CN112142358A - Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption - Google Patents
Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption Download PDFInfo
- Publication number
- CN112142358A CN112142358A CN202010953597.7A CN202010953597A CN112142358A CN 112142358 A CN112142358 A CN 112142358A CN 202010953597 A CN202010953597 A CN 202010953597A CN 112142358 A CN112142358 A CN 112142358A
- Authority
- CN
- China
- Prior art keywords
- parts
- reducing agent
- agent
- anhydrous
- reaction kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
- C04B24/2658—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a formula of an anhydrous polycarboxylic acid water reducing agent, which mainly comprises the following raw materials in parts by weight: 250-350 parts of polycarboxylate superplasticizer mother liquor, 20-70 parts of slow-release high-efficiency water reducing agent, 250-350 parts of unsaturated polyoxyethylene ether macromonomer, 30-60 parts of acrylic acid, 20-30 parts of crosslinking monomer, 50-60 parts of alcohol amine substance, 3-5 parts of antiseptic bactericide, 30-80 parts of sodium gluconate, 100-200 parts of unsaturated amide small monomer, 10-12 parts of thermal decomposition initiator, 13-17 parts of thickening agent, 9-12 parts of organic reducing agent, 10-16 parts of chain transfer agent, 21-23 parts of oxidant, 10-20 parts of auxiliary agent and 10-12 parts of neutralizing agent. The invention has the technical effects of realizing the product performance of low mixing amount, high water reduction and high slump loss resistance, realizing high production efficiency and low energy consumption.
Description
Technical Field
The invention relates to the technical field of anhydrous polycarboxylate superplasticizer formulas and processes, in particular to an anhydrous polycarboxylate superplasticizer formula and a vacuum-pumping preparation method capable of quickly saving energy consumption.
Background
The preparation of the anhydrous polycarboxylic acid water reducing agent comprises a spray drying method, a vacuum dehydration method and a bulk polymerization method at present. The spray drying is suitable for spraying the mother liquid of the water reducing type polycarboxylate superplasticizer with high vitrification temperature. The vacuum dehydration method is suitable for all the polycarboxylic acid water reducing agent mother liquor. The performance of the anhydrous polycarboxylic acid water reducing agent prepared by bulk polymerization is poorer than that of a spray drying method and a vacuum dehydration method. In the vacuum dehydration method, as the water is pumped less and less, the water-reducing concentration of the polycarboxylic acid is higher and lower, the water is dehydrated more and more slowly, so that the production efficiency is low and the energy consumption is high.
Disclosure of Invention
The invention aims to provide a formula of an anhydrous polycarboxylic acid water reducing agent and a vacuum-pumping preparation method capable of quickly saving energy consumption so as to solve the problems in the background technology.
In order to realize the purpose, the invention provides the following technical scheme: the formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 250-350 parts of polycarboxylate superplasticizer mother liquor, 20-70 parts of slow-release high-efficiency water reducing agent, 250-350 parts of unsaturated polyoxyethylene ether macromonomer, 30-60 parts of acrylic acid, 20-30 parts of crosslinking monomer, 50-60 parts of alcohol amine substance, 3-5 parts of antiseptic bactericide, 30-80 parts of sodium gluconate, 100-200 parts of unsaturated amide small monomer, 10-12 parts of thermal decomposition initiator, 13-17 parts of thickening agent, 9-12 parts of organic reducing agent, 10-16 parts of chain transfer agent, 21-23 parts of oxidant, 10-20 parts of auxiliary agent and 10-12 parts of neutralizing agent.
Preferably, the crosslinking monomer is a silicone crosslinking monomer, and comprises one or more of ethyl orthosilicate, methyl orthosilicate and trimethoxy silane.
Preferably, the unsaturated polyoxyethylene ether macromonomer is formed by gradually performing addition polymerization on ethylene oxide and water or ethylene glycol.
Preferably, the thermal decomposition initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, azodiisobutyronitrile dimethyl ester, ammonium persulfate and potassium persulfate.
