CN109133698A - A kind of water-reducing agent and preparation method thereof improving strength cement-based grouting material high temperature performance - Google Patents
A kind of water-reducing agent and preparation method thereof improving strength cement-based grouting material high temperature performance Download PDFInfo
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- CN109133698A CN109133698A CN201810951619.9A CN201810951619A CN109133698A CN 109133698 A CN109133698 A CN 109133698A CN 201810951619 A CN201810951619 A CN 201810951619A CN 109133698 A CN109133698 A CN 109133698A
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- water
- reducing agent
- preparation
- abietyl modified
- modified organic
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—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
- 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
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- 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)
- General Chemical & Material Sciences (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of water-reducing agent for improving strength cement-based grouting material high temperature performance is provided, the raw material for preparing of the water-reducing agent includes: prenyl polyethylene glycol, acrylamido (methyl) propane sulfonic acid, methallylsulfonic acid sodium, acrylic acid, Abietyl modified organic siliconresin, acrylamide.Gained water-reducing agent is used for grouting material, significantly improves the high and low temperature resistance of grouting material, buckle resistance energy.
Description
Technical field
The present invention relates to a kind of additives of strength cement-based grouting material, more particularly to a kind of Abietyl modified silicone-modified water
Mud base grouting material and preparation method thereof.
Background technique:
The performance of strength cement-based grouting material is always determine building and Pavement Performance intensity and high and low temperature resistance one
The cracking on a importance, building and road surface is most related with the thermal expansion and cold contraction effect of cement-based material, is especially assembling
In formula building, sleeve grouting connection accounts for precast concrete assembled architecture vertically connects market 80% or more, and sleeve
Important composition material of the grouting material as reinforced bar sleeve grouting connection, performance determine connecting portion reliability of structure and matter
Stability is measured, it is even more so in the biggish northern area of Temperature Difference Ratio.
Fine silica powder (silicon ash) has stronger hydrophily and activity, in water easy formation-Si-OH, through dry de-
Water is built bridge, and forms siloxanes [- Si-O-Si-] reticular structure, in siloxane network, silicon oxygen bond not only high temperature resistant, and with
The raising of temperature, intensity are continuously improved, in addition, fine silica powder has stronger activity, form colloidal particle in water, are added
Dispersing agent appropriate, the ion that the two dissociates meet, because of surface charge on the contrary, when micelle surface electrostatic repulsion is less than its gravitation
When, Coagulating binding occurs, enhances mobility, pours performance to improve.
Include a carboxylic acid and two double bonds in the structure of rosin, has anti-corrosion, moisture-proof, insulation, bonding, emulsification etc. excellent
Performance, Abietyl modified organic siliconresin are modified using rosin, and introducing in organic siliconresin has the hydrogen of certain rigidity luxuriant and rich with fragrance
Ring structure has many advantages, such as heat resistance, adhesive force, durable, weather-proof, but it is also water-fast simultaneously.
Summary of the invention
Present applicant introduces creatively in the preparation process of carboxylic acid water reducer with heat-resisting, weather-proof, bullet
Property it is good the advantages that, but its also water-fast Abietyl modified organic siliconresin, gained water-reducing agent are used for grouting material simultaneously, significantly improve
The high and low temperature resistance of grouting material, buckle resistance energy.
Specifically, the application provides a kind of water-reducing agent, and the raw material for preparing of the water-reducing agent includes: the poly- second two of prenyl
Alcohol, acrylamido (methyl) propane sulfonic acid, methallylsulfonic acid sodium, acrylic acid, Abietyl modified organic siliconresin, acryloyl
Amine.
Preferably, aforementioned water-reducing agent includes the raw material of following parts by weight:
It is preferred that the molecular weight regulator is methylpropene sodium sulfonate, mercaptopropionic acid or combinations thereof, the initiator was
Oxide or hydrogen peroxide.In addition, aforementioned water-reducing agent prepares raw material this further includes water, dosage is usually the poly- second two of isoprene
0.5-1.5 times of alcohol further includes if necessary pH adjusting agent, and dosage makes the pH value of gained water-reducing agent between 6-8.
It is preferred that the structural formula of the Abietyl modified organic siliconresin is as shown in following formula I:
The preparation method of the Abietyl modified organic siliconresin includes the following steps:
(1) tetramethyl divinyl disiloxane polymerize with octamethylcy-clotetrasiloxane, generates the poly- silicon oxygen of ethenyl blocking
The polymer of alkane；(2) polymer of vinyl terminated polysiloxane is reacted with rosin progress Diels-Alder generates the rosin
Modified organic silicone resin.
More specifically, in the preparation method of the Abietyl modified organic siliconresin,
(1) polymerization reaction of tetramethyl divinyl disiloxane and octamethylcy-clotetrasiloxane (D4) are according to chemical reaction
It is added in reaction kettle after molar ratio stoichiometry in equation, stirring is started, according to the amount of the 1-15% of reactant gross mass
Catalyst is added, is being warming up to 60-120 DEG C, normal pressure heat-insulating is stirred to react 6-10 hours, then is down to 50 DEG C or less removing catalysis
Agent, pressure 133Kpa following temperature in 120-160 DEG C removing low molecule 5-8 hours, obtain the poly- of intermediate vinyl sealing end
Siloxanes, low-molecular material are reusable.
The polymerisation catalysts are the concentrated sulfuric acid or strongly acidic styrene's resin.
(2) the Diels-Alder addition reaction of vinyl terminated polysiloxane and rosin
Vinyl terminated polysiloxane, rosin is anti-according to being added after the molar ratio stoichiometry in chemical equation
It answers in kettle, opens stirring, add the catalyst for accounting for rosin quality 0.1~0.5%, be warming up at 170-220 DEG C and carry out
Diels-Alde addition reaction is evacuated to 3mmHg after reaction 6-8 hours, removes low boiling impurity, and product is cooled to room temperature,
The addition product of vinyl terminated polysiloxane and rosin is obtained, i.e., the described Abietyl modified organic siliconresin.
The mole ratio of vinyl terminated polysiloxane and rosin is 4.5~2.5: 1.
The rosin, abietic acid content, which is not more than, is equal to 85%；
The ethylene terminated polysiloxane, contents of ethylene are more than or equal to 10%；
Catalyst used in the Diels-Alder addition reaction is for phosphoric acid or hydroquinone or to methylbenzene sulphur
Acid.
The preparation method of aforementioned water-reducing agent, includes the following steps,
One, prepared by bottom material
By deionized water, prenyl polyethylene glycol, 2- acrylamide group methyl propane sulfonic acid, Abietyl modified organosilicon tree
Rouge, acrylamide, the mixing of methallylsulfonic acid sodium, and temperature is made to reach 20-30 DEG C, hydrogen peroxide is then added, bottom is made
Material；
Two, the preparation of dropping material A
Acrylic acid is dissolved in deionized water, acrylic acid aqueous solution namely dropping material A is prepared；
Three, the preparation of dropping material B
Methylpropene sodium sulfonate is add to deionized water, the dropping material B is made；
Four, prepared by water-reducing agent finished product
Stirring so that in bottom material each component be uniformly mixed, start simultaneously at be added dropping material A and dropping material B, be added dropwise with
Afterwards, continue to stir, increase temperature to 40-45 DEG C, constant temperature aging 1-3 hours, sodium hydroxide solution is then added and is neutralized, does
It is dry.
A kind of purposes of Abietyl modified organic siliconresin in water-reducing agent preparation, the knot of the Abietyl modified organic siliconresin
Structure formula is as follows:
Specific embodiment
The preparation embodiment 1 of Abietyl modified organic siliconresin
(1) 10.0kg tetramethyl divinyl disiloxane, 50kg octamethylcy-clotetrasiloxane (D4) is taken to be placed in reaction kettle
In, blender is started, while the 3.0kg concentrated sulfuric acid is added and makees catalyst, is heated to 60 DEG C, it is small that normal pressure heat-insulating is stirred to react 6
When, then be down to 50 DEG C or less removing filtering agents, pressure 133Kpa following temperature in 120-160 DEG C removing low molecule 5-8 hours,
The polysiloxanes of intermediate vinyl sealing end is obtained, low-molecular material is reusable.
(2) after reaction by above-mentioned (1), 40kg rosin and 0.08kg hydroquinone catalyst is added, is warming up to 200 DEG C
Lower progress Diels-Alder addition reaction is evacuated to 3mmHg after reaction 6 hours, removes low boiling impurity, and product is cooled to
Room temperature obtains the Abietyl modified organic siliconresin.
Water-reducing agent prepares embodiment 1
One, prepared by bottom material
By 30 kilograms of deionized waters, 60 kilograms of prenyl polyethylene glycol (molecular weight 2000), 0.2 kilogram of 2- acryloyl
Aminomethyl propane sulfonic acid, 2 kilograms of Abietyl modified organic siliconresins, 0.3 kilogram of acrylamide, 0.35 kilogram of methylpropene sodium sulfonate
Mixing, and temperature is made to reach 22 DEG C, 0.25 kilogram of hydrogen peroxide of 50% is then added, bottom material is made；
Two, the preparation of dropping material A
3 kilograms of acrylic acid are dissolved in 15 kilograms of deionized waters, acrylic acid aqueous solution namely dropping material A is prepared；
Three, the preparation of dropping material B
0.3 kilogram of methylpropene sodium sulfonate is added in 5 kilograms of deionized waters, the dropping material B is made；
Four, prepared by water-reducing agent finished product
Stirring so that in bottom material each component be uniformly mixed, start simultaneously at dropping material A and dropping material B, after being added dropwise, after
Continuous stirring increases temperature to 42 DEG C, constant temperature aging 1-3 hours, the sodium hydroxide solution that 1.2 kilograms of concentration are 50% is then added
It is neutralized, it is dry.
Water-reducing agent prepares embodiment 2
Other steps are same as Example 1, the difference is that 2 kilograms of Abietyl modified organic siliconresins are not added in bottom material,
But 3 kilograms of acrylic acid are added, 3 kilograms of acrylic acid are added without in dropping material A, and 2 kilograms of Abietyl modified organic siliconresins are added.
Water-reducing agent prepares embodiment 3
Other conditions are same as Example 1, the difference is that the additional amount of Abietyl modified organic siliconresin is 0.4 thousand
Gram.
Water-reducing agent prepares embodiment 4
Other conditions are same as Example 1, the difference is that the additional amount of Abietyl modified organic siliconresin is 5 kilograms.
Water-reducing agent prepares embodiment 5
Other conditions are same as Example 1, the difference is that the additional amount of Abietyl modified organic siliconresin is 0.8 thousand
Gram.
Water-reducing agent prepares embodiment 6
Other conditions are same as Example 1, the difference is that the additional amount of Abietyl modified organic siliconresin is 3 kilograms.
Water-reducing agent comparative example 1
Other steps are same as Example 1, the difference is that only be added without in the preparation of bottom material it is Abietyl modified organic
Silicone resin.
Water-reducing agent comparative example 2
Other steps are same as Example 2, the difference is that only be added without in the preparation of dropping material A it is Abietyl modified organic
Silicone resin.
Application Example 1
A kind of strength cement-based grouting material, preparation process include that 8 parts by weight are prepared polycarboxylic acids diminishing obtained in embodiment 1
Agent, 1.5 parts by weight of lemon acid are firstly added stirrer for mixing, then by the strong of the mixture being mixed to get and 550 parts by weight
Quartz sand, the 1.5 parts sulfuric acid lithiums of ordinary portland cement, 300 parts by weight that degree grade is 42.5 are added in batch mixer
Mixing obtains grouting material dry powder through being mixed.
