CN106380558B - A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate - Google Patents
A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate Download PDFInfo
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- CN106380558B CN106380558B CN201610726748.9A CN201610726748A CN106380558B CN 106380558 B CN106380558 B CN 106380558B CN 201610726748 A CN201610726748 A CN 201610726748A CN 106380558 B CN106380558 B CN 106380558B
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
-
- 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
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The present invention relates to water-reducing agent production technical fields, and in particular to a kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate；The water-reducing agent is made of the raw material of following parts by weight: crude sodium sulfanilate 120-150 parts, 80-100 parts of formaldehyde, 300-450 parts of alpha-Naphthol industrial wastes, 20-30 parts of sodium sulfite, naphthalene sulfonic dyestuff intermediate pre-processes waste liquid 50-80 parts, 5-30 parts of PH regulator, 50-150 parts of water；The present invention prepares the water-reducing agent of high added value using naphthalene sulfonic dyestuff intermediate waste liquid, is not only able to achieve waste utilization, but also can obtain a kind of convenience, the economic waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, has broad application prospects.
Description
Technical field
The present invention relates to water-reducing agent production technical fields, and in particular to a kind of waste liquid modified height of naphthalene sulfonic dyestuff intermediate
Imitate water-reducing agent.
Background technique
The waste water that dyestuff intermediate production process generates, difficulty of governance is very big, wherein especially with the production of naphthalene series dye intermediate
The difficulty of governance of waste water is very.Naphthalene series dye intermediate product include naphthylamines class, aphthols, naphthalene sulfonic acids class, naphthylamine sulfonic acid class,
Croceine acid class, hydroxy amino naphthalene sulfonic acids class and naphthalene-carboxylic acid class, naphthalene series dye intermediate are using naphthalene as raw material, and process is a series of
Dyestuff intermediate made from organic synthesis unit process (such as sulfonation, nitrification, reduction, amination, hydrolysis etc.).This kind of intermediate has
Naphthalene nucleus contains the substituent groups such as amino, hydroxyl, sulfonic group on naphthalene nucleus.
Water-reducing agent is a kind of under conditions of keeping concrete flowability essentially identical, can be reduced the additional of mixing water amount
Agent is the concrete admixture studied and be most widely used at present.Incorporation water-reducing agent, which can be improved, in use newly mixes
Workability, the mobility of concrete, and the intensity of concrete can be improved, extend the service life of concrete component, therefore diminishing
Agent is indispensable a kind of additive in concrete.Existing amido sulfoacid series high-efficiency water reducer production cost currently on the market
It is higher, it is easy bleeding, realistic scale is low.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of slump-loss and bleeding are small, product workability is good
The waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, is made of the raw material of following parts by weight: thick
Sodium sulfanilate 120-150 parts processed, 80-100 parts of formaldehyde, 300-450 parts of alpha-Naphthol industrial wastes, sodium sulfite 20-30
Part, naphthalene sulfonic dyestuff intermediate pre-processes waste liquid 50-80 parts, 5-30 parts of PH regulator, 50-150 parts of water.
Further, the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, by following parts by weight
Raw material composition: crude sodium sulfanilate 120-130 parts, 80-90 parts of formaldehyde, 300-400 parts of alpha-Naphthol industrial wastes, sulfurous
Sour sodium 20-25 parts, naphthalene sulfonic dyestuff intermediate pre-processes waste liquid 50-60 parts, 5-10 parts of PH regulator, 50-100 parts of water.
Further, the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, by following parts by weight
Raw material composition: crude sodium sulfanilate 130-150 parts, 90-100 parts of formaldehyde, 400-450 parts of alpha-Naphthol industrial wastes, sub-
25-30 parts of sodium sulphate, waste liquid 60-80 parts of naphthalene sulfonic dyestuff intermediate pretreatment, 10-30 parts of PH regulator, water 100-150
Part.
Further, the preprocess method of the naphthalene sulfonic dyestuff intermediate waste liquid are as follows: after collecting waste liquid, use extraction
Separate organic phase and water phase；Retain organic phase, is stripped with sodium hydroxide solution useless to get naphthalene sulfonic dyestuff intermediate
The pretreatment fluid of liquid.
A kind of preparation method of the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, includes the following steps:
(1) dissolve, filter: water is added into reaction kettle, then put into respectively crude sodium sulfanilate, sodium sulfite and
Reaction kettle is warming up to 85-95 DEG C by alpha-Naphthol industrial wastes, is heated while stirring no less than 1 hour；
(2) addition: being slowly added to PH regulator into reaction kettle, adjusts solution PH to 7.5-8.5；
(3) polycondensation: reaction kettle is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, keeps formaldehyde small in 1.5-2
When it is interior drip off, heat preservation no less than 2 hours；
(4) be copolymerized: into reaction kettle be added naphthalene sulfonic dyestuff intermediate waste liquid, keep solution temperature 78-88 DEG C it
Between react 1-2 hours, water use regulation solid content is to get finished product.
