CN111423148A - Environment-friendly steam-pressure-free pipe pile water reducing agent and preparation method thereof - Google Patents
Environment-friendly steam-pressure-free pipe pile water reducing agent and preparation method thereof Download PDFInfo
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- CN111423148A CN111423148A CN202010485450.XA CN202010485450A CN111423148A CN 111423148 A CN111423148 A CN 111423148A CN 202010485450 A CN202010485450 A CN 202010485450A CN 111423148 A CN111423148 A CN 111423148A
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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
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
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- 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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0638—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with at least three nitrogen atoms in the ring
- C08G73/0644—Poly(1,3,5)triazines
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0638—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with at least three nitrogen atoms in the ring
- C08G73/065—Preparatory processes
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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
- 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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Abstract
The invention discloses an environment-friendly steam-free pipe pile water reducing agent which is characterized by comprising the following components in parts by weight: 10-20 parts of 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 5-10 parts of 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl benzene boric acid copolymer, 1-3 parts of 9-fluorenylformic acid, 0.3-0.6 part of initiator, 2-5 parts of plant polysaccharide and 35-45 parts of water. The invention also discloses a preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent. The environment-friendly autoclaved-free pipe pile water reducer disclosed by the invention has the advantages of obvious water reducing effect, small mixing amount, excellent plasticizing performance, no obvious negative influence on the comprehensive performance of concrete, good energy-saving and environment-friendly performance in the preparation and use processes, high reaction activity and low reaction temperature, can effectively enhance the compressive strength, obviously reduce the hardening and viscosity of concrete, and increase the construction performance of concrete.
Description
Technical Field
The invention relates to the technical field of concrete additives, in particular to an environment-friendly autoclaved pipe pile water reducing agent and a preparation method thereof.
Background
With the rapid development of engineering construction technology and the continuous updating of foundation treatment engineering construction process and mechanical equipment, the high-strength concrete prestressed static-pressure pipe pile is widely applied to foundation treatment of high-rise building engineering in large and medium cities, and is the most commonly adopted concrete member in building foundations. At present, the pipe pressing piles in China are mainly produced by a two-stage production process of normal-pressure steam curing and high-pressure steam curing, and the medicine reaches the preset strength and needs to be subjected to two procedures of steam curing and high-temperature and high-pressure steam curing. The production process needs to consume a large amount of energy, and the reduction of the two processes can save a large amount of energy consumption for a pipe pile factory, reduce the emission of boiler waste gas and reduce the investment of environment-friendly equipment.
The high-pressure steam curing link of tubular pile production is cancelled, and the problem can be effectively solved only by adopting the non-steam-pressing tubular pile subjected to normal-pressure steam curing, so that more researches are made in recent years. However, in the past, naphthalene water reducing agents are mostly adopted, and the production process of the naphthalene water reducing agents is polluted greatly, so that a plurality of adverse effects are brought to the environment and the health of constructors; some researches on the adoption of a polycarboxylic acid water reducing agent have shown that the curing time with a mold is usually 10-16 h, the production efficiency is low, and the industrialization is difficult.
The invention discloses a Chinese patent with application number of 201711168992.9, which relates to a special water reducing agent for a steam-curing-free and steam-pressing-free pipe pile used in winter and a preparation method thereof, wherein the water reducing agent comprises, by weight, β -naphthalenesulfonate formaldehyde condensate 80%, aliphatic hydroxysulfonate formaldehyde condensate 10%, sulfamate polymer 5%, triethanolamine 2% and regulator 3%.
Therefore, the environment-friendly steam-free pipe pile water reducer with good water reducing effect, small mixing amount, excellent plasticizing performance and no obvious negative effect on the comprehensive performance of concrete is developed, the energy-saving and environment-friendly pipe pile water reducer with good performance in preparation and use meets the market demand, has wide market value and application prospect, and has very important significance for promoting the development of the concrete additive industry.
