CN100366565C - Preparation method of powder polycarboxylic acids water reducing agent - Google Patents
Preparation method of powder polycarboxylic acids water reducing agent Download PDFInfo
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- CN100366565C CN100366565C CNB2005100290664A CN200510029066A CN100366565C CN 100366565 C CN100366565 C CN 100366565C CN B2005100290664 A CNB2005100290664 A CN B2005100290664A CN 200510029066 A CN200510029066 A CN 200510029066A CN 100366565 C CN100366565 C CN 100366565C
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Abstract
The invention discloses a preparing method of powder polycarboxylic dehydragent, which comprises the following steps: making polycarboxylic dehydragent form droplet in the atomizer; spraying in the drying chamber with the same flowing direction of hot air and material; setting the inlet temperature at 120-200 deg.c and vent temperature at 50-110 deg.c; drying; sedimenting to obtain the product.
Description
Technical field
The present invention relates to a kind of preparation method of polyacrylic dispersion agent powder, especially a kind of preparation method of powder polycarboxylic acids water reducing agent.
Background technology
Concrete is a material commonly used in the engineerings such as bridge, road, building, along with developing rapidly of construction industry and hydro project, to concrete demands for higher performance.Adding water reducer is one of means that improve concrete performance.
The development of water reducer has long history.Successful respectively beta-naphthalenesulfonic-acid formaldehyde condensation compound sodium salt (SNF) and these the two kinds of high efficiency water reducing agents of sulfonated melamine compound condenses (SMF) developed of Japan and Germany make the development of concrete technology rise to a stage from early stage sulfonated lignin to the sixties in last century.This three classes water reducer all has the product supply of material of powder and liquid form.
External polymeric superplasticizer since the mid-80 Development of New Generation in last century, as polycarboxylic acid series and modified polyether series high-efficiency water-reducing agents such as acrylic acid series, toxilic acid systems, water-reducing rate up to more than 30%, volume is few, function of slump protection good, amount of air entrainment and continuous index such as coagulate are comparatively moderate, suit to prepare high workability, self-compacting concrete, thereby be subjected to the favor of engineering circle.Because the characteristics of this class water reducer operational path, make its overwhelming majority supply with the form of liquid, the mode of supplly of this class water reducer is accepted extensively by the client because of its high-performance, but its tangible weak point, because be the liquid form supply of material, its effective content is common to be 22% the aqueous solution, and the cost of long-distance transportation is very high; In some use field, need the polycarboxylic acids dehydragent of powder in addition, as dry-mix etc.At present, the powder polycarboxylic acids water reducing agent powder seldom, its major cause has following two aspects: the one, because the aqueous solution polymerization technology of polycarboxylic acids dehydragent has caused its water content height, generally between 45%-78%, it to be prepared into powder and need very high energy consumption, expensive tooling cost has brought difficulty for the deep processing of this series products: the 2nd, because the molecular weight of polycarboxylic acids dehydragent is less relatively, the softening temperature of dry back powder is low, when processing temperature is higher than softening temperature for a long time, can cause the reactive group of this water reducer that side reactions such as inferior amidation may take place, cause the product appearance xanthochromia, simultaneously to the decline of concrete dispersing property.
Summary of the invention
The preparation method that a kind of powder polycarboxylic acids water reducing agent of providing at the deficiencies in the prior art is provided.
The object of the present invention is achieved like this:
A kind of preparation method of powder polycarboxylic acids water reducing agent: it is characterized in that polycarboxylate water-reducer solution is formed droplet by spraying gun, injection enters kiln, the hot air flow that enters kiln is identical with flow direction of material, the kiln inlet temperature is 120-200 ℃, air outlet temperature is 50-110 ℃, and drying, sedimentation obtain powder polycarboxylic acids water reducing agent.
Described polycarboxylate water-reducer is a comb shaped molecular structure, and main chain is formed through radical polymerization by unsaturated monomer, and side chain is made up of oxyethane (EO) n, propylene oxide (PO) m of different polymerization degree, and side chain is connected with ester bond or ehter bond mode with main chain.
Described unsaturated monomer comprises: (methyl) vinylformic acid, maleic anhydride, acrylamide, vinyl acetate, allylic monomers.
Among described oxyethane (EO) n among n, propylene oxide (PO) m polymerization degree of m be: 0-70.
The apparent viscosity of described polycarboxylate water-reducer is 10-800cp.
