CN108623767A - A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols - Google Patents
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols Download PDFInfo
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- CN108623767A CN108623767A CN201810482500.1A CN201810482500A CN108623767A CN 108623767 A CN108623767 A CN 108623767A CN 201810482500 A CN201810482500 A CN 201810482500A CN 108623767 A CN108623767 A CN 108623767A
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- parts
- waste residue
- production process
- phenols
- formaldehyde
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Classifications
-
- 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
- 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
-
- 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 provides a kind of modified amido sulfoacid series water-reducing agent of the waste residue in the production process containing phenols, is related to building material field, includes the raw material composition of following parts by weight：30 80 parts of waste residue, 80 110 parts of phenol in 100 180 parts of p-aminobenzene sulfonic acid, 80 150 parts of liquid caustic soda, 130 280 parts of formaldehyde, phenols production process, synthetic method includes the following steps：(1) above-mentioned raw materials are weighed；(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, be warming up to 40 60 DEG C of 1 3h of stirring, input phenol, the waste residue in phenols production process, the reaction was continued 30min；(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, 95 DEG C are heated to after being added dropwise, continues 3 4h of insulation reaction, cools down after insulation reaction, the present invention not only solves environmental issue, and creates economic benefit again.
Description
Technical field
The present invention relates to building material fields, and in particular to a kind of modified amido of the waste residue in the production process containing phenols
Sulfonic acid based water reducer.
Background technology
Water-reducing agent is a kind of under conditions of maintaining concrete slump to be basically unchanged, and can reduce the coagulation of mixing water amount
Native additive.Belong to anion surfactant mostly, there is lignosulfonates, naphthalene sulphonate formaldehyde polymer etc..It is added mixed
There is peptizaiton to cement granules after solidifying soil mixture, its workability can be improved, reduce unit consumption of water, improve concrete mixing
The mobility of object；Or unit cement consumption is reduced, save cement.
Either phenolic compound is synthetically produced in the useless residue generated in the process or a small amount of residual mother liquor containing different phenol
The substances such as propyl benzene, phenol, acetone, phenolic compound, belong to hazardous waste, are unable to direct emission, mostly use distillation, essence at present
The modes separating-purifying such as evaporate, extract, it is of high cost, energy consumption is big, it is not only solved if rationally utilizing it for producing water-reducing agent
It has determined environmental issue, and has created economic benefit again.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of modified amidos of the waste residue in production process containing phenols
Sulfonic acid based water reducer not only solves environmental issue, and creates economic benefit again.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 100-180 parts of p-aminobenzene sulfonic acid, 80-150 parts of liquid caustic soda, 130-280 parts of formaldehyde, phenols production process
30-80 parts of slag, 80-110 parts of phenol.
Preferably, including the raw material of following parts by weight forms：120-160 parts of p-aminobenzene sulfonic acid, 85-140 parts of liquid caustic soda,
85-100 parts of 40-70 parts of waste residue, phenol in 140-260 parts of formaldehyde, phenols production process.
Preferably, including the raw material of following parts by weight forms：130-150 parts of p-aminobenzene sulfonic acid, 90-130 parts of liquid caustic soda,
90-95 parts of 50-60 parts of waste residue, phenol in 150-250 parts of formaldehyde, phenols production process.
Preferably, including the raw material of following parts by weight forms：140 parts of p-aminobenzene sulfonic acid, 120 parts of liquid caustic soda, formaldehyde 200
Part, 55 parts of waste residue in phenols production process, 92 parts of phenol.
Preferably, a concentration of the 37% of the formaldehyde.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 40-60 DEG C and stirs
Mix 1-3h, the waste residue in input phenol, phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, 95 DEG C are heated to after being added dropwise, continues insulation reaction 3-4h,
Cool down after insulation reaction.
Preferably, the rate of addition of formaldehyde is controlled, is added dropwise in 1.5-4h.
Preferably, the modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, volume
For the 0.8-3.0% of cement weight.
(3) advantageous effect
The present invention provides a kind of modified amido sulfoacid series water-reducing agent of the waste residue in production process containing phenols, have with
Lower advantageous effect：
(1) present invention is directly using the useless residue generated in a kind of phenol or phenolic compound production process, without through appointing
Where reason is directly used in the pollution that synthesis modification amido sulfoacid series high-efficiency water reducer avoids waste discharge to environment, and solves
Useless Slag recovering processing is more complex, and not disposable, energy consumption is big, it is of high cost the problems such as, belong to the environment-friendly type of hazardous waste recycling
Invention.
