CN111004362A - Preparation method of naphthalene-based superplasticizer - Google Patents

Preparation method of naphthalene-based superplasticizer Download PDF

Info

Publication number
CN111004362A
CN111004362A CN201911398647.3A CN201911398647A CN111004362A CN 111004362 A CN111004362 A CN 111004362A CN 201911398647 A CN201911398647 A CN 201911398647A CN 111004362 A CN111004362 A CN 111004362A
Authority
CN
China
Prior art keywords
naphthalene
preparation
reaction
based superplasticizer
hours
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.)
Granted
Application number
CN201911398647.3A
Other languages
Chinese (zh)
Other versions
CN111004362B (en
Inventor
陈铁海
吴文明
马永腾
张慢
董小丽
寇明泽
白永昇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gansu Academy Of Civil Engineering Sciences Co Ltd
Original Assignee
Gansu Academy Of Civil Engineering Sciences Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Gansu Academy Of Civil Engineering Sciences Co Ltd filed Critical Gansu Academy Of Civil Engineering Sciences Co Ltd
Priority to CN201911398647.3A priority Critical patent/CN111004362B/en
Publication of CN111004362A publication Critical patent/CN111004362A/en
Application granted granted Critical
Publication of CN111004362B publication Critical patent/CN111004362B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G16/00Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
    • C08G16/02Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
    • C08G16/0212Condensation 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
    • C08G16/0218Condensation 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
    • C08G16/0237Condensation 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16Sulfur-containing compounds
    • C04B24/20Sulfonated aromatic compounds
    • C04B24/22Condensation or polymerisation products thereof
    • C04B24/226Sulfonated naphtalene-formaldehyde condensation products
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G16/00Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
    • C08G16/02Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
    • C08G16/04Chemically modified polycondensates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention relates to the field of water reducing agents, and discloses a preparation method of a naphthalene-based superplasticizer, which is characterized in that washing oil, concentrated sulfuric acid, formaldehyde, sodium lignosulphonate and other raw materials are adopted to prepare the naphthalene-based superplasticizer; in the sulfonation reaction process, washing oil is added to replace part of industrial naphthalene, so that the sulfonation reaction time is reduced, and the production efficiency is improved; the sodium lignosulfonate solution is added in the neutralization reaction process, so that sodium lignosulfonate also fully participates in the neutralization reaction, the yield of finished products is improved, and the production cost is saved. The invention solves the problems of long time consumption, low production efficiency and high production cost in the production and preparation process of the existing naphthalene-based superplasticizer.