Described injection is to adopt the centrifugal spraying method, and polycarboxylate water-reducer solution is transported on the spraying gun that horizontally rotates at a high speed by peristaltic pump, makes feed liquid be dispersed into droplet by centrifugal force, and the rotating speed of spraying gun is 15000-30000rpm.
Described kiln diameter is 2-8m.
The inventive method has solved the problem of the cost costliness of liquid polycarboxylate water-reducer long-distance transportation; Widened the Application Areas of product, can be applicable to that general liquid polycarboxylate water-reducer can not direct applied dry-mix; In preparation process, avoided simultaneously material to glue unfavorable factors such as side reaction easily takes place under wall, the high temperature; The powder of preparation is easy to use, is easy to suitability for industrialized production.
Embodiment
Spray-dired principle is: under normal pressure, with atomisation unit material is atomized, it is contacted with warm air in drying tower, because evaporation area is big, the moisture in the material just is evaporated in several seconds, and solids constituent then powdered falls at the bottom of the device.Spray drying technology roughly divides 3 kinds according to atomizing type: air-flowing type; Mechanical type; Centrifugal.Centrifugal spraying drying is by electric heater, tower body, spraying gun, exhaust system, negative pressure device.Whirlwind separator, tail gas device for recovering powder are formed.Its principal feature is as follows: 1) dry device structure is simple relatively, and production process is simplified, convenient operation and control, but moving control is conigenous in continuous large-scale production and implementation; 2) rate of drying fast (general 5～40 seconds) is suitable for the drying of heat-sensitive material especially; 3) can satisfy quality index such as product appearance, size-grade distribution, physicochemical property (dust content, flowability, dispersiveness, instantly-soluble etc.) and the using property data etc. of various products according to technologic requirement timely adjusting parameter in operating process.
In general, there are two systems in the spraying drying, the one, material system, material rely on centrifugal force or pressure to send spraying drying to, become water vapour and powder after the drying, and powder has fallen into storage hopper; Another is an air system, and warm air relies on blower fan to send spraying drying to, is accompanied by water vapour again and extracts out from blower fan.Consider stablizing between these two systems, generally speaking, control negative pressure, charging aperture, material pressure (speed of rotation, gas velocity) in inlet temperature, temperature out, the tower.
Adopt spray-dired method to prepare powder polycarboxylic acids water reducing agent runs into the sticking wall of material through regular meeting problem; because temperature is higher than 120 ℃ in the drying tower; make polymkeric substance generation chemical reaction easily; as the inferior amidation between amide group; yellow more in the long more powder color of dwell time in the tower from seeing the material that is bonded on the wall in appearance, the degree of mobilization and the slump keep the effect before performance all is not so good as original spraying when seeing concrete experiments on application performance.
The sticking wall of material is mainly from the toughness of half-dried material in the spray-drying tower.Material is injected come out after because gob is in by hot-air drying process, when the time was still not enough, the surface is complete drying not. formed so-called half-dried material. this material has bigger toughness.So the direction along material sprays is easy to adhere on it if run into Ta Bize.Next, the exsiccant material is because the vortex disturbance of hot blast in tower. and material also may fly to the tower wall and adhere on it.But the sticking wall of this material, adhesivity are not firm. very easily come off.Generally speaking, the kind of what and the position on the tower wall of the sticking wall of material and spraying gun and working parameter, hot blast speed and hot blast factors such as moving situation in tower are relevant.In order to prevent that material from gluing wall, suitably strengthen tower wall diameter. half-dried material is bumped less than wall just drop downwards.Can effectively solve sticking wall problem.
Embodiment
Polycarboxylate water-reducer stoste with the different solid contents of 2kg, be fed in the spraying gun with the flow velocity of peristaltic pump with 2.2 liters/hour, the rotating speed of spraying gun is 23000rpm, the diameter of drying tower, inlet temperature and air outlet temperature see the following form, air-flow is identical with droplet direction of motion, through super-dry, whirlwind discharging.
