CN108033706A - A kind of synthetic method of modified naphthalene series sulfonate water reducer - Google Patents
A kind of synthetic method of modified naphthalene series sulfonate water reducer Download PDFInfo
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- CN108033706A CN108033706A CN201711468726.8A CN201711468726A CN108033706A CN 108033706 A CN108033706 A CN 108033706A CN 201711468726 A CN201711468726 A CN 201711468726A CN 108033706 A CN108033706 A CN 108033706A
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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
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of synthetic method of modified naphthalene series sulfonate water reducer, include the following steps：(1) sulfonation；(2) hydrolyze；(3) it is condensed；(4) neutralize.The present invention opens the new way of processing and the comprehensive utilization of recovery acid in isooctane production process; the pollution situation of isooctane industry can effectively be improved; both environment is protected; again so that caused recovery acid is comprehensively utilized in isooctane production process, with good economic efficiency and environmental benefit.
Description
Technical field
The invention belongs to build additive technical field, and in particular to a kind of synthesis side of modified naphthalene series sulfonate water reducer
Method.
Background technology
Isooctane is reconciliation component important in China's gasoline, and isooctane is steamed with its high-octane rating, low sensitivity, low thunder
Vapour pressure, volatility, the advantages that flammability and shock resistance are preferable, become a kind of high-quality and indispensable gasoline and reconcile component.Mesh
Before, isooctane generally industrially is prepared using the liquid acid alkylation processes of iso-butane and butylene, reaction member is with dense sulphur
Acid is in the presence of catalyst, iso-butane and butylene is quickly alkylated reaction in isooctane reactor, after the completion of reaction, production
A series of dedoping steps such as thing is washed using the concentrated sulfuric acid, alkali cleaning and washing.
Above-mentioned technique experienced sulfuric acid catalysis, acid cleaning process, generate substantial amounts of high concentration recycling sulfuric acid.At present, China
Sulfur waste acid treatment mainly has Waste Sulfuric Acid concentration, Pintsch process, chemical oxidation, extraction, crystallization, the production work such as chemical fertilizer and neutralisation treatment
Skill.Each enterprise generally takes not according to purposes of sulfuric acid after Waste Sulfuric Acid amount, sulfur waste acid concentration, impurity component and content, processing etc.
Same treatment process, it is sometimes desirable to which several techniques are used cooperatively.In these methods, processing high-concentration sulfuric acid is required for spending high
Cost, the financial cost of relevant enterprise is considerably increased, nor the processing method of whole level.
The cost of conventional process high concentration recycling sulfuric acid is generally all higher, as patent CN106976896A reports a kind of profit
With the method for waste sulfuric acid from alkylation production epsom salt, this method needs to carry out pyrolytic, dedusting to waste sulfuric acid from alkylation
It is lower with respect to sexual valence etc. complex process link.For another example patent CN103351108A is reported discharges in diarylethane production
Thing synthesizes cement water reducing agent technique with byproduct, and a small amount of waste sulfuric acid from alkylation collocation dense sulphur of national standard is only make use of in the patent
Acid, and the high waste oil foot of its by-product is added to prepare concrete high efficiency water reducing agent.It is big for being produced in isooctane production process
Amount high concentration recycling sulfuric acid does not have the ultimate administering method that a financial cost is low, service efficiency is high also.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided a kind of synthesis side of modified naphthalene series sulfonate water reducer
Method.
Technical scheme is as follows：
A kind of synthetic method of modified naphthalene series sulfonate water reducer, includes the following steps：
(1) sulfonation：In parts by mass, toward 95~125 parts of crude naphthalenes of addition in reaction kettle, 120~135 DEG C are heated to
When, start 115~165 parts of recovery acids of dropwise addition, be added dropwise in 0.5~1.5h；It is warm in reaction kettle after recovery acid is added dropwise
Degree control continues 3~5h of insulation at 145~175 DEG C；Above-mentioned recovery acid is the catalysis concentrated sulfuric acid in isooctane production process and washes
The mixture of both concentrated sulfuric acids is washed, wherein the content of titratable acid is 89~91%, and contains organo-sulfate and iso-butane；
(2) hydrolyze：In parts by mass, the material obtained by step (1) is cooled to 105~120 DEG C, adds 40~65 parts
Water, is hydrolyzed 17~45min of reaction；
(3) it is condensed：In parts by mass, the material obtained by step (2) is cooled to 85~100 DEG C, 45~85 parts of dropwise addition is dense
The formalin for 36~40wt% is spent, is added dropwise in 2~4h, then heats to 103~112 DEG C, keeps the temperature 3~8h, is protected
During temperature points 2 times it is each add 14~33 parts of hot water not less than 60 DEG C to adjust material viscosity, finally according to demand with 180~
420 parts of water are diluted；
(4) neutralize：Liquid adjusting PH with base is added into the material obtained by step (3) to 7~9, after being cooled to room temperature, up to described
Modified naphthalene series sulfonate water reducer.
