CN105542100A - High-performance water-reducing agent and preparation method thereof - Google Patents
High-performance water-reducing agent and preparation method thereof Download PDFInfo
- Publication number
- CN105542100A CN105542100A CN201510917349.6A CN201510917349A CN105542100A CN 105542100 A CN105542100 A CN 105542100A CN 201510917349 A CN201510917349 A CN 201510917349A CN 105542100 A CN105542100 A CN 105542100A
- Authority
- CN
- China
- Prior art keywords
- compound
- reducing agent
- formula
- performance water
- water reducing
- 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.)
- Granted
Links
Classifications
-
- 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
-
- 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
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/30—Condensation polymers of aldehydes or ketones
-
- 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
- C08G2/00—Addition polymers of aldehydes or cyclic oligomers thereof or of ketones; Addition copolymers thereof with less than 50 molar percent of other substances
- C08G2/18—Copolymerisation of aldehydes or ketones
- C08G2/26—Copolymerisation of aldehydes or ketones with compounds containing carbon-to-carbon unsaturation
-
- 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)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a high-performance water-reducing agent with a molecular structural formula as described in the specification. In the formula, R1, R2, R3, R4, R5 and R6 are H or alkyl groups with carbon numbers in a range of 1 to 4; and a, b and c are chain numbers of repetitive units. The high-performance water-reducing agent has a molecular weight of 20, 000, 000 to 30, 000, 000 and good adaptability to cement.
Description
Technical field
The present invention relates to technical field of concrete additives, more particularly, it relates to a kind of high-performance water reducing agent, also relates to and the preparation method of high-performance water reducing agent simultaneously.
Background technology
Concrete is basic material of construction, and along with the raising of China's construction criteria, high-strength high perdurable concrete is more universal and important, and as the concrete admixture of one of concrete component, particularly concrete high efficiency water reducing agent is widely used.Current water reducer mainly contains: naphthalene system, melamine series, and sulfamate system etc., shortcoming mainly comprises: the concrete viscosity of its preparation is large, pumping difficulties, unfavorable construction.
High efficiency water reducing agent water-reducing rate can reach more than 20%, mainly naphthalene system, melamine series and and sulfamate system etc.Naphthalene water reducer is that the current turnout of China is maximum, uses the widest high efficiency water reducing agent (accounting for more than 70% of water reducer consumption), is often used to prepare large fluidity, high-strength, high performance concrete.
The concrete slump loss of simple admixture naphthalene water reducer is very fast.Existing application number be 201310747129.4 Chinese patent disclose a kind of naphthalene system poly carboxylic acid anti-subsided water reducer, although solve this technical problem, but naphthalene water reducer and cement adaptability also need to improve, this is because the adaptability problem of cement and water reducer has become the difficult problem perplexing concreter author, affects the effect of admixture and applies.
Summary of the invention
For the deficiency that prior art exists, the object of the present invention is to provide a kind of high-performance water reducing agent, itself and cement have extraordinary adaptability, another object of the present invention is to the preparation method providing described high-performance water reducing agent.
For achieving the above object, the invention provides following technical scheme:
A kind of high-performance water reducing agent, its molecular structural formula is:
Wherein, R
1, R
2, R
3, R
4, R
5, R
6for H or carbon number are the alkyl of 1 ~ 4, a, b, c are the chain number of repeating unit, and molecular weight is 20,000,000 ~ 30,000,000.
The adaptability of cement and water reducer comprises three aspects: one, initialization (slump, divergence); Two, clear and definite saturation point whether is had; Three, loss of working performance situation.When cement and water reducer adapt to: water reducer can reach it self water-reducing rate under conventional volume, not segregation and excreting water phenomenon, it is corresponding less that the slump changes loss in time, to performances such as concrete intensity without negative impact; When being not suitable with: initial slump is little, slump-loss is fast, segregation, bleeding, and additive usage increases.
As the preferred embodiment of the present invention, the preparation method of described high-performance water reducing agent comprises the steps: the compound of the compound of the compound of structural formula I, formula II, formula II I, formaldehyde and solvent to add in reactor, add initiator, under pressure is 0.5MPa, in 100 ~ 110 DEG C of reactions 2 ~ 3 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6for H or carbon number are the alkyl of 1 ~ 4.
In method described above, pressure, the temperature and time of polycondensation have great impact to polymerization, are shown by lot of experiments, and in the present invention, the condition of polyreaction is most preferably condition.
As the preferred embodiment of the present invention, the mol ratio of the compound of the described compound of structural formula I, the compound of formula II and formula II I is 1: 0.5 ~ 1.5: 1.5 ~ 2.5.