Preferably, the neutralizing agent is one or more of potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, ethanolamine, diethanolamine and triethanolamine.
Preferably, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
Preferably, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate or polyethylene glycol dimethacrylate.
Preferably, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline and N, N-diethylaniline.
Preferably, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is polyether sodium phosphate and polyether sodium sulfate.
A vacuum-pumping preparation method for an anhydrous polycarboxylic acid water reducing agent, which can quickly save energy consumption, comprises the following steps:
the method comprises the following steps: preparing a slow-release high-efficiency water reducing agent: the relative molar ratio of the unsaturated amide small monomer to the unsaturated polyoxyethylene ether large monomer is 4-5, the molecular weight of the water reducing agent is 15000-25000, the reaction time is 3-6 h, and the reaction temperature is 60-100 ℃ to synthesize the slow-release high-efficiency water reducing agent;
step two: preparing an additive emulsion: stirring and mixing the polycarboxylate superplasticizer mother liquor, acrylic acid and alcohol amine substances for 0.5-1 h at the rotating speed of 800-1000 r/min; adding a crosslinking monomer into the mixed solution obtained in the first step, and mixing and stirring for 0.25-0.5 h to obtain an additive emulsion;
step three: preparing a regulator: adding deionized water into a material preparation pot or a material preparation cylinder according to the formula amount, and placing the mixture under a high-speed dispersion machine; starting a high-speed dispersion machine, adjusting the gear to 300-500 r/min, stirring, uniformly adding an antiseptic bactericide, sodium gluconate and an auxiliary agent according to the formula amount, and stirring for 20-40 min to prepare a regulator;
step four: placing the prepared slow-release high-efficiency water reducing agent, the additive emulsion and the regulator in a thermocouple reaction kettle, keeping the temperature at 50-60 ℃, and continuously stirring for 1-2 hours to prepare a mixed additive;
step five: adding a thermal decomposition initiator and an organic reducing agent into the mixed additive prepared in the fourth step, keeping the temperature at 40-50 ℃, and continuously stirring for 30-50 hours to prepare a prefabricated mixed additive;
step six: preparing an auxiliary preparation: adding a thickening agent, an organic reducing agent, a chain transfer agent and an oxidizing agent into the mixed additive prepared in the fourth step, keeping the temperature at 60-70 ℃, and continuously stirring for 20-40 h to prepare an auxiliary preparation;
step seven: polymerization: mixing and stirring the prepared slow-release high-efficiency water reducing agent, the additive emulsion, the regulator, the prefabricated mixed additive and the auxiliary preparation, keeping 120 revolutions per minute, and stirring for 1-2 hours to obtain a polycarboxylic acid mother solution;
step eight: placing the polycarboxylic acid mother liquor prepared in the seventh step on a reaction kettle, and installing 2 elongated rotten steel pipes by utilizing the principle that a capillary tube generates a boiling center, wherein one end of the elongated rotten steel pipes is placed 15cm away from the bottom of the reaction kettle, and the other end of the elongated rotten steel pipes is provided with a valve outside the reaction kettle; and the other end of the reaction kettle is placed in the middle of the height of the reaction kettle, the other end of the reaction kettle is provided with a valve outside the reaction kettle, certain air quantity is adjusted through the valve during vacuum pumping, a boiling center is formed in the reaction kettle filled with polycarboxylic acid mother liquor, and thus moisture is rapidly pumped out to prepare the anhydrous polycarboxylic acid water reducing agent.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the solvent type or powder type polycarboxylate superplasticizer which is sold in the market at present and has good water reducing and slump retaining performances, the water reducing solid polycarboxylate superplasticizer provided by the invention has the advantages that the performance is unchanged after dissolution, the neat paste dispersing performance, the water reducing and dispersing performance, the fluidity and the slump retaining capacity are excellent, and the product performance with low dosage, high water reducing and high slump retaining is realized.