Disclosure of Invention
In view of the above, the invention aims to provide an environment-friendly steam-free pipe pile water reducing agent which has the advantages of obvious water reducing effect, small mixing amount, excellent plasticizing performance, no obvious negative effect on the comprehensive performance of concrete, good energy-saving and environment-friendly performance in the preparation and use processes, high reaction activity and low reaction temperature, can effectively enhance the compressive strength, remarkably reduce the hardening and viscosity of concrete, and increase the construction performance of concrete. Meanwhile, the invention also provides a preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent, and the preparation method is simple and easy to implement, is suitable for continuous large-scale production, and has higher social value, economic value and ecological value.
In order to achieve the purpose, the invention adopts the technical scheme that:
the environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: 10-20 parts of 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 5-10 parts of 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl benzene boric acid copolymer, 1-3 parts of 9-fluorenylformic acid, 0.3-0.6 part of initiator, 2-5 parts of plant polysaccharide and 35-45 parts of water.
Preferably, the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
Preferably, the plant polysaccharide is at least one of bamboo leaf polysaccharide, tremella polysaccharide and lentinan.
Further, a method for producing the polycondensate of 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid, comprising the steps of: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into an organic solvent, adding an alkaline catalyst into the organic solvent, stirring and reacting for 8 to 10 hours at 70 to 80 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the organic solvent, adding water and n-hexane with the mass fraction of 3:1 into the organic solvent, carrying out liquid separation to obtain an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -triketone/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate.
Preferably, the molar ratio of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, the organic solvent and the alkaline catalyst is 1:1 (6-10) to (0.3-0.5).
Preferably, the organic solvent is one of tetrahydrofuran, acetone and chloroform.
Preferably, the alkaline catalyst is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
Further, the preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into a high boiling point solvent, stirring and reacting for 4-7 hours under the condition of nitrogen or inert gas, and then performing rotary evaporation to remove the solvent to obtain the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer.
Preferably, the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid, the 4,4 '-diaminostilbene-2, 2' -disulfonic acid, the polyethylene glycol monoallyl ether, the 4-vinylphenylboronic acid, the azobisisobutyronitrile and the high-boiling-point solvent is 0.5:2:1:0.2 (0.03-0.05): 14-20.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the inert gas is one of helium, neon and argon.
The invention also aims to provide a preparation method of the environment-friendly autoclaved-free pipe pile water reducer, which is characterized by comprising the following steps: mixing the components uniformly according to a certain proportion, adding sodium hydroxide, regulating pH to 6.5-7.5, and stirring at 60-80 deg.C for 3-5 hr.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent provided by the invention is simple and feasible, low in preparation cost, high in preparation efficiency and yield, suitable for continuous large-scale production, and high in social value, economic value and ecological value.
(2) The environment-friendly steam-free pipe pile water reducing agent provided by the invention overcomes the defects that the traditional water reducing agent has poor water reducing effect, large mixing amount, large negative influence on the comprehensive performance of a concrete body and easy hardening of the concrete, has the advantages of remarkable water reducing effect, small mixing amount, excellent plasticizing performance, no obvious negative influence on the comprehensive performance of the concrete, good energy-saving and environment-friendly performance in the preparation and use processes, high reaction activity and low reaction temperature, can effectively enhance the compressive strength, remarkably reduce the hardening and viscosity of the concrete and increase the construction performance of the concrete.
(3) The invention provides an environment-friendly steam-free pipe pile water reducing agent, which is added with 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, wherein the main chain of the polycondensate contains a triazine structure, hydrophilic active hydroxyl is introduced through the reaction between amino and epoxy, under the action of steric hindrance and lubrication, the fluidity of concrete is improved, the obstruction to the coagulation action among cement particles is larger, and the slump of the concrete is kept good; the introduced carboxyl structure has a dispersing effect, can improve the dispersing effect of cement particles and control slump loss, and because the triazine structure is arranged on the main chain of the polymer, the branched chain contains the introduced carboxyl, and the molecular chain does not contain a formaldehyde structure, the water reducing effect is better than that of the traditional melamine alkene water reducing agent, and the environmental protection property is better.