(2) present invention introduces useless residue in isopropylbenzene, acetone etc. can participate in polymerizeing, can be with amido sulfoacid series
Grafting increases branch quantity, type in aminosulfonic water-reducing agent, can improve the slump effect of concrete.
(3) phenol in residue is utilized, it is possible to reduce the dosage of phenol in reaction process reduces being produced into for water-reducing agent
This.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Embodiment 1：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 140 parts of p-aminobenzene sulfonic acid, 120 parts of liquid caustic soda, a concentration of 37% 200 parts of formaldehyde, phenols production process
55 parts of slag, 92 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 50 DEG C of stirrings
2h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 2h, 95 DEG C are heated to after being added dropwise, continues
Insulation reaction 3.5h cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 2.0% of amount.
Embodiment 2：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 130 parts of p-aminobenzene sulfonic acid, 90 parts of liquid caustic soda, a concentration of 37% 150 parts of formaldehyde, phenols production process
50 parts of slag, 90 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 50 DEG C of stirrings
1.5h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 2.5h, 95 DEG C are heated to after being added dropwise, after
Continue insulation reaction 3.5h, cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 2.0% of amount.
Embodiment 3：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 150 parts of p-aminobenzene sulfonic acid, 130 parts of liquid caustic soda, a concentration of 37% 250 parts of formaldehyde, phenols production process
60 parts of slag, 95 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 45 DEG C of stirrings
1.5h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 2h, 95 DEG C are heated to after being added dropwise, continues
Insulation reaction 3.2h cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 1.5% of amount.
Embodiment 4：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 120 parts of p-aminobenzene sulfonic acid, 85 parts of liquid caustic soda, a concentration of 37% 140 parts of formaldehyde, phenols production process
40 parts of slag, 85 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 55 DEG C of stirrings
2.5h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 2.5h, 95 DEG C are heated to after being added dropwise, after
Continue insulation reaction 3.8h, cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 2.5% of amount.
Embodiment 5：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 160 parts of p-aminobenzene sulfonic acid, 140 parts of liquid caustic soda, a concentration of 37% 260 parts of formaldehyde, phenols production process
70 parts of slag, 100 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 50 DEG C of stirrings
1.5h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 2.5h, 95 DEG C are heated to after being added dropwise, after
Continue insulation reaction 3.5h, cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 1.0% of amount.
Embodiment 6：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 100 parts of p-aminobenzene sulfonic acid, 80 parts of liquid caustic soda, a concentration of 37% 130 parts of formaldehyde, phenols production process
30 parts of slag, 80 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 40 DEG C of stirrings
1h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 1.5h, 95 DEG C are heated to after being added dropwise, after
Continue insulation reaction 3h, cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 0.8% of amount.
Embodiment 7：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 180 parts of p-aminobenzene sulfonic acid, 150 parts of liquid caustic soda, a concentration of 37% 280 parts of formaldehyde, phenols production process
80 parts of slag, 110 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 60 DEG C of stirrings
3h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 4h, 95 DEG C are heated to after being added dropwise, continues
Insulation reaction 4h cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 3.0% of amount.
Embodiment 8：
A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols, including following parts by weight
Raw material forms：It is useless in 110 parts of p-aminobenzene sulfonic acid, 90 parts of liquid caustic soda, a concentration of 37% 140 parts of formaldehyde, phenols production process
40 parts of slag, 90 parts of phenol.
The modified amido sulfoacid series water-reducing agent of waste residue in the above-mentioned production process containing phenols, synthetic method include following
Step：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, is warming up to 40 DEG C of stirrings
3h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, is added dropwise in 1.5h, 95 DEG C are heated to after being added dropwise, after
Continue insulation reaction 4h, cools down after insulation reaction.
Above-mentioned modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
The 0.8% of amount.
The following table 1 is the water-reducing rate comparing result of product and commercially available aminosulfonic water-reducing agent prepared by the embodiment of the present invention 1：
The following table 2 is the slump comparing result of product and commercially available aminosulfonic water-reducing agent prepared by the embodiment of the present invention 1：
Table 1：
Table 2：
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
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, it will be understood by those of ordinary skill in the art that：It still can be to aforementioned each implementation
Technical solution recorded in example is modified or equivalent replacement of some of the technical features；And these modification or
It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of modified amido sulfoacid series water-reducing agent of the waste residue in production process containing phenols, which is characterized in that including following
The raw material of parts by weight forms：100-180 parts of p-aminobenzene sulfonic acid, 80-150 parts of liquid caustic soda, 130-280 parts of formaldehyde, phenols production
80-110 parts of 30-80 parts of waste residue, phenol in the process.