2. The anhydrous polycarboxylic acid water reducing agent formula and the vacuum pumping preparation method capable of quickly saving energy consumption utilize the principle that a capillary tube generates a boiling center, 2 slender and unbroken steel tubes are arranged on a reaction kettle, one end of each tube is placed 15cm away from the bottom of the reaction kettle, and the other end of each tube is provided with a valve outside the reaction kettle; the other end is arranged in the middle of the height of the reaction kettle, and the other end is provided with a valve outside the reaction kettle. During the evacuation, a certain amount of air is adjusted through a valve, a boiling center is formed in a reaction kettle filled with the polycarboxylic acid mother liquor, so that moisture is rapidly pumped out, and the production efficiency is high and the energy consumption is low.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 250 parts of polycarboxylate superplasticizer mother liquor, 20 parts of slow-release high-efficiency water reducing agent, 250 parts of unsaturated polyoxyethylene ether macromonomer, 30 parts of acrylic acid, 20 parts of crosslinking monomer, 50 parts of alcohol amine substance, 3 parts of antiseptic bactericide, 30 parts of sodium gluconate, 100 parts of unsaturated amide small monomer, 10 parts of thermal decomposition initiator, 13 parts of thickener, 9 parts of organic reducing agent, 10 parts of chain transfer agent, 21 parts of oxidant, 10 parts of assistant and 10 parts of neutralizer.
In this embodiment, the crosslinking monomer is an organic silicon crosslinking monomer, and includes one or more of tetraethoxysilane, methyl orthosilicate, and trimethoxysilane.
In this embodiment, the unsaturated polyoxyethylene ether macromonomer is formed by stepwise addition polymerization of ethylene oxide and water or ethylene glycol.
In this embodiment, the thermal decomposition initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, and potassium persulfate.
In this embodiment, the neutralizing agent is one or more of a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution, ethanolamine, diethanolamine, and triethanolamine.
In this embodiment, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
In this embodiment, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate, or polyethylene glycol dimethacrylate.
In this embodiment, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline, and N, N-diethylaniline.
In this embodiment, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
Example two
The formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 350 parts of polycarboxylic acid water reducer mother liquor, 70 parts of slow-release high-efficiency water reducer, 350 parts of unsaturated polyoxyethylene ether macromonomer, 60 parts of acrylic acid, 30 parts of crosslinking monomer, 60 parts of alcohol amine substance, 5 parts of antiseptic bactericide, 80 parts of sodium gluconate, 200 parts of unsaturated amide small monomer, 12 parts of thermal decomposition initiator, 17 parts of thickener, 12 parts of organic reducing agent, 16 parts of chain transfer agent, 23 parts of oxidant, 20 parts of auxiliary agent and 12 parts of neutralizing agent.
In this embodiment, the crosslinking monomer is an organic silicon crosslinking monomer, and includes one or more of tetraethoxysilane, methyl orthosilicate, and trimethoxysilane.
In this embodiment, the unsaturated polyoxyethylene ether macromonomer is formed by stepwise addition polymerization of ethylene oxide and water or ethylene glycol.
In this embodiment, the thermal decomposition initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, and potassium persulfate.
In this embodiment, the neutralizing agent is one or more of a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution, ethanolamine, diethanolamine, and triethanolamine.
In this embodiment, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
In this embodiment, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate, or polyethylene glycol dimethacrylate.
In this embodiment, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline, and N, N-diethylaniline.
In this embodiment, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
EXAMPLE III
The formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 300 parts of polycarboxylate superplasticizer mother liquor, 45 parts of slow-release high-efficiency water reducing agent, 300 parts of unsaturated polyoxyethylene ether macromonomer, 45 parts of acrylic acid, 25 parts of crosslinking monomer, 55 parts of alcohol amine substance, 4 parts of antiseptic bactericide, 60 parts of sodium gluconate, 150 parts of unsaturated amide small monomer, 11 parts of thermal decomposition initiator, 15 parts of thickener, 10.5 parts of organic reducing agent, 12 parts of chain transfer agent, 22 parts of oxidant, 15 parts of assistant and 11 parts of neutralizer.