Description

Preparation method of naphthalene-based superplasticizer
Technical Field
The invention relates to the field of water reducing agents, in particular to a preparation method of a naphthalene-based high-efficiency water reducing agent
Background
The water reducing agent is a concrete admixture capable of reducing the water consumption for mixing under the condition of maintaining the slump constant of concrete basically. Most of them are anionic surfactants, such as lignosulfonate and naphthalene sulfonate formaldehyde polymer. After the concrete mixture is added, the dispersion effect on cement particles is achieved, the workability of the concrete mixture can be improved, the unit water consumption is reduced, and the fluidity of the concrete mixture is improved; or the unit cement consumption is reduced, and the cement is saved. Wherein the naphthalene-based high-efficiency water reducing agent is a non-air-entraining high-efficiency water reducing agent synthesized by chemical engineering. The chemical name is naphthalene sulfonate formaldehyde condensate which has strong dispersion effect on cement particles.
The conventional naphthalene-based superplasticizer on the market generally undergoes four chemical reaction processes, namely sulfonation reaction, hydrolysis reaction, condensation reaction and neutralization reaction, wherein the time required by each chemical reaction is approximately as follows: sulfonation reaction for more than 2.5 hours, hydrolysis reaction for 1.0 hour, condensation reaction for 3.0 hours, and neutralization reaction for more than 4.5 hours. Therefore, the whole process flow needs more than 11 hours, the cost of producing the naphthalene based superplasticizer mother liquor with the solid content of 40 percent is calculated to be about 1200 yuan per ton, and the cost mainly comprises material cost, labor cost, mechanical loss cost, fuel gas cost and the like.
Therefore, the problems of long time consumption and low production efficiency exist in the preparation process of the conventional naphthalene-based superplasticizer, more fuel gas is used, more labor is consumed, the mechanical loss is increased, and the like in the preparation process, so that the problem of high production cost is caused.
Disclosure of Invention
Based on the technical problems, the invention provides a preparation method of a naphthalene based superplasticizer, which solves the problems of long time consumption, low production efficiency and high production cost in the production and preparation process of the existing naphthalene based superplasticizer.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a naphthalene-based superplasticizer comprises the following steps:
the method comprises the following steps: dissolving naphthalene, namely putting industrial naphthalene and washing oil into a naphthalene dissolving device, heating to 130-140 ℃, and keeping the temperature to ensure that the industrial naphthalene is dissolved and fully mixed with the washing oil, wherein the mass ratio of the industrial naphthalene to the washing oil is 1: 0.25-0.67;
step two: sulfonation, transferring the mixed liquid of the industrial naphthalene and the wash oil obtained in the step one to a sulfonation device, heating to 165 ℃, keeping the temperature, then dropwise adding concentrated sulfuric acid with the concentration of 98%, and continuously stirring, wherein the dropwise adding duration of the concentrated sulfuric acid is 0.5-1 hour, and after dropwise adding of the concentrated sulfuric acid, performing sulfonation reaction for 1.5-2.5 hours to obtain a naphthalene sulfonic acid solution, wherein the mass ratio of the mixed liquid of the industrial naphthalene and the wash oil to the concentrated sulfuric acid is 1: 1.4;
step three: hydrolyzing, namely transferring the naphthalenesulfonic acid solution obtained in the step two into a hydrolysis device, cooling to 105 ℃, keeping the temperature, adding water, continuously stirring, adding water, stirring for 0.5 hour, performing hydrolysis reaction for 1 hour, and fully hydrolyzing until the acidity is 28-30%;
step four: condensing, namely transferring the naphthalenesulfonic acid solution hydrolyzed in the step three into a condensing device, cooling to 88 ℃, keeping the temperature, dropwise adding a formaldehyde solution with the concentration of 37%, and then carrying out condensation reaction for 3 hours to obtain a naphthalenesulfonic acid-formaldehyde condensate, wherein the mass ratio of the naphthalenesulfonic acid solution to the formaldehyde is 1: 1;
step five: neutralizing, namely transferring the naphthalenesulfonic acid formaldehyde condensate obtained in the fourth step into a neutralization device, cooling to 60 ℃, preserving heat, simultaneously adding sodium lignosulfonate solution with the solid content of 30-40% and liquid caustic soda with the concentration of 35% into the neutralization device, then carrying out neutralization reaction for 3.5-4.5 hours, and adjusting the pH value to 6.5-7.5 to obtain a naphthalene water reducer mother liquor;
step six: and D, further drying the naphthalene water reducer mother liquor obtained in the fifth step to obtain a finished product of the solid naphthalene water reducer.
As a preferred mode, the mass ratio of the industrial naphthalene to the wash oil in the first step is 7: 3.
In a preferred embodiment, the sulfonation reaction time in step two is 2 hours.
In a preferred mode, the solid content of the sodium lignosulfonate solution in the fifth step is 40%.
As a preferred mode, the neutralization reaction time in the fifth step is 3.5 hours.
