CN107043446A - A kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2 - Google Patents
A kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2 Download PDFInfo
- Publication number
- CN107043446A CN107043446A CN201710257741.1A CN201710257741A CN107043446A CN 107043446 A CN107043446 A CN 107043446A CN 201710257741 A CN201710257741 A CN 201710257741A CN 107043446 A CN107043446 A CN 107043446A
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- CN
- China
- Prior art keywords
- parts
- fluorenone
- waste liquid
- carboxylic acids
- reducing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
-
- 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
-
- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
-
- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/14—Block or graft polymers prepared by polycondensation of aldehydes or ketones on to macromolecular compounds
-
- 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 present invention relates to a kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2;Include the raw material of following parts by weight:250 320 parts of 9 Fluorenone, 2 carboxylic acid industrial wastes, 80 90 parts of p-aminobenzene sulfonic acid, industrial 70 90 parts of waste phenol dregs, 20 30 parts of sodium pyrosulfite, 100 140 parts of formaldehyde, 3 10 parts of sodium peroxydisulfate, 0 80 parts of PH conditioning agents, 0 100 parts of water;The present invention both contributes to reduce production cost, the carboxylic acid industrial wastes of 9 Fluorenone 2 is made full use of again, effectively realize business cycle, and the perfect adaptation of industry interchain, the waste liquid modified high efficiency water reducing agent molecular weight of the carboxylic acid of 9 Fluorenone 2 of synthesis is big, molecular chain length, water-reducing rate is high, and function of slump protection is strong.
Description
Technical field
The present invention relates to water reducer production technical field, and in particular to a kind of 9-Fluorenone -2- carboxylic acids are waste liquid modified efficiently to be subtracted
Aqua.
Background technology
Concrete admixture, abbreviation additive refers to mix to change before mixing concrete mixing or during mix
The material of kind concrete performance.Because additive can effectively improve the performance of concrete, and with good economic benefit,
It is widely used in many countries, the application in engineering is increasingly taken seriously, as indispensable in concrete
Material.Wherein water reducer is most important a kind of additive in concrete, and it can be in concrete workability and cement consumption
Under permanence condition, mixing water amount can be reduced, concrete strength is improved;Or under workability and intensity permanence condition, save water
Mud consumption.But used water reducer there is water-reducing rate low, poor fluidity, the shortcoming of low intensity in the market, it is impossible to
Meet the requirement in market.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of good 9-Fluorenone -2- carboxylic acids of economic and environment-friendly, water-reducing effect
Waste liquid modified high efficiency water reducing agent.
To realize object above, the present invention is achieved by the following technical programs:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
250-320 parts of industrial wastes, 80-90 parts of p-aminobenzene sulfonic acid, industrial waste phenol dregs 70-90 parts, 20-30 parts of sodium pyrosulfite, first
100-140 parts of aldehyde, 3-10 parts of sodium peroxydisulfate, 0-80 parts of PH conditioning agents, 0-100 parts of water.
Further, the described waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the original of following parts by weight
Material:260-290 parts of 9-Fluorenone -2- carboxylic acid industrial wastes, 84-88 parts of p-aminobenzene sulfonic acid, industrial waste phenol dregs 75-80 parts, Jiao Ya
22-24 parts of sodium sulphate, 110-120 parts of formaldehyde, 4-6 parts of sodium peroxydisulfate, 10-30 parts of PH conditioning agents, 40-60 parts of water.
Further, the described waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the original of following parts by weight
Material:275 parts of 9-Fluorenone -2- carboxylic acids industrial wastes, 86 parts of p-aminobenzene sulfonic acid, industrial 76 parts of waste phenol dregs, 22 parts of sodium pyrosulfite,
112 parts of formaldehyde, 5 parts of sodium peroxydisulfate, 18 parts of PH conditioning agents, 30 parts of water.
Further, the 9-Fluorenone -2- carboxylic acids industrial wastes is pretreatment waste liquid, and the preprocess method is:Collect
After waste liquid, organic phase and aqueous phase are separated with extraction;Retain organic phase, be stripped with sodium hydroxide solution, produce 9- fluorenes
Ketone -2- carboxylic acids pre-process industrial wastes.
