CN105859979A - Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof - Google Patents
Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof Download PDFInfo
- Publication number
- CN105859979A CN105859979A CN201610263545.0A CN201610263545A CN105859979A CN 105859979 A CN105859979 A CN 105859979A CN 201610263545 A CN201610263545 A CN 201610263545A CN 105859979 A CN105859979 A CN 105859979A
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- China
- Prior art keywords
- slump retaining
- retaining agent
- agent
- polycarboxylic acid
- chamotte mould
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Classifications
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- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses an anti-mud polycarboxylic acid slump retaining agent. The slump retaining agent is prepared from the following raw materials by weight percent: 50-75% of unsaturated polyoxyethylene ether monomer, 4-8% of acrylic acid, 6-12% of maleic anhydride, 11-20% of hydroxyethyl acrylate or hydroxypropyl acrylate, 0.5-3.0% of chain transfer agents, 0.1-5% of initiators and 0.01-2% of initiating additives. The invention also discloses a preparation method of the slump retaining agent. The preparation method comprises the following steps: dropwise adding a solution of acrylic acid, hydroxyethyl acrylate and hydroxypropyl acrylate and dropwise adding the initiating additives for 2-3.5 hours, and adding a sodium hydroxide solution to regulate the pH value to 6-7 after insulating for 1-1.5 hours, thus obtaining the anti-mud polycarboxylic acid slump retaining agent with solid content of 40-45%. The slump retaining agent has an obvious anti-mud effect in concrete and has an excellent slump retaining capacity.
Description
Technical field
The present invention relates to technical field of concrete additives, be specifically related to a kind of anti-chamotte mould polycarboxylic acid slump retaining agent preparation and
Method.
Technical background
Since polycarboxylate water-reducer starts application at home, its development is the rapidest.Particularly polycarboxylate water-reducer
It is designated as the concrete admixture that railway engineering is special, greatly facilitates popularization and the application of polycarboxylate water-reducer especially.
Compared with traditional water reducer, polycarboxylate water-reducer has more advantage, and as volume is low, water-reducing rate is high, and adaptability is preferable.But
During practical engineering application, current existing polycarboxylate water-reducer shows some problems.Mainly former along with concrete
The fluctuation of material quality, as cement change, the clay content etc. of sandstone cause the service behaviour of concrete can show obvious rising
Volt, wherein shows particularly evident in terms of slump-loss.The method of such issues that solve at present is mainly joined by adjustment
Composition and division in a proportion, use increase polycarboxylate water-reducer consumption or use retarder slow setting, but these measures or operation on the most numerous
Trivial, or cost increases, or it is easily caused accident.Exploitation one really has adaptability and workability and to concrete
The material quality insensitive sustained-release polycarboxylic water reducer of fluctuation seems the most urgent and important.
Patent CN103641959A discloses a kind of sustained-release polycarboxylic water reducer preparation and method, the poly-carboxylic of this spacetabs type
Acid water reducer be by polyoxyethylene ether, acrylic acid and methyl methacrylate be polymerization monomer, mercaptoethanol as chain-transferring agent,
It is polymerized under the conditions of 80 DEG C and obtains.This sustained-release polycarboxylic water reducer described in invention needs high temperature polymerization, and production cost is higher,
Obvious effect is not had for the concrete that clay content is bigger.
Summary of the invention
It is an object of the invention to the defect for prior art, it is provided that the preparation of a kind of anti-chamotte mould polycarboxylic acid slump retaining agent and
Method.
The present invention, from the chemical constitution of high performance water reducing agent of polyocarboxy acid and the mechanism of action, uses macromolecular design former
Reason, with isopentene group polyoxyethylene ether (TPEG), acrylic acid (AA), maleic anhydride (MA), 2-(Acryloyloxy)ethanol or acrylic acid hydroxyl
Propyl ester primary raw material constitutes slow-releasing system, uses the chain-transferring agent of novel phosphorus-containing acid groups as anti-mud component, finally giving property
The anti-chamotte mould polycarboxylic acid slump retaining agent that energy is excellent.