In this embodiment, the crosslinking monomer is an organic silicon crosslinking monomer, and includes one or more of tetraethoxysilane, methyl orthosilicate, and trimethoxysilane.
In this embodiment, the unsaturated polyoxyethylene ether macromonomer is formed by stepwise addition polymerization of ethylene oxide and water or ethylene glycol.
In this embodiment, the thermal decomposition initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, and potassium persulfate.
In this embodiment, the neutralizing agent is one or more of a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution, ethanolamine, diethanolamine, and triethanolamine.
In this embodiment, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
In this embodiment, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate, or polyethylene glycol dimethacrylate.
In this embodiment, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline, and N, N-diethylaniline.
In this embodiment, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
Example four
The formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: the slow-release efficient water reducing agent comprises, by weight, 20 parts of a slow-release efficient water reducing agent, 250 parts of an unsaturated polyoxyethylene ether macromonomer, 30 parts of acrylic acid, 20 parts of a crosslinking monomer, 50 parts of alcohol amine substances, 3 parts of an anticorrosive bactericide, 30 parts of sodium gluconate, 100 parts of an unsaturated amide small monomer, 10 parts of a thermal decomposition initiator, 13 parts of a thickening agent, 9 parts of an organic reducing agent, 10 parts of a chain transfer agent, 21 parts of an oxidizing agent, 10 parts of an auxiliary agent and 10 parts of a neutralizing agent.
In this embodiment, the crosslinking monomer is an organic silicon crosslinking monomer, and includes one or more of tetraethoxysilane, methyl orthosilicate, and trimethoxysilane.
In this embodiment, the unsaturated polyoxyethylene ether macromonomer is formed by stepwise addition polymerization of ethylene oxide and water or ethylene glycol.
In this embodiment, the thermal decomposition initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, and potassium persulfate.
In this embodiment, the neutralizing agent is one or more of a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution, ethanolamine, diethanolamine, and triethanolamine.
In this embodiment, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
In this embodiment, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate, or polyethylene glycol dimethacrylate.
In this embodiment, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline, and N, N-diethylaniline.
In this embodiment, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
EXAMPLE five
The formula of the anhydrous polycarboxylate superplasticizer mainly comprises the following raw materials in parts by weight: 250 parts of polycarboxylate superplasticizer mother liquor, 250 parts of unsaturated polyoxyethylene ether macromonomer, 30 parts of acrylic acid, 20 parts of crosslinking monomer, 50 parts of alcohol amine substance, 3 parts of antiseptic bactericide, 30 parts of sodium gluconate, 100 parts of unsaturated amide small monomer, 10 parts of thermal decomposition initiator, 13 parts of thickening agent, 9 parts of organic reducing agent, 10 parts of chain transfer agent, 21 parts of oxidant, 10 parts of auxiliary agent and 10 parts of neutralizing agent.
In this embodiment, the crosslinking monomer is an organic silicon crosslinking monomer, and includes one or more of tetraethoxysilane, methyl orthosilicate, and trimethoxysilane.
In this embodiment, the unsaturated polyoxyethylene ether macromonomer is formed by stepwise addition polymerization of ethylene oxide and water or ethylene glycol.
In this embodiment, the thermal decomposition initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, and potassium persulfate.
In this embodiment, the neutralizing agent is one or more of a potassium hydroxide aqueous solution, a sodium hydroxide aqueous solution, ethanolamine, diethanolamine, and triethanolamine.
In this embodiment, the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of a carboxyl-containing graft copolymer.
In this embodiment, the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate, or polyethylene glycol dimethacrylate.
In this embodiment, the organic reducing agent is one or more of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline, and N, N-diethylaniline.
In this embodiment, the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is sodium polyether phosphate and sodium polyether sulfate.
