CN106977678A - A kind of synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent - Google Patents
A kind of synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent Download PDFInfo
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- CN106977678A CN106977678A CN201710267656.3A CN201710267656A CN106977678A CN 106977678 A CN106977678 A CN 106977678A CN 201710267656 A CN201710267656 A CN 201710267656A CN 106977678 A CN106977678 A CN 106977678A
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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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
- C04B24/226—Sulfonated naphtalene-formaldehyde condensation products
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation 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
- C07C303/04—Preparation 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
- C07C303/06—Preparation 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation 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
- C07C303/22—Preparation 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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Abstract
The invention belongs to naphthalene series high-efficiency water-reducing agent synthesis technical field, a kind of synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent is disclosed, naphthalene and recovery naphthalene are manually put into 1000mL there-necked flasks, 110 DEG C of molten naphthalenes are warming up to；Started to warm up after naphthalene fusing, to 140 DEG C after start that sulfuric acid is added dropwise, the amount ratio of the material of naphthalene and sulfuric acid is 1:1.4；It is 162 DEG C 165 DEG C to control temperature；And keeping temperature 162 DEG C 165 DEG C 2.5 hours；Sampling detection hydrolytic acidity 28.5% 30.5%；Regulation temperature of charge starts to be added dropwise formaldehyde at 95 DEG C 100 DEG C, the ratio between amount of naphthalene and formaldehyde material 1:1.1；Add rear constant temperature；30%NaOH is added, whole course of reaction is completed after being 8 10, solid content 45% to pH value.The present invention can comprehensively utilize limited resource, reduce production cost；It make use of recovery naphthalene well.
Description
Technical field
The invention belongs to naphthalene series high-efficiency water-reducing agent synthesis technical field, more particularly to a kind of inexpensive naphthalene series high-efficiency water-reducing agent
Synthetic method.
Background technology
Naphthalene series high-efficiency water-reducing agent, because its characteristic is still in occupation of major part market, is mainly because amino sulphur at this stage
The easy bleeding of Barbiturates, polycarboxylic acids dehydragent is expensive bad with cement adaptability etc..Naphthalene water reducer has in itself
Plurality of advantages, can work well with a variety of water reducer compound uses again.Moreover, the hair of naphthalene series high-efficiency water-reducing agent existing decades
History is opened up, more ripe production technology has been have accumulated, abundant practical application experience can be pre- well using process progress
Survey.Naphthalene series high-efficiency water-reducing agent still has development potentiality in engineer applied in general.The high water reducer low cost optimization life of naphthalene system
Production can comprehensively utilize limited resource, and raw material is maximally utilized to the concept for also complying with Green Chemistry, and even more reduction is produced into
This effective means.High temperature sulfonating reaction is produced in naphthalene series high-efficiency water-reducing agent, some naphthalene is understood and condensation chamber is entered with steam.And
In condensation chamber crystallisation by cooling, this part draws out the naphthalene come from condensation chamber and is referred to as reclaiming naphthalene.
In summary, the problem of prior art is present be：It is higher to there is production cost in the current high water reducer of naphthalene system, wastes
The energy.
The content of the invention
The problem of existing for prior art, the invention provides a kind of synthesis side of inexpensive naphthalene series high-efficiency water-reducing agent
Method.
The present invention is achieved in that a kind of synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent, the inexpensive naphthalene system
In the synthetic method of high efficiency water reducing agent：
Step one, naphthalene and recovery naphthalene are manually put into 1000mL there-necked flasks, is warming up to 110 DEG C of molten naphthalenes；
Step 2, is started to warm up after naphthalene fusing, to 140 DEG C after start that sulfuric acid is added dropwise, the amount ratio of the material of naphthalene and sulfuric acid is
1:1.4；It is 162 DEG C -165 DEG C to control temperature；And keeping temperature 162 DEG C -165 DEG C 2.5 hours；Sampling, detects sulfonation acidity；Acid
125 DEG C of -130 DEG C of moisturizings are cooled to after degree is qualified, maintain temperature to be hydrolyzed within 30 minutes at 120 DEG C -125 DEG C afterwards；After finishing
Sampling detects hydrolytic acidity 28.5%-30.5% again；
Step 3, regulation temperature of charge starts to be added dropwise formaldehyde at 95 DEG C -100 DEG C, the ratio between amount of naphthalene and formaldehyde material 1:
1.1；Add rear constant temperature；
Step 4, adds 30%NaOH, and whole course of reaction is completed after being 8-10, solid content 45% to pH value.