By grouting material dry powder obtained above, the water of 100 parts by weight is added, is placed in mortar mixer stirring, is in the milk
Material 1.
Application Example 2-6
Other conditions are same as Example 1, the difference is that only and correspondingly obtained in water-reducing agent preparation embodiment 2-6
Water-reducing agent replace water-reducing agent preparation embodiment 1 obtained in water-reducing agent, respectively obtain grouting material 2-6.
Comparison study example 1-2
Other conditions are same as Example 1, the difference is that only and are prepared into using in water-reducing agent comparative example 1-2
The water-reducing agent arrived replaces water-reducing agent obtained in water-reducing agent preparation embodiment 1, obtains comparison grouting material I and II respectively.
According to GB/T25181-2010 " premixing mortar ", JG/T985-2005 " ground cement-based self-leveling mortar ",
The regulation of JGJ/T70-2009 " building mortar basic performance tests method standard " is detected.The performance data of grouting material is shown in Table
1:
The performance of 1 Application Example of table and the Comparison study example grouting material
Claims (7)
1. a kind of water-reducing agent for improving strength cement-based grouting material high temperature performance, the raw material for preparing of the water-reducing agent includes: isoamyl two
Alkenyl polyethylene glycol, acrylamido (methyl) propane sulfonic acid, methallylsulfonic acid sodium, acrylic acid, Abietyl modified organosilicon tree
Rouge, acrylamide.
2. water-reducing agent described in claim 1, the raw material including following parts by weight:
3. water-reducing agent as claimed in claim 2, the molecular weight regulator is methylpropene sodium sulfonate, mercaptopropionic acid or its group
It closes, the initiator is peroxide or hydrogen peroxide.
4. the described in any item water-reducing agents of claim 1-3, the structural formula of the Abietyl modified organic siliconresin such as following formula I institute
Show:
5. water-reducing agent as claimed in claim 4, wherein the preparation method of the Abietyl modified organic siliconresin includes the following steps:
(1) tetramethyl divinyl disiloxane polymerize with octamethylcy-clotetrasiloxane, generates vinyl terminated polysiloxane
Polymer；(2) polymer of vinyl terminated polysiloxane and rosin carry out Diels-Alder react generation described Abietyl modified
Organic siliconresin.
6. the described in any item water-reducing agents of claim 1-5, the preparation method of the water-reducing agent include the following steps,
One, prepared by bottom material
By deionized water, prenyl polyethylene glycol, 2- acrylamide group methyl propane sulfonic acid, Abietyl modified organic siliconresin,
Acrylamide, the mixing of methallylsulfonic acid sodium, and temperature is made to reach 20-30 DEG C, hydrogen peroxide is then added, bottom material is made；
Two, the preparation of dropping material A
Acrylic acid is dissolved in deionized water, acrylic acid aqueous solution namely dropping material A is prepared；
Three, the preparation of dropping material B
Methylpropene sodium sulfonate is add to deionized water, the dropping material B is made；
Four, prepared by water-reducing agent finished product
Stirring so that in bottom material each component be uniformly mixed, start simultaneously at be added dropping material A and dropping material B, after being added dropwise, after
Continuous stirring increases temperature to 40-45 DEG C, constant temperature aging 1-3 hours, and sodium hydroxide solution is then added and is neutralized, dry.
7. a kind of purposes of Abietyl modified organic siliconresin in water-reducing agent preparation, the structure of the Abietyl modified organic siliconresin
Formula is as follows:
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| CN108329836A (en) * | 2018-01-31 | 2018-07-27 | 枞阳县三金颜料有限责任公司 | A kind of organic siliconresin that rosin resin is modified |
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2018
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