The anti-chamotte mould polycarboxylic acid slump retaining agent that the present invention provides, by following raw material according to percentage by weight: unsaturated polyoxy second
Alkene ether monomer is 50-75%, and acrylic acid is 4-8%, maleic anhydride be 6-12%, 2-(Acryloyloxy)ethanol or Hydroxypropyl acrylate be 11-
20%, chain-transferring agent is 0.5-3.0%, and initiator amount is 0.1-5%, and initiation auxiliary agent is 0.01-2%.
Described unsaturated polyoxyethylene ether is isopentyl polyoxyethylene ether, and mean molecule quantity is 2400.
Described chain-transferring agent is one or more in dibastic sodium phosphate, sodium dihydrogen phosphate, tertiary sodium phosphate, sodium hypophosphite.
Described initiator is one or both in Ammonium persulfate., potassium peroxydisulfate or hydrogen peroxide (30%).
Described initiation auxiliary agent is one or more in L-AA, sodium formaldehyde sulfoxylate sodium sulfite, sodium sulfite.
The content of described 2-(Acryloyloxy)ethanol is 98%.
The content of described Hydroxypropyl acrylate is 98%.
Present invention also offers the preparation method of above-mentioned anti-chamotte mould polycarboxylic acid slump retaining agent, comprise the following steps:
(1) acrylic acid, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate are dissolved in deionized water that to be made into dropping liquid A material standby, will draw
Send out auxiliary agent be dissolved in deionized water be made into dropping liquid B material standby, initiator is dissolved in water be made into C material standby；
(2) add unsaturated polyethenoxy ether class monomer in a reservoir and deionized water stirs and makes it dissolve, add maleic acid
Acid anhydride stirring and dissolving, dropping initial temperature is 25-30 DEG C, adds chain-transferring agent and stirs 10 minutes, adds initiator C and expects stirring 10
Minute, in end liquid, at the uniform velocity drip A material simultaneously and B expects；
(3) A gob adds 1.5-3 hour, and B gob adds 2-3.5 hour, then is incubated 1 hour；
(4) adding sodium hydroxide solution regulation reacting solution pH value is 6-7, obtains the polycarboxylate water-reducer that solid content is 40-45%.
The present invention uses lower temperature synthesis technique, dropping process without heating, to considerably reduce production cost.Use
Novel chain transfer agent, production process is more environmentally friendly, additionally, the chain-transferring agent phosphoric acid group that the present invention uses, anti-in concrete
Mud effect is obvious, has the slump holding capacity of excellence.
Detailed description of the invention
Acrylic acid described in Examples below, maleic anhydride, 2-(Acryloyloxy)ethanol, chain-transferring agent, initiator and initiation help
Agent is same batch technical grade.
Example 1:
Acrylic acid 4g, 2-(Acryloyloxy)ethanol 11g are dissolved in deionized water that to be made into dropping liquid A material standby, by chain-transferring agent time phosphorus
Hydrochlorate 1.1g and cause auxiliary agent VC0.45g be dissolved in deionized water be made into dropping liquid B material standby, by initiator hydrogen peroxide (30%)
1.4g be dissolved in water be made into C material standby.Isopentene group polyoxyethylene ether (TPEG) 155g and deionized water is added in 500ml container
110g stirs and makes it dissolve, and waits and adds maleic anhydride 3.2g stirring after fully dissolving, and dropping initial temperature to be dissolved is 25-30
DEG C, add chain-transferring agent and stir 10 minutes, add initiator C material stirring 10 minutes, at the uniform velocity drip in end liquid simultaneously A material and
B expects.A gob added 2 hours, and B gob adds 2.5 hours, insulation 1 hour；Adding sodium hydroxide solution regulation reaction solution PH
Value is 6-7, the most anti-chamotte mould polycarboxylic acid slump retaining agent.