(4) The invention provides an environment-friendly steam-free pipe pile water reducing agent, which is added with a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer as a water reducing agent, and because the branched chain of the copolymer contains more active hydrophilic groups, the copolymer is easy to adsorb on the surface of cement due to bridging action, so that the surface of cement particles is provided with the same charge (usually negative charge), an electrostatic repulsion action is formed, the cement particles are promoted to be mutually dispersed, a flocculation structure is disintegrated, and wrapped water is released to participate in flowing, so that the fluidity of a concrete mixture is effectively increased; because the hydrophilic groups have strong polarity, the water reducing agent adsorption film on the surface of the cement particles can form a stable solvated water film with water molecules, and the water film has good lubricating effect and can effectively reduce the sliding resistance among the cement particles, so that the fluidity of concrete is further improved; the water reducing agent has hydrophilic branched chains in the structure and extends into the water solution, so that a hydrophilic three-dimensional adsorption layer with a certain thickness is formed on the surface of the adsorbed cement particles. When the cement particles are close to each other, the adsorption layers begin to overlap, namely, steric hindrance is generated among the cement particles, the more the overlap is, the larger the steric hindrance repulsive force is, the larger the obstruction to the coagulation among the cement particles is, and the slump of the concrete is kept good. The introduced phenylboronic acid structure can further improve the water reducing effect and the comprehensive performance of concrete.
(5) According to the environment-friendly steam-free pipe pile water reducing agent provided by the invention, polyether is introduced into a molecular branched chain to reduce the surface tension of the pipe pile water reducing agent, the internal pore parameters of pipe pile concrete are obviously improved to enhance the compressive strength of the pipe pile water reducing agent, and 9-fluorenecarboxylic acid and plant polysaccharide are introduced to improve the early strength of the pipe pile water reducing agent so as to achieve a steam-free effect.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially.
Example 1
The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: the adhesive comprises, by weight, 10 parts of a 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 5 parts of a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer, 1 part of 9-fluorenylformic acid, 0.3 part of azobisisobutyronitrile, 2 parts of bamboo leaf polysaccharide and 35-45 parts of water.
The preparation method of the polycondensate of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid comprises the following steps: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into tetrahydrofuran, adding sodium hydroxide into the tetrahydrofuran, stirring the mixture to react for 8 hours at 70 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the tetrahydrofuran, adding water and n-hexane with the mass fraction of 3:1 into the mixture, separating the mixture, taking an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate; the molar ratio of the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, tetrahydrofuran and sodium hydroxide is 1:1:6: 0.3.
The preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 4-7 hours under nitrogen, and then performing rotary evaporation to remove the solvent to obtain a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer; the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid to the 4,4 '-diaminostilbene-2, 2' -disulfonic acid to the polyethylene glycol monoallyl ether to the 4-vinylphenylboronic acid to the azobisisobutyronitrile to the dimethyl sulfoxide is 0.5:2:1:0.2:0.03: 14.
The preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent is characterized by comprising the following steps of: the components are uniformly mixed according to a proportion, then sodium hydroxide is added, the PH is adjusted to 6.5, and then the mixture is stirred for 3 hours at the temperature of 60 ℃.
Example 2
The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: 13 parts of 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 6 parts of 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer, 1.5 parts of 9-fluorenylformic acid, 0.4 part of azodiisoheptanonitrile, 3 parts of tremella polysaccharide and 37 parts of water.
The preparation method of the polycondensate of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid comprises the following steps: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into acetone, adding potassium hydroxide into the acetone, stirring and reacting for 8.5 hours at 73 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the acetone, adding water and n-hexane with the mass fraction of 3:1 into the acetone, separating the solution, taking an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate; the molar ratio of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione to the 4, 6-diamino-1, 3, 5-triazine-2-acetic acid to the acetone to the potassium hydroxide is 1:1:7: 0.35.
The preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinylbenzene boric acid and azobisisobutyronitrile into N, N-dimethylformamide, stirring and reacting for 4-7 hours under helium, and then performing rotary evaporation to remove the solvent to obtain a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinylbenzene boric acid copolymer; the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid to the 4,4 '-diaminostilbene-2, 2' -disulfonic acid to the polyethylene glycol monoallyl ether to the 4-vinylphenylboronic acid to the azobisisobutyronitrile to the N, N-dimethylformamide is 0.5:2:1:0.2:0.035: 16.
The preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent is characterized by comprising the following steps of: the components are uniformly mixed according to the proportion, then sodium hydroxide is added, the PH is adjusted to 6.8, and then the mixture is stirred for 3.5 hours at 65 ℃.
Example 3
The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: the adhesive comprises, by weight, 15 parts of a 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 7 parts of a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer, 2 parts of 9-fluorenecarboxylic acid, 0.45 part of azodiisoheptanonitrile, 3.5 parts of lentinan and 40 parts of water.
The preparation method of the polycondensate of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid comprises the following steps: adding 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into chloroform, adding sodium carbonate into the chloroform, stirring and reacting for 9 hours at 75 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the chloroform, adding water and n-hexane with the mass fraction of 3:1 into the chloroform, carrying out liquid separation, taking an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate; the molar ratio of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, chloroform and sodium carbonate is 1:1:8: 0.4.
The preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into N, N-dimethylacetamide, stirring and reacting for 4-7 hours under neon gas, and then performing rotary evaporation to remove the solvent to obtain a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer; the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid to the 4,4 '-diaminostilbene-2, 2' -disulfonic acid to the polyethylene glycol monoallyl ether to the 4-vinylphenylboronic acid to the azobisisobutyronitrile to the N, N-dimethylacetamide is 0.5:2:1:0.2:0.04: 17.
The preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent is characterized by comprising the following steps of: mixing the components uniformly according to a proportion, adding sodium hydroxide, adjusting the pH value to 7, and stirring for 4 hours at 70 ℃.
Example 4
The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: 19 parts of 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 9 parts of 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer, 2.8 parts of 9-fluorenylformic acid, 0.45 part of initiator, 4.5 parts of plant polysaccharide and 44 parts of water; the initiator is formed by mixing azodiisobutyronitrile and azodiisoheptonitrile according to the mass ratio of 3: 5; the plant polysaccharide is formed by mixing bamboo leaf polysaccharide, tremella polysaccharide and lentinan according to a mass ratio of 1:2: 4.
The preparation method of the polycondensate of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid comprises the following steps: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into tetrahydrofuran, adding potassium carbonate into the tetrahydrofuran, stirring and reacting for 9.7 hours at 77 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the tetrahydrofuran, adding water and n-hexane with the mass fraction of 3:1 into the tetrahydrofuran, separating the mixture, taking an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate; the molar ratio of the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, tetrahydrofuran and potassium carbonate is 1:1:9: 0.47.
The preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into a high boiling point solvent, stirring and reacting for 4-7 hours under argon, and then performing rotary evaporation to remove the solvent to obtain a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer; the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid to the 4,4 '-diaminostilbene-2, 2' -disulfonic acid to the polyethylene glycol monoallyl ether to the 4-vinylphenylboronic acid to the azobisisobutyronitrile to the high-boiling-point solvent is 0.5:2:1:0.2:0.045: 19; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:2:3: 2.
The preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent is characterized by comprising the following steps of: the components are uniformly mixed according to the proportion, then sodium hydroxide is added, the PH is adjusted to 7.3, and the mixture is stirred for 4.5 hours at 78 ℃ to obtain the water-based paint.
Example 5
The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: the adhesive comprises, by weight, 20 parts of a 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 10 parts of a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer, 3 parts of 9-fluorenylformic acid, 0.6 part of azobisisobutyronitrile, 5 parts of tremella polysaccharide and 45 parts of water.
The preparation method of the polycondensate of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid comprises the following steps: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into tetrahydrofuran, adding potassium carbonate into the tetrahydrofuran, stirring the mixture for reaction for 10 hours at the temperature of 80 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the tetrahydrofuran, adding water and n-hexane with the mass fraction of 3:1 into the mixture, carrying out liquid separation, taking an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate; the molar ratio of the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, tetrahydrofuran and potassium carbonate is 1:1:10: 0.5.
The preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into N-methyl pyrrolidone, stirring and reacting for 7 hours under nitrogen, and then performing rotary evaporation to remove the solvent to obtain a 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer; the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid to the 4,4 '-diaminostilbene-2, 2' -disulfonic acid to the polyethylene glycol monoallyl ether to the 4-vinylphenylboronic acid to the azobisisobutyronitrile to the N-methylpyrrolidone is 0.5:2:1:0.2:0.05: 20.
The preparation method of the environment-friendly autoclaved-free pipe pile water reducing agent is characterized by comprising the following steps of: mixing the components uniformly according to a proportion, adding sodium hydroxide, adjusting the pH value to 7.5, and stirring at 80 ℃ for 5 hours.
Comparative example 1
This example provides an environment-friendly non-autoclaved water reducer for pipe piles, which has a formulation and a preparation method substantially the same as those of example 1, except that a 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate is not added.
Comparative example 2
The embodiment provides an environment-friendly steam-free pressure pipe pile water reducing agent, the formula and the preparation method of which are basically the same as those in the embodiment 1, except that 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl benzene boric acid copolymer is not added.
Comparative example 3
The embodiment provides an environment-friendly steam-free pressure pipe pile water reducing agent, the formula and the preparation method of which are basically the same as those of embodiment 1, except that 9-fluorenecarboxylic acid and bamboo leaf polysaccharide are not added.
The water reducing agent of the non-autoclaved pipe pile obtained in the embodiments 1-5 and the comparative examples 1-3 adopts southern P.O52.5R cement, the mixing amount is 0.15 percent (folded solid part) of the mass of the cementing material, and the performance of the pipe pile is tested according to GB 13476-; according to GB8076-2008 'concrete admixture', the air content, the slump loss and the like of the concrete are tested. Concrete mixing ratio (kg/m) of non-autoclaved pipe pile3) Comprises the following steps: m (cement), m (mineral powder), m (sand), m (crushed stone), m (water) and m (water reducing agent) are 300:120:710:1350:128: 5.0. Because the influence of the standing time, the heating speed, the constant temperature time, the temperature and the cooling speed on the hydration of the cementing material and the performance of the concrete is complex, the test adopts the following methods: standing for 2 hr after molding, and curing with normal pressure steam (temperature rising rate of 1 deg.C/min, temperature of 90 deg.C, and curing time)4h), cooling to room temperature for 2h, and testing the compressive strength. The results obtained are shown in table 1.
TABLE 1
As can be seen from Table 1, the environment-friendly steam-free pipe pile water reducing agent disclosed by the embodiment of the invention has better water reducing effect, can obviously improve the performances such as the strength of a pipe pile and the like, and has no negative influence on the performance of a concrete body.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The environment-friendly steam-free pressure pipe pile water reducer is characterized by comprising the following components in parts by weight: 10-20 parts of 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate, 5-10 parts of 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl benzene boric acid copolymer, 1-3 parts of 9-fluorenylformic acid, 0.3-0.6 part of initiator, 2-5 parts of plant polysaccharide and 35-45 parts of water.
