CN103864332A - Preparation method of slump loss resistant naphthalene water reducer - Google Patents
Preparation method of slump loss resistant naphthalene water reducer Download PDFInfo
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- CN103864332A CN103864332A CN201410066495.8A CN201410066495A CN103864332A CN 103864332 A CN103864332 A CN 103864332A CN 201410066495 A CN201410066495 A CN 201410066495A CN 103864332 A CN103864332 A CN 103864332A
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Abstract
The invention discloses a preparation method of a slump loss resistant naphthalene water reducer. The naphthalene water reducer is prepared by sulfonating, hydrolyzing, condensing and neutralizing raw materials including crude naphthalene, naphthalene derivatives such as methylnaphthalene, concentrated sulfuric acid, formaldehyde, caustic soda liquid, water and the like. According to the production process, monomer substituents, such as methylnaphthalene and acenaphthene are introduced, an organic solvent azeotropic method is adopted for synthesizing, and finally sodium metasilicate is adopted for neutralizing to adjust pH to 7-10 to obtain the final naphthalene water reducer. The slump loss resistant naphthalene water reducer is prepared by the implementation mode disclosed by the invention, the crude naphthalene is replaced by partial naphthalene derivatives, an effective path of reducing the cost is proposed, naphthalene steam and a solvent are condensed to form a naphthalene solution to be recycled, and thus the product yield is improved and the environmental pollution is reduced.
Description
Technical field
The invention belongs to the technical field of material of construction, relate in particular to a kind of preparation method of collapse protection type naphthalene water reducer.
Background technology
Along with the fast development of China's economy, foundation construction facility constantly perfect, increasing to the consumption demand of concrete admixture.Concrete admixture add the performance such as mobility, workability that can improve fresh concrete, can obviously reduce the consumption of water simultaneously, improve concrete intensity.The advantages such as it is low that naphthalene water reducer has cost, and adaptability is good are the concrete admixture of usage quantity maximum in high efficiency water reducing agent, turnout maximum at present.The production method of naphthalene water reducer, in the stage of maturity, is generally divided into sulfonation, hydrolysis, condensation, neutralization stage.
But NAPTHALENE FLAKES. (INDUSTRIAL GRADE） price volalility is obviously seasonal, as higher in the prices of raw and semifnished materials, NAPTHALENE FLAKES. (INDUSTRIAL GRADE） amount of increase is brought to industrial production naphthalene water reducer and be had a strong impact on.In addition the naphthalene steam producing in sulfonation process, directly discharge meeting to environment.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of collapse protection type naphthalene water reducer, the method replaces NAPTHALENE FLAKES. (INDUSTRIAL GRADE） with part naphthalene derivatives, can reduce costs, naphthalene steam and solvent form the utilization of naphthalene solution circulated through condensation, carry high product yield and reduce environmental pollution.
For solving the problems of the technologies described above, technical solution of the present invention is:
A preparation method for collapse protection type naphthalene water reducer, comprises the following steps:
(1) sulfonation: by mass parts, in the closed reactor A that is connected to cooling and reflux device, add 100～130 parts of NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, 20～40 parts of condensed ring aromatic hydrocarbon, while heating to 120～130 DEG C, start to drip respectively 110～150 parts of vitriol oils and 50～70 parts of organic solvents, in 0.5～1 hour, dropwise; When the vitriol oil dropwises, temperature in the kettle is controlled to 155～170 DEG C, continues insulation 1～2 hour; In reaction process, at the bottom UNICOM steam-pipe of sulfonation reaction still A, pass into steam time 0.5～1h, lower boiling organic solvent enters the cooling and reflux device heat exchange condensation on reactor A top with naphthalene steam, naphthalene steam and solvent form cooling fluid and send constantly into reactor continuation circulating reaction again after condensation, until reaction finishes, the part cooling fluid that remains in the most at last cooling and reflux device reclaims or continues the reaction of next still, because high product yield is finally carried in the utilization of naphthalene steam refrigeration cycle, and reduce environmental pollution;
(2) hydrolysis: after sulfonation reaction finishes, cool to 120～130 DEG C, add 30～45 parts of water, reaction 10～30 minutes is hydrolyzed;
(3) condensation: after hydrolysis reaction finishes, add the sulfonate of 10～20 parts, cool to 85～95 DEG C, drip 60～80 parts of formaldehyde, dropwised in 2～4 hours; Be warming up to 105～115 DEG C, be incubated 2～6 hours; In insulating process, divide and respectively add 10～15 parts of water for 3 times, finally dilute with 120～140 parts of water;
(4) neutralization: after water injection, during material is transferred to and in still B, regulate pH to 7～10, obtain product to room temperature after cooling.