Further, the preparation method of the described waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, including following step
Suddenly:
(1)Dissolving, filtering:Water, then input p-aminobenzene sulfonic acid, industrial waste phenol dregs and pyrosulfurous acid respectively are added into reactor
Sodium, 68-75 DEG C is warming up to by reactor, is heated while stirring no less than 30 minutes;
(2)Addition:PH conditioning agents, regulation solution PH to 7-8 are slowly added into reactor;
(3)Polycondensation:Reactor is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, formaldehyde was dripped in 1-2 hours
Complete, insulation is no less than 2 hours;
(4)Sodium peroxydisulfate is dissolved with appropriate amount of deionized water, and is configured to 12% sodium peroxydisulfate solution;
(5)Copolymerization:9-Fluorenone -2- carboxylic acid industrial wastes, and slow dropwise addition sodium peroxydisulfate solution thereto are added into reactor,
Sodium peroxydisulfate solution was dripped off in 1-2 hours, keep solution temperature to be reacted between 85-95 DEG C 2-3 hours, water use regulation contains
Gu amount, gets product.
6th, the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as any one of claim 1-4, its feature exists
In the volume of the water reducer is the 1.5-1.8wt% of cement weight.
Beneficial effects of the present invention are:
The present invention both contributes to reduce production cost using the raw material that 9-Fluorenone -2- carboxylic acids industrial wastes is graft copolymerization, and right
9-Fluorenone -2- carboxylic acid industrial wastes is made full use of, and effectively realizes business cycle, and industry interchain perfect adaptation,
The waste liquid modified high efficiency water reducing agent molecular weight of 9-Fluorenone -2- carboxylic acids of synthesis is big, molecular chain length, and water-reducing rate is high, and function of slump protection is strong.
The preparation method that the present invention is provided is simple to operation, reacts no waste discharge, helps to save energy consumption, environmental protection warp
Ji.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the implementation of the present invention
Example, the technical scheme in the embodiment of the present invention is clearly and completely described.Based on the embodiment in the present invention, this area
The every other embodiment that those of ordinary skill is obtained under the premise of creative work is not made, belongs to protection of the present invention
Scope.
Embodiment 1:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
275 parts of industrial wastes, 86 parts of p-aminobenzene sulfonic acid, industrial 76 parts of waste phenol dregs, 22 parts of sodium pyrosulfite, 112 parts of formaldehyde, persulfuric acid
5 parts of sodium, 18 parts of PH conditioning agents, 30 parts of water.
Its preparation method, comprises the following steps:
(1)9-Fluorenone -2- carboxylic acids industrial wastes is pre-processed:Collect after waste liquid, organic phase and aqueous phase are separated with extraction;Remain with
Machine phase, is stripped with sodium hydroxide solution, is produced;
(2)Dissolving, filtering:Water, then input p-aminobenzene sulfonic acid, industrial waste phenol dregs and pyrosulfurous acid respectively are added into reactor
Sodium, 68-75 DEG C is warming up to by reactor, is heated while stirring no less than 30 minutes;
(3)Addition:PH conditioning agents, regulation solution PH to 7-8 are slowly added into reactor;
(4)Polycondensation:Reactor is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, formaldehyde was dripped in 1-2 hours
Complete, insulation is no less than 2 hours;
(5)Sodium peroxydisulfate is dissolved with appropriate amount of deionized water, and is configured to 12% sodium peroxydisulfate solution;
(6)Copolymerization:9-Fluorenone -2- carboxylic acid industrial wastes, and slow dropwise addition sodium peroxydisulfate solution thereto are added into reactor,
Sodium peroxydisulfate solution was dripped off in 1-2 hours, keep solution temperature to be reacted between 85-95 DEG C 2-3 hours, water use regulation contains
Gu amount, gets product.
In use, the addition that it is subtracted with accounting for cement weight 1.5-1.8wt% is mixed in fresh concrete.
Embodiment 2:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
260 parts of industrial wastes, 88 parts of p-aminobenzene sulfonic acid, industrial 75 parts of waste phenol dregs, 24 parts of sodium pyrosulfite, 110 parts of formaldehyde, persulfuric acid
6 parts of sodium, 10 parts of PH conditioning agents, 60 parts of water.
Its preparation method be the same as Example 1.
Embodiment 3:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
250 parts of industrial wastes, 90 parts of p-aminobenzene sulfonic acid, industrial 70 parts of waste phenol dregs, 30 parts of sodium pyrosulfite, 100 parts of formaldehyde, persulfuric acid
10 parts of sodium, 2 parts of PH conditioning agents, 100 parts of water.
Its preparation method be the same as Example 1.
Embodiment 4:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
290 parts of industrial wastes, 84 parts of p-aminobenzene sulfonic acid, industrial 80 parts of waste phenol dregs, 22 parts of sodium pyrosulfite, 120 parts of formaldehyde, persulfuric acid
4 parts of sodium, 30 parts of PH conditioning agents, 40 parts of water.