And as a preferable mode, the drying treatment mode in the sixth step is spray drying, wherein the spray drying is to pass the naphthalene water reducer mother liquor through a centrifugal spray dryer, the air inlet temperature of the centrifugal spray dryer is 350-400 ℃, the air outlet temperature of the centrifugal spray dryer is 90-100 ℃, and the naphthalene water reducer powder is obtained after atomization, drying and sedimentation.
As a preferable mode, the naphthalene dissolving device, the sulfonating device, the hydrolyzing device, the condensing device and the neutralizing device are all reaction kettles, and the temperature of the reaction kettles is controlled by a steam heating mode.
Compared with the prior art, the invention has the beneficial effects that:
(1) on the premise of ensuring the quality, the invention adjusts the process and the formula of the sulfonation reaction stage and the neutralization reaction stage in the preparation method of the naphthalene-based superplasticizer, so that the product cost is reduced to about 900 from 1200 of original 40 percent solid content naphthalene-based superplasticizer mother liquor per ton under the condition of unchanged quality, the reduction ratio is close to 26 percent, the product cost is greatly reduced, and the market competitiveness of the product is improved.
(2) The invention replaces partial industrial naphthalene with the washing oil, and changes the raw material of the sulfonation reaction from pure industrial naphthalene into the mixture of the industrial naphthalene and the washing oil. The property of the washing oil is more active compared with that of industrial naphthalene, and the time required for sulfonation reaction is shorter, so that the sulfonation reaction time can be shortened, the sulfonation reaction time is reduced from 2.5 hours to 2 hours, and the production efficiency is improved. Meanwhile, the washing oil is used for replacing part of industrial naphthalene, and the price of the washing oil is lower than that of the industrial naphthalene, so that the raw material cost of production is reduced.
(3) The invention adds sodium lignosulfonate solution in the neutralization reaction stage, so that sodium lignosulfonate also fully participates in the neutralization reaction, the yield of finished products is improved, and the production cost is saved. And the sodium lignosulfonate solution, the condensation product and the liquid alkali react, the neutralization reaction time is shortened, and the neutralization reaction time is reduced from 4.5 hours to 3.5 hours, so that the production efficiency is improved.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions of the embodiments of the present disclosure will be described clearly and completely with reference to the drawings of the embodiments of the present disclosure. It is to be understood that the described embodiments are only a few embodiments of the present disclosure, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the disclosure without any inventive step, are within the scope of protection of the disclosure.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of "first," "second," and similar terms in this disclosure is not intended to indicate any order, quantity, or importance, but rather is used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
A preparation method of a naphthalene-based superplasticizer comprises the following steps:
the method comprises the following steps: dissolving naphthalene, namely putting industrial naphthalene and washing oil into a naphthalene dissolving device, heating to 130-140 ℃, and keeping the temperature to ensure that the industrial naphthalene is dissolved and fully mixed with the washing oil, wherein the mass ratio of the industrial naphthalene to the washing oil is 1: 0.25-0.67;
step two: sulfonation, transferring the mixed liquid of the industrial naphthalene and the wash oil obtained in the step one to a sulfonation device, heating to 165 ℃, keeping the temperature, then dropwise adding concentrated sulfuric acid with the concentration of 98%, and continuously stirring, wherein the dropwise adding duration of the concentrated sulfuric acid is 0.5-1 hour, and after dropwise adding of the concentrated sulfuric acid, performing sulfonation reaction for 1.5-2.5 hours to obtain a naphthalene sulfonic acid solution, wherein the mass ratio of the mixed liquid of the industrial naphthalene and the wash oil to the concentrated sulfuric acid is 1: 1.4;
step three: hydrolyzing, namely transferring the naphthalenesulfonic acid solution obtained in the step two into a hydrolysis device, cooling to 105 ℃, keeping the temperature, adding water, continuously stirring, adding water, stirring for 0.5 hour, performing hydrolysis reaction for 1 hour, and fully hydrolyzing until the acidity is 28-30%;
step four: condensing, namely transferring the naphthalenesulfonic acid solution hydrolyzed in the step three into a condensing device, cooling to 88 ℃, keeping the temperature, dropwise adding a formaldehyde solution with the concentration of 37%, and then carrying out condensation reaction for 3 hours to obtain a naphthalenesulfonic acid-formaldehyde condensate, wherein the mass ratio of the naphthalenesulfonic acid solution to the formaldehyde is 1: 1;
step five: neutralizing, namely transferring the naphthalenesulfonic acid formaldehyde condensate obtained in the fourth step into a neutralization device, cooling to 60 ℃, preserving heat, simultaneously adding sodium lignosulfonate solution with the solid content of 30-40% and liquid caustic soda with the concentration of 35% into the neutralization device, then carrying out neutralization reaction for 3.5-4.5 hours, and adjusting the pH value to 6.5-7.5 to obtain a naphthalene water reducer mother liquor;
step six: and D, further drying the naphthalene water reducer mother liquor obtained in the fifth step to obtain a finished product of the solid naphthalene water reducer.
