CN110963734A - Polycarboxylate superplasticizer containing complex anti-mud structure - Google Patents

Polycarboxylate superplasticizer containing complex anti-mud structure Download PDF

Info

Publication number
CN110963734A
CN110963734A CN201911283761.1A CN201911283761A CN110963734A CN 110963734 A CN110963734 A CN 110963734A CN 201911283761 A CN201911283761 A CN 201911283761A CN 110963734 A CN110963734 A CN 110963734A
Authority
CN
China
Prior art keywords
solution
mud structure
ester monomer
polycarboxylate superplasticizer
mud
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.)
Withdrawn
Application number
CN201911283761.1A
Other languages
Chinese (zh)
Inventor
唐耀华
王光炎
向新姣
唐宏伟
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.)
Hubei Sanke Building Materials Technology Co ltd
Original Assignee
Hubei Sanke Building Materials Technology 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 Hubei Sanke Building Materials Technology Co ltd filed Critical Hubei Sanke Building Materials Technology Co ltd
Priority to CN201911283761.1A priority Critical patent/CN110963734A/en
Publication of CN110963734A publication Critical patent/CN110963734A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F130/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
    • C08F130/02Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
    • 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

Abstract

A polycarboxylate superplasticizer containing a complexing anti-mud structure is composed of the following raw materials in percentage by mass: sodium aminobenzenesulfonate, unsaturated phosphate ester monomer, chain transfer agent, initiator, anhydrous sodium metasilicate and the balance of deionized water. The preparation method disclosed by the invention is simple and reasonable, has the advantages of high efficiency and low cost, is firmer in structure, smaller and more uniform in pore space, can solve the problem of mud content of engineering building materials, and can reduce the slump loss of the engineering building materials under the condition of low doping amount.

