CN109535347B - Preparation method of block water-retaining concrete admixture - Google Patents
Preparation method of block water-retaining concrete admixture Download PDFInfo
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- CN109535347B CN109535347B CN201811580927.1A CN201811580927A CN109535347B CN 109535347 B CN109535347 B CN 109535347B CN 201811580927 A CN201811580927 A CN 201811580927A CN 109535347 B CN109535347 B CN 109535347B
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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
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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
- C04B24/246—Phosphorus-containing polymers containing polyether side chains
Abstract
The invention belongs to the technical field of building additives, and particularly relates to a preparation method of a block water-retaining concrete additive, which comprises the following steps: adding an unsaturated polyether monomer A, an unsaturated crosslinking monomer, acrylic acid, L-ascorbic acid, a chain transfer agent, ferrous sulfate heptahydrate and deionized water into a reaction kettle, stirring, adding hydrogen peroxide after the materials are completely dissolved, continuing stirring for 1-3 hours, stirring again, adding an unsaturated polyether monomer B, an unsaturated polyether monomer C, acrylic acid, an oxidant and deionized water, heating to raise the temperature, beginning to dropwise add a mixed solution I, dropwise adding a mixed solution II after 10 minutes, adding hydrogen peroxide and sodium phosphate into the reaction kettle after the mixed solution I and the mixed solution II are dropwise added, keeping the temperature for 1 hour, and cooling to obtain the block water-retaining concrete admixture. The invention can improve the cohesiveness of concrete mixture, reduce the segregation and bleeding of concrete and reasonably regulate and control the working state of concrete.
Description
Technical Field
The invention belongs to the technical field of building additives, and particularly relates to a preparation method of a block water-retaining concrete additive.
Background
The concrete admixture is widely applied to deionized cement-based materials, such as deionized cement paste, mortar and concrete, and is very necessary in the field of engineering construction and building structures. The concrete admixture can increase the fluidity of the deionized cement-based material and effectively improve the performances of hardened concrete such as strength, durability and the like. With the development of high performance and multiple functions of concrete, the concrete is required to have high workability, high strength and high durability, and to meet the application requirements in many special cases, and has become an indispensable component in high performance concrete.
The concrete admixture has excellent dispersing performance, can enable concrete to achieve better fluidity under the condition of lower mixing amount, can synthesize a polymerizable structural unit into the concrete admixture with preset structure and performance through free radical copolymerization reaction according to the principle of molecular design in the preparation process, and is usually synthesized by monomers containing carboxylic acid groups, sulfonic acid groups, ester groups, polyoxyethylene groups and the like and having unsaturated groups through the free radical copolymerization reaction. In the polymerization preparation process of the concrete admixture, different monomers are randomly or regularly polymerized together, so that molecules have certain molecular space configuration, and the excellent performance of the concrete admixture is determined by the special structure of the concrete admixture. At present, most of concrete admixtures have linear comb-shaped molecular structures, and the steric resistance effect is weaker in a multi-phase system of concrete, so that the dispersibility, the slump retention, the deionized water retention effect and the universality in deionized water slurry are required to be improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a block water-retaining concrete admixture.
The technical scheme of the invention is as follows:
the weight portion of the material is as follows:
adding 180 parts of unsaturated polyether monomer A of 150-180 parts, 5-10 parts of unsaturated crosslinking monomer, 10-30 parts of acrylic acid, 0.2-2 parts of L-ascorbic acid, 0.4-0.8 part of chain transfer agent, 0.01-0.05 part of ferrous sulfate heptahydrate and 150 parts of deionized water of 100-0 parts into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube;
starting a stirring device for stirring, controlling the temperature of a temperature controller to be 15-35 ℃, adding 1-5 parts of hydrogen peroxide after materials are completely dissolved, continuously stirring for 5min, and stopping stirring;
starting the stirring device again after 1-3h, and adding 20-30 parts of unsaturated polyether monomer B, 5-10 parts of unsaturated polyether monomer C, 3-6 parts of acrylic acid, 2-5 parts of oxidant and 30-50 parts of deionized water into the reaction kettle;
heating to 50-65 ℃, dropwise adding a mixed solution I prepared from 2-5 parts of unsaturated amino compound and 30-40 parts of deionized water by using a dropwise adding device, after 10min, dropwise adding a mixed solution II prepared from 0.2-0.5 part of composite reducing agent, 0.1-0.3 part of chain transfer agent and 30-40 parts of deionized water, after the mixed solution I is dropwise added within 0.5-1h, the mixed solution II is dropwise added within 1-1.5h, after the mixed solution I and the mixed solution II are dropwise added, adding 1-2 parts of hydrogen peroxide and 0.2-0.5 part of sodium phosphate into a reaction kettle, preserving heat for 1h, cooling, and obtaining the block water retention type concrete admixture.
