CN112920343A - Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof - Google Patents
Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof Download PDFInfo
- Publication number
- CN112920343A CN112920343A CN202110153980.9A CN202110153980A CN112920343A CN 112920343 A CN112920343 A CN 112920343A CN 202110153980 A CN202110153980 A CN 202110153980A CN 112920343 A CN112920343 A CN 112920343A
- Authority
- CN
- China
- Prior art keywords
- parts
- methyl
- solution
- concrete
- reaction
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of concrete admixtures, and particularly relates to a polycarboxylic acid water reducing agent suitable for commercial concrete and a preparation method thereof. The water reducing agent is prepared from the following raw materials in parts by weight: 350 parts of methyl allyl polyoxyethylene ether 320-methyl-4-methylthiophenol, 20-23 parts of acrylic acid, 40-45 parts of methyl acrylate, 16-18 parts of ammonium persulfate, 1.5-2 parts of hydrogen peroxide and 3-5 parts of isooctyl 3-mercaptopropionate. The polycarboxylic acid water reducing agent prepared by the invention has low yield, good slump keeping performance, high water reducing rate and good stability, can be suitable for commercial concrete, and can greatly reduce the microbial contamination rate of the concrete and improve the stability and compressive strength of the concrete.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a polycarboxylic acid water reducing agent suitable for commercial concrete and a preparation method thereof.
Background
The commercial concrete is prepared from a cementing material, coarse and fine aggregates, water and other additives according to a proper proportion. The commercial concrete has the advantages of rich raw materials, low cost, good plasticity, high strength and durability. With the rapid development of Chinese economy, people put higher requirements on the construction quality and plan of projects. Although commercial concrete has many advantages, in the field use process of commercial concrete, the phenomena of segregation, blockage and the like of the concrete are easy to occur during unloading and pouring, further treatment is improper, and serious quality accidents can also occur in concrete engineering.
The water reducing agent is used as an important additive of concrete, can reduce the using amount of cement and improve the performance index of the concrete. After the water reducing agent is added into the commercial concrete, the water content of the concrete can be adjusted according to construction requirements, resource consumption is reduced, and engineering cost is controlled. The polycarboxylate superplasticizer is an important component of commercial concrete, but is easily polluted by microorganisms due to the molecular structure of the polycarboxylate superplasticizer, and finally influences the performance of the commercial concrete. Therefore, the research and development of a polycarboxylic acid water reducing agent which is suitable for commercial concrete and has good stability is a problem to be solved urgently.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a polycarboxylic acid water reducing agent suitable for commercial concrete, which improves the performance of the commercial concrete, has good stability and stronger antibacterial and anticorrosive performances.
The invention also provides a preparation method of the polycarboxylate superplasticizer.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the invention provides a polycarboxylic acid water reducing agent suitable for commercial concrete, which comprises the following raw materials in parts by weight: 350 parts of methyl allyl polyoxyethylene ether 320-methyl-4-methylthiophenol, 20-23 parts of acrylic acid, 40-45 parts of methyl acrylate, 16-18 parts of ammonium persulfate, 1.5-2 parts of hydrogen peroxide and 3-5 parts of isooctyl 3-mercaptopropionate.
The invention also provides a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
(1) uniformly mixing 3-methyl-4-methylthiophenol and methyl acrylate, adding an ethanol-glycerol mixed solvent, adding proline-concentrated sulfuric acid for catalytic reaction, heating to 45-50 ℃, stirring for reaction for 45-50 hours, and filtering after the reaction is finished to obtain a white product for later use;
(2) adding parts by weight of methyl allyl polyoxyethylene ether, the product prepared in the step (1) and isooctyl 3-mercaptopropionate into deionized water, and uniformly stirring to form a base solution;
(3) adding acrylic acid into deionized water, and uniformly stirring to form a solution A;
(4) adding ammonium persulfate and hydrogen peroxide into deionized water, and uniformly stirring to form a solution B;
(5) firstly heating the base solution to 50-60 ℃, stirring for a period of time, then continuing heating to 80-90 ℃, and dropwise adding the solution A and the solution B, wherein the dropwise adding time of the solution A is 1 hour, and the dropwise adding time of the solution B is 1.5 hours;
(6) after the dropwise addition is finished, the reaction is carried out for 25min under the condition of heat preservation, after the reaction is finished, the pH value is adjusted to 6-7, and the stirring is carried out for 30min under the condition of heat preservation.