Described condensed ring aromatic hydrocarbon is the one in methylnaphthalene, acenaphthene, anthracene.
Described organic solvent is the one in hexanaphthene, acetic acid, methylene dichloride.
Described sulfonate is the one in Sodium styrene sulfonate, sodium naphthalene sulfonate, p-hydroxy benzenyl sulfonate sodium.
In described step (4), regulate pH value to adopt 25～45 parts of Starsos.
Because the present invention adds suitable organic solvent recovered steam in sulfonation process, recycle, reduces tail gas discharging pollutant, be conducive to economize on resources, and protection of the environment.In addition, for the present invention, the naphthalene derivatives such as methylnaphthalene, anthracene, acenaphthene suitably replaces part NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, can alleviate a part of pressure, improves the market competitiveness of naphthalene water reducer.In addition, the present invention also introduces sulfonate component, and in the condensation stage, by strengthening with the molecular structure controllability of the synthetic naphthalene water reducer of formaldehyde condensation, suitable introducing sulfonate also can improve its over-all properties, improves the application of naphthalene water reducer.
In a word, the present invention replaces NAPTHALENE FLAKES. (INDUSTRIAL GRADE） with part naphthalene derivatives, has proposed the effective way that reduces costs, and naphthalene steam and solvent form the utilization of naphthalene solution circulated through condensation, have improved product yield and have reduced environmental pollution.
Embodiment
Below in conjunction with specific embodiment, the inventive method is described in further detail, makes the person skilled of this area have more deep understanding to the present invention.
Embodiment 1
(1) sulfonation: in the closed reactor A that is connected to cooling and reflux device, add 100kg NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, 20kg methylnaphthalene, while heating to 120～130 DEG C, starts to drip respectively the 110kg vitriol oil and 50kg hexanaphthene, dropwises in 0.5 hour.When the vitriol oil dropwises, temperature in the kettle is controlled to 160～170 DEG C, continues insulation 1.5 hours.In reaction process, at the bottom UNICOM steam-pipe of sulfonation reaction still A, pass into steam time 0.5～1h, hexanaphthene enters the cooling and reflux device heat exchange condensation on reactor A top with naphthalene steam, naphthalene steam and hexanaphthene form cooling fluid and send constantly into reactor continuation circulating reaction after condensation, until reaction finishes, the part cooling fluid that remains in the most at last cooling and reflux device reclaims or continues the reaction of next still.
(2) hydrolysis: after sulfonation reaction finishes, cool to 125 DEG C, add 30kg water, reaction 20 minutes is hydrolyzed.
(3) condensation: after hydrolysis reaction finishes, add the Sodium styrene sulfonate of 10kg, cool to 85～95 DEG C, drip 60kg formaldehyde, dropwised in 2 hours.Be warming up to 105 DEG C, be incubated 3 hours.In insulating process, divide and respectively add 10kg water 3 times, finally dilute with 120kg water.
(4) neutralization: after water injection, during material is transferred to and in still B, add 25kg Starso, regulate pH value to 7～10, obtain product to room temperature after cooling.
Embodiment 2
(1) sulfonation: in the closed reactor A that is connected to cooling and reflux device, add 130kg NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, 40kg acenaphthene, while heating to 130 DEG C, starts to drip respectively the 150kg vitriol oil and 60kg acetic acid, dropwises in 0.5 hour.When the vitriol oil dropwises, temperature in the kettle is controlled to 155～165 DEG C, continues insulation 2 hours.In reaction process, at the bottom UNICOM steam-pipe of sulfonation reaction still A, pass into steam time 0.5～1h, acetic acid enters the cooling and reflux device heat exchange condensation on reactor A top with naphthalene steam, naphthalene steam and acetic acid form cooling fluid and send constantly into reactor continuation circulating reaction after condensation, until reaction finishes, the part cooling fluid that remains in the most at last cooling and reflux device reclaims or continues the reaction of next still.
(2) hydrolysis: after sulfonation reaction finishes, cool to 120 DEG C, add 30kg water, reaction 30 minutes is hydrolyzed.