As the preferred embodiment of the present invention, the compound of described structural formula I and the mol ratio of formaldehyde are: 1: 1.5 ~ 2.
As the preferred embodiment of the present invention, described solvent is at least one in methyl alcohol, ethanol, propyl alcohol.
As the preferred embodiment of the present invention, described initiator is at least one in sulfuric acid, ammonium sulfate, ammonium persulphate, sulfoxylic acid ammonium.
The beneficial effect that the present invention is compared to the prior art had:
1. the present invention's high-performance water reducing agent of adopting chiral molecules to prepare and cement have good adaptability;
2. the present invention adopts (R)-binaphthol derivative to prepare water reducer, has plurality of advantages, and this is because dinaphthol and derivative thereof are that a class does not contain chiral centre but has C
2the asymmetric compound of symmetry axis, dinaphthol and derivative thereof have rigid backbone but can with C
2symmetry axis overturns, different groups can be modified on different positions and molecular axis asymmetric but have the chiral configuration of high stability.Namely high-performance water reducing agent of the present invention has the stability of rigidity and height.
3. in addition, because (R)-binaphthol derivative has higher activity, so high-performance water reducing agent of the present invention and cement have better adaptability.
Accompanying drawing explanation
Fig. 1 is the building-up process of Compounds of structural formula I;
Fig. 2 is the nucleus magnetic hydrogen spectrum spectrogram of Compounds of structural formula I.
Embodiment
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.
Embodiment one:
High-effect water reducer described in the present embodiment adopts following methods to be prepared from:
The compound of the compound of the compound of structural formula I, formula II a, formula II Ia, formaldehyde and methyl alcohol are added in reactor, adds sulfuric acid as initiator, under pressure is 0.5MPa, in 110 DEG C of reactions 3 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6be H atom; The mol ratio of the compound of described structural formula I, the compound of formula II a, the compound of formula II Ia and formaldehyde is 1: 1: 1: 2.
Embodiment two:
High-effect water reducer described in the present embodiment adopts following methods to be prepared from:
The compound of the compound of the compound of structural formula I, formula II b, formula II Ib, formaldehyde and ethanol are added in reactor, adds ammonium sulfate as initiator, under pressure is 0.5MPa, in 100 DEG C of reactions 2 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6be-CH
3; The mol ratio of the compound of described structural formula I, the compound of formula II b, the compound of formula II Ib and formaldehyde is 1: 0.5: 1.5: 1.5.
Embodiment three:
High-effect water reducer described in the present embodiment adopts following methods to be prepared from:
The compound of the compound of the compound of structural formula I, formula II c, formula II Ic, formaldehyde and n-propyl alcohol are added in reactor, add ammonium persulphate as initiator, under pressure is 0.5MPa, in 105 DEG C of reactions 2.5 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6be-CH
2cH
2cH
2cH
3; The mol ratio of the compound of described structural formula I, the compound of formula II c, the compound of formula II Ic and formaldehyde is 1: 1.5: 1.5: 1.8.
Embodiment four:
High-effect water reducer described in the present embodiment adopts following methods to be prepared from:
The compound of the compound of the compound of structural formula I, formula II d, formula II Id, formaldehyde and n-propyl alcohol are added in reactor, add sulfoxylic acid ammonium as initiator, under pressure is 0.5MPa, in 110 DEG C of reactions 2.5 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6be-CH
2cH
3; The mol ratio of the compound of described structural formula I, the compound of formula II d, the compound of formula II Id and formaldehyde is 1: 1.5: 2.5: 2.
Embodiment five:
High-effect water reducer described in the present embodiment adopts following methods to be prepared from:
The compound of the compound of the compound of structural formula I, formula II a, formula II Id, formaldehyde and Virahol are added in reactor, add ammonium persulphate as initiator, under pressure is 0.5MPa, in 110 DEG C of reactions 2.5 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3be H, R
4, R
5, R
6be-CH
2cH
3; The mol ratio of the compound of described structural formula I, the compound of formula II a, the compound of formula II Id and formaldehyde is 1: 1.25: 1.75: 2.
Further, high-performance water reducing agent of the present invention and P.O42.5 cement adaptability are studied.
Comparative group one: do not add the concrete that any water reducer makes,
Comparative group two: adopt in prior art and be added with the concrete that massfraction is the naphthalene water reducer making of 0.4%, wherein, naphthalene water reducer is buied by Guangdong Redwall New Materials Co., Ltd..
Experimental group one: the high-performance water reducing agent adopting embodiment one to obtain replaces the concrete that the naphthalene water reducer in comparative group makes.
Experimental group two: the concrete adopting the high-performance water reducing agent that obtains of embodiment two to replace the naphthalene water reducer in comparative group to make, wherein, this two kinds of water reducers identical in quality.
