CN111423551A - System for producing high-concentration naphthalene water reducer by naphthalene excess method and production method thereof - Google Patents
System for producing high-concentration naphthalene water reducer by naphthalene excess method and production method thereof Download PDFInfo
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- CN111423551A CN111423551A CN202010253668.2A CN202010253668A CN111423551A CN 111423551 A CN111423551 A CN 111423551A CN 202010253668 A CN202010253668 A CN 202010253668A CN 111423551 A CN111423551 A CN 111423551A
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- naphthalene
- temperature
- pipeline
- reaction kettle
- concentration
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- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 21
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000009833 condensation Methods 0.000 claims abstract description 17
- 230000005494 condensation Effects 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 48
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 238000006277 sulfonation reaction Methods 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KVBGVZZKJNLNJU-UHFFFAOYSA-N naphthalene-2-sulfonic acid Chemical compound C1=CC=CC2=CC(S(=O)(=O)O)=CC=C21 KVBGVZZKJNLNJU-UHFFFAOYSA-N 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000008030 superplasticizer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
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
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/0212—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds
- C08G16/0218—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen
- C08G16/0237—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen containing sulfur
-
- 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 invention discloses a system for producing a high-concentration naphthalene water reducing agent by a naphthalene excess method, which comprises a reaction kettle, a conveying device and a condenser, wherein the reaction kettle is communicated with the conveying device through a pipeline; a production method for producing a high-concentration naphthalene water reducer by a naphthalene excess method comprises the following steps of S1; s2, sulfonation; s3, naphthalene removal; s4, distributing materials; s5, condensation; and S6, neutralizing. The invention has the advantages that: can meet the requirements of quickly dispersing and mixing the sulfonating agent, avoiding multi-sulfonation, saving energy, reducing exhaust emission and improving production efficiency.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a system for producing a high-concentration naphthalene water reducer by a naphthalene excess method and a production method thereof.
Background
The naphthalene water reducer is a high-efficiency water reducer widely applied, is a superplasticizer, has good water reducing and early strengthening effects, is mostly applied to the concrete industry, and is also applied to the industries of gypsum boards, coal water slurries, ceramics, oil wells and the like, the production process mainly comprises the steps of putting industrial naphthalene into a reaction kettle, heating to a certain temperature, stirring while dropwise adding concentrated sulfuric acid for sulfonation, preserving heat, hydrolyzing, adding formaldehyde for condensation, neutralizing and drying, and the production process of the naphthalene water reducer generally comprises two methods, namely, the first method comprises the steps of sulfonating in the reaction kettle, dropwise adding formaldehyde for condensation in the same reaction kettle after sulfonation, and the other method comprises the steps of sulfonating in the reaction kettle, transferring to another condensation kettle after sulfonation, and dropwise adding formaldehyde for condensation, wherein the first method comprises the following four problems that (1) during large-scale production, the heat loss is large because a refrigerant and a heating medium are alternately used, the heat loss is high, (2) the second method comprises the steps of seriously losing heat during single-batch operation, the heat release is not fully utilized, and (3) the reaction area is large, the waste gas volatilization amount of waste gas is large, the production efficiency is realized, the continuous production efficiency is low, the effect of the continuous production efficiency, the concentrated sulfuric acid is not affected, the next step, the second method is not only when the concentrated sulfuric acid is 355%, the concentrated sulfuric acid is easily reduced, and the concentrated sulfuric acid is easily used, and the concentrated sulfuric acid is easily reduced, and.
Disclosure of Invention
The invention aims to solve the technical problem of providing a production system for producing a naphthalene water reducer by a naphthalene excess method and a production method thereof, which can meet the requirements of quickly dispersing and mixing a sulfonating agent, avoiding multi-sulfonation, saving energy, reducing waste gas emission and improving production efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the utility model provides a high enriched naphthalene water reducing agent system of excessive method production of naphthalene, includes reation kettle, conveying equipment and condenser, reation kettle passes through pipeline and conveying equipment intercommunication, conveying equipment has industry naphthalene storage device, condensation cauldron and solvent storage device through the pipeline intercommunication, reation kettle has the condenser through the pipeline intercommunication, the condenser has the separator through the pipeline intercommunication, the separator with through pipeline and solvent storage device intercommunication, the separator has water storage device through the pipeline intercommunication.
As an improvement, a mixer is arranged on a pipeline between the reaction kettle and the conveying device, and the mixer is communicated with a sulfonating agent storage device through a pipeline.
As an improvement, the reaction kettle adopts a reaction kettle with a stirring shaft.