Further, in the step (1), the concentration of the 3-methyl-4-methylthiophenol in the mixed solvent is 20-25%; the volume ratio of ethanol to glycerol in the mixed solvent is 5: 1.
further, in the step (1), the addition amount of the proline-concentrated sulfuric acid accounts for 2.5% of the mass of the 3-methyl-4-methylthiophenol; the mass ratio of the proline to the concentrated sulfuric acid is 0.3: 1.
the pH value is adjusted by adopting concentrated alkali.
The concentrated alkali is sodium hydroxide solution with the mass concentration of 30%.
According to the invention, firstly, the 3-methyl-4-methylthiophenol and the methyl acrylate are synthesized into the polymeric monomer, the introduction of the monomer can greatly improve the antibacterial capability of the polycarboxylic acid water reducing agent, the microbial pollution of the concrete water reducing agent is greatly reduced, and then the monomer methyl allyl polyoxyethylene ether and the acrylic acid are used for synthesizing the modified polycarboxylic acid water reducing agent under the action of the chain transfer agent and the composite initiator.
The invention has the beneficial effects that: the polycarboxylic acid water reducing agent prepared by the invention has low yield, good slump keeping performance, high water reducing rate and good stability, can be suitable for commercial concrete, and can greatly reduce the microbial contamination rate of the concrete and improve the stability and compressive strength of the concrete.
Detailed Description
The technical solution of the present invention is further explained and illustrated by the following specific examples.
Example 1
A polycarboxylic acid water reducing agent suitable for commercial concrete comprises the following components in percentage by weight: 320 parts of methyl allyl polyoxyethylene ether, 20 parts of 3-methyl-4-methylthiophenol, 42 parts of acrylic acid, 16 parts of methyl acrylate, 2 parts of ammonium persulfate, 1.5 parts of hydrogen peroxide and 3 parts of isooctyl 3-mercaptopropionate.
The preparation method comprises the following steps:
(1) uniformly mixing 3-methyl-4-methylthiophenol and methyl acrylate in parts by weight, adding 50mL of ethanol and 10mL of glycerol mixed solvent, adding proline-concentrated sulfuric acid accounting for 2.5% of the mass of the 3-methyl-4-methylthiophenol for catalytic reaction, heating to 45-50 ℃, stirring for reacting for 45 hours, and filtering after the reaction is finished to obtain a white product for later use;
(2) adding parts by weight of methyl allyl polyoxyethylene ether, the product prepared in the step (1) and isooctyl 3-mercaptopropionate into deionized water, and uniformly stirring to form a base solution;
(3) adding acrylic acid into deionized water, and uniformly stirring to form a solution A;
(4) adding ammonium persulfate and hydrogen peroxide into deionized water, and uniformly stirring to form a solution B;
(5) firstly heating the base solution to 50-60 ℃, stirring for a period of time, then continuing heating to 80-90 ℃, and dropwise adding the solution A and the solution B, wherein the dropwise adding time of the solution A is 1 hour, and the dropwise adding time of the solution B is 1.5 hours;
(6) after the dropwise addition is finished, the reaction is carried out for 25min under the condition of heat preservation, after the reaction is finished, the pH value is adjusted to 6-7, and the stirring is carried out for 30min under the condition of heat preservation.
Meanwhile, it is noted that, in the synthesis process of the step (1), when the synthesis is performed only with concentrated sulfuric acid, the reaction progress is monitored by TLC (developing solvent is composed of ethyl acetate and petroleum ether in a volume ratio of 1: 3), and it takes 70 hours for the reaction to end.
Example 2
A polycarboxylic acid water reducing agent suitable for commercial concrete comprises the following components in percentage by weight: 350 parts of methyl allyl polyoxyethylene ether, 23 parts of 3-methyl-4-methylthiophenol, 45 parts of acrylic acid, 18 parts of methyl acrylate, 3 parts of ammonium persulfate, 1.5 parts of hydrogen peroxide and 5 parts of isooctyl 3-mercaptopropionate.
The preparation method is the same as example 1.
Example 3
A polycarboxylic acid water reducing agent suitable for commercial concrete comprises the following components in percentage by weight: 335 parts of methyl allyl polyoxyethylene ether, 23 parts of 3-methyl-4-methylthiophenol, 42 parts of acrylic acid, 18 parts of methyl acrylate, 3 parts of ammonium persulfate, 2 parts of hydrogen peroxide and 4 parts of isooctyl 3-mercaptopropionate.