In a preferred embodiment of the invention, the step (1) is：In parts by mass, toward adding in reaction kettle
100~120 parts of crude naphthalenes, when heating to 120~130 DEG C, start 120~160 parts of recovery acids of dropwise addition, in 0.5~1.5h
Inside it is added dropwise；After recovery acid is added dropwise, reactor temperature is controlled at 150~170 DEG C, continues 3~5h of insulation.
In a preferred embodiment of the invention, the step (2) is：In parts by mass, by obtained by step (1)
Material cools to 110~120 DEG C, adds 40~60 parts of water, 20~40min of reaction is hydrolyzed.
In a preferred embodiment of the invention, the step (3) is：In parts by mass, by obtained by step (2)
Material cools to 90~98 DEG C, and the formalin that 50~80 parts of concentration are 36~40wt% is added dropwise, is added dropwise in 2~4h,
103~110 DEG C are then heated to, keeps the temperature 3~8h, 2 each 15~30 parts of hot water for being not less than 60 DEG C of addition are divided in insulating process
To adjust material viscosity, finally it is diluted according to demand with 200~400 parts of water.
In a preferred embodiment of the invention, the concentration of the formalin is 37wt%.
The beneficial effects of the invention are as follows：
1st, the present invention provide not only a kind of ultimate processing method of caused recovery acid in isooctane production process, more
It is important that provide a kind of new method of the caused recovery acid utilization of resources in isooctane production process.In industrial production,
Caused recycling acid yield is big in isooctane production process, concentration is high, processing cost is high.The present invention opens isooctane life
The new way of processing and the comprehensive utilization of recovery acid during production, can effectively improve the pollution situation of isooctane industry, both
Environment is protected, and make it that caused recovery acid is comprehensively utilized in isooctane production process, there is good economic effect
Benefit and environmental benefit.
2nd, using the method for the present invention, modified naphthalene series sulfonic acid is made using caused recovery acid in isooctane production process
Salt
Water-reducing agent, because containing the accessory substances such as a small amount of organo-sulfate, iso-butane in recovery acid, in high-temperature sulfuric acid sulfonation
Cheng Zhong, generates more small molecule, changes this low defect of naphthalene sulfonic salt amount of air entrainment so that is prepared using the present invention
Modified naphthalene series sulfonate water reducer has the characteristics that dispersion performance is good, amount of air entrainment is high, workability is good.
3rd, using the modified naphthalene series sulfonate water reducer for preparing of the present invention because using caused by isooctane production process
Recovery acid can substantially reduce the cost of material of naphthalene sulfonic salt water-reducing agent as raw material, improve cost performance and the enterprise of product
Benefit.
Embodiment
Technical scheme is further detailed and described below by way of embodiment.
Recovery acid in following embodiments is the catalysis concentrated sulfuric acid and both washing concentrated sulfuric acids in isooctane production process
The content of mixture, wherein titratable acid is 89~91%, and contains a small amount of organo-sulfate and iso-butane.
Embodiment 1
(1) sulfonation：In parts by mass, toward 100 parts of crude naphthalenes of addition in reaction kettle, when heating to 120 DEG C, start to drip
Add 130 parts of recovery acids, be added dropwise in 1h；When recovery acid is added dropwise, reactor temperature is controlled at 160 DEG C, after continuation of insurance
Warm 3h；
(2) hydrolyze：In parts by mass, after sulfonating reaction, 120 DEG C are cooled to, 50 parts of water is added, reaction is hydrolyzed
30min；
(3) it is condensed：In parts by mass, after hydrolysis, 98 DEG C are cooled to, the first that 60 parts of concentration are 37wt% is added dropwise
Aldehyde solution, is added dropwise in 2h；103 DEG C are warming up to, keeps the temperature 3h；Point 2 each 15 parts of additions are not less than 60 DEG C in insulating process
Hot water adjust material viscosity, be finally diluted according to demand with 300 parts of water；
(4) neutralize：After insulation, 200 parts of liquid adjusting PH with base are added to 7~9, after being cooled to room temperature, up to product.