Example 2:
Acrylic acid 6g, Hydroxypropyl acrylate 15g are dissolved in deionized water that to be made into dropping liquid A material standby, by chain-transferring agent time phosphorus
Hydrochlorate 1.5g and cause auxiliary agent VC0.6g be dissolved in deionized water be made into dropping liquid B material standby, by initiator hydrogen peroxide (30%) 2.8g
Be dissolved in water be made into C material standby.Isopentene group polyoxyethylene ether (TPEG) 170g and deionized water 120g is added in 500ml container
Stirring and make it dissolve, waiting and add maleic anhydride 5.3g stirring after fully dissolving, dropping initial temperature to be dissolved is 25-30 DEG C, adds
Enter chain-transferring agent to stir 10 minutes, add initiator C material stirring 10 minutes, in end liquid, at the uniform velocity drip A material simultaneously and B expects.A
Gob added 3 hours, and B gob adds 3.5 hours, insulation 1 hour；It is 6-adding sodium hydroxide solution regulation reaction solution pH value
7, the most anti-chamotte mould polycarboxylic acid slump retaining agent.
Example 3:
By acrylic acid 4.5g, 2-(Acryloyloxy)ethanol 8.6g, Hydroxypropyl acrylate 3.8g is dissolved in deionized water and is made into dropping liquid A material
Standby, by chain-transferring agent hypophosphites 1.2g and cause auxiliary agent VC0.85g be dissolved in deionized water be made into dropping liquid B material standby, will
Initiator hydrogen peroxide (30%) 3.2g be dissolved in water be made into C material standby.Isopentene group polyoxyethylene ether is added in 500ml container
(TPEG) 165g and deionized water 115g stirs and makes it dissolve, and waits and adds maleic anhydride 4.5g stirring after fully dissolving, to be dissolved
Dropping initial temperature is 25-30 DEG C, adds chain-transferring agent and stirs 10 minutes, adds initiator C material stirring 10 minutes, simultaneously to
At the uniform velocity drip A material in end liquid and B expects.A gob added 2.5 hours, and B gob adds 3.0 hours, insulation 1.5 hours；Adding hydrogen-oxygen
Changing sodium solution regulation reaction solution pH value is 6-7, the most anti-chamotte mould polycarboxylic acid slump retaining agent.
Application effect below by concrete test explanation embodiment 1～3:
Anti-chamotte mould polycarboxylic acid slump retaining agent
With reference to standard GB/T 8,076 2008 " concrete admixture " relevant regulations, adjust water consumption and make fresh concrete initial
The slump is (210 ± 10) mm, test material: Carnis Rapanae thomasianae P O42.5 cement；It is limited that permanent new material science and technology share built by Guizhou ferrum
Company (hereinafter referred to as Heng Fa company) water reducer: TJ-S5(is admittedly containing 40%) 60%+ anti-chamotte mould polycarboxylic acid slump retaining agent 40%.
Select the polycarboxylic acid slump retaining agent 1# of certain offshore company and the anti-chamotte mould polycarboxylic acid slump retaining agent of the present invention to experiment gained
Sample is tested, and the results are shown in Table 1 testing concrete performance result.
Table 1 testing concrete performance result
From above-mentioned concrete data it can be seen that the anti-chamotte mould polycarboxylic acid slump retaining agent of the present invention has superior slump retaining
Can, basic free of losses in 2-3 hour can be kept.
Claims (8)
1. an anti-chamotte mould polycarboxylic acid slump retaining agent, is characterized in that, this slump retaining agent is calculated in percentage by weight by following raw material: no
Saturated polyoxyethylene ether monomer is 50-75%, and acrylic acid is 4-8%, and maleic anhydride is 6-12%, 2-(Acryloyloxy)ethanol or acrylic acid
Hydroxypropyl acrylate is 11-20%, and chain-transferring agent is 0.5-3.0%, and initiator is 0.1-5%, and initiation auxiliary agent is 0.01-2%.
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, described unsaturated polyoxyethylene ether is different
Amyl group polyoxyethylene ether, mean molecule quantity is 2400.
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, described chain-transferring agent be dibastic sodium phosphate,
One or more in sodium dihydrogen phosphate, tertiary sodium phosphate, sodium hypophosphite.
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, described initiator is Ammonium persulfate., mistake
One or both in potassium sulfate or hydrogen peroxide (30%).
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, described initiation auxiliary agent is L-Vitamin C
One or more in acid, sodium formaldehyde sulfoxylate sodium sulfite, sodium sulfite.