The anhydrous polycarboxylic acid water reducing agent is prepared by the following preparation methods in the embodiments:
a vacuum-pumping preparation method for an anhydrous polycarboxylic acid water reducing agent, which can quickly save energy consumption, comprises the following steps:
the method comprises the following steps: preparing a slow-release high-efficiency water reducing agent: the relative molar ratio of the unsaturated amide small monomer to the unsaturated polyoxyethylene ether large monomer is 4-5, the molecular weight of the water reducing agent is 15000-25000, the reaction time is 3-6 h, and the reaction temperature is 60-100 ℃ to synthesize the slow-release high-efficiency water reducing agent;
step two: preparing an additive emulsion: stirring and mixing the polycarboxylate superplasticizer mother liquor, acrylic acid and alcohol amine substances for 0.5-1 h at the rotating speed of 800-1000 r/min; adding a crosslinking monomer into the mixed solution obtained in the first step, and mixing and stirring for 0.25-0.5 h to obtain an additive emulsion;
step three: preparing a regulator: adding deionized water into a material preparation pot or a material preparation cylinder according to the formula amount, and placing the mixture under a high-speed dispersion machine; starting a high-speed dispersion machine, adjusting the gear to 300-500 r/min, stirring, uniformly adding an antiseptic bactericide, sodium gluconate and an auxiliary agent according to the formula amount, and stirring for 20-40 min to prepare a regulator;
step four: placing the prepared slow-release high-efficiency water reducing agent, the additive emulsion and the regulator in a thermocouple reaction kettle, keeping the temperature at 50-60 ℃, and continuously stirring for 1-2 hours to prepare a mixed additive;
step five: adding a thermal decomposition initiator and an organic reducing agent into the mixed additive prepared in the fourth step, keeping the temperature at 40-50 ℃, and continuously stirring for 30-50 hours to prepare a prefabricated mixed additive;
step six: preparing an auxiliary preparation: adding a thickening agent, an organic reducing agent, a chain transfer agent and an oxidizing agent into the mixed additive prepared in the fourth step, keeping the temperature at 60-70 ℃, and continuously stirring for 20-40 h to prepare an auxiliary preparation;
step seven: polymerization: mixing and stirring the prepared slow-release high-efficiency water reducing agent, the additive emulsion, the regulator, the prefabricated mixed additive and the auxiliary preparation, keeping 120 revolutions per minute, and stirring for 1-2 hours to obtain a polycarboxylic acid mother solution;
step eight: placing the polycarboxylic acid mother liquor prepared in the seventh step on a reaction kettle, and installing 2 elongated rotten steel pipes by utilizing the principle that a capillary tube generates a boiling center, wherein one end of the elongated rotten steel pipes is placed 15cm away from the bottom of the reaction kettle, and the other end of the elongated rotten steel pipes is provided with a valve outside the reaction kettle; and the other end of the reaction kettle is placed in the middle of the height of the reaction kettle, the other end of the reaction kettle is provided with a valve outside the reaction kettle, certain air quantity is adjusted through the valve during vacuum pumping, a boiling center is formed in the reaction kettle filled with polycarboxylic acid mother liquor, and thus moisture is rapidly pumped out to prepare the anhydrous polycarboxylic acid water reducing agent.
Experiment one: the test data of the slump and the slump of the anhydrous polycarboxylate water reducer prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment after being applied to the same concrete are shown in the following table:
and (3) analyzing an experimental result: the fluidity and slump-retaining ability of the anhydrous polycarboxylic acid water reducing agent prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment are obviously higher than those of the anhydrous polycarboxylic acid water reducing agent in the prior art.
Experiment two: the test data of the production efficiency and the energy consumption of the anhydrous polycarboxylate water reducer prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment and the existing anhydrous polycarboxylate water reducer are respectively applied to the same concrete, and are shown in the following table:
and (3) analyzing an experimental result: the production efficiency of the anhydrous polycarboxylic acid water reducer prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment is obviously higher than that of the anhydrous polycarboxylic acid water reducer in the prior art; the energy consumption of the anhydrous polycarboxylic acid water reducer prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment is obviously lower than that of the anhydrous polycarboxylic acid water reducer in the prior art.