Further, the volume of the water-reducing agent is the 1.1-1.4wt% of cement weight.
The invention has the benefit that
(1) it uses crude sodium sulfanilate and alpha-Naphthol industrial wastes as reaction raw materials, helps to economize on resources
With reduce cost of material, effectively improve that amido sulfoacid series high-efficiency water reducer cost is excessive and the problem of practical application hardly possible.
(2) it is grafted on water-reducing agent polymer molecular chain, can either locate using naphthalene sulfonic dyestuff intermediate is waste liquid modified
The dye intermediate wastewater for managing refractory reason, realizes the utilization again of waste liquid, and it can be made to be grafted on water-reducing agent polymer molecule,
The steric hindrance of water-reducing agent is improved, and then improves its dispersibility and water-reducing rate, to reduce the slump-loss of concrete and secrete
Aqueous, so that product workability is good, the present invention prepares the water-reducing agent of high added value using naphthalene sulfonic dyestuff intermediate waste liquid,
Not only it is able to achieve waste utilization, but also a kind of convenience, the economic waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate can be obtained,
It has broad application prospects.
(3) three-waste free discharge in preparation process, safety and environmental protection；Reaction time is short, and preparation method is simple and efficient.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with implementation of the invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1:
A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, is made of the raw material of following parts by weight: thick
150 parts of sodium sulfanilate processed, 90 parts of formaldehyde, 300 parts of alpha-Naphthol industrial wastes, 25 parts of sodium sulfite, naphthalene sulfonic dyestuff
Intermediate pre-processes 80 parts of waste liquid, 5 parts of PH regulator, 100 parts of water.
Preparation method includes the following steps:
(1) waste liquid pre-processes: after collecting waste liquid, separating organic phase and water phase with extraction；Retain organic phase, uses hydroxide
Sodium solution is stripped to get the pretreatment fluid of naphthalene sulfonic dyestuff intermediate waste liquid；
(2) dissolve, filter: water is added into reaction kettle, then put into respectively crude sodium sulfanilate, sodium sulfite and
Reaction kettle is warming up to 85-95 DEG C by alpha-Naphthol industrial wastes, is heated while stirring 2 hours；
(3) addition: being slowly added to PH regulator into reaction kettle, adjusts solution PH to 7.5-8.5；
(4) polycondensation: reaction kettle is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, makes formaldehyde at 1.5 hours
It inside drips off, keeps the temperature 2 hours；
(5) it is copolymerized: naphthalene sulfonic dyestuff intermediate waste liquid being added into reaction kettle, keep solution temperature anti-at 80 DEG C or so
It answers 2 hours, water use regulation solid content is to get finished product.
In use, the water-reducing agent is added use to account for the volume of cement weight 1.2wt%.
Embodiment 2:
A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, is made of the raw material of following parts by weight: thick
120 parts of sodium sulfanilate processed, 80 parts of formaldehyde, 450 parts of alpha-Naphthol industrial wastes, 20 parts of sodium sulfite, naphthalene sulfonic dyestuff
Intermediate pre-processes 50 parts of waste liquid, 30 parts of PH regulator, 50 parts of water.
Preparation method includes the following steps:
(1) waste liquid pre-processes: after collecting waste liquid, separating organic phase and water phase with extraction；Retain organic phase, uses hydroxide
Sodium solution is stripped to get the pretreatment fluid of naphthalene sulfonic dyestuff intermediate waste liquid；
(2) dissolve, filter: water is added into reaction kettle, then put into respectively crude sodium sulfanilate, sodium sulfite and
Reaction kettle is warming up to 85-95 DEG C by alpha-Naphthol industrial wastes, is heated while stirring 1.5 hours；
(3) addition: being slowly added to PH regulator into reaction kettle, adjusts solution PH to 7.5-8.5；
(4) polycondensation: reaction kettle is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, makes formaldehyde in 2 hours
It drips off, keeps the temperature 3 hours；
(5) be copolymerized: into reaction kettle be added naphthalene sulfonic dyestuff intermediate waste liquid, keep solution temperature 78-88 DEG C it
Between react 1.5 hours, water use regulation solid content is to get finished product.
In use, the water-reducing agent is added use to account for the volume of cement weight 1.1wt%.