Experimental group three: the concrete adopting the high-performance water reducing agent that obtains of embodiment three to replace the naphthalene water reducer in comparative group to make, wherein, this two kinds of water reducers identical in quality.
Experimental group four: the concrete adopting the high-performance water reducing agent that obtains of embodiment four to replace the naphthalene water reducer in comparative group to make, wherein, this two kinds of water reducers identical in quality.
Experimental group five: the concrete adopting the high-performance water reducing agent that obtains of embodiment five to replace the naphthalene water reducer in comparative group to make, wherein, this two kinds of water reducers identical in quality.
The concrete of table 1 comparative group and experimental group one to five and the adaptive detection result of P.O42.5 cement
Can be found out by the detected result of table 1: high-effect water reducer of the present invention has high water reducing rate, low bleeding rate, the high slump and high divergence hold facility, occurs without segregation phenomenon, add concrete resistance to compression degree simultaneously.
The saturation point research of the high-performance water reducing agent that table 2 adopts embodiment one to obtain and different cement
| Cement type | Saturation point (%) |
| Portland pozzolana cement | 0.6 |
| Portland fly ash cement | 0.7 |
| Moderate-heat portland cement | 0.5 |
| Low-heat slag salt cement | 0.4 |
| Ordinary Portland cement | 0.4 |
| Sulfate resisting Portland cement | 0.8 |
| Masonry cement | 0.5 |
| Oil well cement | 0.6 |
| Portland blast furnace slag cement | 0.7 |
| Composite Portland cement | 0.4 |
Can be found out by the detected result of table 2: the high-performance water reducing agent that embodiment one obtains and different types of cement all have clear and definite saturation point.
In sum, high-performance water reducing agent of the present invention and cement have good adaptability.
The above is only the preferred embodiment of the present invention, protection scope of the present invention be not only confined to above-described embodiment, and all technical schemes belonged under thinking of the present invention all belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. a high-performance water reducing agent, is characterized in that, its molecular structural formula is:
Wherein, R
1, R
2, R
3, R
4, R
5, R
6for H or carbon number are the alkyl of 1 ~ 4, a, b, c are the chain number of repeating unit, and molecular weight is 20,000,000 ~ 30,000,000.
2. high-performance water reducing agent according to claim 1, it is characterized in that, the preparation method of described high-performance water reducing agent comprises the steps: the compound of the compound of the compound of structural formula I, formula II, formula II I, formaldehyde and solvent to add in reactor, add initiator, under pressure is 0.5MPa, in 100 ~ 110 DEG C of reactions 2 ~ 3 hours, obtain described high-performance water reducing agent;
Wherein, R
1, R
2, R
3, R
4, R
5, R
6for H or carbon number are the alkyl of 1 ~ 4.
3. high-performance water reducing agent according to claim 2, is characterized in that: the mol ratio of the compound of the described compound of structural formula I, the compound of formula II and formula II I is 1: 0.5 ~ 1.5: 1.5 ~ 2.5.
4. according to claim 2, it is characterized in that: the compound of described structural formula I and the mol ratio of formaldehyde are: 1: 1.5 ~ 2.
5. according to claim 2, it is characterized in that: described solvent is at least one in methyl alcohol, ethanol, propyl alcohol.