Further, to starting after 140 DEG C that sulfuric acid is added dropwise, rate of addition is controlled, sulfuric acid was added at -45 minutes 35 minutes.
Further, optimum hydrolysis acidity is 29.5%；Reaction time is 4h.
Further, rear 100 DEG C -105 DEG C of constant temperature is added to be kept for -4.5 hours 4 hours.
Further, reclaim naphthalene volume be 5% in the case of, the ratio between the amount of material of naphthalene and sulfuric acid be 1:1.4th, naphthalene with
The ratio between amount of material of formaldehyde is 1:1st, the condensation time is 4h.
Another object of the present invention is to provide a kind of synthetic method by the inexpensive naphthalene series high-efficiency water-reducing agent to synthesize
Water reducer.
Advantages of the present invention and good effect are：It is that naphthalene series high-efficiency water-reducing agent volatilizees during high―temperature nuclei to reclaim naphthalene
Part naphthalene out, purity is higher.Part crude naphthalene is substituted if can will reclaim naphthalene and recycle, can be dropped to a certain extent
The cost of low naphthalene water reducer, and avoid causing the waste of resource.And the analysis of property content on reclaiming naphthalene etc. is not
There is more literature research, the reasonable processing on reclaiming naphthalene does not have preferable scheme；Because reclaiming in naphthalene and containing sour gas
Body sulfur oxide and other methyl naphthalenes etc. can influence the synthesis of naphthalene series high-efficiency water-reducing agent；The high water reducer low cost optimization of naphthalene system
Production can comprehensively utilize limited resource, and raw material is maximally utilized to the concept for also complying with Green Chemistry, even more reduction production
Cost effective manner；It make use of well and condensation chamber entered with steam in naphthalene series high-efficiency water-reducing agent production high temperature sulfonating reaction
Reclaim naphthalene.The method of the present invention is simple, and the energy has been saved well, production cost is reduced.
Brief description of the drawings
Fig. 1 is the synthetic method flow chart of inexpensive naphthalene series high-efficiency water-reducing agent provided in an embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent provided in an embodiment of the present invention includes following step
Suddenly：
S101：Molten naphthalene, 102.54g (naphthalene is by 96.85% conversion) crude naphthalenes and 5.4g are reclaimed naphthalene (94.39) and manually put into
Into 1000mL there-necked flasks, 110 DEG C of molten naphthalenes are warming up to；
S102：Sulfonation, naphthalene fusing after start to warm up, to 140 DEG C after start be added dropwise sulfuric acid (61.5ml), control be added dropwise speed
Degree, makes sulfuric acid be added at -45 minutes 35 minutes.It is 162 DEG C -165 DEG C to control temperature.And keeping temperature 162 DEG C is -165 DEG C 2.5 small
When.Sampling, detection sulfonation acidity (be normally 30.5% -33.0% or so, beyond this scope it is excessive when should check down
Whether wrong feed intake)；
S103：125 DEG C of -130 DEG C of moisturizings are cooled to after acidity is qualified, rate of water make-up calculates (consulting reference materials).Temperature is maintained afterwards
It is hydrolyzed within 30 minutes at 120 DEG C -125 DEG C.After finishing again sampling detection hydrolytic acidity (28.5% -30.5%, typically with
28.5%-29.5% is optimal), if acidity value is unqualified, acid or moisturizing should be mended again until detecting qualified；
S104：Condensation, regulation temperature of charge starts that formaldehyde (64ml), plus temperature control during formaldehyde is added dropwise at 95 DEG C -100 DEG C
Make between 100 DEG C -108 DEG C (plus rate of addition should be controlled during formaldehyde, electric jacket heating removes electric jacket when temperature is high
, it is not necessary to use cooling water), about 2.0 hours time added.In 100 DEG C of -105 DEG C of constant temperature -4.5 hours 4 hours after adding；
S105：Neutralize, add 30%NaOH (at a slow speed plus, prevent flash), be 8-10 or so to pH value, solid content 45% is left
Whole course of reaction is completed behind the right side.