The invention has the beneficial effects that: compared with the solvent type or powder type polycarboxylate superplasticizer which is sold in the market at present and has good water reducing and slump retaining performances, the water reducing solid polycarboxylate superplasticizer provided by the invention has the advantages that the performance is unchanged after dissolution, the neat paste dispersing performance, the water reducing and dispersing performance, the fluidity and the slump retaining capacity are excellent, and the product performance with low dosage, high water reducing and high slump retaining is realized. The anhydrous polycarboxylic acid water reducing agent formula and the vacuum pumping preparation method capable of quickly saving energy consumption utilize the principle that a capillary tube generates a boiling center, 2 slender and unbroken steel tubes are arranged on a reaction kettle, one end of each tube is placed 15cm away from the bottom of the reaction kettle, and the other end of each tube is provided with a valve outside the reaction kettle; the other end is arranged in the middle of the height of the reaction kettle, and the other end is provided with a valve outside the reaction kettle. During the evacuation, a certain amount of air is adjusted through a valve, a boiling center is formed in a reaction kettle filled with the polycarboxylic acid mother liquor, so that moisture is rapidly pumped out, and the production efficiency is high and the energy consumption is low.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. The formula of the anhydrous polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight: the raw material components mainly comprise the following components in parts by weight: 250-350 parts of polycarboxylate superplasticizer mother liquor, 20-70 parts of slow-release high-efficiency water reducing agent, 250-350 parts of unsaturated polyoxyethylene ether macromonomer, 30-60 parts of acrylic acid, 20-30 parts of crosslinking monomer, 50-60 parts of alcohol amine substance, 3-5 parts of antiseptic bactericide, 30-80 parts of sodium gluconate, 100-200 parts of unsaturated amide small monomer, 10-12 parts of thermal decomposition initiator, 13-17 parts of thickening agent, 9-12 parts of organic reducing agent, 10-16 parts of chain transfer agent, 21-23 parts of oxidant, 10-20 parts of auxiliary agent and 10-12 parts of neutralizing agent.
2. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the crosslinking monomer is an organic silicon crosslinking monomer and comprises one or more of tetraethoxysilane, methyl orthosilicate and trimethoxy silane.
3. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the unsaturated polyoxyethylene ether macromonomer is formed by gradually carrying out addition polymerization on ethylene oxide and water or ethylene glycol.
4. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the thermal decomposition initiator is one or a mixture of azodiisobutyronitrile, azodiisoheptonitrile, dimethyl azodiisobutyrate, ammonium persulfate and potassium persulfate.
5. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the neutralizing agent is one or more of potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, ethanolamine, diethanolamine and triethanolamine.
6. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the polycarboxylate superplasticizer mother liquor is a surfactant with a molecular structure of carboxyl-containing graft copolymer.
7. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the crosslinking monomer is ethylene glycol dimethacrylate, triethylene glycol dimethacrylate or polyethylene glycol dimethacrylate.
8. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the organic reducing agent is one or a mixture of L-ascorbic acid, N-methylaniline, N-ethylaniline, N-dimethylaniline and N, N-diethylaniline.
9. The anhydrous polycarboxylate water reducer formula according to claim 1, characterized in that: the oxidant is hydrogen peroxide and ammonium persulfate, and the auxiliary agent is polyether sodium phosphate and polyether sodium sulfate.