Embodiment 2
(1) sulfonation：In parts by mass, toward 100 parts of crude naphthalenes of addition in reaction kettle, when heating to 120 DEG C, start to drip
Add 135 parts of recovery acids, be added dropwise in 1.5h；When recovery acid is added dropwise, reactor temperature is controlled at 160 DEG C, is continued
Keep the temperature 3h；
(2) hydrolyze：In parts by mass, after sulfonating reaction, 120 DEG C are cooled to, 50 parts of water is added, reaction is hydrolyzed
30min；
(3) it is condensed：In parts by mass, after hydrolysis, 98 DEG C are cooled to, the first that 63 parts of concentration are 37wt% is added dropwise
Aldehyde solution, is added dropwise in 2h；103 DEG C are warming up to, keeps the temperature 3h；Point 2 each 15 parts of additions are not less than 60 DEG C in insulating process
Hot water adjust material viscosity, be finally diluted according to demand with 300 parts of water；
(4) neutralize：After insulation, 200 parts of liquid adjusting PH with base are added to 7~9, after being cooled to room temperature, up to product.
Embodiment 3
(1) sulfonation：In parts by mass, toward 100 parts of crude naphthalenes of addition in reaction kettle, when heating to 120 DEG C, start to drip
Add 1358 parts of recovery acids, be added dropwise in 1.5h；When recovery acid is added dropwise, reactor temperature is controlled at 162 DEG C, is continued
Keep the temperature 4h；
(2) hydrolyze：In parts by mass, after sulfonating reaction, 120 DEG C are cooled to, 55 parts of water is added, reaction is hydrolyzed
30min；
(3) it is condensed：In parts by mass, after hydrolysis, 98 DEG C are cooled to, the first that 63 parts of concentration are 37wt% is added dropwise
Aldehyde solution, is added dropwise in 3h；105 DEG C are warming up to, keeps the temperature 5h；Point 2 each 18 parts of additions are not less than 60 DEG C in insulating process
Hot water adjust material viscosity, be finally diluted according to demand with 300 parts of water；
(4) neutralize：After insulation, 200 parts of liquid adjusting PH with base are added to 7~9, after being cooled to room temperature, up to product.
Embodiment 4
(1) sulfonation：In parts by mass, toward 100 parts of crude naphthalenes of addition in reaction kettle, when heating to 125 DEG C, start to drip
Add 1358 parts of recovery acids, be added dropwise in 1.5h；When recovery acid is added dropwise, reactor temperature is controlled at 165 DEG C, is continued
Keep the temperature 4h；
(2) hydrolyze：In parts by mass, after sulfonating reaction, 115 DEG C are cooled to, 60 parts of water is added, reaction is hydrolyzed
30min；
(3) it is condensed：In parts by mass, after hydrolysis, 95 DEG C are cooled to, the first that 65 parts of concentration are 37wt% is added dropwise
Aldehyde solution, is added dropwise in 3h；105 DEG C are warming up to, keeps the temperature 5h；Point 2 each 20 parts of additions are not less than 60 DEG C in insulating process
Hot water adjust material viscosity, be finally diluted according to demand with 300 parts of water；
(4) neutralize：After insulation, 200 parts of liquid adjusting PH with base are added to 7~9, after being cooled to room temperature, up to product.
Embodiment 5
(1) sulfonation：In parts by mass, toward 110 parts of crude naphthalenes of addition in reaction kettle, when heating to 125 DEG C, start to drip
Add 1358 parts of recovery acids, be added dropwise in 1.5h；When recovery acid is added dropwise, reactor temperature is controlled at 165 DEG C, is continued
Keep the temperature 4h；
(2) hydrolyze：In parts by mass, after sulfonating reaction, 115 DEG C are cooled to, 60 parts of water is added, reaction is hydrolyzed
30min；
(3) it is condensed：In parts by mass, after hydrolysis, 100 DEG C are cooled to, it is 37wt%'s that 65 parts of concentration, which are added dropwise,
Formalin, is added dropwise in 3h；110 DEG C are warming up to, keeps the temperature 5h；Point 2 each 20 parts of additions are not less than 60 in insulating process
DEG C hot water adjust material viscosity, be finally diluted according to demand with 300 parts of water；
(4) neutralize：After insulation, 200 parts of liquid adjusting PH with base are added to 7~9, after being cooled to room temperature, up to product.