Its preparation method be the same as Example 1.
Embodiment 5:
A kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, includes the raw material of following parts by weight:9-Fluorenone -2- carboxylic acids
320 parts of industrial wastes, 80 parts of p-aminobenzene sulfonic acid, industrial 90 parts of waste phenol dregs, 20 parts of sodium pyrosulfite, 140 parts of formaldehyde, persulfuric acid
3 parts of sodium, 80 parts of PH conditioning agents, 20 parts of water.
Its preparation method be the same as Example 1.
It is as shown in the table using water reducer properties data made from embodiment 1-5:
As seen from the above table, with water reducer and national standard made from embodiment 1-5《Concrete admixture》Testing standard compare, diminishing
Rate is higher, and air content is lower, and 28d shrinkage ratios are low, and obtained concrete crushing strength is high.
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
The present invention is described in detail, it will be understood by those within the art that:It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic;And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (6)
1. a kind of waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids, it is characterised in that include the raw material of following parts by weight:
250-320 parts of 9-Fluorenone -2- carboxylic acid industrial wastes, 80-90 parts of p-aminobenzene sulfonic acid, industrial waste phenol dregs 70-90 parts, pyrosulfurous acid
20-30 parts of sodium, 100-140 parts of formaldehyde, 3-10 parts of sodium peroxydisulfate, 0-80 parts of PH conditioning agents, 0-100 parts of water.
2. the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as claimed in claim 1, it is characterised in that including following weight
Measure the raw material of number:260-290 parts of 9-Fluorenone -2- carboxylic acid industrial wastes, 84-88 parts of p-aminobenzene sulfonic acid, industrial waste phenol dregs 75-
80 parts, 22-24 parts of sodium pyrosulfite, 110-120 parts of formaldehyde, 4-6 parts of sodium peroxydisulfate, 10-30 parts of PH conditioning agents, 40-60 parts of water.
3. the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as claimed in claim 1, it is characterised in that including following weight
Measure the raw material of number:275 parts of 9-Fluorenone -2- carboxylic acids industrial wastes, 86 parts of p-aminobenzene sulfonic acid, industrial 76 parts of waste phenol dregs, Jiao Ya
22 parts of sodium sulphate, 112 parts of formaldehyde, 5 parts of sodium peroxydisulfate, 18 parts of PH conditioning agents, 30 parts of water.
4. the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as claimed in claim 1, it is characterised in that the 9-Fluorenone -
2- carboxylic acids industrial wastes is pretreatment waste liquid, and the preprocess method is:Collect after waste liquid, organic phase and water are separated with extraction
Phase;Retain organic phase, be stripped with sodium hydroxide solution, produce 9-Fluorenone -2- carboxylic acids pretreatment industrial wastes.
5. the preparation method of the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as any one of claim 1-4, its
It is characterised by, comprises the following steps:
(1)Dissolving, filtering:Water, then input p-aminobenzene sulfonic acid, industrial waste phenol dregs and pyrosulfurous acid respectively are added into reactor
Sodium, 68-75 DEG C is warming up to by reactor, is heated while stirring no less than 30 minutes;
(2)Addition:PH conditioning agents, regulation solution PH to 7-8 are slowly added into reactor;
(3)Polycondensation:Reactor is warming up to 90-95 DEG C, formalin is slowly added dropwise thereto, formaldehyde was dripped in 1-2 hours
Complete, insulation is no less than 2 hours;
(4)Sodium peroxydisulfate is dissolved with appropriate amount of deionized water, and is configured to 12% sodium peroxydisulfate solution;
(5)Copolymerization:9-Fluorenone -2- carboxylic acid industrial wastes, and slow dropwise addition sodium peroxydisulfate solution thereto are added into reactor,
Sodium peroxydisulfate solution was dripped off in 1-2 hours, keep solution temperature to be reacted between 85-95 DEG C 2-3 hours, water use regulation contains
Gu amount, gets product.
6. the waste liquid modified high efficiency water reducing agent of 9-Fluorenone -2- carboxylic acids as any one of claim 1-4, it is characterised in that
The volume of the water reducer is the 1.5-1.8wt% of cement weight.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114180906A (en) * | 2021-11-22 | 2022-03-15 | 蒋雨炎 | Environment-friendly pervious concrete and preparation method thereof |
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CN114180906A (en) * | 2021-11-22 | 2022-03-15 | 蒋雨炎 | Environment-friendly pervious concrete and preparation method thereof |
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