10. A vacuum-pumping preparation method for an anhydrous polycarboxylate superplasticizer, which can quickly save energy consumption, is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: preparing a slow-release high-efficiency water reducing agent: the relative molar ratio of the unsaturated amide small monomer to the unsaturated polyoxyethylene ether large monomer is 4-5, the molecular weight of the water reducing agent is 15000-25000, the reaction time is 3-6 h, and the reaction temperature is 60-100 ℃ to synthesize the slow-release high-efficiency water reducing agent;
step two: preparing an additive emulsion: stirring and mixing the polycarboxylate superplasticizer mother liquor, acrylic acid and alcohol amine substances for 0.5-1 h at the rotating speed of 800-1000 r/min; adding a crosslinking monomer into the mixed solution obtained in the first step, and mixing and stirring for 0.25-0.5 h to obtain an additive emulsion;
step three: preparing a regulator: adding deionized water into a material preparation pot or a material preparation cylinder according to the formula amount, and placing the mixture under a high-speed dispersion machine; starting a high-speed dispersion machine, adjusting the gear to 300-500 r/min, stirring, uniformly adding an antiseptic bactericide, sodium gluconate and an auxiliary agent according to the formula amount, and stirring for 20-40 min to prepare a regulator;
step four: placing the prepared slow-release high-efficiency water reducing agent, the additive emulsion and the regulator in a thermocouple reaction kettle, keeping the temperature at 50-60 ℃, and continuously stirring for 1-2 hours to prepare a mixed additive;
step five: adding a thermal decomposition initiator and an organic reducing agent into the mixed additive prepared in the fourth step, keeping the temperature at 40-50 ℃, and continuously stirring for 30-50 hours to prepare a prefabricated mixed additive;
step six: preparing an auxiliary preparation: adding a thickening agent, an organic reducing agent, a chain transfer agent and an oxidizing agent into the mixed additive prepared in the fourth step, keeping the temperature at 60-70 ℃, and continuously stirring for 20-40 h to prepare an auxiliary preparation;
step seven: polymerization: mixing and stirring the prepared slow-release high-efficiency water reducing agent, the additive emulsion, the regulator, the prefabricated mixed additive and the auxiliary preparation, keeping 120 revolutions per minute, and stirring for 1-2 hours to obtain a polycarboxylic acid mother solution;
step eight: placing the polycarboxylic acid mother liquor prepared in the seventh step on a reaction kettle, and installing 2 elongated rotten steel pipes by utilizing the principle that a capillary tube generates a boiling center, wherein one end of the elongated rotten steel pipes is placed 15cm away from the bottom of the reaction kettle, and the other end of the elongated rotten steel pipes is provided with a valve outside the reaction kettle; and the other end of the reaction kettle is placed in the middle of the height of the reaction kettle, the other end of the reaction kettle is provided with a valve outside the reaction kettle, certain air quantity is adjusted through the valve during vacuum pumping, a boiling center is formed in the reaction kettle filled with polycarboxylic acid mother liquor, and thus moisture is rapidly pumped out to prepare the anhydrous polycarboxylic acid water reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010953597.7A CN112142358A (en) | 2020-09-11 | 2020-09-11 | Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010953597.7A CN112142358A (en) | 2020-09-11 | 2020-09-11 | Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112142358A true CN112142358A (en) | 2020-12-29 |
Family
ID=73890981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010953597.7A Pending CN112142358A (en) | 2020-09-11 | 2020-09-11 | Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112142358A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409296A (en) * | 2022-01-20 | 2022-04-29 | 陈襄雨 | Anti-corrosion and anti-rust water reducing agent and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815882A (en) * | 2012-08-03 | 2012-12-12 | 山西科腾环保科技有限公司 | High-performance water reducer of polycarboxylic acid, and preparation method thereof |
| CN105111387A (en) * | 2015-10-08 | 2015-12-02 | 南京瑞迪高新技术有限公司 | Preparation method of low entrained-air type solid polycarboxylic water reducer |