(3) condensation: after hydrolysis reaction finishes, add the sodium naphthalene sulfonate of 20kg, cool to 85～95 DEG C, drip 80kg formaldehyde, dropwised in 3 hours.Be warming up to 115 DEG C, be incubated 5 hours.In insulating process, divide and respectively add 10kg water 3 times, finally dilute with 140kg water.
(4) neutralization: after water injection, during material is transferred to and in still B, add 45kg Starso, regulate pH value to 7～10, obtain product to room temperature after cooling.
Embodiment 3
(1) sulfonation: in the closed reactor A that is connected to cooling and reflux device, add 120kg NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, 25kg anthracene, while heating to 125 DEG C, starts to drip respectively the 150kg vitriol oil and 70kg methylene dichloride, dropwises in 1 hour.When the vitriol oil dropwises, temperature in the kettle is controlled to 160～170 DEG C, continues insulation 2 hours.In reaction process, at the bottom UNICOM steam-pipe of sulfonation reaction still A, pass into steam time 0.5～1h, methylene dichloride enters the cooling and reflux device heat exchange condensation on reactor A top with naphthalene steam, naphthalene steam and methylene dichloride form cooling fluid and send constantly into reactor continuation circulating reaction after condensation, until reaction finishes, the part cooling fluid that remains in the most at last cooling and reflux device reclaims or continues the reaction of next still.
(2) hydrolysis: after sulfonation reaction finishes, cool to 125 DEG C, add 30kg water, reaction 20 minutes is hydrolyzed.
(3) condensation: after hydrolysis reaction finishes, add the 4-Vinyl phenol sodium sulfonate of 15kg, cool to 85～95 DEG C, drip 70kg formaldehyde, dropwised in 3 hours.Be warming up to 110 DEG C, be incubated 5 hours.In insulating process, divide and respectively add 10kg water 3 times, finally dilute with 140kg water.
(4) neutralization: after water injection, during material is transferred to and in still B, add 30kg Starso, regulate pH value to 7～10, obtain product to room temperature after cooling.
By embodiment 1～3 synthetic sample obtaining and the contrast of common naphthalene water reducer, measure the slump and the each age strength of concrete.
Table 1 embodiment concrete contrast properties
Test-results explanation, is used concrete initial flow and the function of slump protection that product of the present invention is prepared to be all better than common naphthalene water reducer performance in the market, and does not affect other workabilities.
The above, be only preferred embodiment of the present invention, not technical scope of the present invention is imposed any restrictions, thus variation or the modification in every case done according to claim of the present invention and specification sheets, within all should belonging to the scope that patent of the present invention contains.
Claims (5)
1. a preparation method for collapse protection type naphthalene water reducer, is characterized in that comprising the following steps:
(1) sulfonation: by mass parts, in the closed reactor A that is connected to cooling and reflux device, add 100 ~ 130 parts of NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, 20 ~ 40 parts of condensed ring aromatic hydrocarbon, while heating to 120 ~ 130 DEG C, start to drip respectively 110 ~ 150 parts of vitriol oils and 50 ~ 70 parts of organic solvents, in 0.5 ~ 1 hour, dropwise; When the vitriol oil dropwises, temperature in the kettle is controlled to 155 ~ 170 DEG C, continues insulation 1 ~ 2 hour; In reaction process, at the bottom UNICOM steam-pipe of sulfonation reaction still A, pass into steam time 0.5 ~ 1h, lower boiling organic solvent enters the cooling and reflux device heat exchange condensation on reactor A top with naphthalene steam, naphthalene steam and solvent form cooling fluid and send constantly into reactor continuation circulating reaction again after condensation, until reaction finishes, the part cooling fluid that remains in the most at last cooling and reflux device reclaims or continues the reaction of next still;
(2) hydrolysis: after sulfonation reaction finishes, cool to 120 ~ 130 DEG C, add 30 ~ 45 parts of water, reaction 10 ~ 30 minutes is hydrolyzed;
(3) condensation: after hydrolysis reaction finishes, add the sulfonate of 10 ~ 20 parts, cool to 85 ~ 95 DEG C, drip 60 ~ 80 parts of formaldehyde, dropwised in 2 ~ 4 hours; Be warming up to 105 ~ 115 DEG C, be incubated 2 ~ 6 hours; In insulating process, divide and respectively add 10 ~ 15 parts of water for 3 times, finally use 120 ~ 140 parts of water to dilute;
(4) neutralization: after water injection, during material is transferred to and in still B, regulate pH to 7 ~ 10, obtain product to room temperature after cooling.
