CN110790879A - Production process of water reducing agent - Google Patents

Production process of water reducing agent Download PDF

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Publication number
CN110790879A
CN110790879A CN201910951462.4A CN201910951462A CN110790879A CN 110790879 A CN110790879 A CN 110790879A CN 201910951462 A CN201910951462 A CN 201910951462A CN 110790879 A CN110790879 A CN 110790879A
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kettle
water
neutralization
materials
reaction
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邵玉田
常程
潘湫泽
徐国鹏
邱宇飞
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Anhui Source Of Students Chemical Co Ltd
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    • 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
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/04Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
    • C07C303/06Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/22Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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    • 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
    • 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

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the technical field of water reducing agents and discloses a production process of a water reducing agent, which comprises the following steps of sulfonating, injecting 70L of methylnaphthalene in a methylnaphthalene absorption system into a 6300L sulfonation kettle by a pump, supplementing fresh methylnaphthalene to the methylnaphthalene absorption system after the injection is finished, conveying 93 ℃ liquid naphthalene from a liquid naphthalene raw material tank to a workshop metering tank by the pump, and injecting the liquid naphthalene into a 6300L enamel sulfonation kettle after the quantity is confirmed. This production technology of water-reducing agent, send to the formaldehyde metering tank from the head tank through with the pump for the formaldehyde solution, then control the velocity of flow and slowly pour into the condensation reaction cauldron into, carry out condensation reaction, the reaction finishes, pour into workshop recovery system water or industrial water into, dilute the material, then the autonomous flow to the neutralization kettle, the product outside the water-reducing agent of producing has obtained abundant utilization, the pollution produces less and the conversion ratio of raw and other materials is high, corresponding water-reducing agent manufacturing cost reduces, user's vexation has been removed from, user's use has been made things convenient for.

Description

Production process of water reducing agent
Technical Field
The invention relates to the technical field of water reducing agents, in particular to a production process of a water reducing agent.
Background
The water reducing agent is a concrete admixture capable of reducing the mixing water consumption under the condition of maintaining the slump constant of concrete, most of the water reducing agent belongs to anionic surfactants, and comprises lignosulfonate, naphthalene sulfonate formaldehyde polymer and the like, and the water reducing agent has a dispersing effect on cement particles after being added into a concrete mixture, can improve the workability of the concrete mixture, reduces the unit water consumption, improves the fluidity of the concrete mixture, or reduces the unit cement consumption, and saves cement.
The traditional water reducer production process has complicated steps and large waste of used materials, the raw materials are not completely utilized, the production cost is greatly increased while a large amount of pollutants are generated, and the cost of the water reducer is increased, so that the production process of the water reducer is provided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a production process of a water reducing agent, which has the advantages of low production cost and the like, and solves the problems that the traditional water reducing agent production process has complicated steps, large waste of used materials, incomplete utilization of raw materials, production cost greatly increased while a large amount of pollutants are generated, and the cost of the water reducing agent is increased.
(II) technical scheme
In order to achieve the aim of low production cost, the invention provides the following technical scheme: a production process of a water reducing agent comprises the following steps:
1) sulfonating, namely injecting 70L of methylnaphthalene in a 6300L sulfonating kettle by using a pump, supplementing fresh methylnaphthalene to the methylnaphthalene absorption system after the injection is finished, conveying 93 ℃ liquid naphthalene from a liquid naphthalene raw material tank to a workshop metering tank by using the pump, after the quantity is confirmed, injecting the liquid naphthalene into a 6300L enamel sulfonating kettle, heating the reaction kettle to 120 ℃ through a jacket oil temperature, stopping heating, then slowly injecting 98% sulfuric acid, adjusting the flow rate along with the change of the internal temperature of the reaction kettle, controlling the internal temperature of the reaction kettle to be within 150 ℃, after the addition of the sulfuric acid is finished, slowly raising the internal temperature of the reaction kettle to 160-165 ℃, reacting for 2h, raising the temperature to 160-165 ℃ so as to convert α -naphthalenesulfonic acid which is reacted in advance into β -naphthalenesulfonic acid as far as possible, wherein α -naphthalenesulfonic acid is about 15% and β -naphthalenesulfonic acid is about 85% in the material after the sulfonation is finished, emptying the naphthalene metering tank of the sulfonating part and the sulfonating reaction kettle firstly absorb sublimated naphthalene through the methylnaphthalene absorption system, and then spraying the tail gas to recover alkali liquid naphthalene;
the above process is represented by the following reaction formula:
2) hydrolysis, namely opening a bottom valve of the reaction kettle, automatically injecting the sulfonated material into a 12000L condensation reaction kettle, cooling the material to 120 ℃ by jacket cooling water, then adding 1230L hydrolysis water, and forcibly cooling the material to the temperature of 90-95 ℃ after 0.5h of hydrolysis, wherein the hydrolysis aims at reducing α -naphthalenesulfonic acid which is not beneficial to the product quality into acid and naphthalene;
the above process is represented by the following reaction formula:
Figure BDA0002225887680000022
3) conveying the formaldehyde solution from a raw material tank to a formaldehyde metering tank by a pump, then slowly injecting the formaldehyde solution into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, injecting the formaldehyde solution into workshop recovery system water or industrial water to dilute the materials, and then automatically flowing the materials to a neutralization kettle;
the above process is represented by the following reaction formula:
4) after the neutralization kettle receives the condensed material, controlling the flow and adding 32 percent of liquid caustic soda for neutralization, after the PH meets the requirement, finishing the neutralization, and feeding the kettle material into a post-treatment working section;
the above process is represented by the following reaction formula:
5) and (3) post-treatment, namely after neutralization is finished, directly selling a part of the kettle materials as products, adding sodium sulfate into a part of the kettle materials for compounding to be sold as products, adding sodium chloride into a part of the kettle materials for compounding to be sold as products, adding calcium oxide into a part of the kettle materials for removing part of sulfate radical ions, then carrying out filter pressing, selling the filtrate as the products, selling the filter residues as calcium sulfate serving as a byproduct, and reducing the water content of the rest of the kettle materials of the neutralization kettle by spray drying to be sold as the products.
Preferably, after the hydrolysis and sulfonation in the step 2 are finished, opening a bottom valve of the reaction kettle, automatically injecting the sulfonated material into a 12000L condensation reaction kettle, cooling the material to 120 ℃ by jacket cooling water, then adding 1230L water for hydrolysis, carrying out hydrolysis for 0.5h, then forcibly cooling to the temperature in the kettle to 90-95 ℃, and discharging tail gas during hydrolysis to absorb sublimed naphthalene and acid mist through a methyl tea naphthalene absorption system and a liquid alkali water spraying system in a workshop.
Preferably, in the condensation in step 3, the formaldehyde solution is sent to a formaldehyde metering tank from a raw material tank by a pump, then the formaldehyde solution is slowly injected into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, the formaldehyde solution is injected into workshop recovery system water or industrial water to dilute the materials, then the diluted materials automatically flow into a neutralization kettle, the temperature of the condensation kettle is controlled within 100 ℃ in the formaldehyde injection process, if the condensation temperature exceeds 100 ℃, the formaldehyde flow is adjusted, after the formaldehyde injection is finished, the condensation temperature is slowly increased to 103-105 ℃, the temperature is stopped to perform the condensation reaction, the pressure of the reaction kettle is controlled at 0.03Mp α, the temperature is 105-110 ℃, and the reaction lasts for 4-5 hours.
Preferably, after the neutralization kettle in the step 4 receives the condensation material, 32% liquid caustic soda is added in the neutralization kettle in a controlled flow manner for neutralization, after the PH meets the requirement, the neutralization is finished, the kettle material enters a post-treatment working section, cooling water is added in the neutralization kettle in a jacket manner while the neutralization kettle is neutralized, and the temperature of the neutralization kettle is controlled.
Preferably, after the post-treatment in step 5, after neutralization, part of the kettle material is directly sold as a product, part of the kettle material is added with sodium sulfate for compounding and then sold as a product, part of the kettle material is added with sodium chloride for compounding and then sold as a product, part of the kettle material is added with calcium oxide for removing part of sulfate ions, then, filter pressing is carried out, filtrate is sold as a product, filter residue is calcium sulfate and sold as a byproduct, the rest of the kettle material in the neutralization kettle is sold as a product after the moisture content is reduced by spray drying, and dust generated in the drying process is subjected to secondary cyclone dust removal and water film dust removal treatment.
(III) advantageous effects
Compared with the prior art, the invention provides a production process of a water reducing agent, which has the following beneficial effects:
1. the production process of the water reducing agent comprises the steps of conveying a formaldehyde solution to a formaldehyde metering tank from a raw material tank by a pump, controlling the flow rate, slowly injecting the formaldehyde solution into a condensation reaction kettle, carrying out condensation reaction, injecting the formaldehyde solution into a workshop for recovering system water or industrial water, diluting the materials, automatically flowing the diluted materials into a neutralization kettle, controlling the flow rate, adding 32% liquid caustic soda into the neutralization kettle for neutralization after receiving the condensation materials, after the pH value meets the requirement, directly selling a part of kettle materials as a product after the neutralization is finished, selling a part of the kettle materials as a product after adding sodium sulfate for compounding, selling a part of the product after adding sodium chloride for compounding, removing a part of sulfate ions by adding calcium oxide, carrying out filter pressing, selling a filtrate as a product, selling filter residues as calcium sulfate as a byproduct, reducing the moisture content of the rest of the kettle materials by spray drying, and selling the rest of the water reducing agent as a product, wherein the produced water reducing agent product is fully, the pollution is less, the conversion ratio of raw materials is high, the production cost of the corresponding water reducing agent is reduced, the trouble of a user is avoided, and the use of the user is facilitated.
2. The production process of the water reducer comprises the steps of sulfonating, injecting 70L of methylnaphthalene in a methylnaphthalene absorption system into a 6300L sulfonating kettle by a pump, supplementing fresh methylnaphthalene to the methylnaphthalene absorption system after injection, conveying 93 ℃ liquid naphthalene from a liquid naphthalene raw material tank to a workshop metering tank by the pump, after quantity confirmation, injecting into a 6300L enamel sulfonating kettle, raising the temperature of the reaction kettle to 120 ℃ by a jacket oil temperature, stopping temperature rise, then slowly injecting 98% sulfuric acid, regulating the flow rate along with the change of the internal temperature of the reaction kettle, controlling the internal temperature of the reaction kettle to be within 150 ℃, after the sulfuric acid is completely added, slowly raising the internal temperature of the reaction kettle to be 160-165 ℃ for 2h, raising the temperature to be 160-165 ℃ for the purpose of converting α -naphthalenesulfonic acid which is subjected to early reaction into β -naphthalenesulfonic acid as far as possible, allowing α -naphthalenesulfonic acid to be about 15% in the materials after sulfonation, allowing 3982-naphthalenesulfonic acid to be about 85%, allowing the naphthalene metering tank and the tail gas of the naphthalene absorption system and tail gas of the sulfonation reaction to enter a hydrolysis reaction kettle after sulfonation, after the tail gas is discharged, allowing the tail gas to enter a hydrolysis reaction kettle, after the hydrolysis reaction kettle is opened, forcibly cooling, injecting the hydrolysis reaction kettle, injecting the sulfonation kettle, injecting the naphthalene reaction kettle to be about 3995-naphthalene reaction kettle, injecting the hydrolysis reaction kettle, injecting the naphthalene reaction kettle.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A production process of a water reducing agent comprises the following steps:
1) sulfonating, namely injecting 70L of methylnaphthalene in a 6300L sulfonating kettle by using a pump, supplementing fresh methylnaphthalene to the methylnaphthalene absorption system after the injection is finished, conveying 93 ℃ liquid naphthalene from a liquid naphthalene raw material tank to a workshop metering tank by using the pump, after the quantity is confirmed, injecting the liquid naphthalene into a 6300L enamel sulfonating kettle, heating the reaction kettle to 120 ℃ through a jacket oil temperature, stopping heating, then slowly injecting 98% sulfuric acid, adjusting the flow rate along with the change of the internal temperature of the reaction kettle, controlling the internal temperature of the reaction kettle to be within 150 ℃, after the addition of the sulfuric acid is finished, slowly raising the internal temperature of the reaction kettle to 160-165 ℃, reacting for 2h, raising the temperature to 160-165 ℃ so as to convert α -naphthalenesulfonic acid which is reacted in advance into β -naphthalenesulfonic acid as far as possible, wherein α -naphthalenesulfonic acid is about 15% and β -naphthalenesulfonic acid is about 85% in the material after the sulfonation is finished, emptying the naphthalene metering tank of the sulfonating part and the sulfonating reaction kettle firstly absorb sublimated naphthalene through the methylnaphthalene absorption system, and then spraying the tail gas to recover alkali liquid naphthalene;