In the preparation method, the product produced by using the material with high naphthalene content has small air-entraining property and better performance of the naphthalene water reducer, so 95 percent of industrial naphthalene or refined naphthalene is mostly used in the current water reducer production plants to be beneficial to the stable quality of the product.
The sulfuric acid used for sulfonation is usually concentrated sulfuric acid with the concentration of 98 percent, the sulfonation reaction is electrophilic reaction, and the reaction is not anionic SO and HSO but cationic H3SOAnd neutral molecule SO3The sulfonation reaction is that concentrated sulfuric acid acts on naphthalene, and a sulfonic acid group replaces hydrogen atoms of the naphthalene, so that naphthalene sulfonic acid is generated as a reaction result, the quality of the sulfonation reaction is controlled, the β -naphthalene sulfonic acid content is directly influenced, and the quality of the product after condensation is greatly influenced.
In the process of sulfonation reaction, when β -naphthalenesulfonic acid is produced, part of α -naphthalenesulfonic acid is also generated, in order to hydrolyze α -naphthalenesulfonic acid and facilitate the subsequent polycondensation, α -naphthalenesulfonic acid should be hydrolyzed, the reactant is cooled to about 120 ℃ during the hydrolysis reaction, water is added, at this time, β -naphthalenesulfonic acid is stable, α -naphthalenesulfonic acid is easy to hydrolyze, the product after α -naphthalenesulfonic acid hydrolysis is naphthalene and sulfuric acid, and the separated product can be used as a raw material to continuously participate in sulfonation reaction.
After the hydrolysis reaction is finished, formaldehyde is dripped into the condensation device, and the formaldehyde reacts with β -naphthalenesulfonic acid to generate a naphthalenesulfonic acid-formaldehyde condensation compound, in the condensation process, materials become thick, so that the materials are solidified in the condensation device, therefore, the acidity of the materials after the hydrolysis reaction is kept at 28-30% and cannot be too high, the formaldehyde cannot be excessive, the formaldehyde addition speed cannot be too high, and the formaldehyde must be dripped slowly.
And transferring the material after the condensation reaction into a neutralization device, adding the sodium lignosulfonate solution and the liquid alkali with solid contents into the neutralization device simultaneously to neutralize the sulfuric acid excessive in the sulfonation reaction, and obtaining the naphthalene water reducer mother liquor when the pH value is stabilized at 6.5-7.5.
And finally, further drying the naphthalene water reducer mother liquor to obtain a finished product of the solid naphthalene water reducer. The drying treatment mode can adopt spray drying, wherein the spray drying is to pass the naphthalene water reducer mother liquor through a centrifugal spray dryer, the air inlet temperature of the centrifugal spray dryer is 350-400 ℃, the air outlet temperature is 90-100 ℃, and the naphthalene water reducer powder is obtained after atomization, drying and sedimentation. The spray drying speed is high. After the feed liquid is centrifugally sprayed, the surface area is greatly increased, 95-98% of water can be instantly evaporated in high-temperature airflow, and the drying time is only a few seconds. And the solution and the emulsion can be directly dried into powder or granular products, and the working procedures of evaporation, crushing and the like can be omitted.
And the naphthalene dissolving device, the sulfonating device, the hydrolyzing device, the condensing device and the neutralizing device in the reaction are all reaction kettles, and the temperature of the reaction kettles is controlled by a steam heating mode.
Examples 1 to 9:
the difference of the preparation method of the naphthalene-based superplasticizer is that different mass ratios of industrial naphthalene to wash oil and different sulfonation reaction times are adopted in the sulfonation reaction stage.
TABLE 1 analysis of results of examples 1 to 9
Figure BDA0002345060540000051
The water reducing rate parameters of the naphthalene water reducing agent prepared in the embodiment 1-9 are shown in table 1, the water reducing rate of the high-efficiency water reducing agent is qualified when the water reducing rate is more than 14%, the raw material cost of different mass ratios of industrial naphthalene to wash oil and the power consumption cost of different sulfonation reaction time are integrated, and when the mass ratio of the industrial naphthalene to the wash oil is 7: 3 and the sulfonation reaction duration is 2 hours, the cost performance is highest.
Examples 10 to 16:
the preparation method of the naphthalene-based high-efficiency water reducing agent is characterized in that sodium lignosulfonate with different solid contents and different neutralization reaction times are adopted in the neutralization reaction stage.
TABLE 2 analysis tables of results of examples 10 to 16
Figure BDA0002345060540000052
Figure BDA0002345060540000061
The water reducing rate parameters of the naphthalene water reducing agent prepared in the embodiment 10-16 are shown in table 2, the water reducing rate of the high-efficiency water reducing agent is qualified when the water reducing rate is more than 14%, the raw material cost of sodium lignosulfonate with different solid contents and the power consumption cost of different neutralization reaction times are integrated, and when the solid content of the sodium lignosulfonate is 40% and the neutralization reaction duration is 3.5 hours, the cost performance is highest.