A production method for producing a naphthalene water reducer by a naphthalene excess method comprises the following steps:
s1, feeding, namely adding accurately-metered liquid naphthalene into a reaction kettle, and opening steam to increase the temperature;
s2, sulfonating, namely slowly adding metered sulfuric acid at a constant speed when the temperature of naphthalene is 140-145 ℃, adding acid for 55-65 min, continuously adding steam for heating, keeping the temperature when the temperature is 160 ℃, controlling the temperature to be 160-165 ℃, keeping the temperature for 2.5 hours, and keeping the temperature above 160 ℃ when the temperature is finished;
s3, removing naphthalene, opening a steam inlet and outlet valve, filling steam into the reaction kettle, adjusting feeding according to the condensation temperature, enabling a large amount of acid water to flow out of the separator and a large amount of liquid naphthalene to flow out of the separator, stopping filling steam when the naphthalene amount reaches a designed value, taking 5-10 hours, and sampling to measure the acidity to be 20-25%;
s4, distributing materials, opening heat-preservation steam of a feeding pipeline, melting the materials in the pipeline, opening a feeding valve of the condensation kettle, closing all other valves, and feeding through a feeding pump;
s5, condensing, namely adding metered formaldehyde in a trickle mode, adding the formaldehyde for 2-3 hours, observing the temperature, keeping the temperature within 100 ℃, stopping adding the formaldehyde when the temperature exceeds 100 ℃, continuing adding the formaldehyde after the temperature is reduced to 95-100 ℃, raising the temperature to 105-115 ℃ after adding the formaldehyde, keeping the temperature of the tail gas at the upper part not more than 60 ℃, condensing for 6-8 hours, stopping condensing when the net current rise value reaches 10-12A, immediately adding 200 liters of wastewater, and continuing stirring for 1-2 hours;
and S6, neutralizing, namely adding caustic soda for neutralization until the pH value is 7-9.
As an improvement, the concentration of the sulfuric acid added in the S2 is 92-105%.
Compared with the prior art, the system and the production method have the advantages that the system for producing the high-concentration naphthalene water reducing agent by the naphthalene excess method adopts sulfonation with lower complex acid amount, is not easy to produce disulfonic acid or polysulfonic acid, improves the selectivity of β -naphthalenesulfonic acid, improves the quality of the water reducing agent, reduces waste residue discharge, adopts naphthalene as a water-carrying agent, recycles naphthalene during sulfonation of the next batch, does not use a solvent during sulfonation, is clean and environment-friendly, omits a hydrolysis process, saves electric energy during stirring, adopts a large-volume reaction kettle for centralized sulfonation, fully utilizes reaction heat, maintains the temperature of the reaction kettle, reduces steam usage, adopts the large-volume reaction kettle for centralized sulfonation, reduces waste gas discharge, adopts steam heat preservation for a pipeline, and avoids material condensation.
Drawings
FIG. 1 is a block diagram of a system for producing a high-concentration naphthalene water reducer by a naphthalene excess method.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments:
examples
A system for producing a high-concentration naphthalene water reducer by a naphthalene excess method comprises a reaction kettle, a pipeline for conveying equipment, a pipeline for communicating an upper inlet of the reaction kettle with an upper opening of a condenser, the pipeline for communicating the conveying equipment with a condensation kettle, a pipeline for communicating a lower interface of the condenser with an upper inlet of a separator, a pipeline for communicating an upper interface of the separator with a water storage device, a pipeline for communicating a lower interface of the separator with a solvent device, a pipeline for communicating a lower interface of the conveying equipment with a lower interface of the solvent storage device, a pipeline for communicating an inlet of the conveying equipment with an industrial naphthalene storage device, and a pipeline for symmetrically connecting a left inlet and a right inlet of a mixer with the outlet of the conveying equipment. The mixer is positioned on a pipeline for connecting the conveying equipment and the reaction kettle, and the mixer is connected with the sulfonating agent storage equipment by a pipeline.
A production method for producing a naphthalene water reducer by a naphthalene excess method comprises the following steps:
s1, feeding, namely adding accurately-metered liquid naphthalene into a reaction kettle, and opening steam to increase the temperature;
s2, sulfonating, when the temperature of naphthalene is 145 ℃, slowly and uniformly adding metered sulfuric acid, adding acid for 60min, continuously adding steam for heating, when the temperature is 160 ℃, starting heat preservation, controlling the temperature to be 160-165 ℃, preserving the heat for 2.5 hours, and when the heat preservation is finished, keeping the temperature to be above 160 ℃;
s3, removing naphthalene, opening a steam inlet and outlet valve, filling steam into the reaction kettle, adjusting feeding according to the condensation temperature, enabling a large amount of acid water to flow out of the separator and a large amount of liquid naphthalene to flow out of the separator, stopping filling steam when the naphthalene amount reaches a designed value, and sampling to measure the acidity to be 25% when the time is 8 hours;
s4, distributing materials, opening heat-preservation steam of a feeding pipeline, melting the materials in the pipeline, opening a feeding valve of the condensation kettle, closing all other valves, and feeding through a feeding pump;
s5, condensation, namely adding metered formaldehyde in a trickle mode, adding the formaldehyde for 2.5 hours, observing the temperature, keeping the temperature within 100 ℃, stopping adding the formaldehyde when the temperature exceeds 100 ℃, continuing adding the formaldehyde after the temperature is reduced to 95 ℃, raising the temperature to 110 ℃ after the formaldehyde is added, keeping the temperature of the upper tail gas below 60 ℃, terminating the condensation for 7 hours, immediately adding 200 liters of wastewater when the net current rise value reaches 10-12A, and continuing stirring for 2 hours;
and S6, neutralizing, namely adding caustic soda for neutralization until the pH value is 7-9.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. All such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention.