Description

Polycarboxylate superplasticizer containing complex anti-mud structure
Technical Field
The invention relates to the technical field of building materials, in particular to a polycarboxylic acid water reducing agent containing a complexing anti-mud structure.
Background
In recent decades, with the continuous development of concrete preparation and construction technology, the application of preparing high-performance concrete by using a polycarboxylic acid water reducing agent becomes more and more extensive, and the concrete becomes a development trend of concrete. The polycarboxylic acid water reducing agent has the advantages of small mixing amount, high water reducing rate, good cement adaptability, excellent collapse degree maintaining performance, low chloride ion content and alkali content, small shrinkage, good durability and the like, and is environment-friendly, so that the polycarboxylic acid water reducing agent is widely applied to house building and infrastructure construction engineering. However, in the practical application process, the sand content has a large adverse effect on the concrete doped with the polycarboxylate superplasticizer. The interlayer structure of the soil in the sand and high-valence metal ions such as magnesium ions, aluminum ions and the like contained in the sand can adsorb a large amount of polycarboxylic acid water reducing agent molecules, so that the water reducing agent loses activity. In recent years, natural sand resources are in short supply, and as sand with high mud content is directly used in concrete, the workability of fresh concrete doped with polycarboxylic acid water reducing agent is deteriorated, the slump retention capacity is reduced, and the strength and durability of the concrete are even affected.
At present, an effective method for solving the problems is not available, the problems can be solved only by increasing the mixing amount of the polycarboxylic acid water reducing agent, the cost of concrete is increased, and meanwhile, the troubles of other processes are increased.
Disclosure of Invention
The invention aims to provide a polycarboxylic acid water reducing agent containing a complexing anti-mud structure, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a polycarboxylate superplasticizer containing a complexing anti-mud structure is composed of the following raw materials in percentage by mass: sodium aminobenzenesulfonate, unsaturated phosphate ester monomer, chain transfer agent, initiator, anhydrous sodium metasilicate and the balance of deionized water;
a preparation method of a polycarboxylic acid water reducing agent containing a complexing anti-mud structure comprises the following steps:
1) sequentially adding sodium aminobenzenesulfonate and anhydrous sodium metasilicate into a stirring kettle, uniformly mixing and stirring, stirring at the rotating speed of 160-210 revolutions per minute for 8-15 min to prepare an aqueous solution, neutralizing the aqueous solution with 30% NaOH to obtain a solution with the pH value of 6-7, and marking the solution as No. I;
2) dissolving an initiator and a complexing agent in water to prepare a solution II, beginning to drip the solution I, beginning to drip the solution II when the temperature reaches a set value, adding the initiator for 10-15 min, adding an unsaturated phosphate ester monomer and a chain transfer agent within 4.5h, reacting for 3-5 h at 80-110 ℃, stopping the reaction by using a small amount of ascorbic acid solution, and cooling to room temperature to obtain the polycarboxylic acid water reducer containing the complex anti-mud structure.
Preferably, the unsaturated phosphate ester monomer is prepared by the following method: reacting a phosphating agent with an unsaturated ester monomer at 70-90 ℃ for 1-1.5 hours, adding polyoxometallate, continuously reacting for 0.5-3 hours, adding deionized water, and continuously reacting for 1-3 hours at 90-120 ℃ to obtain the unsaturated phosphate ester monomer.
Preferably, the chain transfer agent is sodium methallylsulfonate.
Preferably, the initiator is hydrogen peroxide (H)202) And ascorbic acid (Vc).
Preferably, the complexing agent is one of ethylene diamine tetraacetic acid dipotassium salt, diethylenetriamine pentamethylene phosphonic acid potassium salt, ethylene diamine tetra methylene phosphonic acid potassium salt and bis 1, 6-hexylidene triamine pentamethylene phosphonic acid potassium salt.
The preparation method disclosed by the invention is simple and reasonable, has the advantages of high efficiency and low cost, is firmer in structure, smaller and more uniform in pore space, can solve the problem of mud content of engineering building materials, and can reduce the slump loss of the engineering building materials under the condition of low doping amount.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
A preparation method of a polycarboxylic acid water reducing agent containing a complexing anti-mud structure comprises the following steps:
1) sequentially adding sodium aminobenzenesulfonate and anhydrous sodium metasilicate into a stirring kettle, uniformly mixing and stirring, stirring for 15min at the rotating speed of 160-210 revolutions per minute, preparing an aqueous solution, neutralizing the aqueous solution with 30% NaOH to obtain a solution with the pH value of 6-7, and marking the solution as No. I;
2) dissolving hydrogen peroxide and ethylene diamine tetraacetic acid dipotassium salt in water to prepare a solution II, beginning to dropwise add the solution I, beginning to dropwise add the solution II when the temperature reaches a set value, adding an initiator for 15min, controlling the addition of an unsaturated phosphate ester monomer and methyl allyl sodium sulfonate within 4.5h, reacting for 5 hours at 110 ℃, stopping the reaction by using a small amount of ascorbic acid solution, and cooling to room temperature to obtain the polycarboxylic acid water reducer containing the complex anti-mud structure.
The unsaturated phosphate ester monomer is prepared by the following method: reacting a phosphating agent with an unsaturated ester monomer at 90 ℃ for 1.5 hours, adding polyoxometallate to continue reacting for 3 hours, adding deionized water to continue reacting at 90 ℃ for 1 hour to obtain the unsaturated phosphate ester monomer.
Example 2
A preparation method of a polycarboxylic acid water reducing agent containing a complexing anti-mud structure comprises the following steps:
1) sequentially adding sodium aminobenzenesulfonate and anhydrous sodium metasilicate into a stirring kettle, uniformly mixing and stirring, stirring at the rotating speed of 160-210 revolutions per minute for 10min to prepare an aqueous solution, neutralizing the aqueous solution with 30% NaOH to obtain a solution with the pH value of 6-7, and marking the solution as No. I;
2) dissolving hydrogen peroxide and ethylene diamine tetramethylene phosphonic acid potassium salt in water to prepare a solution II, beginning to dropwise add the solution I, beginning to dropwise add the solution II when the temperature reaches a set value, adding an initiator for 12min, controlling the unsaturated phosphate ester monomer and the sodium methallylsulfonate to be added within 4.5h, reacting for 4 hours at 100 ℃, stopping the reaction by using a small amount of ascorbic acid solution, and cooling to room temperature to obtain the polycarboxylic acid water reducer containing the complex anti-mud structure.
The unsaturated phosphate ester monomer is prepared by the following method: reacting a phosphating agent with an unsaturated ester monomer at 80 ℃ for 1.2 hours, then adding polyoxometallate to continue reacting for 2 hours, adding deionized water to continue reacting for 2 hours at 110 ℃ to obtain the unsaturated phosphate ester monomer.
Example 3
A preparation method of a polycarboxylic acid water reducing agent containing a complexing anti-mud structure comprises the following steps:
1) sequentially adding sodium aminobenzenesulfonate and anhydrous sodium metasilicate into a stirring kettle, uniformly mixing and stirring, stirring at the rotating speed of 160-210 revolutions per minute for 8min to prepare an aqueous solution, neutralizing the aqueous solution with 30% NaOH to obtain a solution with the pH value of 6-7, and marking the solution as No. I;
2) dissolving hydrogen peroxide and ethylene diamine tetraacetic acid dipotassium salt in water to prepare a solution II, beginning to dropwise add the solution I, beginning to dropwise add the solution II when the temperature reaches a set value, adding an initiator for 10min, controlling the addition of an unsaturated phosphate ester monomer and methyl allyl sodium sulfonate within 4.5h, reacting for 3 hours at 80 ℃, stopping the reaction by using a small amount of ascorbic acid solution, and cooling to room temperature to obtain the polycarboxylic acid water reducer containing the complex anti-mud structure.
The unsaturated phosphate ester monomer is prepared by the following method: reacting a phosphating agent with an unsaturated ester monomer at 70 ℃ for 1 hour, adding polyoxometallate to continue reacting for 0.5 hour, adding deionized water to continue reacting at 120 ℃ for 3 hours to obtain the unsaturated phosphate ester monomer.
Comparative example
Adding part of water and 4-hydroxybutyl vinyl polyether macromonomer into a reaction kettle by adopting water-soluble free radical polymerization, quickly stirring, respectively and uniformly adding a mixed aqueous solution of acrylic acid, end-capped amide phosphate and propionic acid and a rongalite aqueous solution into the reaction kettle when the 4-hydroxybutyl vinyl polyether macromonomer is completely dissolved and the temperature is stabilized at 20 ℃, continuing for 2 hours, and continuing to keep the temperature for 2 hours after the reaction is finished. And cooling to room temperature, neutralizing with 30% sodium hydroxide aqueous solution until the pH value is 6.0-7.0, adding water to adjust the solid content to 40%, and obtaining the anti-mud polycarboxylic acid water reducer.
The details of the assay are given in the following table:
table 1: fluidity test for examples 1-3 and comparative example
Figure 656460DEST_PATH_IMAGE002
As can be seen from Table 1, when the mixing amount of the polycarboxylic acid water reducer containing the complex anti-mud structure is 0.25%, the fluidity of the polycarboxylic acid water reducer reaches 180mm, and the polycarboxylic acid water reducer has certain loss after 1 hour and good dispersibility on concrete; the slump retaining agent shows a gradually-decreasing trend along with the prolonging of the standing time, and the fluidity trend of the slump retaining agent is obviously smaller than that of a comparative example, so that the slump retaining agent has good slump retaining performance and is better than that of the comparative example.
The concrete performance test shows that the folded solid content of the additive is 1.5% of the montmorillonite dosage, the montmorillonite used is 6g, and the test results are shown in Table 2.
Table 2: the examples 1-3 and comparative examples were tested for performance:
Figure 42442DEST_PATH_IMAGE004
the compressive strength of the concrete is obviously improved and is enhanced along with time, which shows that the polycarboxylic acid water reducer containing the complex anti-mud structure has the anti-mud property and also has an obvious improvement effect on the concrete strength. Compared with concrete with the same admixture anchoring amount in the comparative example, the concrete has higher compressive strength and better performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (5)

1. A polycarboxylate superplasticizer containing a complexing anti-mud structure is characterized by being implemented according to the following steps:
1) sequentially adding sodium aminobenzenesulfonate and anhydrous sodium metasilicate into a stirring kettle, uniformly mixing and stirring, stirring at the rotating speed of 160-210 revolutions per minute for 8-15 min to prepare an aqueous solution, neutralizing the aqueous solution with 30% NaOH to obtain a solution with the pH value of 6-7, and marking the solution as No. I;
2) dissolving an initiator in water to prepare a solution II, beginning to dropwise add the solution I, beginning to dropwise add the solution II when the temperature reaches a set value, adding the initiator for 10-15 min, controlling the unsaturated phosphate ester monomer and the chain transfer agent to be added within 4.5h, reacting for 3-5 h at 80-110 ℃, stopping the reaction by using a small amount of ascorbic acid solution, and cooling to room temperature to obtain the polycarboxylic acid water reducer containing the complex anti-mud structure.
2. The polycarboxylate superplasticizer containing the complex anti-mud structure according to claim 1, characterized in that the unsaturated phosphate ester monomer is prepared by the following method: reacting a phosphating agent with an unsaturated ester monomer at 70-90 ℃ for 1-1.5 hours, adding polyoxometallate, continuously reacting for 0.5-3 hours, adding deionized water, and continuously reacting for 1-3 hours at 90-120 ℃ to obtain the unsaturated phosphate ester monomer.
3. The polycarboxylate superplasticizer with the complexed anti-mud structure according to claim 1, wherein said chain transfer agent is sodium methallylsulfonate.
4. The polycarboxylate superplasticizer containing the complex anti-mud structure as claimed in claim 1, wherein said initiator is one or more of hydrogen peroxide and ascorbic acid.
5. The polycarboxylate water reducer with the complexing anti-mud structure as claimed in claim 1, wherein the complexing agent is one of dipotassium ethylenediamine tetraacetate, potassium diethylenetriamine pentamethylenephosphonic acid, potassium ethylenediamine tetramethylene phosphonic acid and potassium bis-1, 6-hexylenediamine pentamethylenephosphonic acid.
CN201911283761.1A 2019-12-13 2019-12-13 Polycarboxylate superplasticizer containing complex anti-mud structure Withdrawn CN110963734A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911283761.1A CN110963734A (en) 2019-12-13 2019-12-13 Polycarboxylate superplasticizer containing complex anti-mud structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911283761.1A CN110963734A (en) 2019-12-13 2019-12-13 Polycarboxylate superplasticizer containing complex anti-mud structure