Further, the unsaturated polyether monomer a comprises the following structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1＝CH2 (a)
wherein p is an integer, and p is more than or equal to 5 and less than or equal to 10; q is an integer, and q is more than or equal to 1 and less than or equal to 2; r1Is H or CH3。
Further, the unsaturated crosslinking monomer is one of triallyl phosphite, diallyl allylphosphonate and triallyl phosphate.
Further, the chain transfer agent is one of thioglycolic acid, mercaptopropionic acid and mercaptoethanol.
Further, the unsaturated polyether monomer B comprises the following structure (B):
CH3CH2O(CH2CH2O)m(CH2CH2CH2O)nCH2CH2OOCH2CR2＝CH2 (b)
wherein m is an integer, and m is more than or equal to 20 and less than or equal to 25; n is an integer of 1 to lessn≤3；R2Is H or CH3。
Further, the unsaturated polyether monomer C comprises the following structure (C):
CH2＝CR3CH2OO(CH2CH2CH2O)x(CH2CH2O)yOCH2CR4＝CH2 (c)
wherein x is an integer, and x is more than or equal to 1 and less than or equal to 2; y is an integer, and y is more than or equal to 5 and less than or equal to 10; r3，R4Is H or CH3。
Further, the oxidant is one of hydrogen peroxide, ammonium persulfate, sodium persulfate and potassium persulfate.
Further, the unsaturated amino compound isD-allylglycine、2-amino-4-methyl-4-pentenoic acid、2-Ammonia 3-butenoic acidAnd 2-amino-5-hexenoic acid.
Further, the composite reducing agent has the following composition in parts by weight:
2-hydroxy-2-sulfinato zinc acetate: 40-60 percent;
2-hydroxy-2-sulfonic acid zinc acetate: 1 to 4 percent;
l-ascorbic acid: 1 to 5 percent;
one of sodium hydrosulfite, potassium hydrosulfite or zinc hydrosulfite: 15 to 35 percent;
one of sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate: 10 to 20 percent.
The invention has the beneficial effects that: the block polymer is prepared by aqueous solution free radical copolymerization and by adopting unsaturated monomers, initiators, chain transfer agents and the like through a two-step method, and the preparation method has the characteristics of strong operability, easy control of reaction process, low sensitivity to reaction conditions, easy industrial production and the like. Polyether side chains of different types and lengths are introduced into the molecular side chains, so that the spatial configuration and the stretching degree of the concrete admixture in a concrete multiphase system can be regulated and controlled; by introducing crosslinking monomers, unsaturated amino compounds and the like into a molecular main chain, the lubricating effect and the hydrophilic state of particles in a concrete multi-item system can be improved, the cohesiveness of a concrete mixture is improved, the segregation and bleeding of concrete are reduced, and the working state of the concrete is reasonably regulated and controlled.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In examples 1 to 4, the components and the proportions of the composite reducing agent used are shown in table 1.
