CN108641037B - Concrete synergist containing phosphoric acid group and preparation method thereof - Google Patents
Concrete synergist containing phosphoric acid group and preparation method thereof Download PDFInfo
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- CN108641037B CN108641037B CN201810625131.7A CN201810625131A CN108641037B CN 108641037 B CN108641037 B CN 108641037B CN 201810625131 A CN201810625131 A CN 201810625131A CN 108641037 B CN108641037 B CN 108641037B
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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
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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
- C04B24/243—Phosphorus-containing polymers
Abstract
The invention provides a concrete synergist containing phosphoric acid groups and a preparation method thereof, wherein the concrete synergist comprises the following steps: (1) adding tea saponin, isopropenylphosphoric acid, methacrylamidopropyl trimethylammonium chloride and water into a reaction tank, starting stirring and heating; (2) after the temperature is raised to 60-120 ℃, starting to dropwise add an initiator solution with the mass percentage concentration of 1-10%, wherein the initiator solution is prepared from the initiator and part of the water, the dropwise adding time is controlled to be 3-5 hours, and the temperature is controlled to be 90-120 ℃ during dropwise adding; (3) and after the dripping is finished, adding inorganic alkali, keeping the temperature, continuing to react for 1-3 hours, cooling and discharging to obtain the concrete synergist.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, and particularly relates to a concrete synergist containing phosphoric acid groups and a preparation method thereof.
Background
Concrete is currently the largest and most widely used material worldwide because of its many advantages. Research data shows that about 20-30% of cement in concrete does not participate in hydration reaction in the conventional environment, only plays a role in filling fine aggregates, cannot effectively exert the strength of the cement, and causes great waste of resources. On the other hand, different water reducing agents have different influence mechanisms on cement adsorption and the like, so that the water reducing agents hardly play a role in concrete after being added to a certain degree, and the economical efficiency and the workability are difficult to guarantee. How to develop a new concrete admixture to solve the problems, the surplus cement is saved, and the basic performance and strength of the concrete can be guaranteed, thereby having very important practical significance for concrete enterprises.
The concrete synergist is used for stimulating the action of each unit of cement molecule to the maximum extent and stimulating the performance of the water reducing agent by improving the dispersion degree of cement particles and mineral fine aggregates. The cement particles are more dispersed, so that the hydration action of the cement is more sufficient, namely most of the cement particles are fully mixed and stirred with water, sand, stone and the like, and then can be fully contacted with other materials (such as a water reducing agent) around the cement particles and react, so that the comprehensive performance of the concrete is enhanced, and the original cement consumption in the concrete is saved.
The invention provides a concrete synergist containing phosphoric acid groups. The concrete synergist is a novel concrete admixture, can reduce the cement consumption of the concrete with medium and low strength grades, can ensure the workability, the strength and the durability of the concrete, and has wide application prospect.
Disclosure of Invention
Therefore, aiming at the content, the invention provides the concrete synergist containing the phosphoric acid group and the preparation method thereof, the concrete synergist is a novel concrete admixture, and for the concrete with medium and low strength grade, the concrete synergist can reduce the using amount of cement, and can ensure the workability, strength and durability, thereby having wide application prospect.
In order to achieve the purpose, the invention is realized by the following technical scheme: a concrete synergist containing phosphoric acid groups is mainly prepared from the following raw materials in parts by weight:
the initiator is one or a mixture of more of sodium persulfate, potassium persulfate and ammonium persulfate.
The inorganic base is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
A preparation method of a concrete synergist containing phosphoric acid groups is realized by the following steps:
(1) adding tea saponin, isopropenylphosphoric acid, methacrylamidopropyl trimethylammonium chloride and water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 60-120 ℃, starting to dropwise add an initiator solution with the mass percentage concentration of 1-10%, wherein the initiator solution is prepared from the initiator and part of the water, the dropwise adding time is controlled to be 3-5 hours, and the temperature is controlled to be 90-120 ℃ during dropwise adding;
(3) and after the dripping is finished, adding inorganic alkali, keeping the temperature, continuing to react for 1-3 hours, cooling and discharging to obtain the concrete synergist.
Compared with the prior art, the invention has the following remarkable effects:
1. tea saponin is used as a basic raw material, and is modified by adding a plurality of modifiers, so that phosphate groups, amide groups, ester groups and the like are introduced, and the performance of the product is improved.
2. The product is non-toxic and harmless, is not limited by seasons and regions in use, and is convenient to transport and store;
3. the product has simple production process and mild conditions, the feeding and the conditions in the production process are easy to control, and the whole process has no three wastes, thus being a green, environment-friendly, pollution-free and clean production process.
Detailed Description
The present invention is further illustrated in detail by the following examples.
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the initiator is one or a mixture of more of sodium persulfate, potassium persulfate and ammonium persulfate.
The inorganic base is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
The invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding tea saponin, isopropenylphosphoric acid, methacrylamidopropyl trimethylammonium chloride and water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 60-120 ℃, starting to dropwise add an initiator solution with the mass percentage concentration of 1-10%, wherein the initiator solution is prepared from the initiator and part of the water, the dropwise adding time is controlled to be 3-5 hours, and the temperature is controlled to be 90-120 ℃ during dropwise adding;
(3) and after the dripping is finished, adding inorganic alkali, keeping the temperature, continuing to react for 1-3 hours, cooling and discharging to obtain the concrete synergist.
The present invention will be described in detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 28 parts of tea saponin, 6 parts of isopropenylphosphoric acid, 2 parts of methacrylamidopropyl trimethylammonium chloride and 45 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 70 ℃, beginning to dropwise add a sodium persulfate solution with the mass percentage concentration of 2%, wherein the sodium persulfate solution is prepared from 0.1 part of sodium persulfate and 4.9 parts of water, the dropwise adding time is controlled to be 4.5 hours, and the temperature is controlled to be 95 ℃ during dropwise adding;
(3) and after the dropwise addition, adding 14 parts of sodium hydroxide, keeping the temperature, continuing to react for 1.5 hours, cooling and discharging to obtain the concrete synergist.
Example 2
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 30 parts of tea saponin, 7.5 parts of isopropenylphosphoric acid, 3.5 parts of methacrylamidopropyl trimethylammonium chloride and 42 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 85 ℃, beginning to dropwise add sodium persulfate solution with the mass percentage concentration of 6%, wherein the sodium persulfate solution is prepared from 0.3 part of sodium persulfate and 4.7 parts of water, the dropwise adding time is controlled to be 3.8 hours, and the temperature is controlled to be 98 ℃ during dropwise adding;
(3) and after the dropwise addition, adding 12 parts of sodium hydroxide, keeping the temperature, continuing to react for 2 hours, cooling and discharging to obtain the concrete synergist.
Example 3
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 32 parts of tea saponin, 9 parts of isopropenylphosphoric acid, 5 parts of methacrylamidopropyl trimethylammonium chloride and 35 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 98 ℃, beginning to dropwise add a potassium persulfate solution with the mass percentage concentration of 7.5 percent, wherein the potassium persulfate solution is prepared from 0.6 part of potassium persulfate and 7.4 parts of water, the dropwise adding time is controlled to be 3.2 hours, and the temperature is controlled to be 105 ℃ during dropwise adding;
(3) and after the dripping is finished, adding 11 parts of potassium hydroxide, keeping the temperature for continuously reacting for 2.5 hours, cooling and discharging to obtain the concrete synergist.
Example 4
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 34 parts of tea saponin, 11 parts of isopropenylphosphoric acid, 6.5 parts of methacrylamidopropyl trimethylammonium chloride and 26 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 108 ℃, beginning to dropwise add a potassium persulfate solution with the mass percentage concentration of 8%, wherein the potassium persulfate solution is prepared from 1 part of potassium persulfate and 11.5 parts of water, the dropwise adding time is controlled to be 3.5 hours, and the temperature is controlled to be 115 ℃ during dropwise adding;
(3) and after the dripping is finished, adding 10 parts of potassium hydroxide, keeping the temperature, continuing to react for 2.8 hours, cooling and discharging to obtain the concrete synergist.
Example 5
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 38 parts of tea saponin, 12.5 parts of isopropenylphosphoric acid, 8 parts of methacrylamidopropyl trimethyl ammonium chloride and 13.5 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 118 ℃, beginning to dropwise add an ammonium persulfate solution with the mass percentage concentration of 7.5 percent, wherein the ammonium persulfate solution is prepared from 1.5 parts of ammonium persulfate and 18.5 parts of water, the dropwise adding time is controlled to be 4.5 hours, and the temperature is controlled to be 102 ℃ during dropwise adding;
(3) and after the dripping is finished, 8 parts of potassium carbonate is added, the temperature is kept, the reaction is continued for 2.2 hours, and the concrete synergist is obtained after cooling and discharging.
Example 6
The invention relates to a concrete synergist containing phosphoric acid groups, which is prepared from the following raw materials in parts by weight:
the initiator is a mixture of sodium persulfate and potassium persulfate, and the mass ratio of the sodium persulfate to the potassium persulfate is 1:2, namely, the usage amounts of the sodium persulfate and the potassium persulfate are respectively 0.6 part and 1.2 part.
The invention relates to a preparation method of a concrete synergist containing phosphoric acid groups, which is realized by the following steps:
(1) adding 39 parts of tea saponin, 14 parts of isopropenylphosphoric acid, 9.5 parts of methacrylamidopropyl trimethyl ammonium chloride and 11.5 parts of water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 101 ℃, starting to dropwise add an initiator solution with the mass percentage concentration of 9 percent, wherein the initiator solution is prepared by 0.6 part of sodium persulfate, 1.2 parts of potassium persulfate and 18.2 parts of water, the dropwise adding time is controlled to be 4 hours, and the temperature is controlled to be 115 ℃ during dropwise adding;
(3) and after the dripping is finished, adding 6 parts of potassium carbonate, keeping the temperature for continuously reacting for 2 hours, cooling and discharging to obtain the concrete synergist.
In the following test, the concrete grade C30 commonly used in concrete enterprises is used as a reference for comparison and inspection. The concrete application test using the concrete synergist of the invention shows the effect.
TABLE 1C 30 concrete mixing ratio kg/m3
| Mixing ratio | Cement | Water (W) | Fly ash | Slag of mine | River sand | Crushed stone of 5-31.5 mm |
| Datum | 210 | 150 | 98 | 54 | 790 | 1038 |
| After adjustment | 189 | 150 | 98 | 54 | 790 | 1059 |
Remarking:
1. the cement is P.O 42.5 cement;
2. 10 percent of fly ash with the fineness of 45 mu m, 94 percent of water requirement ratio, 0.3 percent of water content and 1.7 percent of loss on ignition are adopted;
3. the slag is 95-grade slag with a specific surface area of 420m2Kg, fluidity ratio of 102%, 7d compressive strength of 78MPa, 28d compressive strength of 98 MPa;
4. the selected river sand has the fineness modulus of 2.6, the mud content of 1.5 and the mud block content of 0 percent;
5. the graded broken stone is 5-31.5 mm broken stone, the needle sheet content is 8.2%, the crushing index is 11.1%, the mud content is 0.5%, and the mud block content is 0%;
6. the water reducing agent is low-concentration polycarboxylic acid water reducing agent JSS, and the water reducing rate is 20%.
The concrete synergist provided by the invention has a reinforcing effect on cement, and improves workability; under the condition that the standard formula condition of the concrete is not changed, the prepared concrete is good in workability, easy to construct and small in slump loss, the 7d and 28d compressive strengths have obvious improving effects, and the concrete strength experimental results are shown in the following table:
TABLE 2 application effect of concrete synergist prepared in examples 1-6 of the present invention
Remarking:
1. selecting a reference mixing ratio;
2. the water reducing agent is a polycarboxylic acid water reducing agent, and the dosage of the water reducing agent is 9.8kg/m3；
2. The dosage of the synergist is three ten-thousandth of the dosage of the cement.
The concrete synergist provided by the invention has a reinforcing effect on cement, and improves workability; compared with the reference mixing ratio, the concrete under the condition of the adjusted mixing ratio (the cement dosage is reduced by 10%) shows that the compressive strength of 7d and 28d is not reduced and even is improved, and the concrete synergist provided by the invention has the effect of reducing the cement dosage. The concrete strength test results are shown in the following table:
TABLE 3 Effect of concrete synergist prepared in examples 1-6 of the present invention
Remarking:
1. the reference mixing ratio is selected for the comparative sample experiment, and the adjusted mixing ratio is selected in the examples 1-6;
2. the dosage of the polycarboxylate superplasticizer is 9.8kg/m3；
3. The dosage of the synergist is three ten-thousandth of the dosage of the cement.
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.
Claims (1)
1. A preparation method of a concrete synergist containing phosphoric acid groups is characterized in that: the method is realized by the following steps:
(1) adding tea saponin, isopropenylphosphoric acid, methacrylamidopropyltrimethylammonium chloride and water into a reaction tank, starting stirring and heating;
(2) after the temperature is raised to 60-120 ℃, starting to dropwise add an initiator solution with the mass percentage concentration of 1-10%, wherein the initiator solution is prepared from the initiator and water, the dropwise adding time is controlled to be 3-5 hours, and the temperature is controlled to be 90-120 ℃ during dropwise adding;
(3) after the dripping is finished, adding inorganic base, keeping the temperature, continuing to react for 1-3 hours, cooling and discharging to obtain the concrete synergist;
the material is mainly prepared from the following raw materials in parts by weight:
25-40 parts of tea saponin
5-15 parts of isopropenylphosphoric acid
1-10 parts of methacrylamidopropyl trimethyl ammonium chloride
0.05-2 parts of initiator
5-15 parts of inorganic base
25-55 parts of water;
the initiator is one or a mixture of more of sodium persulfate, potassium persulfate and ammonium persulfate;
the inorganic base is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104496266A (en) * | 2015-01-15 | 2015-04-08 | 科之杰新材料集团有限公司 | Concrete synergist and preparation method thereof |
| CN105036587A (en) * | 2015-09-06 | 2015-11-11 | 山东宏艺科技股份有限公司 | High-performance concrete synergist and preparing method thereof |
| CN105949385A (en) * | 2016-07-15 | 2016-09-21 | 刘碧霞 | Naphthalene series ceramic dispersing agent and preparation method thereof |
| CN106674435A (en) * | 2016-07-15 | 2017-05-17 | 刘碧霞 | Composite ceramic dispersant and preparation method thereof |
| CN106904867A (en) * | 2017-04-20 | 2017-06-30 | 福建清源科技有限公司 | Concrete synergist containing chitosan sodium sulfonate and preparation method thereof |
| CN105217995B (en) * | 2015-11-06 | 2017-09-15 | 科之杰新材料集团有限公司 | A kind of Concrete synergist and preparation method thereof |
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- 2018-06-17 CN CN201810625131.7A patent/CN108641037B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104496266A (en) * | 2015-01-15 | 2015-04-08 | 科之杰新材料集团有限公司 | Concrete synergist and preparation method thereof |
| CN105036587A (en) * | 2015-09-06 | 2015-11-11 | 山东宏艺科技股份有限公司 | High-performance concrete synergist and preparing method thereof |
| CN105217995B (en) * | 2015-11-06 | 2017-09-15 | 科之杰新材料集团有限公司 | A kind of Concrete synergist and preparation method thereof |
| CN105949385A (en) * | 2016-07-15 | 2016-09-21 | 刘碧霞 | Naphthalene series ceramic dispersing agent and preparation method thereof |
| CN106674435A (en) * | 2016-07-15 | 2017-05-17 | 刘碧霞 | Composite ceramic dispersant and preparation method thereof |
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