Claims (5)
1. The system for producing the high-concentration naphthalene water reducing agent by the naphthalene excess method comprises a reaction kettle, conveying equipment and a condenser, and is characterized in that: the reaction kettle is communicated with the conveying equipment through a pipeline, the conveying device is communicated with the industrial naphthalene storage device, the condensation kettle and the solvent storage device through pipelines, the reaction kettle is communicated with the condenser through a pipeline, the condenser is communicated with the separator through a pipeline, the separator is communicated with the solvent storage device through a pipeline, and the separator is communicated with the water storage device through a pipeline.
2. The system for producing the high-concentration naphthalene water reducer by the naphthalene excess method according to claim 1, which is characterized in that: and a mixer is arranged on the pipeline between the reaction kettle and the conveying device, and the mixer is communicated with a sulfonating agent storage device through a pipeline.
3. The system for producing the high-concentration naphthalene water reducer by the naphthalene excess method according to claim 1, which is characterized in that: the reaction kettle adopts a reaction kettle with a stirring shaft.
4. A production method for producing a high-concentration naphthalene water reducer by a naphthalene excess method is characterized by comprising the following steps:
s1, feeding, namely adding accurately-metered liquid naphthalene into a reaction kettle, and opening steam to increase the temperature;
s2, sulfonating, namely slowly adding metered sulfuric acid at a constant speed when the temperature of naphthalene is 140-145 ℃, adding acid for 55-65 min, continuously adding steam for heating, keeping the temperature when the temperature is 160 ℃, controlling the temperature to be 160-165 ℃, keeping the temperature for 2.5 hours, and keeping the temperature above 160 ℃ when the temperature is finished;
s3, removing naphthalene, opening a steam inlet and outlet valve, filling steam into the reaction kettle, adjusting feeding according to the condensation temperature, enabling a large amount of acid water to flow out of the separator and a large amount of liquid naphthalene to flow out of the separator, stopping filling steam when the naphthalene amount reaches a designed value, taking 5-10 hours, and sampling to measure the acidity to be 20-25%;
s4, distributing materials, opening heat-preservation steam of a feeding pipeline, melting the materials in the pipeline, opening a feeding valve of the condensation kettle, closing all other valves, and feeding through a feeding pump;
s5, condensing, namely adding metered formaldehyde in a trickle mode, adding the formaldehyde for 2-3 hours, observing the temperature, keeping the temperature within 100 ℃, stopping adding the formaldehyde when the temperature exceeds 100 ℃, continuing adding the formaldehyde after the temperature is reduced to 95-100 ℃, raising the temperature to 105-115 ℃ after adding the formaldehyde, keeping the temperature of the tail gas at the upper part not more than 60 ℃, condensing for 6-8 hours, stopping condensing when the net current rise value reaches 10-12A, immediately adding 200 liters of wastewater, and continuing stirring for 1-2 hours;
and S6, neutralizing, namely adding caustic soda for neutralization until the pH value is 7-9.
5. The production method for producing the high-concentration naphthalene water reducer by the naphthalene excess method according to claim 4 is characterized in that: the concentration of the sulfuric acid added in the S2 is 92-105%.
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CN202010253668.2A CN111423551A (en) | 2020-04-01 | 2020-04-01 | System for producing high-concentration naphthalene water reducer by naphthalene excess method and production method thereof |
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CN202010253668.2A CN111423551A (en) | 2020-04-01 | 2020-04-01 | System for producing high-concentration naphthalene water reducer by naphthalene excess method and production method thereof |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102464464A (en) * | 2010-11-09 | 2012-05-23 | 浙江龙盛集团股份有限公司 | Preparation method of naphthalene series water reducer |
CN105236798A (en) * | 2014-12-26 | 2016-01-13 | 上虞吉龙化学建材有限公司 | Preparation method of naphthalene-series water reducing agent |
CN106082756A (en) * | 2016-06-24 | 2016-11-09 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production system of naphthalene water reducer |
CN106117481A (en) * | 2016-06-24 | 2016-11-16 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production method of naphthalene water reducer |
CN107573471A (en) * | 2017-08-31 | 2018-01-12 | 浙江吉盛化学建材有限公司 | A kind of production technology of FDN high efficiency water reducing agents |
-
2020
- 2020-04-01 CN CN202010253668.2A patent/CN111423551A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102464464A (en) * | 2010-11-09 | 2012-05-23 | 浙江龙盛集团股份有限公司 | Preparation method of naphthalene series water reducer |
CN105236798A (en) * | 2014-12-26 | 2016-01-13 | 上虞吉龙化学建材有限公司 | Preparation method of naphthalene-series water reducing agent |
CN106082756A (en) * | 2016-06-24 | 2016-11-09 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production system of naphthalene water reducer |
CN106117481A (en) * | 2016-06-24 | 2016-11-16 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the condensation of sulfonation separate mealing type to produce the production method of naphthalene water reducer |
CN107573471A (en) * | 2017-08-31 | 2018-01-12 | 浙江吉盛化学建材有限公司 | A kind of production technology of FDN high efficiency water reducing agents |
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