By integrating the above embodiments, when the mass ratio of the industrial naphthalene to the wash oil is 7: 3, the duration of the sulfonation reaction is 2 hours, the solid content of the sodium lignosulfonate is 40%, and the duration of the neutralization reaction is 3.5 hours, the cost performance of the whole preparation method is highest, at this time, the cost of the naphthalene series water reducer mother liquor with 40% of solid content per ton is reduced from 1200 to about 900, and the reduction ratio is close to 26%. The total time of the whole process flow is reduced from about 11 hours to about 9.5 hours, and the power consumption cost of the equipment is reduced.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only used for clearly illustrating the verification process of the invention and are not used for limiting the patent protection scope of the invention, which is defined by the claims, and all the equivalent structural changes made by using the contents of the description and the drawings of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The preparation method of the naphthalene-based superplasticizer is characterized by comprising the following steps:
the method comprises the following steps: dissolving naphthalene, namely putting industrial naphthalene and washing oil into a naphthalene dissolving device, heating to 130-140 ℃, and keeping the temperature to ensure that the industrial naphthalene is dissolved and fully mixed with the washing oil, wherein the mass ratio of the industrial naphthalene to the washing oil is 1: 0.25-0.67;
step two: sulfonation, transferring the mixed liquid of the industrial naphthalene and the wash oil obtained in the step one to a sulfonation device, heating to 165 ℃, keeping the temperature, then dropwise adding concentrated sulfuric acid with the concentration of 98%, and continuously stirring, wherein the dropwise adding duration of the concentrated sulfuric acid is 0.5-1 hour, and after dropwise adding of the concentrated sulfuric acid, performing sulfonation reaction for 1.5-2.5 hours to obtain a naphthalene sulfonic acid solution, wherein the mass ratio of the mixed liquid of the industrial naphthalene and the wash oil to the concentrated sulfuric acid is 1: 1.4;
step three: hydrolyzing, namely transferring the naphthalenesulfonic acid solution obtained in the step two into a hydrolysis device, cooling to 105 ℃, keeping the temperature, adding water, continuously stirring, adding water, stirring for 0.5 hour, performing hydrolysis reaction for 1 hour, and fully hydrolyzing until the acidity is 28-30%;
step four: condensing, namely transferring the naphthalenesulfonic acid solution hydrolyzed in the step three into a condensing device, cooling to 88 ℃, keeping the temperature, dropwise adding a formaldehyde solution with the concentration of 37%, and then carrying out condensation reaction for 3 hours to obtain a naphthalenesulfonic acid-formaldehyde condensate, wherein the mass ratio of the naphthalenesulfonic acid solution to the formaldehyde is 1: 1;
step five: neutralizing, namely transferring the naphthalenesulfonic acid formaldehyde condensate obtained in the fourth step into a neutralization device, cooling to 60 ℃, preserving heat, simultaneously adding sodium lignosulfonate solution with the solid content of 30-40% and liquid caustic soda with the concentration of 35% into the neutralization device, then carrying out neutralization reaction for 3.5-4.5 hours, and adjusting the pH value to 6.5-7.5 to obtain a naphthalene water reducer mother liquor;
step six: and D, further drying the naphthalene water reducer mother liquor obtained in the fifth step to obtain a finished product of the solid naphthalene water reducer.
2. The preparation method of the naphthalene based superplasticizer according to claim 1, characterized by comprising the following steps: the mass ratio of the industrial naphthalene to the wash oil in the first step is 7: 3.
3. The preparation method of the naphthalene based superplasticizer according to claim 2, characterized by comprising the following steps: and in the second step, the sulfonation reaction time is 2 hours.
4. The preparation method of the naphthalene based superplasticizer according to claim 1, characterized by comprising the following steps: and in the fifth step, the solid content of the sodium lignosulfonate solution is 40%.
5. The preparation method of the naphthalene based superplasticizer according to claim 4, characterized by comprising the following steps: and the neutralization reaction time in the step five is 3.5 hours.
6. The preparation method of the naphthalene based superplasticizer according to claim 1, characterized by comprising the following steps: and the drying treatment mode in the sixth step is spray drying, wherein the spray drying is to pass the naphthalene water reducer mother liquor through a centrifugal spray dryer, the air inlet temperature of the centrifugal spray dryer is 350-400 ℃, the air outlet temperature of the centrifugal spray dryer is 90-100 ℃, and the naphthalene water reducer powder is obtained after atomization, drying and sedimentation.
7. The preparation method of the naphthalene based superplasticizer according to claim 1, characterized by comprising the following steps: the naphthalene dissolving device, the sulfonating device, the hydrolyzing device, the condensing device and the neutralizing device are all reaction kettles, and the temperature of the reaction kettles is controlled in a steam heating mode.
CN201911398647.3A 2019-12-30 2019-12-30 Preparation method of naphthalene-based superplasticizer Active CN111004362B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911398647.3A CN111004362B (en) 2019-12-30 2019-12-30 Preparation method of naphthalene-based superplasticizer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911398647.3A CN111004362B (en) 2019-12-30 2019-12-30 Preparation method of naphthalene-based superplasticizer