The preparation method is the same as example 1.
Comparative example 1
A polycarboxylic acid water reducing agent suitable for commercial concrete comprises the following components in percentage by weight: 320 parts of methyl allyl polyoxyethylene ether, 42 parts of acrylic acid, 16 parts of methyl acrylate, 2 parts of ammonium persulfate, 1.5 parts of hydrogen peroxide and 3 parts of 3-isooctyl mercaptopropionate.
The preparation method comprises the following steps:
(1) adding parts by weight of methyl allyl polyoxyethylene ether, methyl methacrylate and 3-isooctyl mercaptopropionate into deionized water, and uniformly stirring to form a base solution;
(2) adding acrylic acid into deionized water, and uniformly stirring to form a solution A;
(3) adding ammonium persulfate and hydrogen peroxide into deionized water, and uniformly stirring to form a solution B;
(4) firstly heating the base solution to 50-60 ℃, stirring for a period of time, then continuing heating to 80-90 ℃, and dropwise adding the solution A and the solution B, wherein the dropwise adding time of the solution A is 1 hour, and the dropwise adding time of the solution B is 1.5 hours;
(5) after the dropwise addition is finished, the reaction is carried out for 25min under the condition of heat preservation, after the reaction is finished, the pH value is adjusted to 6-7, and the stirring is carried out for 30min under the condition of heat preservation.
Effects of the embodiment
Carrying out relevant detection according to a test method provided by GB/T8076-2008, wherein the folding and fixing doping amount of the water reducing agent is 0.12%, and reference cement is adopted; the concrete free flowing time is concrete with the strength grade of C50, and the concrete comprises the following components: 365 of cement, 90 of mineral powder, 45 of fly ash, 1750 of sandstone and 150 of water; specific results are shown in table 1.
TABLE 1
And (II) respectively taking 500 parts of the water reducing agents prepared in the examples and the comparative examples, adding 50 parts of sucrose, respectively inoculating cultured moulds into the water reducing agents, standing for 6 months at room temperature, wherein the water reducing agents prepared in the comparative example 1 have more surface microorganisms and have putrefactive odor, bacterial plaques slightly appear on the surfaces of the water reducing agents prepared in the invention, and the performance change is little after the test.
Claims (6)
1. The polycarboxylic acid water reducing agent suitable for commercial concrete is characterized by comprising the following raw materials in parts by weight: 350 parts of methyl allyl polyoxyethylene ether 320-methyl-4-methylthiophenol, 20-23 parts of acrylic acid, 40-45 parts of methyl acrylate, 16-18 parts of ammonium persulfate, 1.5-2 parts of hydrogen peroxide and 3-5 parts of isooctyl 3-mercaptopropionate.
2. The preparation method of the polycarboxylate superplasticizer according to claim 1, characterized by comprising the following steps:
(1) uniformly mixing 3-methyl-4-methylthiophenol and methyl acrylate, adding an ethanol-glycerol mixed solvent, adding proline-concentrated sulfuric acid for catalytic reaction, heating to 45-50 ℃, stirring for reaction for 45-50 hours, and filtering after the reaction is finished to obtain a white product for later use;
(2) adding parts by weight of methyl allyl polyoxyethylene ether, the product prepared in the step (1) and isooctyl 3-mercaptopropionate into deionized water, and uniformly stirring to form a base solution;
(3) adding acrylic acid into deionized water, and uniformly stirring to form a solution A;
(4) adding ammonium persulfate and hydrogen peroxide into deionized water, and uniformly stirring to form a solution B;
(5) firstly heating the base solution to 50-60 ℃, stirring for a period of time, then continuing heating to 80-90 ℃, and dropwise adding the solution A and the solution B, wherein the dropwise adding time of the solution A is 1 hour, and the dropwise adding time of the solution B is 1.5 hours;
(6) after the dropwise addition is finished, the reaction is carried out for 25min under the condition of heat preservation, after the reaction is finished, the pH value is adjusted to 6-7, and the stirring is carried out for 30min under the condition of heat preservation.
3. The production method according to claim 2, wherein in the step (1), the concentration of the 3-methyl-4-methylthiophenol in the mixed solvent is 20 to 25%; the volume ratio of ethanol to glycerol in the mixed solvent is 5: 1.