the above process is represented by the following reaction formula:
Figure BDA0002225887680000061
2) hydrolysis, namely opening a bottom valve of the reaction kettle, automatically injecting the sulfonated material into a 12000L condensation reaction kettle, cooling the material to 120 ℃ by jacket cooling water, then adding 1230L hydrolysis water, and forcibly cooling the material to the temperature of 90-95 ℃ after 0.5h of hydrolysis, wherein the hydrolysis aims at reducing α -naphthalenesulfonic acid which is not beneficial to the product quality into acid and naphthalene;
the above process is represented by the following reaction formula:
Figure BDA0002225887680000062
3) conveying the formaldehyde solution from a raw material tank to a formaldehyde metering tank by a pump, then slowly injecting the formaldehyde solution into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, injecting the formaldehyde solution into workshop recovery system water or industrial water to dilute the materials, and then automatically flowing the materials to a neutralization kettle;
the above process is represented by the following reaction formula:
Figure BDA0002225887680000063
4) after the neutralization kettle receives the condensed material, controlling the flow and adding 32 percent of liquid caustic soda for neutralization, after the PH meets the requirement, finishing the neutralization, and feeding the kettle material into a post-treatment working section;
the above process is represented by the following reaction formula:
Figure BDA0002225887680000071
5) and (3) post-treatment, namely after neutralization is finished, directly selling a part of the kettle materials as products, adding sodium sulfate into a part of the kettle materials for compounding to be sold as products, adding sodium chloride into a part of the kettle materials for compounding to be sold as products, adding calcium oxide into a part of the kettle materials for removing part of sulfate radical ions, then carrying out filter pressing, selling the filtrate as the products, selling the filter residues as calcium sulfate serving as a byproduct, and reducing the water content of the rest of the kettle materials of the neutralization kettle by spray drying to be sold as the products.
And 2, after hydrolysis and sulfonation are finished, opening a bottom valve of the reaction kettle, automatically injecting sulfonated materials into a 12000L condensation reaction kettle, cooling the materials to 120 ℃ by jacket cooling water, then adding 1230L hydrolysis water, carrying out hydrolysis for 0.5h, then carrying out forced cooling until the temperature in the kettle reaches 90-95 ℃, and discharging tail gas during hydrolysis to absorb sublimed naphthalene and acid mist by a methyl tea naphthalene absorption system and a liquid alkali water spraying system in a workshop.
And 3, condensing, namely conveying the formaldehyde solution from a raw material tank to a formaldehyde metering tank by using a pump, then slowly injecting the formaldehyde solution into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, injecting the formaldehyde solution into workshop recovery system water or industrial water to dilute the materials, then automatically flowing the materials into a neutralization kettle, controlling the temperature of the condensation kettle within 100 ℃ in the formaldehyde injection process, regulating the formaldehyde flow if the condensation temperature exceeds 100 ℃, after the formaldehyde injection is finished, slowly increasing the condensation temperature to 103-105 ℃, stopping heating, performing the condensation reaction, controlling the pressure of the reaction kettle at 0.03Mp α, controlling the temperature at 105-110 ℃, and reacting for 4-5 hours.
And 4, after the neutralization kettle receives the condensed materials, controlling the flow rate and adding 32% of liquid caustic soda for neutralization, after the PH meets the requirement, finishing the neutralization, enabling the kettle materials to enter a post-treatment working section, starting jacket cooling water of the neutralization kettle while neutralizing, and controlling the temperature of the neutralization kettle.
And 5, post-treatment, wherein after neutralization is finished, a part of the kettle material is directly sold as a product, a part of the kettle material is added with sodium sulfate for compounding and then sold as a product, a part of the kettle material is added with sodium chloride for compounding and then sold as a product, a part of the kettle material is added with calcium oxide for removing part of sulfate ions, then, filter pressing is carried out, filtrate is sold as a product, filter residue is calcium sulfate and sold as a byproduct, the rest of the kettle material in the neutralization kettle is subjected to spray drying for reducing the moisture content and then sold as a product, and dust generated in the drying process is subjected to secondary cyclone dust.
The production process of the water reducer has the advantages that formaldehyde solution is conveyed to a formaldehyde metering tank from a raw material tank by a pump, then the formaldehyde solution is slowly injected into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, the formaldehyde solution is injected into a workshop recovery system water or industrial water to dilute the materials, then the materials automatically flow to a neutralization kettle, after the neutralization kettle receives the condensation materials, 32% liquid alkali is added at a controlled flow rate to neutralize the materials, after the pH reaches the requirement, a part of kettle materials are directly sold as products, a part of kettle materials are sold as products after sodium sulfate is added for compounding, a part of products are sold as products after sodium chloride is added for compounding, a part of products are sold as calcium oxide to remove partial sulfate ions, then filter pressing is performed, filtrate is sold as products, filter residues are calcium sulfate and sold as byproducts, the rest neutralization kettle materials are sold as products after the moisture content is reduced by spray drying, the products are sold, the water reducer products other than the produced are fully utilized, the water reducer products are produced, the pollution is generated with a low production cost, the corresponding production cost is reduced, the oil temperature of the user occupies the trouble, the use of oil, the use of the tail gas is facilitated, the tail gas is utilized, the tail gas is firstly, the tail gas is filled into a sulfonation reaction kettle, the sulfonation reaction kettle, the sulfonation kettle is filled into a sulfonation kettle, the sulfonation reaction kettle, the sulfonation kettle is filled into a sulfonation reaction kettle, the sulfonation kettle is filled into a sulfonation kettle, the sulfonation kettle is filled into the sulfonation reaction kettle, the sulfonation kettle is filled into the sulfonation kettle, the sulfonation kettle is filled into the sulfonation reaction kettle is filled into the sulfonation kettle, the sulfonation kettle is filled into the sulfonation kettle, the sulfonation reaction kettle, the sulfonation reaction kettle is filled into the sulfonation kettle, the sulfonation kettle is filled into the sulfonation reaction kettle, the sulfonation kettle is filled into the sulfonation kettle, the sulfonation kettle is filled into the sulfonation kettle, the sulfonation kettle.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. The production process of the water reducing agent is characterized by comprising the following steps of:
1) sulfonating, namely injecting 70L of methylnaphthalene in a 6300L sulfonating kettle by using a pump, supplementing fresh methylnaphthalene to the methylnaphthalene absorption system after the injection is finished, conveying 93 ℃ liquid naphthalene from a liquid naphthalene raw material tank to a workshop metering tank by using the pump, after the quantity is confirmed, injecting the liquid naphthalene into a 6300L enamel sulfonating kettle, heating the reaction kettle to 120 ℃ through a jacket oil temperature, stopping heating, then slowly injecting 98% sulfuric acid, adjusting the flow rate along with the change of the internal temperature of the reaction kettle, controlling the internal temperature of the reaction kettle to be within 150 ℃, after the addition of the sulfuric acid is finished, slowly raising the internal temperature of the reaction kettle to 160-165 ℃, reacting for 2h, raising the temperature to 160-165 ℃ so as to convert α -naphthalenesulfonic acid which is reacted in advance into β -naphthalenesulfonic acid as far as possible, wherein α -naphthalenesulfonic acid is about 15% and β -naphthalenesulfonic acid is about 85% in the material after the sulfonation is finished, emptying the naphthalene metering tank of the sulfonating part and the sulfonating reaction kettle firstly absorb sublimated naphthalene through the methylnaphthalene absorption system, and then spraying the tail gas to recover alkali liquid naphthalene;
the above process is represented by the following reaction formula:
Figure FDA0002225887670000011
2) hydrolysis, namely opening a bottom valve of the reaction kettle, automatically injecting the sulfonated material into a 12000L condensation reaction kettle, cooling the material to 120 ℃ by jacket cooling water, then adding 1230L hydrolysis water, and forcibly cooling the material to the temperature of 90-95 ℃ after 0.5h of hydrolysis, wherein the hydrolysis aims at reducing α -naphthalenesulfonic acid which is not beneficial to the product quality into acid and naphthalene;
the above process is represented by the following reaction formula:
Figure FDA0002225887670000012
3) conveying the formaldehyde solution from a raw material tank to a formaldehyde metering tank by a pump, then slowly injecting the formaldehyde solution into a condensation reaction kettle at a controlled flow rate to perform condensation reaction, after the reaction is finished, injecting the formaldehyde solution into workshop recovery system water or industrial water to dilute the materials, and then automatically flowing the materials to a neutralization kettle;
the above process is represented by the following reaction formula:
Figure FDA0002225887670000021
4) after the neutralization kettle receives the condensed material, controlling the flow and adding 32 percent of liquid caustic soda for neutralization, after the PH meets the requirement, finishing the neutralization, and feeding the kettle material into a post-treatment working section;
the above process is represented by the following reaction formula:
Figure FDA0002225887670000022
2NaOH+H2SO4→Na2SO4+2H2O
5) and (3) post-treatment, namely after neutralization is finished, directly selling a part of the kettle materials as products, adding sodium sulfate into a part of the kettle materials for compounding to be sold as products, adding sodium chloride into a part of the kettle materials for compounding to be sold as products, adding calcium oxide into a part of the kettle materials for removing part of sulfate radical ions, then carrying out filter pressing, selling the filtrate as the products, selling the filter residues as calcium sulfate serving as a byproduct, and reducing the water content of the rest of the kettle materials of the neutralization kettle by spray drying to be sold as the products.
2. The production process of the water reducing agent according to claim 1, characterized in that: and 2, after the hydrolysis and sulfonation are finished, opening a bottom valve of the reaction kettle, automatically injecting the sulfonated material into a 12000L condensation reaction kettle, cooling the material to 120 ℃ by jacket cooling water, then adding 1230L hydrolysis water, carrying out hydrolysis for 0.5h, then forcibly cooling to the temperature in the kettle to 90-95 ℃, and discharging tail gas during hydrolysis to absorb sublimed naphthalene and acid mist by a methyl tea naphthalene absorption system and a liquid alkali water spraying system in a workshop.
3. The production process of the water reducing agent according to claim 1, characterized in that in the condensation in step 3, the formaldehyde solution is pumped from a raw material tank to a formaldehyde metering tank, then the flow rate is controlled to be slowly injected into a condensation reaction kettle for condensation reaction, after the reaction is finished, the formaldehyde solution is injected into a workshop to recover system water or industrial water, the material is diluted and then automatically flows into a neutralization kettle, the temperature of the condensation kettle is controlled within 100 ℃ during the injection of the formaldehyde, if the condensation temperature exceeds 100 ℃, the formaldehyde flow is adjusted, after the injection of the formaldehyde is finished, the condensation temperature is slowly increased to 103-105 ℃, the temperature is stopped to be increased, the condensation reaction is carried out, the pressure of the reaction kettle is controlled to be 0.03Mp α, the temperature is 105-110 ℃, and the reaction is carried out for 4-5 hours.
4. The production process of the water reducing agent according to claim 1, characterized in that: and 4, after the neutralization kettle receives the condensed materials, controlling the flow rate, adding 32% of liquid caustic soda for neutralization, after the PH meets the requirement, finishing the neutralization, enabling the kettle materials to enter a post-treatment working section, starting jacket cooling water of the neutralization kettle while neutralizing, and controlling the temperature of the neutralization kettle.
5. The production process of the water reducing agent according to claim 1, characterized in that: and 5, after the post-treatment and neutralization are finished, directly selling a part of the kettle materials as products, adding sodium sulfate into a part of the kettle materials for compounding to be sold as products, adding sodium chloride into a part of the kettle materials for compounding to be sold as products, adding calcium oxide into a part of the kettle materials to remove part of sulfate ions, then performing filter pressing, selling the filtrate as products, selling the filter residues as calcium sulfate serving as byproducts, reducing the water content of the rest of the kettle materials for neutralization through spray drying to be sold as products, and performing secondary cyclone dust removal and water film dust removal treatment on dust generated in the drying process.
CN201910951462.4A 2019-10-08 2019-10-08 Production process of water reducing agent Pending CN110790879A (en)

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