CN114772971A - Preparation method of powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar - Google Patents
Preparation method of powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar Download PDFInfo
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- CN114772971A CN114772971A CN202210381070.0A CN202210381070A CN114772971A CN 114772971 A CN114772971 A CN 114772971A CN 202210381070 A CN202210381070 A CN 202210381070A CN 114772971 A CN114772971 A CN 114772971A
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- water
- gypsum
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- calcium hydroxide
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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
- 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
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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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method of a powder polycarboxylate water reducer for gypsum-based dry powder mortar, which is prepared from the following components: polyether macromonomer, acrylic acid, chain transfer agent, oxidant, reduction initiator, alkaline substance, separant, soft water and water; the polyether macromonomer is methyl allyl polyoxyethylene ether 3000; the alkaline substance is calcium hydroxide; the chain transfer agent is mercaptopropionic acid; the separant is a mixture of white carbon black and calcium hydroxide; the oxidant is hydrogen peroxide, and the reducing agent is sodium formaldehyde sulfoxylate; the invention reduces the influence of free sulfate on the polycarboxylic acid water reducing agent dispersed gypsum. That is, free sulfate radicals and calcium ions are combined to form insoluble calcium sulfate, so that the influence of a polycarboxylate water reducing agent on gypsum dispersion is reduced or not influenced.
Description
Technical Field
The invention relates to preparation of a powdery polycarboxylate superplasticizer, in particular to a powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar.
Background
At present, the main domestic rubber materials are divided into two types of dry powder mortar: cement-based dry-mixed mortar and gypsum-based dry-mixed mortar.
A set of mature technology has been formed in China for the powder polycarboxylate superplasticizer for the cement-based dry powder mortar, and the powder polycarboxylate superplasticizer for the gypsum-based dry powder mortar is used for dry start. In recent years, the reuse of industrial gypsum by-products has been on the rise for environmental reasons and the call for the reuse of by-products has increased. China is a country with large discharge amount of industrial by-product gypsum and a country with large utilization of gypsum resources. The application of the industrial side gypsum has positive environmental protection significance and can save precious natural gypsum resources.
The original powder polycarboxylate superplasticizer is suitable for portland cement, but is not suitable for sulfate gypsum, and causes more or less problems. Such as insufficient water reduction or insufficient retention. Therefore, the invention of the powdery polycarboxylate superplasticizer suitable for gypsum-based dry mortar is urgent.
Disclosure of Invention
The invention discloses a preparation method of a powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar, aiming at the problems in the prior art, and based on the principle that the gypsum contains free sulfate because the gypsum has low water reducing rate or low retentivity, and the free sulfate reduces the polycarboxylate superplasticizer to disperse the gypsum, the powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar of the invention can solve the defects in the prior art.
The invention is realized by the following steps:
a preparation method of a powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar is characterized in that the superplasticizer is prepared from the following components: polyether macromonomer, acrylic acid, chain transfer agent, oxidant, reduction initiator, alkaline substance, separant, soft water and water; the polyether macromonomer is methyl allyl polyoxyethylene ether 3000; the alkaline substance is calcium hydroxide; the chain transfer agent is mercaptopropionic acid; the separant is a mixture of white carbon black and calcium hydroxide, wherein the white carbon black accounts for 2% of the powdery polycarboxylic acid water reducer, and the calcium hydroxide accounts for 5-10% of the powdery polycarboxylic acid water reducer; the oxidant is hydrogen peroxide, and the reducing agent is sodium formaldehyde sulfoxylate.
Further, the soft water and the water are added in batches.
Further, the acrylic acid, the mercaptopropionic acid and the soft water are used as materials A, the rongalite and the water are used as materials B, and the preparation method of the water reducing agent comprises the following steps:
starting stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dripping device, adding soft water, methallyl polyoxyethylene ether 3000 and hydrogen peroxide, and then dripping a material A and a material B simultaneously, wherein the material A is as follows: acrylic acid, mercaptopropionic acid, and soft water; the material B is as follows: uniformly dripping the sodium formaldehyde sulfoxylate blocks, water and the material A for 3 hours, uniformly dripping the material B for 3.5 hours, curing the material B for 1.5 hours after the material B is dripped, then adding a calcium hydroxide aqueous suspension, adjusting the pH to 9-10, and supplementing water until the solid content is 40% to obtain a 40% polycarboxylic acid water reducing agent solution;
pumping 40% of polycarboxylate superplasticizer solution into a centrifugal spray drying tower through a peristaltic pump, and simultaneously uniformly adding a separant into an air inlet pipeline; and controlling the air inlet temperature and the air outlet temperature to obtain the polycarboxylic acid water reducing agent powder with good fluidity.