| CN106478896A (en) * | 2016-10-31 | 2017-03-08 | 科之杰新材料集团有限公司 | A kind of preparation method of comprehensive polycarboxylate water-reducer |
| CN107163197A (en) * | 2017-04-28 | 2017-09-15 | 江苏尼高科技有限公司 | High-performance solid polycarboxylate water-reducer and preparation method thereof |
| CN107555831A (en) * | 2017-09-30 | 2018-01-09 | 江苏兆佳建材科技有限公司 | A kind of chlorine-free type polycarboxylate water-reducer |
-
2020
- 2020-09-11 CN CN202010953597.7A patent/CN112142358A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815882A (en) * | 2012-08-03 | 2012-12-12 | 山西科腾环保科技有限公司 | High-performance water reducer of polycarboxylic acid, and preparation method thereof |
| CN105111387A (en) * | 2015-10-08 | 2015-12-02 | 南京瑞迪高新技术有限公司 | Preparation method of low entrained-air type solid polycarboxylic water reducer |
| CN106478896A (en) * | 2016-10-31 | 2017-03-08 | 科之杰新材料集团有限公司 | A kind of preparation method of comprehensive polycarboxylate water-reducer |
| CN107163197A (en) * | 2017-04-28 | 2017-09-15 | 江苏尼高科技有限公司 | High-performance solid polycarboxylate water-reducer and preparation method thereof |
| CN107555831A (en) * | 2017-09-30 | 2018-01-09 | 江苏兆佳建材科技有限公司 | A kind of chlorine-free type polycarboxylate water-reducer |
Non-Patent Citations (1)
| Title |
|---|
| 张开诚: "《化学实验教程》", 28 February 2014, 华中科技大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409296A (en) * | 2022-01-20 | 2022-04-29 | 陈襄雨 | Anti-corrosion and anti-rust water reducing agent and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104496256B (en) | Polycarboxylate superplasticizer and preparation method thereof | |
| CN108948288B (en) | Preparation method of crosslinking type polycarboxylate superplasticizer by adopting carboxyl functional monomer | |
| CN105236800B (en) | A kind of poly carboxylic acid series water reducer mother liquor and its preparation method and application | |
| CN106317342B (en) | A kind of sustained release Early-strength polycarboxylate superplasticizer and preparation method thereof | |
| CN104692699B (en) | A kind of early-strength ethers polycarboxylic acid water reducing agent and preparation method thereof | |
| CN114195421A (en) | Preparation method of polycarboxylic acid admixture for machine-made sand concrete | |
| CN104774293B (en) | A kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof | |
| CN106749983A (en) | A kind of ultra early-strength polycarboxylate water-reducer and preparation method thereof | |
| CN108707211A (en) | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof | |
| CN110229285B (en) | Preparation method of early-strength polycarboxylate superplasticizer | |
| CN109053972A (en) | A kind of anti-chamotte mould polycarboxylate water-reducer preparation method of barrier intercalation | |
| CN112142358A (en) | Anhydrous polycarboxylate superplasticizer formula and vacuum-pumping preparation method capable of quickly saving energy consumption | |
| CN107200839B (en) | Methallyl alcohol random polyether and preparation method thereof | |
| CN112126022A (en) | Formula and preparation method of polycarboxylate superplasticizer | |
| CN105524230B (en) | A kind of preparation method of high-efficiency water-reducing agent of poly-carboxylic acid | |
| CN110698609A (en) | High-performance polycarboxylic acid water reducing agent synthesized at normal temperature, preparation method and application thereof | |
| CN109053970B (en) | Preparation method of anti-mud polycarboxylic slump retaining agent adopting carboxyl functional monomer | |
| CN114349914B (en) | Ferrocene modified anti-mud polycarboxylate water reducer and preparation method thereof | |
| CN112358221A (en) | Formula and preparation method of water-reducing solid polycarboxylate superplasticizer | |
| CN112028533A (en) | Early-strength viscosity-reduction type polycarboxylate superplasticizer and preparation method thereof | |
| CN108218278A (en) | A kind of preparation method of esters high dispersive high-slump-retentionpolycarboxylate polycarboxylate water reducer | |
| CN111087552A (en) | Synthetic method of polycarboxylic acid water reducer with high water reducing rate and mud resistance | |
| CN106883403A (en) | The preparation method of maleic acid mono alkyl ester polyether | |
| CN113278112A (en) | Polycarboxylate superplasticizer miscible with defoaming agent and preparation method thereof | |
| CN111825372B (en) | Polycarboxylic acid high-performance water reducing agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201229 |
|
| RJ01 | Rejection of invention patent application after publication |