Publications (2)

Publication Number Publication Date
CN111004362A true CN111004362A (en) 2020-04-14
CN111004362B CN111004362B (en) 2022-09-02

Family

ID=70119465

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911398647.3A Active CN111004362B (en) 2019-12-30 2019-12-30 Preparation method of naphthalene-based superplasticizer

Country Status (1)

Country Link
CN (1) CN111004362B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105514A (en) * 2021-12-24 2022-03-01 莱芜市兆信新材料股份有限公司 Preparation method of naphthalene water reducer for middle east high-heat area

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0578157A (en) * 1991-09-24 1993-03-30 Kao Corp Method for producing cement dispersant
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
CN109369059A (en) * 2018-12-06 2019-02-22 山东万山化工有限公司 A kind of synthetic method of the naphthalene water reducer based on 2,6- naphthalenedisulfonic acid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0578157A (en) * 1991-09-24 1993-03-30 Kao Corp Method for producing cement dispersant
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
CN109369059A (en) * 2018-12-06 2019-02-22 山东万山化工有限公司 A kind of synthetic method of the naphthalene water reducer based on 2,6- naphthalenedisulfonic acid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105514A (en) * 2021-12-24 2022-03-01 莱芜市兆信新材料股份有限公司 Preparation method of naphthalene water reducer for middle east high-heat area

Also Published As

Publication number Publication date
CN111004362B (en) 2022-09-02

Similar Documents

Publication Publication Date Title
CN114315202B (en) Protein gypsum retarder and preparation method thereof
CN106117482B (en) A kind of modified high-thin arch dam naphthalene water reducer and preparation method thereof
CN105236798B (en) A kind of preparation method of naphthalene water reducer
CN102464464B (en) Preparation method of naphthalene series water reducer
CN101474543B (en) Method for preparing composite dispersing agent
CN106517849A (en) Oxidation-sulfonation starch water reducing agent preparation method
CN111004362B (en) Preparation method of naphthalene-based superplasticizer
CN104403349B (en) A kind of industrialized preparing process of pigment yellow 97
CN106810412B (en) Method for improving sulfonation reaction efficiency and production method of dispersing agent MF
CN1800075A (en) Simplified method for preparing low alkaline naphthalene series concrete water reducing agent
CN104628605B (en) A kind of naphthalene continuous catalysis method of sulfonating and device thereof
CN106632938B (en) A kind of energy saving preparation method and its special equipment of naphthalene water reducer
CN101182301B (en) Method for preparing 2-amido-8-naphthol-6-sulfonic acid
CN111909061B (en) Production process of 2-amino-3, 6, 8-naphthalene trisulfonic acid
CN103011665A (en) Aliphat water reducer and naphthalene water reducer chemical compound process
CN109534712B (en) Light yellow naphthalene water reducing agent and preparation method thereof
CN108003070B (en) Sulfonation method in H acid production
CN103739449B (en) A kind of preparation method of 1,5-dihydroxy naphthlene
CN109705610A (en) A kind of directly preparation method of blended light yellow D-GL
CN105293973A (en) Naphthalene type efficient water reducing agent and preparation method thereof
CN109705609A (en) A kind of industrialized preparing process of the low aniline value paratonere 57:1 of mother liquid coming
CN102177777B (en) Delinting penetrant for cotton-seed processing
CN111470793B (en) High-dispersity high-quality naphthalene-based high-efficiency water reducing agent and preparation method thereof
CN101676274A (en) Method for preparing N-tertiary butyl benzothiazole sulfonamide
CN101723616A (en) Method for preparing concrete water reducing agent

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant