CN108641037A - A kind of Concrete synergist and preparation method thereof of phosphorous acid groups - Google Patents
A kind of Concrete synergist and preparation method thereof of phosphorous acid groups Download PDFInfo
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- CN108641037A CN108641037A CN201810625131.7A CN201810625131A CN108641037A CN 108641037 A CN108641037 A CN 108641037A CN 201810625131 A CN201810625131 A CN 201810625131A CN 108641037 A CN108641037 A CN 108641037A
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- concrete
- acid groups
- phosphorous acid
- concrete synergist
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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
- C08F230/00—Copolymers 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
- C08F230/02—Copolymers 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
-
- 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
- C04B24/243—Phosphorus-containing polymers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention provides a kind of Concrete synergist and preparation method thereof of phosphorous acid groups, and its step are as follows：(1) Tea Saponin, isopropyl alkenyl phosphoric acid, methacryl amido propyl ester trimethyl ammonium chloride and water are added in retort, open and stirs and heat up；(2) start that the initiator solution that mass percent concentration is 1~10% is added dropwise after being warming up to 60 DEG C~120 DEG C, this initiator solution is formulated by the initiator and the part water, time for adding control temperature at 3~5 hours, dropwise addition is controlled at 90 DEG C~120 DEG C；(3) inorganic base holding temperature is added after dripping, and the reaction was continued 1~3 hour, and cooling discharge is to get the Concrete synergist.
Description
Technical field
The invention belongs to field of fine chemical, more particularly to the Concrete synergist of a kind of phosphorous acid groups and its preparation side
Method.
Background technology
Concrete becomes current whole world dosage maximum and the most wide material of use scope because of having the advantages that a series of
Material.Research data shows have the cement there are about 20%~30% to be not engaged in hydration reaction in concrete under conventional environment, only
The fine filling effect that gathers materials is played, strength of cement cannot be effectively played, causes the significant wastage of resource.On the other hand, due to
The Influencing Mechanism of different Water-reducing Admixtures To Cements absorption etc. is different, after adding to a certain extent, is difficult to recur to concrete
Effect, economy and application property are difficult to be protected.How new concrete admixture is developed to solve the above problems, it will be rich
The basic performance and intensity that can ensure concrete while remaining cement saves again have Concrete Enterprises particularly significant
Realistic meaning.
Concrete synergist is the dispersion degree by improving cement granules and mineral fine aggregate, is excited to the maximum extent each
The effect of unit cement molecule, excites the performance of water-reducing agent.Since cement granules are more dispersed, the hydration of cement is more abundant,
That is most cement granules are after He Shui, sand, stone etc. are sufficiently mixed stirring, and then the other materials of energy and its periphery
(such as water-reducing agent) comes into full contact with and reacts, and to enhance the comprehensive performance of concrete, and saves original water in concrete
Mud dosage.
The present invention provides a kind of Concrete synergists of phosphorous acid groups.This Concrete synergist is a kind of novel mixes
Solidifying soil additive, for for Medium and low intensity grade concrete, cement consumption can be reduced, while can guarantee again its workability,
Intensity and durability have a wide range of application prospect.
Invention content
Therefore, for the above content, the present invention provides a kind of Concrete synergist and preparation method thereof of phosphorous acid groups,
The Concrete synergist is a kind of novel concrete admixture, for that for Medium and low intensity grade concrete, can reduce water
Mud dosage, while can guarantee its workability, intensity and durability again, there is a wide range of application prospect.
In order to achieve the above objectives, the present invention is achieved by the following technical solutions：A kind of concrete of phosphorous acid groups
Synergist, the raw material components mainly matched by following mass fractions are made：
The initiator is the mixture of one or more of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate.
The inorganic base is the mixture of one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
A kind of preparation method of the Concrete synergist of phosphorous acid groups, is achieved by the steps of：
(1) Tea Saponin, isopropyl alkenyl phosphoric acid, methacryl amido propyl ester trimethyl ammonium chloride and water are added to retort
In, it opens and stirs and heat up；
(2) start that the initiator solution that mass percent concentration is 1~10% is added dropwise after being warming up to 60 DEG C~120 DEG C,
This initiator solution is formulated by the initiator and the part water, time for adding control temperature at 3~5 hours, dropwise addition
Degree control is at 90 DEG C~120 DEG C；
(3) inorganic base holding temperature is added after dripping, and the reaction was continued 1~3 hour, and cooling discharge is to get the concrete
Synergist.
Compared with prior art, the present invention has following remarkable result：
1, it is basic raw material with Tea Saponin, a variety of modifying agent is added, it is modified, to introduce phosphate group, amide
Group, ester group etc. improve the performance of product.
2, the product is nontoxic, using not limited by season and region, is readily transported and stores；
3, the product processes are simple, mild condition, and production process charging, condition are all easy to control, entire technique mistake
Journey is discharged without " three wastes ", is a kind of environmental type, pollution-free cleanly production technique.
Specific implementation mode
The present invention is further elaborated on reference to embodiments.
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
The initiator is the mixture of one or more of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate.
The inorganic base is the mixture of one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) Tea Saponin, isopropyl alkenyl phosphoric acid, methacryl amido propyl ester trimethyl ammonium chloride and water are added to retort
In, it opens and stirs and heat up；
(2) start that the initiator solution that mass percent concentration is 1~10% is added dropwise after being warming up to 60 DEG C~120 DEG C,
This initiator solution is formulated by the initiator and the part water, time for adding control temperature at 3~5 hours, dropwise addition
Degree control is at 90 DEG C~120 DEG C；
(3) inorganic base holding temperature is added after dripping, and the reaction was continued 1~3 hour, and cooling discharge is to get the concrete
Synergist.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment 1
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 28 parts of Tea Saponins, 6 parts of isopropyl alkenyl phosphoric acids, 2 parts of methacryl amido propyl ester trimethyl ammonium chlorides and 45 parts
Water is added in retort, is opened and is stirred and heat up；
(2) start that the sodium peroxydisulfate solution that mass percent concentration is 2%, this sodium peroxydisulfate is added dropwise after being warming up to 70 DEG C
Solution is formulated by 0.1 part of sodium peroxydisulfate and 4.9 parts of water, and time for adding control temperature at 4.5 hours, dropwise addition is controlled 95
℃；
(3) 14 parts of sodium hydroxides holding temperature are added after dripping, and the reaction was continued 1.5 hours, and cooling discharge is to get described
Concrete synergist.
Embodiment 2
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 30 parts of Tea Saponins, 7.5 parts of isopropyl alkenyl phosphoric acids, 3.5 parts of methacryl amido propyl ester trimethyl ammonium chlorides and
42 parts of water are added in retort, are opened and are stirred and heat up；
(2) start that the sodium peroxydisulfate solution that mass percent concentration is 6%, this sodium peroxydisulfate is added dropwise after being warming up to 85 DEG C
Solution is formulated by 0.3 part of sodium peroxydisulfate and 4.7 parts of water, and time for adding control temperature at 3.8 hours, dropwise addition is controlled 98
℃；
(3) 12 parts of sodium hydroxides holding temperature are added after dripping, and the reaction was continued 2 hours, and cooling discharge is to get described mixed
Solidifying soil synergist.
Embodiment 3
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 32 parts of Tea Saponins, 9 parts of isopropyl alkenyl phosphoric acids, 5 parts of methacryl amido propyl ester trimethyl ammonium chlorides and 35 parts
Water is added in retort, is opened and is stirred and heat up；
(2) start that the potassium persulfate solution that mass percent concentration is 7.5%, this persulfuric acid is added dropwise after being warming up to 98 DEG C
Potassium solution is formulated by 0.6 part of potassium peroxydisulfate and 7.4 parts of water, and time for adding control temperature control at 3.2 hours, dropwise addition exists
105℃；
(3) 11 parts of potassium hydroxide holding temperature are added after dripping, and the reaction was continued 2.5 hours, and cooling discharge is to get described
Concrete synergist.
Embodiment 4
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 34 parts of Tea Saponins, 11 parts of isopropyl alkenyl phosphoric acids, 6.5 parts of methacryl amido propyl ester trimethyl ammonium chlorides and
26 parts of water are added in retort, are opened and are stirred and heat up；
(2) start that the potassium persulfate solution that mass percent concentration is 8%, this persulfuric acid is added dropwise after being warming up to 108 DEG C
Potassium solution is formulated by 1 part of potassium peroxydisulfate and 11.5 parts of water, and time for adding control temperature control at 3.5 hours, dropwise addition exists
115℃；
(3) 10 parts of potassium hydroxide holding temperature are added after dripping, and the reaction was continued 2.8 hours, and cooling discharge is to get described
Concrete synergist.
Embodiment 5
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 38 parts of Tea Saponins, 12.5 parts of isopropyl alkenyl phosphoric acids, 8 parts of methacryl amido propyl ester trimethyl ammonium chlorides and
13.5 parts of water are added in retort, are opened and are stirred and heat up；
(2) start that the ammonium persulfate solution that mass percent concentration is 7.5%, this over cure is added dropwise after being warming up to 118 DEG C
Acid ammonium solution is formulated by 1.5 parts of ammonium persulfates and 18.5 parts of water, and time for adding controls the temperature control at 4.5 hours, dropwise addition
System is at 102 DEG C；
(3) 8 parts of potassium carbonate holding temperature are added after dripping, and the reaction was continued 2.2 hours, and cooling discharge is to get the coagulation
Native synergist.
Embodiment 6
A kind of Concrete synergist of phosphorous acid groups of the present invention, the raw material components system matched by following mass fractions
At：
Wherein, the initiator is the mixture of sodium peroxydisulfate and potassium peroxydisulfate, and the matter of sodium peroxydisulfate and potassium peroxydisulfate
Amount is than being 1:2, that is, the dosage of sodium peroxydisulfate and potassium peroxydisulfate is respectively 0.6 part and 1.2 parts.
A kind of preparation method of the Concrete synergist of phosphorous acid groups of the present invention, is achieved by the steps of：
(1) by 39 parts of Tea Saponins, 14 parts of isopropyl alkenyl phosphoric acids, 9.5 parts of methacryl amido propyl ester trimethyl ammonium chlorides and
11.5 parts of water are added in retort, are opened and are stirred and heat up；
(2) start that the initiator solution that mass percent concentration is 9% is added dropwise after being warming up to 101 DEG C, this initiator is molten
Liquid is formulated by 0.6 part of sodium peroxydisulfate, 1.2 parts of potassium peroxydisulfates and 18.2 parts of water, and time for adding is controlled at 4 hours, dropwise addition
Temperature is controlled at 115 DEG C；
(3) 6 parts of potassium carbonate holding temperature are added after dripping, and the reaction was continued 2 hours, and cooling discharge is to get the concrete
Synergist.
Following tests match ratio on the basis of the common concrete grade C30 of Concrete Enterprises carries out comparison test.It uses
The concrete application test that the Concrete synergist of the present invention carries out, illustrates its effect.
1 C30 concrete mixs kg/m of table3
| Match ratio | Cement | Water | Flyash | Slag | River sand | 5~31.5mm rubbles |
| Benchmark | 210 | 150 | 98 | 54 | 790 | 1038 |
| After adjustment | 189 | 150 | 98 | 54 | 790 | 1059 |
Remarks：
1, the cement of cement selection PO42.5；
2, it for the flyash of (45 μm) is 10% to use fineness, water demand ratio 94%, water content 0.3%, and loss on ignition is
1.7%；
3, slag selects 95 grades of slags, specific surface area 420m2/ kg, fluidity ratio are that 102%, 7d compression strength is
78MPa, 28d compression strength are 98MPa；
4, the river sand selected, fineness modulus 2.6, clay content 1.5, clod content are 0%；
5, the grading of rubble is the rubble of 5~31.5mm, elongated particles 8.2%, crush index 11.1%, clay content
0.5%, clod content 0%；
6, water-reducing agent uses low dense polycarboxylate water-reducer JSS, water-reducing rate 20%.
A kind of Concrete synergist provided by the invention has enhancing effect to cement, improves workability；Concrete is in benchmark
In the case that formulation condition is constant, the concrete workability of preparation is good, is easy to construct, and loss of slump is smaller, and 7d and 28d is anti-
Compressive Strength is obviously improved effect, and the experimental results are shown inthe following table for concrete strength：
The application effect of Concrete synergist prepared by 2 embodiment of the present invention 1~6 of table
Remarks：
1, match ratio selects benchmark match ratio；
2, water-reducing agent is polycarboxylate water-reducer, dosage 9.8kg/m3；
2, the dosage of synergist is 3/10000ths of cement consumption.
A kind of Concrete synergist provided by the invention has enhancing effect to cement, improves workability；Concrete is adjusting
Under the conditions of match ratio afterwards (cement consumption reduces 10%), contrast experiment is carried out with benchmark match ratio, finds 7d and 28d pressure resistances
Degree will not decline, or even also increase, it is known that, Concrete synergist provided by the invention is reduced the effect of cement consumption.
The experimental results are shown inthe following table for concrete strength：
The application effect of Concrete synergist prepared by 3 embodiment of the present invention 1~6 of table
Remarks：
1, comparative sample experiment selects benchmark match ratio, Examples 1 to 6 to select the match ratio after adjustment；
2, the dosage of polycarboxylate water-reducer is 9.8kg/m3；
3, the dosage of synergist is 3/10000ths of cement consumption.
The foregoing descriptions are merely the embodiment using this origination techniques content, any those skilled in the art use this wound
Make done modifications and changes, all belong to the scope of the claims of this creation opinion, and is not limited to those disclosed embodiments.
Claims (4)
1. a kind of preparation method of the Concrete synergist of phosphorous acid groups, it is characterised in that：It is achieved by the steps of：
(1) Tea Saponin, isopropyl alkenyl phosphoric acid, methacryl amido propyl ester trimethyl ammonium chloride and water are added in retort,
It opens and stirs and heat up；
(2) start that the initiator solution that mass percent concentration is 1~10% is added dropwise after being warming up to 60 DEG C~120 DEG C, this draws
Hair agent solution is formulated by the initiator and water, and time for adding control temperature at 3~5 hours, dropwise addition is controlled at 90 DEG C
~120 DEG C；
(3) inorganic base holding temperature is added after dripping, and the reaction was continued 1~3 hour, and cooling discharge is to get Concrete synergist.
2. a kind of preparation method of the Concrete synergist of phosphorous acid groups according to claim 1, it is characterised in that：It is main
The raw material components to be matched by following mass fractions are made：
3. a kind of preparation method of the Concrete synergist of phosphorous acid groups according to claim 1, it is characterised in that：Institute
State the mixture that initiator is one or more of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate.
4. a kind of preparation method of the Concrete synergist of phosphorous acid groups according to claim 1, it is characterised in that：Institute
State the mixture that inorganic base is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
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| CN201810625131.7A CN108641037B (en) | 2018-06-17 | 2018-06-17 | Concrete synergist containing phosphoric acid group and preparation method thereof |
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| CN201810625131.7A CN108641037B (en) | 2018-06-17 | 2018-06-17 | Concrete synergist containing phosphoric acid group and preparation method thereof |
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| CN108641037A true CN108641037A (en) | 2018-10-12 |
| CN108641037B CN108641037B (en) | 2020-05-08 |
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