing water consumption under the condition of keeping the slump of concrete basically unchanged, most of the water reducing agent belongs to anionic surfactants, and comprises lignosulfonate, naphthalene sulfonate formaldehyde polymer and the like, and after the water reducing agent is added into a concrete mixture, the water reducing agent has a dispersing effect on cement particles, so that the workability of the concrete mixture can be improved, the unit water consumption is reduced, and the fluidity of the concrete mixture is improved; or the unit cement consumption is reduced, and the cement is saved;
along with the vigorous development of the building industry, higher requirements are put forward on the quality, construction speed, construction environment and comprehensive cost of building construction, under the condition, the advanced water reducer is increasingly used with excellent water reducing, plastic retaining, early strengthening or retarding, economy, construction convenience and other performances, and at present, the high-efficiency water reducer in the market mainly has three major varieties: the naphthalene-based superplasticizer, the melamine-based superplasticizer and the wood turbulent superplasticizer are characterized in that the naphthalene-based superplasticizer is used in the largest amount, and the naphthalene-based superplasticizer is mainly prepared from industrial naphthalene, so that the naphthalene-based superplasticizer has high production cost due to large fluctuation of the price and market sources in recent years, is limited to a certain extent in building construction, provides a new way for reducing the production cost, and simultaneously provides a method for synthesizing the naphthalene-based superplasticizer from residues of phthalic anhydride prepared by a naphthalene method.
Disclosure of Invention
The invention aims to provide a method for synthesizing a naphthalene water reducer by using residues of phthalic anhydride prepared by a naphthalene method, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for synthesizing a naphthalene water reducer by using residues of phthalic anhydride prepared by a naphthalene method comprises the following steps;
the method comprises the following steps: crushing 30-40 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dropping 3-5 parts of sulfonating agent during stirring, and maintaining the temperature at 220-250 ℃ for 100-fold glass for 120 minutes;
step two: cooling to 120-140 ℃, adding water for hydrolysis for 90-110 minutes, and cooling to 90-100 ℃ again;
step three: pouring 10-15 parts of industrial naphthalene oil into a reaction bottle, heating to 70-80 ℃, stirring, pouring into a reaction kettle after heating to 90-110 ℃, adding 2-4 parts of modifier into the reaction kettle, and stirring uniformly;
step four: dripping 3-5 parts of formaldehyde solution into the reaction kettle, controlling the reaction temperature at 100-120 ℃, maintaining for 60-70 minutes after dripping, and then cooling to 60-70 ℃;
step five: adding 20-30 parts of liquid caustic soda into a reaction kettle, stirring, adding the liquid caustic soda to neutralize the solvent in the reaction kettle to be alkalescent with the pH of 8-10, filtering, discharging, drying, and evaporating water to obtain the solid powdery water reducing agent.
Preferably, after the fourth step, 3 to 5 parts of retarder and 0.5 to 0.8 part of flocculant are sequentially added into the reaction kettle and stirred for 40 to 50 minutes.
Preferably, the retarder is lignosulfonate, and the flocculating agent is inorganic polymer polyaluminium oxide.
Preferably, the sulfonating agent is any one of concentrated sulfuric acid, chlorosulfonic acid, sulfur trioxide, sulfamic acid and sulfite.
Preferably, the liquid alkali is prepared by mixing and stirring a sodium hydroxide solution and a small amount of a sodium bicarbonate solution.
The method for synthesizing the naphthalene water reducer by using the residue of the phthalic anhydride prepared by the naphthalene method has the beneficial effects that:
the residue of phthalic anhydride prepared by adopting a naphthalene method is used as a raw material, a modifier is added into naphthalene oil after sulfonation by heating to participate in condensation together, so that a novel additive with the performance not lower than that of a tea-series water reducing agent is prepared, meanwhile, a formaldehyde solution and liquid alkali are heated, so that the high-efficiency water reducing agent can be worth of, the phthalic anhydride residue contains more carbonyl, carboxyl, hydroxyl and other groups, the groups have the functions similar to the hydroxyl in a citric acid retarder, and in the cement hydration process, a certain effect of hindering the cement hydration is achieved, so that the production cost is effectively reduced while the effect of the original water reducing agent is not lower.
Drawings
FIG. 1 is a comparative graph of the use effect of the concrete prepared by the invention
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
the method comprises the following steps: crushing 35 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dropping 5 parts of concentrated sulfuric acid in the stirring process, and maintaining the temperature at 220 ℃ for 110 minutes;
step two: cooling to 135 deg.C, adding water for hydrolysis for 90 min, and cooling to 93 deg.C;
step three: pouring 10 parts of industrial naphthalene oil into a reaction bottle, heating to 70 ℃, stirring, pouring into a reaction kettle after heating to 90 ℃, adding 2 parts of modifier into the reaction kettle, and stirring uniformly;
step four: dripping 3 parts of formaldehyde solution into a reaction kettle, controlling the reaction temperature at 120 ℃, maintaining for 70 minutes after dripping, cooling to 70 ℃, sequentially adding 4 parts of lignosulfonate and 0.8 part of polymeric alumina into the reaction kettle, and stirring for 48 minutes;
step five: adding 28 parts of liquid caustic soda prepared by mixing and stirring a sodium hydroxide solution and a small amount of sodium bicarbonate solution into a reaction kettle, stirring, neutralizing a solvent in the reaction kettle to be alkalescent with the pH of 9 by adding the liquid caustic soda, and filtering, discharging, drying and evaporating water to obtain the solid powdery water reducing agent.
the method comprises the following steps: crushing 38 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dropping 5 parts of concentrated sulfuric acid in the stirring process, and maintaining the temperature at 240 ℃ for 110 minutes;
step two: cooling to 140 ℃, adding water for hydrolysis for 95 minutes, and cooling to 90 ℃ again;
step three: pouring 12 parts of industrial naphthalene oil into a reaction bottle, heating to 80 ℃, stirring, pouring into a reaction kettle after heating to 100 ℃, adding 4 parts of modifier into the reaction kettle, and stirring uniformly;
step four: dripping 3 parts of formaldehyde solution into a reaction kettle, controlling the reaction temperature at 120 ℃, maintaining for 70 minutes after dripping, cooling to 65 ℃, sequentially adding 4 parts of lignosulfonate and 0.6 part of polymeric alumina into the reaction kettle, and stirring for 45 minutes;
step five: adding 25 parts of liquid caustic soda prepared by mixing and stirring a sodium hydroxide solution and a small amount of sodium bicarbonate solution into a reaction kettle, stirring, neutralizing a solvent in the reaction kettle to be alkalescent with the pH of 9 by adding the liquid caustic soda, and filtering, discharging, drying and evaporating water to obtain the solid powdery water reducing agent.
Embodiment 3, the present invention provides a technical solution: a method for synthesizing a naphthalene water reducer by using residues of phthalic anhydride prepared by a naphthalene method comprises the following steps;
the method comprises the following steps: crushing 30 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dripping 4 parts of sulfamic acid in the stirring process, and maintaining the temperature at 230 ℃ for 110 minutes;
step two: cooling to 130 ℃, adding water for hydrolysis for 100 minutes, and cooling to 95 ℃ again;
step three: pouring 11 parts of industrial naphthalene oil into a reaction bottle, heating to 70 ℃, stirring, pouring into a reaction kettle after heating to 110 ℃, adding 4 parts of modifier into the reaction kettle, and stirring uniformly;
step four: dripping 3 parts of formaldehyde solution into a reaction kettle, controlling the reaction temperature at 110 ℃, maintaining for 65 minutes after dripping, cooling to 60 ℃, sequentially adding 3-5 parts of lignosulfonate and 0.6 part of polymeric alumina into the reaction kettle, and stirring for 45 minutes;
step five: adding 25 parts of liquid caustic soda prepared by mixing and stirring a sodium hydroxide solution and a small amount of sodium bicarbonate solution into a reaction kettle, stirring, neutralizing a solvent in the reaction kettle to be alkalescent with the pH of 8 by adding the liquid caustic soda, and filtering, discharging, drying and evaporating water to obtain the solid powdery water reducing agent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for synthesizing a naphthalene water reducer by using residues of phthalic anhydride prepared by a naphthalene method is characterized by comprising the following steps: comprises the following steps;
the method comprises the following steps: crushing 30-40 parts of phthalic anhydride residues by using crushing equipment, putting the crushed phthalic anhydride residues into a reaction kettle, stirring the phthalic anhydride residues, slowly dropping 3-5 parts of sulfonating agent during stirring, and maintaining the temperature at 220-250 ℃ for 100-fold glass for 120 minutes;
step two: cooling to 120-140 ℃, adding water for hydrolysis for 90-110 minutes, and cooling to 90-100 ℃ again;
step three: pouring 10-15 parts of industrial naphthalene oil into a reaction bottle, heating to 70-80 ℃, stirring, pouring into a reaction kettle after heating to 90-110 ℃, adding 2-4 parts of modifier into the reaction kettle, and stirring uniformly;
step four: dripping 3-5 parts of formaldehyde solution into the reaction kettle, controlling the reaction temperature at 100-120 ℃, maintaining for 60-70 minutes after dripping, and then cooling to 60-70 ℃;
step five: adding 20-30 parts of liquid caustic soda into a reaction kettle, stirring, adding the liquid caustic soda to neutralize the solvent in the reaction kettle to be alkalescent with the pH of 8-10, filtering, discharging, drying, and evaporating water to obtain the solid powdery water reducing agent.
2. The method for synthesizing the naphthalene water reducer by using the residue of the phthalic anhydride prepared by the naphthalene method according to claim 1, which is characterized by comprising the following steps of: and after the fourth step, 3-5 parts of retarder and 0.5-0.8 part of flocculant can be sequentially added into the reaction kettle, and the mixture is stirred for 40-50 minutes.
3. The method for synthesizing the naphthalene water reducer by using the residue of the phthalic anhydride prepared by the naphthalene method according to claim 2, which is characterized by comprising the following steps of: the retarder is lignosulfonate, and the flocculating agent is inorganic polymer polyaluminium oxide.
4. The method for synthesizing the naphthalene water reducer by using the residue of the phthalic anhydride prepared by the naphthalene method according to claim 1, which is characterized by comprising the following steps of: the sulfonating agent is any one of concentrated sulfuric acid, chlorosulfonic acid, sulfur trioxide, sulfamic acid and sulfite.
5. The method for synthesizing the naphthalene water reducer by using the residue of the phthalic anhydride prepared by the naphthalene method according to claim 1, which is characterized by comprising the following steps of: the liquid alkali is prepared by mixing and stirring a sodium hydroxide solution and a small amount of sodium bicarbonate solution.
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Citations (4)
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|---|---|---|---|---|
| CA2783526A1 (en) * | 2011-08-11 | 2013-02-11 | Afton Chemical Corporation | Lubricant compositions containing a functionalized dispersant |
| CN208583336U (en) * | 2018-07-12 | 2019-03-08 | 新泰市中泰新材料科技有限公司 | Phthalic anhydride Slag recovering system |
| CN111996047A (en) * | 2020-08-26 | 2020-11-27 | 安徽鑫固环保股份有限公司 | Method for synthesizing naphthalene-based coal water slurry dispersant from residue of phthalic anhydride prepared by naphthalene method |
| CN112048046A (en) * | 2020-09-02 | 2020-12-08 | 安徽鑫固环保股份有限公司 | Method for synthesizing naphthalene water reducer by residue of phthalic anhydride prepared by naphthalene method |
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2021
- 2021-09-15 CN CN202111084422.8A patent/CN113683335A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2783526A1 (en) * | 2011-08-11 | 2013-02-11 | Afton Chemical Corporation | Lubricant compositions containing a functionalized dispersant |
| CN208583336U (en) * | 2018-07-12 | 2019-03-08 | 新泰市中泰新材料科技有限公司 | Phthalic anhydride Slag recovering system |
| CN111996047A (en) * | 2020-08-26 | 2020-11-27 | 安徽鑫固环保股份有限公司 | Method for synthesizing naphthalene-based coal water slurry dispersant from residue of phthalic anhydride prepared by naphthalene method |
| CN112048046A (en) * | 2020-09-02 | 2020-12-08 | 安徽鑫固环保股份有限公司 | Method for synthesizing naphthalene water reducer by residue of phthalic anhydride prepared by naphthalene method |
Non-Patent Citations (3)
| Title |
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| 宋波等: "聚羧酸改性萘系高效减水剂的制备与性能", 《新型建筑材料》 * |
| 宋波等: "萘系高效减水剂的改性研究", 《安徽化工》 * |
| 寿崇琦等: "苯酐残渣合成高效减水剂的研究", 《山东建材》 * |
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Application publication date: 20211123 |