Embodiment 6
Embodiment 6 is the performance test of modified naphthalene series sulfonate water reducer made from embodiment 1~5.
Embodiment 1~5 is synthesized into obtained modified naphthalene series sulfonate water reducer and common naphthalene sulfonic salt water-reducing agent (FDN)
Concrete performance contrast, using southern P.O42.5R cement, volume for glue material quality 0.5% (folding solid part), according to
GB8076-2008《Concrete admixture》, test its glue sand water-reducing rate, concrete slump, air content and concrete and easily
Property.Concrete mix is：Water：170Kg, cement (P.O42.5R)：250Kg, coal ash (II grades)：50Kg, miberal powder (S95)：
60Kg, river sand：570Kg, fine sand：200Kg, stone 1020Kg, it is as shown in the table for acquired results.
1 embodiment performance comparison of table
Note："+" represents that workability is good and bad, and "+" is more, and workability is better.
Those of ordinary skill in the art understand, when technical parameter of the invention changes in following ranges, remain able to
To same as the previously described embodiments or similar technique effect, protection scope of the present invention is still fallen within：
A kind of synthetic method of modified naphthalene series sulfonate water reducer, includes the following steps：
(1) sulfonation：In parts by mass, toward 95~125 parts of crude naphthalenes of addition in reaction kettle, 120~135 DEG C are heated to
When, start 115~165 parts of recovery acids of dropwise addition, be added dropwise in 0.5~1.5h；It is warm in reaction kettle after recovery acid is added dropwise
Degree control continues 3~5h of insulation at 145~175 DEG C；Above-mentioned recovery acid is the catalysis concentrated sulfuric acid in isooctane production process and washes
The mixture of both concentrated sulfuric acids is washed, wherein the content of titratable acid is 89~91%, and contains organo-sulfate and iso-butane；It is excellent
Choosing, in parts by mass, 100~120 parts of crude naphthalenes are added into reaction kettle, when heating to 120~130 DEG C, start to drip
Add 120~160 parts of recovery acids, be added dropwise in 0.5~1.5h；After recovery acid is added dropwise, reactor temperature control exists
150~170 DEG C, continue 3~5h of insulation；
(2) hydrolyze：In parts by mass, the material obtained by step (1) is cooled to 105~120 DEG C, adds 40~65 parts
Water, is hydrolyzed 17~45min of reaction；Preferably, in parts by mass, the material obtained by step (1) is cooled to 110~120
DEG C, 40~60 parts of water are added, 20~40min of reaction is hydrolyzed；
(3) it is condensed：In parts by mass, the material obtained by step (2) is cooled to 85~100 DEG C, 45~85 parts of dropwise addition is dense
The formalin for 36~40wt% is spent, is added dropwise in 2~4h, then heats to 103~112 DEG C, keeps the temperature 3~8h, is protected
During temperature points 2 times it is each add 14~33 parts of hot water not less than 60 DEG C to adjust material viscosity, finally according to demand with 180~
420 parts of water are diluted；Preferably, in parts by mass, the material obtained by step (2) is cooled to 90~98 DEG C, it is added dropwise 50~
80 parts of concentration are the formalin of 36~40wt%, are added dropwise in 2~4h, then heat to 103~110 DEG C, insulation 3~
8h, in insulating process points 2 times it is each add 15~30 parts of hot water not less than 60 DEG C to adjust material viscosity, finally use according to demand
200~400 parts of water are diluted；
(4) neutralize：Liquid adjusting PH with base is added into the material obtained by step (3) to 7~9, after being cooled to room temperature, up to described
Modified naphthalene series sulfonate water reducer.
The foregoing is only a preferred embodiment of the present invention, therefore cannot limit the scope that the present invention is implemented according to this, i.e.,
The equivalent changes and modifications made according to the scope of the claims of the present invention and description, all should still belong in the range of the present invention covers.
Claims (5)
- A kind of 1. synthetic method of modified naphthalene series sulfonate water reducer, it is characterised in that：Include the following steps：(1) sulfonation：In parts by mass, toward adding 95~125 parts of crude naphthalenes in reaction kettle, when heating to 120~135 DEG C, Start 115~165 parts of recovery acids of dropwise addition, be added dropwise in 0.5~1.5h；After recovery acid is added dropwise, reactor temperature Control continues 3~5h of insulation at 145~175 DEG C；Above-mentioned recovery acid is the catalysis concentrated sulfuric acid and washing in isooctane production process The content of the mixture of both concentrated sulfuric acids, wherein titratable acid is 89~91%, and contains organo-sulfate and iso-butane；(2) hydrolyze：In parts by mass, the material obtained by step (1) is cooled to 105~120 DEG C, adds 40~65 parts of water, into 17~45min of row hydrolysis；(3) it is condensed：In parts by mass, the material obtained by step (2) is cooled to 85~100 DEG C, 45~85 parts of concentration, which are added dropwise, is The formalin of 36~40wt%, is added dropwise in 2~4h, then heats to 103~112 DEG C, keeps the temperature 3~8h, kept the temperature Point 2 each 14~33 parts of hot water not less than 60 DEG C of addition are to adjust material viscosity in journey, finally according to demand with 180~420 Part water is diluted；(4) neutralize：Liquid adjusting PH with base is added into the material obtained by step (3) to 7~9, after being cooled to room temperature, up to the modification Naphthalene sulfonic salt water-reducing agent.
- 2. synthetic method as claimed in claim 1, it is characterised in that：The step (1) is：In parts by mass, toward reaction kettle 100~120 parts of crude naphthalenes of middle addition, when heating to 120~130 DEG C, start 120~160 parts of recovery acids of dropwise addition, 0.5 It is added dropwise in~1.5h；After recovery acid is added dropwise, reactor temperature is controlled at 150~170 DEG C, continues 3~5h of insulation.
- 3. synthetic method as claimed in claim 1, it is characterised in that：The step (2) is：In parts by mass, by step (1) The material of gained cools to 110~120 DEG C, adds 40~60 parts of water, 20~40min of reaction is hydrolyzed.
- 4. synthetic method as claimed in claim 1, it is characterised in that：The step (3) is：In parts by mass, by step (2) The material of gained cools to 90~98 DEG C, and the formalin that 50~80 parts of concentration are 36~40wt% is added dropwise, is added dropwise in 2~4h Finish, then heat to 103~110 DEG C, keep the temperature 3~8h, divide 2 each 15~30 parts of additions to be not less than 60 DEG C in insulating process Hot water is finally diluted with 200~400 parts of water according to demand with adjusting material viscosity.
- 5. the synthetic method as described in any claim in Claims 1-4, it is characterised in that：The formalin it is dense Spend for 37wt%.
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| CN108609887A (en) * | 2018-05-18 | 2018-10-02 | 萧县沃德化工科技有限公司 | The method that the spent lye of mercerization prepares modified naphthalene series water-reducing agent |
| CN109279803A (en) * | 2018-12-03 | 2019-01-29 | 广东科隆智谷新材料股份有限公司 | The improvement of naphthalene water reducer preparation method and its control method of quality index |
| CN109534712A (en) * | 2018-10-25 | 2019-03-29 | 浙江龙盛化工研究有限公司 | A kind of light yellow naphthalene water reducer and preparation method thereof |
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| CN108609887A (en) * | 2018-05-18 | 2018-10-02 | 萧县沃德化工科技有限公司 | The method that the spent lye of mercerization prepares modified naphthalene series water-reducing agent |
| CN109534712A (en) * | 2018-10-25 | 2019-03-29 | 浙江龙盛化工研究有限公司 | A kind of light yellow naphthalene water reducer and preparation method thereof |
| CN109534712B (en) * | 2018-10-25 | 2021-09-21 | 浙江龙盛化工研究有限公司 | Light yellow naphthalene water reducing agent and preparation method thereof |
| CN109279803A (en) * | 2018-12-03 | 2019-01-29 | 广东科隆智谷新材料股份有限公司 | The improvement of naphthalene water reducer preparation method and its control method of quality index |
| CN109279803B (en) * | 2018-12-03 | 2021-05-07 | 广东科隆智谷新材料股份有限公司 | Improvement of naphthalene series water reducing agent preparation method and control method of quality index thereof |
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| CN108033706B (en) | 2020-10-09 |
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