4. the production method according to claim 2 or 3, wherein in the step (1), the proline-concentrated sulfuric acid is added in an amount of 2.5% by mass of the 3-methyl-4-methylthiophenol; the mass ratio of the proline to the concentrated sulfuric acid is 0.3: 1.
5. the process according to any one of claims 2 to 4, wherein the pH adjustment in the step (6) is carried out using a concentrated alkali.
6. The production method according to claim 5, wherein the concentrated alkali is a sodium hydroxide solution having a mass concentration of 30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110153980.9A CN112920343A (en) | 2021-02-04 | 2021-02-04 | Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110153980.9A CN112920343A (en) | 2021-02-04 | 2021-02-04 | Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112920343A true CN112920343A (en) | 2021-06-08 |
Family
ID=76170304
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110153980.9A Pending CN112920343A (en) | 2021-02-04 | 2021-02-04 | Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112920343A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN109400820A (en) * | 2018-10-31 | 2019-03-01 | 山西奥瑞特建材科技有限公司 | A kind of polycarboxylate water-reducer and preparation method |
| CN113149507A (en) * | 2021-04-16 | 2021-07-23 | 江苏超力建材科技有限公司 | Preparation method of comprehensive slump-retaining polycarboxylate superplasticizer |
-
2021
- 2021-02-04 CN CN202110153980.9A patent/CN112920343A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN109400820A (en) * | 2018-10-31 | 2019-03-01 | 山西奥瑞特建材科技有限公司 | A kind of polycarboxylate water-reducer and preparation method |
| CN113149507A (en) * | 2021-04-16 | 2021-07-23 | 江苏超力建材科技有限公司 | Preparation method of comprehensive slump-retaining polycarboxylate superplasticizer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114195421B (en) | Preparation method of polycarboxylic acid additive for machine-made sand concrete | |
| CN109400821B (en) | Concrete bleeding-resistant inhibitor with water reducing function and preparation method thereof | |
| CN105924592B (en) | Viscosity-reducing polycarboxylic acid water reducer and preparation method thereof | |
| CN109369860B (en) | Slow-release controllable polycarboxylate superplasticizer mother liquor and preparation method thereof | |
| CN108948288B (en) | Preparation method of crosslinking type polycarboxylate superplasticizer by adopting carboxyl functional monomer | |
| CN111393583B (en) | Amino propane sulfonic acid inner salt type amphoteric concrete water reducer and preparation method thereof | |
| CN111100253A (en) | Concrete anti-sensitive polycarboxylate superplasticizer and preparation method thereof | |
| CN111439947A (en) | Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof | |
| CN104356316A (en) | Polycarboxylic acid water reducer prepared from running water and preparation method of polycarboxylic acid water reducer | |
| CN104628293A (en) | Early strength type polycarboxylic acid water reducing agent, preparation method and use method thereof | |
| CN111153627A (en) | Anti-mud additive suitable for machine-made sand concrete and compounding method thereof | |
| CN109053970B (en) | Preparation method of anti-mud polycarboxylic slump retaining agent adopting carboxyl functional monomer | |
| CN108558261B (en) | Additive for inhibiting assembled concrete bleeding and preparation method thereof | |
| CN111961148B (en) | Reaction air-entraining type polycarboxylate superplasticizer and preparation method thereof | |
| CN111808244B (en) | Polycarboxylate superplasticizer with high water reduction and high adaptability and preparation method thereof | |
| CN112521099A (en) | Production process of quick-setting concrete | |
| CN109721271B (en) | Polycarboxylate water reducing agent composition for self-compacting high-workability concrete | |
| CN110606695A (en) | Modified polycarboxylate superplasticizer and preparation method thereof | |
| CN108706899B (en) | Preparation method of modified cement dispersant | |
| CN112920343A (en) | Polycarboxylate superplasticizer suitable for commercial concrete and preparation method thereof | |
| CN111019059B (en) | Polycarboxylate superplasticizer synthesized at normal temperature and synthesis method thereof | |
| CN108219079B (en) | Polycarboxylic acid water reducing agent, and preparation method and use method thereof | |
| CN111825372B (en) | Polycarboxylic acid high-performance water reducing agent and preparation method thereof | |
| CN109111556B (en) | Ester ether crosslinking polycarboxylic acid workability regulator and preparation method thereof | |
| CN113149507A (en) | Preparation method of comprehensive slump-retaining polycarboxylate superplasticizer |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210608 |
|
| RJ01 | Rejection of invention patent application after publication |