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, the content of described 2-(Acryloyloxy)ethanol is
98%。
Anti-chamotte mould polycarboxylic acid slump retaining agent the most according to claim 1, is characterized in that, the content of described Hydroxypropyl acrylate is
98%。
8. a preparation method for anti-chamotte mould polycarboxylic acid slump retaining agent, is characterized in that, comprise the following steps:
(1) acrylic acid, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate are dissolved in deionized water that to be made into dropping liquid A material standby, will draw
Send out auxiliary agent be dissolved in deionized water be made into dropping liquid B material standby, initiator is dissolved in water be made into C material standby；
(2) add unsaturated polyethenoxy ether class monomer in a reservoir and deionized water stirs and makes it dissolve, add maleic acid
Acid anhydride stirring and dissolving, dropping initial temperature is 25-30 DEG C, adds chain-transferring agent and stirs 10 minutes, adds initiator C and expects stirring 10
Minute, in end liquid, at the uniform velocity drip A material simultaneously and B expects；
(3) A gob adds 1.5-3 hour, and B gob adds 2-3.5 hour, then is incubated 1 hour；
(4) adding sodium hydroxide solution regulation reacting solution pH value is 6-7, obtains the anti-chamotte mould polycarboxylic acids that solid content is 40-45% and protects
Collapse agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263545.0A CN105859979A (en) | 2016-04-26 | 2016-04-26 | Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof |
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| CN201610263545.0A CN105859979A (en) | 2016-04-26 | 2016-04-26 | Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof |
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Cited By (8)
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| CN107721233A (en) * | 2017-10-23 | 2018-02-23 | 南京建高新材料科技有限公司 | A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer |
| CN106366256B (en) * | 2016-09-13 | 2018-06-26 | 科之杰新材料集团有限公司 | A kind of preparation method of the anti-mud collapse protective poly-carboxylic acid water reducing agent of esters |
| CN108585590A (en) * | 2018-04-28 | 2018-09-28 | 武汉理工大学 | A kind of premixing mortar open hour adjusting control agent and preparation method thereof |
| CN108911561A (en) * | 2018-05-25 | 2018-11-30 | 湖北工业大学 | 2200 molecular weight polyether polycarboxylic acid slump retaining agents of one kind and preparation method |
| CN109400825A (en) * | 2018-11-28 | 2019-03-01 | 山西格瑞特建筑科技股份有限公司 | A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect |
| CN110713573A (en) * | 2019-09-18 | 2020-01-21 | 山东申鑫建材科技有限公司 | Method for synthesizing polycarboxylate superplasticizer slump-retaining mother liquor |
| CN113336466A (en) * | 2021-06-30 | 2021-09-03 | 苏州弗克技术股份有限公司 | Slump-retaining and mud-resisting stabilizing agent for concrete and mortar and preparation method thereof |
| CN114907528A (en) * | 2022-05-19 | 2022-08-16 | 广东建盛高新材料有限公司 | Anti-mud mother liquor and preparation method and application thereof |
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| CN108585590A (en) * | 2018-04-28 | 2018-09-28 | 武汉理工大学 | A kind of premixing mortar open hour adjusting control agent and preparation method thereof |
| CN108585590B (en) * | 2018-04-28 | 2020-11-17 | 武汉理工大学 | Premixed mortar opening time regulating agent and preparation method thereof |
| CN108911561A (en) * | 2018-05-25 | 2018-11-30 | 湖北工业大学 | 2200 molecular weight polyether polycarboxylic acid slump retaining agents of one kind and preparation method |
| CN109400825A (en) * | 2018-11-28 | 2019-03-01 | 山西格瑞特建筑科技股份有限公司 | A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect |
| CN110713573A (en) * | 2019-09-18 | 2020-01-21 | 山东申鑫建材科技有限公司 | Method for synthesizing polycarboxylate superplasticizer slump-retaining mother liquor |
| CN113336466A (en) * | 2021-06-30 | 2021-09-03 | 苏州弗克技术股份有限公司 | Slump-retaining and mud-resisting stabilizing agent for concrete and mortar and preparation method thereof |
| CN114907528A (en) * | 2022-05-19 | 2022-08-16 | 广东建盛高新材料有限公司 | Anti-mud mother liquor and preparation method and application thereof |
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Application publication date: 20160817 |