Embodiment 3:
A kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, is made of the raw material of following parts by weight: thick
130 parts of sodium sulfanilate processed, 90 parts of formaldehyde, 400 parts of alpha-Naphthol industrial wastes, 30 parts of sodium sulfite, naphthalene sulfonic dyestuff
Intermediate pre-processes 60 parts of waste liquid, 10 parts of PH regulator, 150 parts of water.
Preparation method includes the following steps:
(1) waste liquid pre-processes: after collecting waste liquid, separating organic phase and water phase with extraction；Retain organic phase, uses hydroxide
Sodium solution is stripped to get the pretreatment fluid of naphthalene sulfonic dyestuff intermediate waste liquid；
(2) dissolve, filter: water is added into reaction kettle, then put into respectively crude sodium sulfanilate, sodium sulfite and
Reaction kettle is warming up to 85-95 DEG C by alpha-Naphthol industrial wastes, is heated while stirring 1 hour；
(3) addition: being slowly added to PH regulator into reaction kettle, adjusts solution PH to 7.5-8.5；
(4) polycondensation: reaction kettle is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, makes formaldehyde at 1.5 hours
It inside drips off, keeps the temperature 3 hours；
(5) be copolymerized: into reaction kettle be added naphthalene sulfonic dyestuff intermediate waste liquid, keep solution temperature 78-88 DEG C it
Between react 1 hour, water use regulation solid content is to get finished product.
In use, the water-reducing agent is added use to account for the volume of cement weight 1.4wt%.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (5)
1. a kind of waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate, which is characterized in that the water-reducing agent is by following weight
The raw material of number forms: crude sodium sulfanilate 120-150 parts, 80-100 parts of formaldehyde, and alpha-Naphthol industrial wastes 300-450
Part, 20-30 parts of sodium sulfite, waste liquid 50-80 parts of naphthalene sulfonic dyestuff intermediate pretreatment, 5-30 parts of pH adjusting agent, water 50-
150 parts；The preparation method of the water-reducing agent, includes the following steps:
(1) it dissolves, filter: water being added into reaction kettle, then puts into crude sodium sulfanilate, sodium sulfite and α-naphthalene respectively
Reaction kettle is warming up to 85-95 DEG C by phenol industrial wastes, is heated while stirring no less than 1 hour；
(2) addition: being slowly added to pH adjusting agent into reaction kettle, adjusts pH value of solution to 7.5-8.5；
(3) polycondensation: reaction kettle is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, makes formaldehyde in 1.5-2 hours
It drips off, heat preservation no less than 2 hours；
(4) it is copolymerized: naphthalene sulfonic dyestuff intermediate being added into reaction kettle and pre-processes waste liquid, keeps solution temperature at 78-88 DEG C
Between react 1-2 hours, water use regulation solid content is to get finished product.
2. the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate as described in claim 1, which is characterized in that by as follows
The raw material of parts by weight forms: crude sodium sulfanilate 120-130 parts, 80-90 parts of formaldehyde, and alpha-Naphthol industrial wastes 300-
400 parts, 20-25 parts of sodium sulfite, waste liquid 50-60 parts of naphthalene sulfonic dyestuff intermediate pretreatment, 5-10 parts of pH adjusting agent, water
50-100 parts.
3. the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate as described in claim 1, which is characterized in that by as follows
The raw material of parts by weight forms: crude sodium sulfanilate 130-150 parts, 90-100 parts of formaldehyde, and alpha-Naphthol industrial wastes
400-450 parts, 25-30 parts of sodium sulfite, naphthalene sulfonic dyestuff intermediate pre-processes waste liquid 60-80 parts, pH adjusting agent 10-30
Part, 100-150 parts of water.
4. the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate as described in claim 1, which is characterized in that the naphthalene
It is the preprocess method of sulfonic acid dye intermediate waste liquid are as follows: after collecting waste liquid, separate organic phase and water phase with extraction；It remains with
Machine phase is stripped with sodium hydroxide solution and pre-processes waste liquid to get naphthalene sulfonic dyestuff intermediate.
5. the waste liquid modified high efficiency water reducing agent of naphthalene sulfonic dyestuff intermediate as described in claim 1-4 is any, which is characterized in that
The volume of the water-reducing agent is the 1.1-1.4wt% of cement weight.
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| CN107043446A (en) * | 2017-04-19 | 2017-08-15 | 邵启明 | A kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2 |
| CN113185156A (en) * | 2021-05-08 | 2021-07-30 | 上海攀昂建筑工程有限公司 | Method for producing seawater corrosion resistant cement by using construction waste |
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| US5153299A (en) * | 1989-09-01 | 1992-10-06 | Sanyo-Kokusaku Pulp Co., Ltd. | Production of novel condensates comprising bisphenols and aromatic aminosulfonic acids, condensates and dispersant, additive and water-reducing agent based thereon |
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