The application principle of the present invention is further described with reference to experiment.
1st, 1. the ratio between amount of material of naphthalene and the concentrated sulfuric acid
It is 1 to control to choose the ratio between amount of material of naphthalene and sulfuric acid in the case that other conditions are certain:1.2、1:1.3、1:
1.4、1：1.5、1:1.6
Influence of the consumption of the concentrated sulfuric acid of table 1 to cement fluidity
2. sulfonation temperature control other conditions it is certain in the case of choose four groups of 155 DEG C -160 DEG C of temperature values, 160 DEG C -
165℃、165℃—170℃、170℃—175℃.It is as shown in the table
Influence of the sulfonation temperature of table 2 to cement fluidity
3. different sulfonation time 1.5h, 2h, 2.5h, 3h are chosen in the case that sulfonation time control other conditions are certain,
Studying synthesis of the sulfonation time on naphthalene series high-efficiency water-reducing agent influences
Influence of the sulfonation time of table 3 to cement fluidity
4. in the case that the ratio between amount of material of naphthalene and formaldehyde control other conditions are certain, the material of naphthalene and formaldehyde is chosen
The ratio between amount 1:0.9、1:1、1:1.1、1:Synthesis of the amount of the material of 1.2 research naphthalenes and formaldehyde on naphthalene series high-efficiency water-reducing agent influences
The influence for comparing cement fluidity of the amount of the material of the naphthalene of table 4 and formaldehyde
5. in the case that condensation time control other conditions are certain, it is 2h, 3h, 4h, 5h, 6h, research to choose the condensation time
Influence of the temperature to naphthalene series high-efficiency water-reducing agent during condensation
Table 5 is condensed influence of the time to cement fluidity
6. condensation controlling pH, selection condensation acidity are 29%, 31%, 33%
Table 6 is condensed influence of the acidity to cement fluidity
Reclaim naphthalene volume and flowing degree of net paste of cement
The ratio between amount of material of naphthalene and the concentrated sulfuric acid and flowing degree of net paste of cement
The ratio between amount of naphthalene and formaldehyde material and flowing degree of net paste of cement
Condensation reaction time and flowing degree of net paste of cement
7. orthogonal optimization test and result
2nd, the synthesis of naphthalene series high-efficiency water-reducing agent
The synthesis master of naphthalene series high-efficiency water-reducing agent is four steps of experience.High temperature sulfonated naphthalene, prepares beta-naphthalenesulfonic-acid；Hydrolysis is removed
Accessory substance α-naphthalenesulfonicacid；Formaldehyde is added dropwise and carries out polycondensation；Neutralization reaction obtains water reducer product mother liquid.
The preparation principle of 2.1 synthesis naphthalene series high-efficiency water-reducing agents：
Molten naphthalene：Naphthalene at normal temperatures be white plates crystal, in order to be able to the more preferable haptoreaction of liquid sulfuric acid, first heating will
Naphthalene melts, and is typically warming up to 110 DEG C or so, it is yellowish-brown liquid that naphthalene melts completely, and the industrial production with scale is usually to use
Liquid naphthalene is produced, and molten naphthalene is the stage most consumed energy in whole synthesis flow, and remaining stage is all exothermic reaction.Li Qiang etc.[83]Closing
When the process modification of high efficiency water reducing agent, naphthalene is cleverly melted standby with 165 DEG C in later stage sulfonating reaction of high temperature, can be big
Big reduction energy consumption, makes full use of the energy.
Sulfonation：Sulfonating agent is made of the concentrated sulfuric acid and occurs sulfonating reaction with crude naphthalene, this is an electrophilic reversible reaction.It is strong electrophilic
The hydrogen atom point α β that group sulfonic group will replace on the hydrogen atom being connected on naphthalene core with carbon atom, naphthalene core, position α electron clouds are close
Degree is big to be easier at low temperature just (60 DEG C) the electrophilic sulfonating reactions of generation[84], β just the opposite, and cloud density is low to be needed
Electrophilic sulfonating reaction just occurs under higher temperature.Liu Yang etc.[85]Drawn in optimization naphthalene series high-efficiency water-reducing agent preparation process condition, sulphur
Change reaction temperature control to start that sulfuric acid is added dropwise more than 135 DEG C, to reduce accessory substance generation.Control is dripped in 30min or so,
Temperature is risen between 160 DEG C -162 DEG C again afterwards, insulation 2h carries out complete sulfonation.
Sulfonating reaction：Can carry out at a certain temperature, but due to poly- β naphthalene sulfonic acids synthesis condition understand, 162 DEG C-
Most beneficial for poly- β naphthalene sulfonic acids is synthesized under conditions of 165 DEG C, the reaction time is 2.5 hours：
Naphthalene generates β naphthalene sulfonic acids with concentrated acid sulfonation
Sulfonation side reaction：
Naphthalene generates α naphthalene sulfonic acids with concentrated acid sulfonation
Hydrolysis：In order to remove the part accessory substance α naphthalene sulfonic acids produced in sulfonating reaction, acidity is surveyed in sampling after the completion of sulfonation
Probably 30.5%~33.0% or so.The acidity for needing to control is condensed according to latter step, amount of water is calculated.It is cooled to 120 DEG C
~125 DEG C or so, add water hydrolysis 30min.
Hydrolysis：
The hydrolysis of α naphthalene sulfonic acids
Condensation：Condensation reaction principle is shown below, and is that formaldehyde molecule is converted into reaction under conditions of hydrogen ion catalysis
Activity very high carbonyl carbonyl cation, then carry out electrophilic condensation reaction with β naphthalene sulfonic acids.The key factor of this reaction is in summary
The bigger degree of polymerization of hydrogen ion concentration, i.e. acidity is bigger, and reaction is more violent, easily occurs implode.Temperature is controlled at 95 DEG C~100 DEG C,
The too high also easy generation implode of temperature.The mass fraction calculated is added dropwise for 37% formalin, notes speed is added dropwise
Degree, control is dripped in 2h, controls temperature to be condensed between 100 DEG C~108 DEG C after dripping.With the progress of reaction, thing
Material can become sticky, and mixing speed can be substantially slack-off, while material wrinkles, it is now general using a small amount of repeatedly moisturizing, protect material
Hold surface smoothly glossy.Bai Jie etc.[88]Point out to replace mass fraction to be 37% formalin with paraformaldehyde, be substantially shorter
Polymerization reaction time, the addition formaldehyde time can foreshorten to 40~45min, and condensation reaction time can also foreshorten to 1~2h, because of its first
Aldehyde is higher, can improve reaction rate, and substantially reduce the dehydration energy of polymerisation.
Condensation reaction:
β naphthalene sulfonic acids and formaldehyde condensation reaction mechanism
Neutralize：With in 3 sodium hydroxide solutions and the complete sulfuric acid of unreacted, product mother liquid is adjusted to neutral or alkalescent, Peng
Hide[89]Pointed out in a kind of patent of the synthetic method of collapse protection type naphthalene series high-efficiency water-reducing agent optimal pH value be 6~7, mainly because
To add alkali excessively to introduce substantial amounts of metal Na+, the scattered retention property of metallic sodium ion pair cement is poor, cause fluidity loss compared with
It hurry up.Note that a small amount of multiple principle should be taken during adding alkali, plus too much, because neutralization reaction occurs for strong acid and strong base, largely
Heat release can trigger flash.
The reaction of poly- β naphthalene sulfonic acids and sodium hydroxide
The present invention synthesizes and optimized the technique of naphthalene series high-efficiency water-reducing agent based on modern production process, has drawn naphthalene and sulfuric acid
The amount ratio of optimisation substance is 1:1.4；160 DEG C~165 DEG C of the temperature of sulfonation；The ratio between amount of naphthalene and formaldehyde material 1:1.1st, it is condensed anti-
It is 29.5% to answer optimum acidity；Condensation reaction time is 4h；And for the realistic problem of naphthalene series high-efficiency water-reducing agent, propose improvement side
Case, explores the suitable addition for recycling crude naphthalene, has tested the thing for reclaiming naphthalene and the concentrated sulfuric acid under naphthalene Different adding amount
The ratio of the amount of matter, the ratio of the amount of naphthalene and formaldehyde material, the influence of the factor to water reducer performance such as reaction temperature has been drawn
The volume for reclaiming naphthalene is in the case of 5%, the ratio between the amount of material of naphthalene and sulfuric acid is 1:1.4th, the amount of the material of naphthalene and formaldehyde it
Than for 1:1st, the condensation time is 4h.The performance that new product acts on cement is tested by paste flowing degree.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
1. a kind of synthetic method of inexpensive naphthalene series high-efficiency water-reducing agent, it is characterised in that the inexpensive naphthalene series high-efficiency water-reducing agent
Synthetic method in：
Step one, naphthalene and recovery naphthalene are manually put into 1000mL there-necked flasks, is warming up to 110 DEG C of molten naphthalenes；
Step 2, is started to warm up after naphthalene fusing, to 140 DEG C after start that sulfuric acid is added dropwise, the amount ratio of the material of naphthalene and sulfuric acid is 1:
1.4；It is 162 DEG C -165 DEG C to control temperature；And keeping temperature 162 DEG C -165 DEG C 2.5 hours；Sampling, detects sulfonation acidity；Acidity
125 DEG C of -130 DEG C of moisturizings are cooled to after qualified, maintain temperature to be hydrolyzed within 30 minutes at 120 DEG C -125 DEG C afterwards；After finishing again
Sub-sampling detection hydrolytic acidity 28.5%-30.5%；
Step 3, regulation temperature of charge starts to be added dropwise formaldehyde at 95 DEG C -100 DEG C, the ratio between amount of naphthalene and formaldehyde material 1:1.1；
Add rear constant temperature；
Step 4, adds 30%NaOH, and whole course of reaction is completed after being 8-10, solid content 45% to pH value.
2. the synthetic method of low cost naphthalene series high-efficiency water-reducing agent as claimed in claim 1, it is characterised in that opened after to 140 DEG C
Begin that sulfuric acid is added dropwise, control rate of addition, sulfuric acid was added at -45 minutes 35 minutes.
3. the synthetic method of low cost naphthalene series high-efficiency water-reducing agent as claimed in claim 1, it is characterised in that hydrolytic acidity is
29.5%；Reaction time is 4h.
4. the synthetic method of low cost naphthalene series high-efficiency water-reducing agent as claimed in claim 1, it is characterised in that add rear constant temperature
100 DEG C -105 DEG C are kept for -4.5 hours 4 hours.
5. the synthetic method of low cost naphthalene series high-efficiency water-reducing agent as claimed in claim 1, it is characterised in that reclaiming mixing for naphthalene
Amount is in the case of 5%, the ratio between the amount of material of naphthalene and sulfuric acid is 1:1.4th, the ratio between amount of material of naphthalene and formaldehyde is 1:1st, contract
The conjunction time is 4h.
6. the diminishing that a kind of synthetic method of naphthalene series high-efficiency water-reducing agent inexpensive described in Claims 1 to 5 any one is synthesized
Agent.
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| CN110747021A (en) * | 2018-07-24 | 2020-02-04 | 国家能源投资集团有限责任公司 | Coal water slurry dispersant, preparation method and application thereof |
| CN110747021B (en) * | 2018-07-24 | 2022-03-22 | 国家能源投资集团有限责任公司 | Coal water slurry dispersant, preparation method and application thereof |
| CN112574072A (en) * | 2020-11-20 | 2021-03-30 | 安徽鑫固环保股份有限公司 | Method for synthesizing dispersant by using acid tar |
| CN114230492A (en) * | 2021-12-29 | 2022-03-25 | 陈会江 | Preparation process of concrete modification additive |
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Application publication date: 20170725 |