2. The environment-friendly steam-free pipe pile water reducer according to claim 1, wherein the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile; the plant polysaccharide is at least one of bamboo leaf polysaccharide, tremella polysaccharide and lentinan.
3. The environment-friendly steam-free pipe pile water reducer according to claim 1, wherein the preparation method of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate comprises the following steps: adding 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione and 4, 6-diamino-1, 3, 5-triazine-2-acetic acid into an organic solvent, adding an alkaline catalyst into the organic solvent, stirring and reacting for 8 to 10 hours at 70 to 80 ℃ in an oxygen atmosphere, then carrying out rotary evaporation to remove the organic solvent, adding water and n-hexane with the mass fraction of 3:1 into the organic solvent, carrying out liquid separation to obtain an organic phase, then carrying out rotary evaporation to remove the n-hexane to obtain the 1, 3-bis (oxiranylmethyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -triketone/4, 6-diamino-1, 3, 5-triazine-2-acetic acid polycondensate.
4. The environment-friendly steam-free pipe pile water reducer according to claim 3, wherein the molar ratio of the 1, 3-bis (ethylene oxide methyl) -5- (2-propenyl) -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, 4, 6-diamino-1, 3, 5-triazine-2-acetic acid, the organic solvent and the alkaline catalyst is 1:1 (6-10): 0.3-0.5.
5. The environment-friendly non-autoclaved pipe pile water reducing agent according to claim 3, wherein the organic solvent is one of tetrahydrofuran, acetone and chloroform.
6. The environment-friendly steam-free pipe pile water reducer according to claim 3, wherein the basic catalyst is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
7. The environment-friendly steam-free pipe pile water reducer according to claim 1, wherein the preparation method of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer comprises the following steps: adding 7-amino-3-vinyl-3-cephem-4-carboxylic acid, 4 '-diaminostilbene-2, 2' -disulfonic acid, polyethylene glycol monoallyl ether, 4-vinyl phenylboronic acid and azobisisobutyronitrile into a high boiling point solvent, stirring and reacting for 4-7 hours under the condition of nitrogen or inert gas, and then performing rotary evaporation to remove the solvent to obtain the 7-amino-3-vinyl-3-cephem-4-carboxylic acid/4, 4 '-diaminostilbene-2, 2' -disulfonic acid/polyethylene glycol monoallyl ether/4-vinyl phenylboronic acid copolymer.
8. The environment-friendly steam-free pipe pile water reducer according to claim 7, wherein the mass ratio of the 7-amino-3-vinyl-3-cephem-4-carboxylic acid, the 4,4 '-diaminostilbene-2, 2' -disulfonic acid, the polyethylene glycol monoallyl ether, the 4-vinylphenylboronic acid, the azobisisobutyronitrile and the high boiling point solvent is 0.5:2:1:0.2 (0.03-0.05): 14-20.
9. The environment-friendly non-autoclaved pipe pile water reducing agent according to claim 7, wherein the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the inert gas is one of helium, neon and argon.
10. The environment-friendly steam-free pipe pile water reducer according to any one of claims 1 to 9, wherein the preparation method of the environment-friendly steam-free pipe pile water reducer comprises the following steps: mixing the components uniformly according to a certain proportion, adding sodium hydroxide, regulating pH to 6.5-7.5, and stirring at 60-80 deg.C for 3-5 hr.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194407A (en) * | 2020-10-30 | 2021-01-08 | 赵金山 | Environment-friendly concrete water reducing agent and preparation method thereof |
| CN114180906A (en) * | 2021-11-22 | 2022-03-15 | 蒋雨炎 | Environment-friendly pervious concrete and preparation method thereof |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194407A (en) * | 2020-10-30 | 2021-01-08 | 赵金山 | Environment-friendly concrete water reducing agent and preparation method thereof |
| CN114180906A (en) * | 2021-11-22 | 2022-03-15 | 蒋雨炎 | Environment-friendly pervious concrete and preparation method thereof |
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