Further, stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dropping device, adding 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide, and then dropping the material A and the material B simultaneously; the material A is as follows: 45 g of acrylic acid, 1.5 g of mercaptopropionic acid, 150 g of soft water); the material B is as follows: 1 g of sodium formaldehyde sulfoxylate and 100 g of water, wherein the material A is uniformly dripped after 3 hours, the material B is uniformly dripped after 3.5 hours, after the material B is dripped, curing is carried out for 1.5 hours, then 32% of calcium hydroxide aqueous suspension is added, the pH value is adjusted to 9-12, and water is supplemented until the solid content is 40% to obtain 40% of polycarboxylic acid water reducing agent solution;
pumping 40% of polycarboxylate superplasticizer solution into a centrifugal spray drying tower through a peristaltic pump, and simultaneously uniformly adding a separant into an air inlet pipeline; the white carbon black accounts for 2 percent of the powdery polycarboxylate water reducer, and the calcium hydroxide accounts for 5 to 10 percent of the powdery polycarboxylate water reducer; and controlling the air inlet temperature and the air outlet temperature to obtain the polycarboxylic acid water reducing agent powder with good fluidity.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method comprises the steps of polymerizing polyether macromonomer and acrylic acid at normal temperature under the conditions of a chain transfer agent, an oxidant and a reduction initiator, adjusting the pH to 8-11 by adopting an alkaline substance after polymerization, and then preparing the powdery polycarboxylate superplasticizer suitable for gypsum dry powder mortar by spray drying and an isolating agent. The water reducing agent disclosed by the invention can reduce the influence of free sulfate on the dispersion of the polycarboxylate water reducing agent in gypsum, namely, the free sulfate is combined with calcium ions to form calcium sulfate which is difficult to dissolve, so that the influence of the polycarboxylate water reducing agent on the gypsum dispersion is reduced or not influenced.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention more clear, the present invention is further described in detail by referring to examples below. It should be noted that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Starting stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dripping device, adding 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide, simultaneously dripping materials A (45 g of acrylic acid, 1.5 g of mercaptopropionic acid and 150 g of soft water) and materials B (1 g of rongalite and 100 g of water), uniformly dripping the materials A for 3 hours, uniformly dripping the materials B for 3.5 hours, curing for 1.5 hours after dripping the materials B, adding 32% of calcium hydroxide aqueous suspension, regulating the pH to 9-10, and supplementing water until the solid content is 40% to obtain a 40% polycarboxylic acid water reducer solution. 40% of polycarboxylate water reducing agent solution is pumped into a centrifugal spray drying tower through a peristaltic pump, and meanwhile, an isolating agent (white carbon black accounts for 2% of the powder polycarboxylate water reducing agent, and calcium hydroxide accounts for 5% of the powder polycarboxylate water reducing agent) is uniformly added at an air inlet pipeline. The polycarboxylate superplasticizer powder with good fluidity can be obtained by controlling certain air inlet temperature and air outlet temperature.
Example two
Stirring is started in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dripping device, 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide are added, then materials A (45 g of acrylic acid, 1.5 g of mercaptopropionic acid and 150 g of soft water) and materials B (1 g of sodium formaldehyde sulfoxylate and 100 g of water) are simultaneously dripped, the materials A are uniformly dripped for 3 hours, the materials B are uniformly dripped for 3.5 hours, after the materials B are dripped, the materials B are cured for 1.5 hours, then 32% of calcium hydroxide aqueous suspension is added, the pH is regulated to 10-11, and water is supplemented until the solid content is 40%, so as to obtain 40% of polycarboxylic acid water reducing agent solution. 40% of polycarboxylate water reducer solution is pumped into a centrifugal spray drying tower through a peristaltic pump, and meanwhile, an isolating agent (white carbon black accounts for 2% of the powder polycarboxylate water reducer and calcium hydroxide accounts for 10% of the powder polycarboxylate water reducer) is uniformly added into an air inlet pipeline. The polycarboxylic acid water reducing agent powder with good fluidity can be obtained by controlling certain air inlet temperature and air outlet temperature.