6. according to claim 2, it is characterized in that: described initiator is at least one in sulfuric acid, ammonium sulfate, ammonium persulphate, sulfoxylic acid ammonium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510917349.6A CN105542100B (en) | 2015-12-10 | 2015-12-10 | A kind of high-performance water reducing agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510917349.6A CN105542100B (en) | 2015-12-10 | 2015-12-10 | A kind of high-performance water reducing agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105542100A true CN105542100A (en) | 2016-05-04 |
| CN105542100B CN105542100B (en) | 2017-10-20 |
Family
ID=55821688
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510917349.6A Expired - Fee Related CN105542100B (en) | 2015-12-10 | 2015-12-10 | A kind of high-performance water reducing agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105542100B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048844A (en) * | 1989-07-15 | 1991-01-30 | 中山大学 | Opticity 1,1 '-preparation method of union-2-naphthol |
| US6302955B1 (en) * | 1998-11-04 | 2001-10-16 | W. R. Grace & Co.-Conn. | Composition for improving freeze/thaw durability of masonry containing fatty acid-based efflorescence control agents |
| CN1887776A (en) * | 2005-06-30 | 2007-01-03 | 东莞市寮步新型建筑材料厂 | Prepn of naphthalene water reducing agent |
| WO2007135935A1 (en) * | 2006-05-22 | 2007-11-29 | Toagosei Co., Ltd. | Dispersing agent |
| CN101851323A (en) * | 2010-05-28 | 2010-10-06 | 浙江五龙化工股份有限公司 | Multi-branched polycarboxylic water reducer with excellent function of slump protection and preparation method thereof |
| CN103804611A (en) * | 2013-12-27 | 2014-05-21 | 江苏创基新材料有限公司 | Method for preparing polycarboxylate high-efficiency water reducing agent |
| CN103804620A (en) * | 2013-12-30 | 2014-05-21 | 广东红墙新材料股份有限公司 | Naphthalene polycarboxylate slump-keeping water reducing agent and preparation method thereof |
-
2015
- 2015-12-10 CN CN201510917349.6A patent/CN105542100B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048844A (en) * | 1989-07-15 | 1991-01-30 | 中山大学 | Opticity 1,1 '-preparation method of union-2-naphthol |
| US6302955B1 (en) * | 1998-11-04 | 2001-10-16 | W. R. Grace & Co.-Conn. | Composition for improving freeze/thaw durability of masonry containing fatty acid-based efflorescence control agents |
| CN1887776A (en) * | 2005-06-30 | 2007-01-03 | 东莞市寮步新型建筑材料厂 | Prepn of naphthalene water reducing agent |
| WO2007135935A1 (en) * | 2006-05-22 | 2007-11-29 | Toagosei Co., Ltd. | Dispersing agent |
| CN101851323A (en) * | 2010-05-28 | 2010-10-06 | 浙江五龙化工股份有限公司 | Multi-branched polycarboxylic water reducer with excellent function of slump protection and preparation method thereof |
| CN103804611A (en) * | 2013-12-27 | 2014-05-21 | 江苏创基新材料有限公司 | Method for preparing polycarboxylate high-efficiency water reducing agent |
| CN103804620A (en) * | 2013-12-30 | 2014-05-21 | 广东红墙新材料股份有限公司 | Naphthalene polycarboxylate slump-keeping water reducing agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105542100B (en) | 2017-10-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102391435B (en) | Slump-retaining polycarboxylic acid type water reducing agent and preparation method thereof | |
| CN105924592B (en) | Viscosity-reducing polycarboxylic acid water reducer and preparation method thereof | |
| WO2022056975A1 (en) | Preparation method for polycarboxylic acid admixture for use in machine-made sand concrete | |
| CN104031216A (en) | Polyether-amide type polycarboxylic high-efficiency water reducer and preparation method thereof | |
| CN104817663A (en) | Preparation method of polycarboxylate water-reducer capable of inhibiting side-effect of montmorillonite and polymeric monomer | |
| CN101200355A (en) | Polycarboxylic acids series water reducer and method for making same | |
| CN101830663A (en) | Collapse protective poly-carboxylic acid water reducing agent and preparation method thereof | |
| CN104628293A (en) | Early strength type polycarboxylic acid water reducing agent, preparation method and use method thereof | |
| CN107815300A (en) | A kind of oily sludge profile control blocking agent and preparation method thereof | |
| CN102807653B (en) | Co-polycarboxylic acid high efficiency water reducer capable of compounding with naphthalene formaldehyde water reducer and method for preparing same | |
| CN109776785B (en) | Anti-mud additive for concrete and preparation method and application thereof | |
| CN103319650A (en) | Phosphoaluminate cement system fluid loss additive and preparation method thereof | |
| CN108529918B (en) | Modified aluminum-silicon particles and modifier thereof | |
| CN104151477A (en) | Preparation method of amphoteric polycarboxylate clay inhibitor | |
| CN103641963B (en) | A kind of poly carboxylic acid series water reducer and preparation method thereof be applicable to containing mud aggregate | |
| CN101781101B (en) | High-performance polycarboxylate based polyether water reducing agent | |
| CN103693885B (en) | A kind of polycarboxylate superplasticizer composition and uses thereof | |
| CN105542100A (en) | High-performance water-reducing agent and preparation method thereof | |
| CN103011674B (en) | Polyether amine modified polycarboxylate-type concrete slump retaining agent and preparation method thereof | |
| CN102408528B (en) | Preparation method for polycarboxylic acid water reducer with strong adaptability | |
| CN111484270A (en) | Ultra-long-distance concrete pumping agent | |
| CN102173639A (en) | Polycarboxylate-based water-reducing agent with effect of inhibiting corrosion of steel bars and preparation method thereof | |
| CN105565700A (en) | Early strength waterproof agent for ordinary Portland cement | |
| CN102173641A (en) | Super-efficient carboxylic acid water reducer without thermal energy consumption | |
| CN101357832B (en) | Comb polymer anti-foaming agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171020 Termination date: 20181210 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |