CN101993215A - Preparation method of sulfonate water reducing agent - Google Patents
Preparation method of sulfonate water reducing agent Download PDFInfo
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- CN101993215A CN101993215A CN 200910017908 CN200910017908A CN101993215A CN 101993215 A CN101993215 A CN 101993215A CN 200910017908 CN200910017908 CN 200910017908 CN 200910017908 A CN200910017908 A CN 200910017908A CN 101993215 A CN101993215 A CN 101993215A
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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
- C04B24/16—Sulfur-containing compounds
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Abstract
The invention relates to a preparation method of sulfonate water reducing agents, wherein the sulfonate water reducing agents are prepared from the raw materials consisting of butyl methacrylate, beta-hydroxyethyl methacrylate and 2-acrylamido-2-methylpropanesulfonic acid by the method of catalytic chain transfer polymerization on condition that azobisiso(nitroaminoethyl)butyl ether is used as initiator, and bis(aqua)bis((difluoroboryl)dimethylglyoximato)cobalt (II) (COBF) is used as catalytic chain transfer agent. The preparation method has the advantages of: being simple in process, easy in industrial production, stable in product performance and wide in suitability, and the prepared water reducing agent has the performances of low doping amount, high water reducing rate, no retardation, low slump loss and the like.
Description
Technical field
The present invention relates to a kind of technology of preparing of water reducer of cement concrete, is to disclose a kind of new synthetic method that has the cement water reducing agent of sulfonic acid group specifically, belongs to building material technical field.
Background technology
The concrete annual production of China surpasses 14 billion cubic meters, and the demand of annual high efficiency water reducing agent surpasses 300,000 tons, and the investment of the particularly current Infrastructure that increases for expanding domestic demand will make to the demand of high efficiency water reducing agent bigger.Water reducer commonly used at present mainly contains sulfonated lignin based water reducer, naphthalenesulfonate based water reducer, melamine based water reducer, melamine resin water reducer etc., the main effective constituent of sulfonated lignin is xylogen, in recent years, because the over-exploitation of forest, badly influence the biogenetic derivation of xylogen, and have influence on its chemical constitution and comprise the various chemical reactions of sulfonation, finally make the water-reducing rate of sulfonated lignin lower, the air content height, and slow setting etc.; It is big through time loss that the deficiency of naphthalenesulfonate based water reducer mainly shows as the slump, and concrete is clamminess a bit, cement/adulterant bad adaptability.
The patent No. is 200310123840 Aliphatic sulfonate superplasticizer and its preparation methods, employing contains the ketone compounds of carbonyl and aldehydes as the condensation monomer, with sulphite is sulphonating agent, carries out condensation reaction in alkaline aqueous solution, makes the water-soluble polymer condenses.Its diminishing dispersion effect and reinforced effects are better than traditional naphthalene series high-efficiency water-reducing agent, facts have proved, the performance of the water reducer of this water reducer also needs to optimize.The patent No. is 200610124100 lignosulfonate series air entraining and water reducing admixture for concrete and preparation method thereof, obtains product and has higher water-reducing rate, has improved concrete intensity to a certain extent, has certain delayed coagulation.The patent No. is 200810048056 polyether modification type sulfamate water reducing agents and preparation method thereof, adopt the principal commander of lower-cost formaldehyde, the sulfanilate grafting poly carboxylic acid series water reducer oxygen Vinyl Ether of reuniting, polycondensation synthesising macromolecule copolymer water reducer, the concrete of preparation has good operation and mechanical property.
The present invention uses Polmerization method of catalysis chain transfer, adopting butyl methacrylate, methacrylic acid-beta-hydroxy ethyl ester, 2-acrylamido-2-methyl propane sulfonic acid is raw material, azo two different (nitrogen amine ethyl) butyl ether is an initiator, bis (aqua) bis ((difluoroboryl) dimethylglyoximato) cobalt (II) is a catalytic chain transfer agent (COBF), has prepared novel Sulfonates water reducer.This method reaction path is short, and the catalytic chain transfer agent add-on of use is few, and catalytic efficiency height, the water reducer that obtains have low incorporation, high water reducing rate, performance such as slow setting, low slump loss not.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of novel Sulfonates water reducer.Prepare water reducer with Polmerization method of catalysis chain transfer.
Another object of the present invention is to use the method for catalytic chain transfer polymerization to prepare the water reducer that has sulfonic acid group efficiently.
Purpose of the present invention is achieved through the following technical solutions
(1) catalytic chain transfer polymerization reaction: in reactor, add 2-acrylamido-2-methyl propane sulfonic acid, N, dinethylformamide stirs, after it is dissolved fully, adding butyl methacrylate, COBF are that catalyst structure is seen figure, azo two different (nitrogen amine ethyl) butyl ether is an initiator, stirring mixes it, sealing, blast high pure nitrogen 1hr, move on in 75 ℃～90 ℃ the oil bath, stirring reaction 10hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, vacuum-drying 24hr gets faint yellow solid.
(2) solid is dissolved in the tetrahydrofuran (THF) fully, adds sodium hydroxide solution, the normal temperature vigorous stirring makes its complete reaction, and underpressure distillation thoroughly steams tetrahydrofuran (THF), obtains high efficiency water reducing agent solution.
The COBF structure
Described 2-acrylamido-2-methyl propane sulfonic acid (AMPS, molar mass is 205), consumption is 205～512.5 parts, butyl methacrylate (BMA, molar mass is 142), consumption is 142～710 parts, the COBF add-on is 0.02% of all monomer masses, azo two different (nitrogen amine ethyl) butyl ether add-on is 0.1% of all monomer masses, N, dinethylformamide (DMF, molar mass is 73), consumption is 0.8 times-1.2 times of 2-acrylamido-2-methyl propane sulfonic acid quality, and the amount of tetrahydrofuran (THF) is 1.2 times of amount of solid.75 ℃～80 ℃ of temperature of reaction, reaction times 7～10hr.
Synthetic Sulfonates water reducer of the present invention is a colourless transparent liquid, and capability and performance is stable, does not precipitate, do not separate out under the low temperature, concentration is 5%～10%, and incorporation is generally about 0.5%～1.5% of cement gross weight in concrete, has the good water-reducing effect and the slump and keeps.Water-reducing rate reaches as high as 36%, and the initial slump of concrete mix can reach 220mm, and concrete 3d ultimate compression strength improves 60%～110%, and 28d ultimate compression strength improves 50%～90%.
The present invention compared with prior art has following outstanding advantage:
(1) Polmerization method of catalysis chain transfer involved in the present invention belongs to the preparation of first Application in the Sulfonates water reducer.Present method has uses catalytic chain transfer agent few, catalytic efficiency height, the advantage that reaction back by product is easy to remove.
(2) the present invention has adopted Polmerization method of catalysis chain transfer synthesising sulfonate class water reducer first, thereby obtains a kind of novel Sulfonates water reducer.
(3) the prepared Sulfonates water reducer of the present invention, the water reducer that obtains have low incorporation, high water reducing rate, performance such as slow setting, low slump loss not, have satisfied the requirement of construction.
Embodiment:
The present invention is described in further detail below in conjunction with embodiment, but the invention embodiment is not limited thereto.
Embodiment 1
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.069g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.347g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 2
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 246g, N, dinethylformamide 246g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.078g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.388g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 3
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 287g, N, dinethylformamide 287g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.086g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.429g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 4
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 328g, N, dinethylformamide 328g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.094g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.470g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 5
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 369g, N, dinethylformamide 369g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.102g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.511g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 6
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 410g, N, dinethylformamide 410g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.110g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.552g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 7
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 451g, N, dinethylformamide 451g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF 0.119g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.593g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 8
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 492g, N, dinethylformamide 492
G, stirring is dissolved it fully, adds butyl methacrylate 142g, catalytic chain transfer agent COBF 0.127g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.634g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 9
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 512.5g, N, dinethylformamide 512.5g, stirring is dissolved it fully, add butyl methacrylate 142g, catalytic chain transfer agent COBF0.131g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.655g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 10
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 213g, catalytic chain transfer agent COBF 0.084g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.418g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 11
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 284g, catalytic chain transfer agent COBF 0.098g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.489g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 12
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 355g, catalytic chain transfer agent COBF 0.112g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.560g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 13
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 426g, catalytic chain transfer agent COBF 0.126g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.631g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 14
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 497g, catalytic chain transfer agent COBF 0.140g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.702g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 15
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 568g, catalytic chain transfer agent COBF 0.155g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.773g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 16
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 639g, catalytic chain transfer agent COBF 0.167g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.844g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
Embodiment 17
(1) method with catalytic chain transfer polymerization prepares polymkeric substance
In reactor, add 2-acrylamido-2-methyl propane sulfonic acid 205g, N, dinethylformamide 205g, stirring is dissolved it fully, add butyl methacrylate 710g, catalytic chain transfer agent COBF 0.183g, initiator azo two different (nitrogen amine ethyl) butyl ether 0.915g, mix, reactor sealing is under the normal temperature behind the logical nitrogen purge gas 2hr, 80 ℃ of reaction 8hr, the product volume ratio is 1: 1 distilled water, a methanol mixed purified solution, and product vacuum-drying 24hr obtains the exsiccant faint yellow solid.
(2) preparation of sulfonate water reducer
Take by weighing previous step and obtain polymkeric substance 300g and be dissolved in the 360g tetrahydrofuran (THF), after the dissolving, add 1% sodium hydroxide solution gradually fully, vigorous stirring under the room temperature, pH to 7～8 are regulated in fully reaction, evaporate 360g liquid, promptly obtain Sulfonates water reducer solution.
With water reducer sulfonated melamine, sodium lignosulfonate, the naphthalene sulfonic salt of using always on the sulfonate water reducer of embodiment 7～9 preparation and the market, add in state, Yihe River cement (group) limited-liability company 42.5 class g cements, the test result under identical conditions sees Table 1.
Table 1 simultaneous test test result
Claims (4)
1. the preparation method of Sulfonates water reducer.
2. the synthesis material of claim 1 is that butyl methacrylate, methacrylic acid-beta-hydroxy ethyl ester, 2-acrylamido-2-methyl propane sulfonic acid are raw material, azo two different (nitrogen amine ethyl) butyl ether is an initiator, and bis (aqua) bis ((difluoroboryl) dimethylglyoximato) cobalt (II) is a catalytic chain transfer agent (COBF).
3. the synthetic method of claim 1 is a Polmerization method of catalysis chain transfer.
4. the preparation of claim 1 is implemented in by following technology and adds 2-acrylamido-2-methyl propane sulfonic acid, N in the reactor, dinethylformamide stirs, after it is dissolved fully, adding butyl methacrylate, COBF are catalyzer, azo two different (nitrogen amine ethyl) butyl ether is an initiator, stirring mixes it, sealing, blast high pure nitrogen 1hr, move on in 75 ℃～90 ℃ the oil bath, stirring reaction 10hr, the product volume ratio is that 1: 1 distilled water, methyl alcohol mixed liquor purified, vacuum-drying 24hr gets faint yellow solid.Solid is dissolved in the tetrahydrofuran (THF) fully, adds the sodium hydroxide solution after dissolving, stirring at normal temperature makes its complete reaction, and underpressure distillation thoroughly steams tetrahydrofuran (THF), obtains high efficiency water reducing agent solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104496253A (en) * | 2014-12-23 | 2015-04-08 | 岳阳东方雨虹防水技术有限责任公司 | Special early-strength polycarboxylate superplasticizer for prefabricated parts and preparation method of special early-strength polycarboxylate superplasticizer |
| CN107586360A (en) * | 2017-10-23 | 2018-01-16 | 中国地质大学（北京） | A kind of Star Polyacrylamide copolymer and preparation method thereof and drilling fluid |
| CN116265494A (en) * | 2021-12-17 | 2023-06-20 | 江苏苏博特新材料股份有限公司 | Side chain macromonomer, preparation method thereof and low-sensitivity high-adaptability polycarboxylate superplasticizer prepared by using side chain macromonomer |
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2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104496253A (en) * | 2014-12-23 | 2015-04-08 | 岳阳东方雨虹防水技术有限责任公司 | Special early-strength polycarboxylate superplasticizer for prefabricated parts and preparation method of special early-strength polycarboxylate superplasticizer |
| CN107586360A (en) * | 2017-10-23 | 2018-01-16 | 中国地质大学（北京） | A kind of Star Polyacrylamide copolymer and preparation method thereof and drilling fluid |
| CN107586360B (en) * | 2017-10-23 | 2018-07-03 | 中国地质大学（北京） | A kind of Star Polyacrylamide copolymer and preparation method thereof and drilling fluid |
| CN116265494A (en) * | 2021-12-17 | 2023-06-20 | 江苏苏博特新材料股份有限公司 | Side chain macromonomer, preparation method thereof and low-sensitivity high-adaptability polycarboxylate superplasticizer prepared by using side chain macromonomer |
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Application publication date: 20110330 |