TABLE 1 Complex Reductant Components and proportions
Example 1
Adding 150 parts by weight of H (OCH) into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube2CH2)5OCH2CH2CH2OCH2CH2CH＝CH25 parts of triallyl phosphite, 10 parts of acrylic acid, 0.2 part of L-ascorbic acid, 0.8 part of thioglycollic acid, 0.05 part of ferrous sulfate heptahydrate and 100 parts of deionized water, starting a stirring device for stirring, controlling the temperature of a temperature controller to be 35 ℃, adding 3 parts of hydrogen peroxide after the materials are completely dissolved, continuing stirring for 5min, stopping stirring, starting the stirring device again after 1h, and adding 25 parts of CH into a reaction kettle3CH2O(CH2CH2O)20CH2CH2CH2OCH2CH2OOCH2CH＝CH25 parts of CH2＝CHCH2OO(CH2CH2CH2O)2(CH2CH2O)5OCH2CCH3＝CH23 parts of acrylic acid, 5 parts of hydrogen peroxide and 35 parts of deionized water, heating to 65 ℃, and beginning to dropwise add 2-5 parts of acrylic acid, 5 parts of hydrogen peroxide and 35 parts of deionized water by using a dropwise adding deviceD-allylglycineAnd 35 parts of deionized water, dropwise adding a mixed solution I prepared from 0.2 part of composite reducing agent, 0.2 part of thioglycolic acid and 35 parts of deionized water after 10min, dropwise adding the mixed solution I within 0.5h, dropwise adding the mixed solution II within 1h, adding 1 part of hydrogen peroxide and 0.5 part of sodium phosphate into the reaction kettle after dropwise adding the mixed solution I and the mixed solution II, preserving heat for 1h, and cooling to obtain the block water retention type concrete admixture.
Example 2
160 parts of H (OCH) are added into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube according to the parts by weight2CH2)6(OCH2CH2CH2)2OCH2CH2CCH3＝CH26 parts of allyl diallyl phosphonate, 30 parts of acrylic acid, 0.5 part of L-ascorbic acid, 0.8 part of thioglycollic acid, 0.03 part of ferrous sulfate heptahydrate and 120 parts of deionized water, starting a stirring device for stirring, controlling the temperature of a temperature controller to be 30 ℃, adding 2 parts of hydrogen peroxide after the materials are completely dissolved, continuing stirring for 5min, stopping stirring, starting the stirring device again for stirring after 2h, and adding 26 parts of CH into a reaction kettle3CH2O(CH2CH2O)22(CH2CH2CH2O)2CH2CH2OOCH2CH＝CH210 parts of CH2＝CCH3CH2OOCH2CH2CH2O(CH2CH2O)7OCH2CH＝CH24 parts of acrylic acid, 2 parts of ammonium persulfate and 40 parts of deionized water, heating to 50 ℃, and beginning to dropwise add 2-5 parts of acrylic acid, 2-5 parts of ammonium persulfate and 40 parts of deionized water by using a dropwise adding device2-amino-4-methyl-4-pentenoic acidAnd 40 parts of deionized water, and after 10min, dropwise adding 0.5 part of composite reducing agent, 0.1 part of mercaptopropionic acid and 40 parts of deionized waterAnd (3) adding the mixed solution II, wherein the adding of the mixed solution I is finished within 1h, the adding of the mixed solution II is finished within 1.5h, adding 1.5 parts of hydrogen peroxide and 0.2 part of sodium phosphate into the reaction kettle after the adding of the mixed solution I and the mixed solution II is finished, preserving heat for 1h, and cooling to obtain the block water-retaining concrete admixture.
Example 3
Adding 170 parts of H (OCH) into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube according to parts by weight2CH2)8(OCH2CH2CH2)3OCH2CH2CCH3＝CH210 parts of triallyl phosphate, 20 parts of acrylic acid, 1 part of L-ascorbic acid, 0.4 part of mercaptopropionic acid, 0.01 part of ferrous sulfate heptahydrate and 150 parts of deionized water, starting a stirring device for stirring, controlling the temperature of a temperature controller to be 15 ℃, adding 1 part of hydrogen peroxide after the materials are completely dissolved, continuing stirring for 5min, stopping stirring, starting the stirring device again for stirring after 3h, and adding 20 parts of CH into a reaction kettle3CH2O(CH2CH2O)23(CH2CH2CH2O)2CH2CH2OOCH2CH＝CH28 parts of CH2＝CCH3CH2OO(CH2CH2CH2O)2(CH2CH2O)10OCH2CCH3＝CH25 parts of acrylic acid, 3 parts of sodium persulfate and 30 parts of deionized water, heating to 55 ℃, and beginning to dropwise add 2-5 parts of acrylic acid, sodium persulfate and deionized water by using a dropwise adding device2-amino-3-butenoic acidAnd 30 parts of deionized water, dropwise adding a mixed solution I prepared from 0.4 part of composite reducing agent, 0.1 part of mercaptoethanol and 30 parts of deionized water after 10min, dropwise adding the mixed solution I within 0.8h, dropwise adding the mixed solution II within 1h, adding 1.8 parts of hydrogen peroxide and 0.4 part of sodium phosphate into the reaction kettle after dropwise adding the mixed solution I and the mixed solution II, preserving heat for 1h, and cooling to obtain the block water-retaining concrete admixture.
Example 4
Adding 180 parts by weight of H (OCH) into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube2CH2)10(OCH2CH2CH2)2OCH2CH2CH＝CH28 parts of triallyl phosphate, 15 parts of acrylic acid, 2 parts of L-ascorbic acid, 0.5 part of mercaptoethanol, 0.04 part of ferrous sulfate heptahydrate and 135 parts of deionized water, starting a stirring device for stirring, controlling the temperature of a temperature controller to be 25 ℃, adding 5 parts of hydrogen peroxide after the materials are completely dissolved, continuing stirring for 5min, stopping stirring, starting the stirring device again for stirring after 1h, and adding 30 parts of CH into a reaction kettle3CH2O(CH2CH2O)25(CH2CH2CH2O)3CH2CH2OOCH2CCH3＝CH210 parts of CH2＝CHCH2OOCH2CH2CH2O(CH2CH2O)9OCH2CH＝CH26 parts of acrylic acid, 4 parts of potassium persulfate and 50 parts of deionized water, when the temperature is raised to 60 ℃, beginning to dropwise add a mixed solution I prepared from 2-5 parts of 2-amino-5-hexenoic acid and 30 parts of deionized water by using a dropwise adding device, after 10min, dropwise adding a mixed solution II prepared from 0.3 part of composite reducing agent, 0.3 part of mercaptoethanol and 40 parts of deionized water, after dropwise adding the mixed solution I in 1h, dropwise adding the mixed solution II in 1.5h, after dropwise adding the mixed solution I and the mixed solution II, adding 2 parts of hydrogen peroxide and 0.3 part of sodium phosphate into a reaction kettle, keeping the temperature for 1h, and cooling to obtain the block water retention type concrete admixture.
The samples obtained by the synthesis in examples 1 to 4 and a reference sample (a commercially available standard high performance water reducing agent, HPWR-S) were subjected to a concrete mixture performance test method and a hardened concrete performance test according to GB/T50080-2016 Standard test method for Performance of ordinary concrete mixtures and GB/T50081-2016 Standard test method for mechanical Performance of ordinary concrete.
The performance test adopts the following main raw materials:
cement (C): P.O 42.5.5 Portland Cement, Tata Hongshi Cement, Inc.;
fly Ash (FA): class II fly ash, Xiamen trade Co Ltd;
mineral powder (SL): grade S95, fujian sanbao iron and steel limited;
sand (S): the fineness modulus is 2.8, the mud content is less than 1 percent, and the mansion gate Wanxiang is the same as the practical company;
stone (G): 5-25mm graded crushed stone, Xiamen Shunli building materials Co Ltd;
test water (W): tap water meets the regulation of JGJ 63-2006 Water for concrete Standard.
The concrete mixing proportion adopted in the performance test is shown in table 2, and the performance test data is shown in table 3.
TABLE 2 concrete mix proportions
| Raw material | C | FA | SL | S | G | W |
| Dosage/(kg/m)3) | 280 | 70 | 70 | 740 | 1020 | 162 |
TABLE 3 concrete test Properties
From the performance test data in table 3, it can be seen that the technical scheme of the present invention has obvious effects of water retention and segregation resistance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, so that any modifications, equivalents and improvements made by the present invention as described in the specification are included in the scope of the present invention.
Claims (4)
1. A preparation method of a block water-retaining concrete admixture is characterized by comprising the following steps: the method comprises the following steps:
the weight portion of the material is as follows:
adding 180 parts of unsaturated polyether monomer A of 150-180 parts, 5-10 parts of unsaturated crosslinking monomer, 10-30 parts of acrylic acid, 0.2-2 parts of L-ascorbic acid, 0.4-0.8 part of chain transfer agent, 0.01-0.05 part of ferrous sulfate heptahydrate and 150 parts of deionized water of 100-0 parts into a reaction kettle with a temperature controller, a stirring device, a dropping device and a nitrogen tube;
starting the stirring device for stirring, controlling the temperature of the temperature controller to be 15-35 ℃, adding 1-5 parts of hydrogen peroxide after the materials are completely dissolved, continuing stirring for 5min, and then stopping stirring;
after 1-3h, starting the stirring device again for stirring, and adding 20-30 parts of unsaturated polyether monomer B, 5-10 parts of unsaturated polyether monomer C, 3-6 parts of acrylic acid, 2-5 parts of oxidant and 30-50 parts of deionized water into the reaction kettle;
heating to 50-65 ℃, beginning to dropwise add a mixed solution I prepared from 2-5 parts of unsaturated amino compound and 30-40 parts of deionized water by using the dropwise adding device, dropwise adding a mixed solution II prepared from 0.2-0.5 part of composite reducing agent, 0.1-0.3 part of chain transfer agent and 30-40 parts of deionized water after 10min, dropwise adding the mixed solution I in 0.5-1h, dropwise adding the mixed solution II in 1-1.5h, adding 1-2 parts of hydrogen peroxide and 0.2-0.5 part of sodium phosphate into the reaction kettle after dropwise adding the mixed solution I and the mixed solution II, preserving heat for 1h, and cooling to obtain the block water-retaining concrete admixture;
the unsaturated polyether monomer A comprises the following structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1=CH2 (a)
wherein p is an integer, and p is more than or equal to 5 and less than or equal to 10; q is an integer, and q is more than or equal to 1 and less than or equal to 2; r1Is H or CH3；
The unsaturated crosslinking monomer is one of triallyl phosphite, diallyl allylphosphonate and triallyl phosphate;
the unsaturated polyether monomer B comprises the following structure (B):
CH3CH2O(CH2CH2O)m(CH2CH2CH2O)nCH2CH2OOCH2CR2=CH2 (b)
wherein m is an integer, and m is more than or equal to 20 and less than or equal to 25; n is an integer, and n is more than or equal to 1 and less than or equal to 3; r2Is H or CH3；
The unsaturated polyether monomer C comprises the following structure (C):
CH2=CR3CH2OO(CH2CH2CH2O)x(CH2CH2O)yOCH2CR4=CH2 (c)
wherein x is an integer, and x is more than or equal to 1 and less than or equal to 2; y is an integer, and y is more than or equal to 5 and less than or equal to 10; r3，R4Is H or CH3；
The unsaturated amino compound is one of D-allyl glycine, 2-amino-4-methyl-4-pentenoic acid, 2-amino-3-butenoic acid and 2-amino-5-hexenoic acid.
2. The method for preparing the block water-retaining concrete admixture according to claim 1, wherein the method comprises the following steps: the chain transfer agent is one of thioglycolic acid, mercaptopropionic acid and mercaptoethanol.
3. The method for preparing the block water-retaining concrete admixture according to claim 1, wherein the method comprises the following steps: the oxidant is one of hydrogen peroxide, ammonium persulfate, sodium persulfate and potassium persulfate.
4. The method for preparing the block water-retaining concrete admixture according to claim 1, wherein the method comprises the following steps: the composite reducing agent comprises the following components in parts by weight:
2-hydroxy-2-sulfinato zinc acetate: 40-60 percent;
2-hydroxy-2-sulfonic acid zinc acetate: 1 to 4 percent;
l-ascorbic acid: 1 to 5 percent;
one of sodium hydrosulfite, potassium hydrosulfite or zinc hydrosulfite: 15 to 35 percent;
one of sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate: 10 to 20 percent.
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