Publications (1)

Publication Number Publication Date
CN110963734A true CN110963734A (en) 2020-04-07

Family

ID=70034218

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911283761.1A Withdrawn CN110963734A (en) 2019-12-13 2019-12-13 Polycarboxylate superplasticizer containing complex anti-mud structure

Country Status (1)

Country Link
CN (1) CN110963734A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113461359A (en) * 2021-06-29 2021-10-01 江苏先帅科技有限公司 Composite polycarboxylate superplasticizer for tube sheet prefabricated member and preparation method thereof
CN114380527A (en) * 2022-03-23 2022-04-22 湖南凝英新材料科技有限公司 Reinforced modifier for concrete admixture and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113461359A (en) * 2021-06-29 2021-10-01 江苏先帅科技有限公司 Composite polycarboxylate superplasticizer for tube sheet prefabricated member and preparation method thereof
CN113461359B (en) * 2021-06-29 2022-05-10 江苏先帅科技有限公司 Composite polycarboxylate superplasticizer for tube sheet prefabricated member and preparation method thereof
CN114380527A (en) * 2022-03-23 2022-04-22 湖南凝英新材料科技有限公司 Reinforced modifier for concrete admixture and preparation method thereof

Similar Documents

Publication Publication Date Title
CN102504126A (en) Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof
CN108794700A (en) A kind of carboxylic acid group polymer and preparation method thereof and sustained-release polycarboxylic water reducer
CN110963734A (en) Polycarboxylate superplasticizer containing complex anti-mud structure
CN106830740B (en) A kind of additive improving polycarboxylate water-reducer and component materials of concrete compatibility
CN104031216A (en) Polyether-amide type polycarboxylic high-efficiency water reducer and preparation method thereof
CN110963732A (en) Environment-friendly alkali-free liquid accelerator and normal-temperature preparation method thereof
CN107954627B (en) Composite concrete retarder and preparation method thereof
CN111763290A (en) Early-strength polycarboxylate superplasticizer
CN106380551B (en) A kind of muting sensitive induction reactance chamotte mould polycarboxylate water-reducer and preparation method thereof
CN114349914B (en) Ferrocene modified anti-mud polycarboxylate water reducer and preparation method thereof
CN107417155B (en) Alkali-free chlorine-free liquid accelerator and preparation method and application thereof
CN114163577A (en) Viscosity-reducing water reducer and preparation method and application thereof
CN109721271B (en) Polycarboxylate water reducing agent composition for self-compacting high-workability concrete
CN112708025A (en) Anti-segregation intermediate, self-compacting concrete anti-segregation agent and preparation method thereof
CN112479624A (en) Low-alkali liquid accelerator for sprayed concrete and preparation method thereof
CN109626860B (en) Preparation method of block viscosity-reducing concrete admixture
CN107603110A (en) A kind of branched chain type suppression mud polycarboxylate water-reducer, its preparation method and application
CN113429134B (en) Method for adjusting fluidity and setting time of chemically-activated cementing material system
CN110776603A (en) Preparation method of polycarboxylic acid mud-resistant water reducer synthesized by sodium lignosulfonate
CN114920890B (en) Viscosity-reducing additive and preparation method and application thereof
CN110885414A (en) ATRP method ester-based amide block polymer modified polycarboxylic acid water reducing agent and preparation method thereof
CN111848881A (en) Cross-linking amphoteric polycarboxylate superplasticizer, preparation method and application
CN114685085B (en) Wet-mixed mortar additive and preparation method thereof
CN108559034B (en) Ether low-sensitivity type polycarboxylate superplasticizer and preparation method thereof
CN109535347B (en) Preparation method of block water-retaining concrete admixture

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20200407