2. the preparation method of a kind of collapse protection type naphthalene water reducer according to claim 1, is characterized in that: described condensed ring aromatic hydrocarbon is the one in methylnaphthalene, acenaphthene, anthracene.
3. the preparation method of a kind of collapse protection type naphthalene water reducer according to claim 1, is characterized in that: described organic solvent is the one in hexanaphthene, acetic acid, methylene dichloride.
4. the preparation method of a kind of collapse protection type naphthalene water reducer according to claim 1, is characterized in that: described sulfonate is the one in Sodium styrene sulfonate, sodium naphthalene sulfonate, p-hydroxy benzenyl sulfonate sodium.
5. the preparation method of a kind of collapse protection type naphthalene water reducer according to claim 1, is characterized in that: in described step (4), regulate pH value to adopt 25 ~ 45 parts of Starsos.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104176968A (en) * | 2014-08-21 | 2014-12-03 | 广东瑞安科技实业有限公司 | Production method for naphthalene high-concentration water reducer |
| CN105884238A (en) * | 2015-08-18 | 2016-08-24 | 科之杰新材料集团有限公司 | Naphthalene-based powder water reducing agent and preparation method thereof |
| 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 |
| CN106117481A (en) * | 2016-06-24 | 2016-11-16 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production method of naphthalene water reducer |
| CN106632938A (en) * | 2016-09-20 | 2017-05-10 | 江苏苏博特新材料股份有限公司 | Energy-saving preparation method of naphthalene water reducer and equipment special for energy-saving preparation method |
| CN107200817A (en) * | 2017-07-07 | 2017-09-26 | 科之杰新材料集团有限公司 | A kind of preparation method of stable type concrete slump controlling agent |
| CN108033706A (en) * | 2017-12-28 | 2018-05-15 | 浙江建研科之杰新材料有限公司 | A kind of synthetic method of modified naphthalene series sulfonate water reducer |
| CN110156368A (en) * | 2019-05-24 | 2019-08-23 | 莱芜市兆信新材料股份有限公司 | A kind of preparation method of gypsum water-reducing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104176968B (en) * | 2014-08-21 | 2015-12-02 | 广东瑞安科技实业有限公司 | The production method of the high dense water reducer of a kind of naphthalene system |
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| CN105884238B (en) * | 2015-08-18 | 2017-12-22 | 科之杰新材料集团有限公司 | A kind of naphthalene system pulvis water reducer and preparation method thereof |
| CN105884238A (en) * | 2015-08-18 | 2016-08-24 | 科之杰新材料集团有限公司 | Naphthalene-based powder water reducing agent and preparation method thereof |
| CN106117481B (en) * | 2016-06-24 | 2018-06-08 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the production method of sulfonation separate mealing type condensation production naphthalene water reducer |
| CN106117481A (en) * | 2016-06-24 | 2016-11-16 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production method of naphthalene water reducer |
| 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 |
| 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 |
| CN106632938A (en) * | 2016-09-20 | 2017-05-10 | 江苏苏博特新材料股份有限公司 | Energy-saving preparation method of naphthalene water reducer and equipment special for energy-saving preparation method |
| CN106632938B (en) * | 2016-09-20 | 2019-01-01 | 江苏苏博特新材料股份有限公司 | A kind of energy saving preparation method and its special equipment of naphthalene water reducer |
| CN107200817A (en) * | 2017-07-07 | 2017-09-26 | 科之杰新材料集团有限公司 | A kind of preparation method of stable type concrete slump controlling agent |
| CN107200817B (en) * | 2017-07-07 | 2019-07-19 | 科之杰新材料集团有限公司 | A kind of preparation method of stable type concrete slump controlling agent |
| CN108033706A (en) * | 2017-12-28 | 2018-05-15 | 浙江建研科之杰新材料有限公司 | A kind of synthetic method of modified naphthalene series sulfonate water reducer |
| CN110156368A (en) * | 2019-05-24 | 2019-08-23 | 莱芜市兆信新材料股份有限公司 | A kind of preparation method of gypsum water-reducing agent |
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