EXAMPLE III
Stirring is started in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser and a dripping device, 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide are added, then materials A (45 g of acrylic acid, 1.5 g of mercaptopropionic acid and 150 g of soft water) and materials B (1 g of sodium formaldehyde sulfoxylate and 100 g of water) are simultaneously dripped, the materials A are uniformly dripped for 3 hours, the materials B are uniformly dripped for 3.5 hours, after the materials B are dripped, the materials B are cured for 1.5 hours, then 32% of calcium hydroxide aqueous suspension is added, the pH is regulated to 11-12, and water is supplemented until the solid content is 40%, so as to obtain 40% of polycarboxylic acid water reducing agent solution. 40% of polycarboxylate water reducing agent solution is pumped into a centrifugal spray drying tower through a peristaltic pump, and meanwhile, an isolating agent (white carbon black accounts for 2% of the powder polycarboxylate water reducing agent, and calcium hydroxide accounts for 5% of the powder polycarboxylate water reducing agent) is uniformly added at an air inlet pipeline. The polycarboxylic acid water reducing agent powder with good fluidity can be obtained by controlling certain air inlet temperature and air outlet temperature.
Example four
Starting stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dripping device, adding 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide, simultaneously dripping materials A (45 g of acrylic acid, 1.5 g of mercaptopropionic acid and 150 g of soft water) and materials B (1 g of rongalite and 100 g of water), uniformly dripping the materials A for 3 hours, uniformly dripping the materials B for 3.5 hours, curing for 1.5 hours after dripping the materials B, adding 32% of calcium hydroxide aqueous suspension, regulating the pH to 11-12, and supplementing water until the solid content is 40% to obtain a 40% polycarboxylic acid water reducer solution. 40% of polycarboxylate water reducer solution is pumped into a centrifugal spray drying tower through a peristaltic pump, and meanwhile, an isolating agent (white carbon black accounts for 2% of the powder polycarboxylate water reducer and calcium hydroxide accounts for 10% of the powder polycarboxylate water reducer) is uniformly added into an air inlet pipeline. The polycarboxylic acid water reducing agent powder with good fluidity can be obtained by controlling certain air inlet temperature and air outlet temperature.
Comparative example
Stirring is started in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser tube and a dripping device, 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide are added, then materials A (45 g of acrylic acid, 1.5 g of mercaptopropionic acid and 150 g of soft water) and materials B (1 g of sodium formaldehyde sulfoxylate and 100 g of water) are simultaneously dripped, the materials A are uniformly dripped for 3 hours, the materials B are uniformly dripped for 3.5 hours, after the materials B are dripped, the materials B are cured for 1.5 hours, then 32% of sodium hydroxide solution is added, the pH is regulated to 10-11, and water is supplemented until the solid content is 40%, so as to obtain 40% of polycarboxylic acid water reducer solution. 40% of polycarboxylate water reducer solution is pumped into a centrifugal spray drying tower through a peristaltic pump, and meanwhile, an isolating agent (white carbon black accounts for 2% of the powder polycarboxylate water reducer and talcum powder accounts for 10% of the powder polycarboxylate water reducer) is uniformly added at an air inlet pipeline.
The water reducing agents obtained in the above examples 1 to 4 and comparative examples were tested for initial fluidity and 30min flow extension, and the comparative results were as follows (evaluation results (execution standard: JC/T1023-:
remarking: 950 g of Xinyang Feng gypsum, 50 g of 42.5 g of cement, 0.8 g of gypsum retarder, 0.6 g of defoamer, 0.6 g of cellulose, 0.4 g of plastic retention agent, 1.5 g of powdery polycarboxylate superplasticizer and 420 g of water.
By comparison, the calcium hydroxide is better than the sodium hydroxide, and the water reducing agent of the invention reduces the influence of free sulfate on the polycarboxylic acid water reducing agent to disperse gypsum. The water reducing agent disclosed by the invention combines free sulfate radicals and calcium ions to form calcium sulfate which is difficult to dissolve, so that influence of the polycarboxylic acid water reducing agent on gypsum dispersion is reduced or not influenced.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications can be made without departing from the principle of the present invention, and these modifications should also be regarded as the protection scope of the present invention.
Claims (4)
1. A preparation method of a powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar is characterized in that the superplasticizer is prepared from the following components: polyether macromonomer, acrylic acid, chain transfer agent, oxidant, reduction initiator, alkaline substance, separant, soft water and water; the polyether macromonomer is methyl allyl polyoxyethylene ether 3000; the alkaline substance is calcium hydroxide; the chain transfer agent is mercaptopropionic acid; the separant is a mixture of white carbon black and calcium hydroxide, wherein the white carbon black accounts for 2% of the powdery polycarboxylic acid water reducer, and the calcium hydroxide accounts for 5-10% of the powdery polycarboxylic acid water reducer; the oxidant is hydrogen peroxide, and the reducing agent is sodium formaldehyde sulfoxylate.
2. The method for preparing the powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar according to claim 1, wherein soft water and water are added in batches.
3. The preparation method of the powder polycarboxylate water reducer for gypsum-based dry powder mortar according to claim 1, wherein the acrylic acid, the mercaptopropionic acid and the soft water are material A, the rongalite and the water are material B, and the preparation method of the water reducer comprises the following steps:
starting stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dripping device, adding soft water, methallyl polyoxyethylene ether 3000 and hydrogen peroxide, and then dripping a material A and a material B simultaneously, wherein the material A is as follows: acrylic acid, mercaptopropionic acid, and soft water; the material B is as follows: uniformly dripping the sodium formaldehyde sulfoxylate, water and the material A for 3 hours, dripping the material B for 3.5 hours, curing for 1.5 hours after the material B is dripped, then adding a calcium hydroxide aqueous suspension, adjusting the pH to 9-10, and replenishing water until the solid content is 40% to obtain a 40% polycarboxylic acid water reducing agent solution;
pumping 40% of polycarboxylate superplasticizer solution into a centrifugal spray drying tower through a peristaltic pump, and simultaneously uniformly adding a separant into an air inlet pipeline; and controlling the air inlet temperature and the air outlet temperature to obtain the polycarboxylic acid water reducing agent powder with good fluidity.
4. The preparation method of the powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar of claim 3 is characterized in that,
starting stirring in a four-neck flask provided with a thermometer, a speed-regulating stirrer, a reflux condenser pipe and a dripping device, adding 200 g of soft water, 365 g of methylallyl polyoxyethylene ether 3000 and 4 g of hydrogen peroxide, and dripping the material A and the material B simultaneously; the material A is as follows: 45 g of acrylic acid, 1.5 g of mercaptopropionic acid, 150 g of soft water); the material B is as follows: 1 g of sodium formaldehyde sulfoxylate and 100 g of water, wherein the material A is uniformly dripped after 3 hours, the material B is uniformly dripped after 3.5 hours, after the material B is dripped, curing is carried out for 1.5 hours, then 32% of calcium hydroxide aqueous suspension is added, the pH value is adjusted to 9-12, and water is supplemented until the solid content is 40% to obtain 40% of polycarboxylic acid water reducing agent solution;
pumping 40% of a polycarboxylic acid water reducing agent solution into a centrifugal spray drying tower through a peristaltic pump, and simultaneously uniformly adding a separant into an air inlet pipeline; the white carbon black accounts for 2 percent of the powdery polycarboxylate water reducer, and the calcium hydroxide accounts for 5 to 10 percent of the powdery polycarboxylate water reducer; and controlling the air inlet temperature and the air outlet temperature to obtain the polycarboxylic acid water reducing agent powder with good fluidity.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962273A (en) * | 2010-09-27 | 2011-02-02 | 上海三瑞化学有限公司 | Method for preparing powdery polycarboxylic acid hyperdispersant |
| CN104987469A (en) * | 2015-06-30 | 2015-10-21 | 同济大学 | Preparing method for high dispersion type polycarboxylate water reducing agent |
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- 2022-04-12 CN CN202210381070.0A patent/CN114772971A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962273A (en) * | 2010-09-27 | 2011-02-02 | 上海三瑞化学有限公司 | Method for preparing powdery polycarboxylic acid hyperdispersant |
| CN104987469A (en) * | 2015-06-30 | 2015-10-21 | 同济大学 | Preparing method for high dispersion type polycarboxylate water reducing agent |
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