2. the modified amido sulfoacid series water-reducing agent containing the waste residue in phenols production process as described in claim 1, feature
It is, includes the raw material composition of following parts by weight：120-160 parts of p-aminobenzene sulfonic acid, 85-140 parts of liquid caustic soda, formaldehyde 140-
260 parts, 40-70 parts of waste residue in phenols production process, 85-100 parts of phenol.
3. the modified amido sulfoacid series water-reducing agent containing the waste residue in phenols production process as claimed in claim 2, feature
It is, includes the raw material composition of following parts by weight：130-150 parts of p-aminobenzene sulfonic acid, 90-130 parts of liquid caustic soda, formaldehyde 150-
250 parts, 50-60 parts of waste residue in phenols production process, 90-95 parts of phenol.
4. the modified amido sulfoacid series water-reducing agent containing the waste residue in phenols production process as claimed in claim 3, feature
It is, includes the raw material composition of following parts by weight：140 parts of p-aminobenzene sulfonic acid, 120 parts of liquid caustic soda, 200 parts of formaldehyde, phenols life
92 parts of 55 parts of waste residue, phenol during production.
5. the modified amido sulfoacid series diminishing containing the waste residue in phenols production process as described in any one of claim 1-4
Agent, which is characterized in that a concentration of the 37% of the formaldehyde.
6. the modified amido sulfoacid series diminishing containing the waste residue in phenols production process as described in any one of claim 1-4
Agent, which is characterized in that its synthetic method includes the following steps：
(1) above-mentioned raw materials are weighed；
(2) it adds water in four-hole boiling flask, p-aminobenzene sulfonic acid, liquid caustic soda is added while stirring, be warming up to 40-60 DEG C of stirring 1-
3h, input phenol, the waste residue in phenols production process, the reaction was continued 30min；
(3) formaldehyde is added dropwise, controls the rate of addition of formaldehyde, 95 DEG C are heated to after being added dropwise, continues insulation reaction 3-4h, heat preservation
Cool down after reaction.
7. the modified amido sulfoacid series water-reducing agent containing the waste residue in phenols production process as claimed in claim 6, feature
It is, controls the rate of addition of formaldehyde, be added dropwise in 1.5-4h.
8. the modified amido sulfoacid series water-reducing agent containing the waste residue in phenols production process as claimed in claim 6, feature
It is, the modified amido sulfoacid series water-reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
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| CN201810482500.1A CN108623767A (en) | 2018-05-18 | 2018-05-18 | A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols |
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| CN201810482500.1A CN108623767A (en) | 2018-05-18 | 2018-05-18 | A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols |
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Cited By (3)
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| CN108586683A (en) * | 2018-05-18 | 2018-09-28 | 萧县沃德化工科技有限公司 | The method that heavy distillat prepares modified aliphatic high efficiency water reducing agent in ethanol production process |
| CN111748067A (en) * | 2020-06-11 | 2020-10-09 | 安徽鑫固环保股份有限公司 | Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater |
| CN112592452A (en) * | 2020-10-27 | 2021-04-02 | 安徽鑫固环保股份有限公司 | Method for resource utilization of resorcinol distillation residues |
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| US20060134335A1 (en) * | 2004-12-17 | 2006-06-22 | David Glassel | Methods for preventing warping in wood products |
| CN102898060A (en) * | 2012-11-01 | 2013-01-30 | 徐友娟 | Efficient sulfamic acid water reducing agent and preparation method thereof |
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| CN108586683A (en) * | 2018-05-18 | 2018-09-28 | 萧县沃德化工科技有限公司 | The method that heavy distillat prepares modified aliphatic high efficiency water reducing agent in ethanol production process |
| CN111748067A (en) * | 2020-06-11 | 2020-10-09 | 安徽鑫固环保股份有限公司 | Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater |
| CN112592452A (en) * | 2020-10-27 | 2021-04-02 | 安徽鑫固环保股份有限公司 | Method for resource utilization of resorcinol distillation residues |
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Application publication date: 20181009 |