| Embodiment | Charging solid content % | Viscosity Cp | Drying tower internal diameter m | Inlet temperature ℃ | Temperature of outgoing air ℃ | Discharge method | Remarks |
| 1 | 22 | 25 | 1.6 | 14-150 | 61-66 | The discharging of broom inwall | Sticking wall |
| 2 | 40 | 270 | 1.6 | 16-170 | 85-89 | Sticking wall | |
| 3 | 40 | 270 | 1.6 | 18-189 | 88-90 | Sticking wall | |
| 4 | 40 | 270 | 1.6 | 19-195 | 85-101 | Sticking wall | |
| 5 | 50 | 500 | 1.2 | 14-155 | 78-96 | Sticking wall | |
| 6 | 50 | 500 | 2 | 150-160 | 85-90 | The whirlwind discharging | Not sticking wall |
Evaluation method
1, the initial clean slurry degree of mobilization simultaneous test of powder polycarboxylic acids water reducing agent
The testing method of flowing degree of net paste of cement: press GB8077-87 " Methods for testing uniformity of concrete admixture " and measure flowing degree of net paste of cement, W/C=0.29 water reducer volume is the percentage ratio that water reducer accounts for cement quality: 1.1% (being converted to liquid 22%).Cement is associating P042.5
| Embodiment | Morphology microstructure | The powder color | Solid content % | Initial clean slurry degree of mobilization mm |
| 1 | The powder agglomates shape | Pale yellow | 97.5 | 155 |
| 2 | The powder agglomates shape | Pale yellow | 98.3 | 155 |
| 3 | The powder agglomates shape | Yellow | 98.2 | 135 |
| 4 | The powder agglomates shape | Yellow | 97.8 | 132 |
| 5 | The powder agglomates shape | Little Huang | 96.35 | 177 |
| 6 | The powdery good fluidity | White | 92.95 | 226 |
| Stoste | Liquid | 22 | 240 |
2, the simultaneous test of powder polycarboxylic acids water reducing agent concrete
Raw material: cement is associating P042.5, and sand is half sand, and stone is the continuous grain grade proportion of 5-25mm:
| Cement | Sand | Stone | Water | Water reducer (parameter 1.1%) |
| 335kg | 765kg | 1100kg | 145kg | Embodiment 6 |
| 335kg | 765kg | 1100kg | 145kg | Stoste |
Test-results:
| Water reducer | Slump |
| Embodiment 6 | 160/450 |
| Stoste | 175/500 |
From test result, embodiment 6 is close with the test result of dry preceding stoste.Cement there are good dispersion effect and slump hold facility.Embodiment 6 compares with the detection data of stoste, works as through the performance and the liquid phase of processing back powder.
Claims (7)
1. the preparation method of a powder polycarboxylic acids water reducing agent, it is characterized in that polycarboxylate water-reducer solution is formed droplet by spraying gun, injection enters kiln, the hot air flow that enters kiln is identical with flow direction of material, the kiln inlet temperature is 120-200 ℃, air outlet temperature is 50-110 ℃, and drying, sedimentation obtain powder polycarboxylic acids water reducing agent.
2. the preparation method of powder polycarboxylic acids water reducing agent according to claim 1, it is characterized in that described polycarboxylate water-reducer is a comb shaped molecular structure, main chain is formed through radical polymerization by unsaturated monomer, side chain is made up of oxyethane, the propylene oxide of different polymerization degree, and side chain is connected with ester bond or ehter bond mode with main chain.
3. the preparation method of powder polycarboxylic acids water reducing agent according to claim 2 is characterized in that described unsaturated monomer comprises: (methyl) vinylformic acid, maleic anhydride, acrylamide, vinyl acetate, allylic monomers.
4. the preparation method of powder polycarboxylic acids water reducing agent according to claim 2 is characterized in that the polymerization degree of described oxyethane, propylene oxide is: 0-70.
5. the preparation method of powder polycarboxylic acids water reducing agent according to claim 1, the apparent viscosity that it is characterized in that described polycarboxylate water-reducer is 10-800cp.
6. the preparation method of powder polycarboxylic acids water reducing agent according to claim 1, it is characterized in that described injection is to adopt the centrifugal spraying method, be transported to polycarboxylate water-reducer solution on the spraying gun that horizontally rotates at a high speed by peristaltic pump, make feed liquid be dispersed into droplet by centrifugal force, the rotating speed of spraying gun is 15000-30000rpm.
7. the preparation method of powder polycarboxylic acids water reducing agent according to claim 1 is characterized in that described kiln diameter is 2-8m.
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| CNB2005100290664A CN100366565C (en) | 2005-08-25 | 2005-08-25 | Preparation method of powder polycarboxylic acids water reducing agent |
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| CNB2005100290664A CN100366565C (en) | 2005-08-25 | 2005-08-25 | Preparation method of powder polycarboxylic acids water reducing agent |
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| CN100366565C true CN100366565C (en) | 2008-02-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935184B (en) * | 2010-08-19 | 2012-08-08 | 上海三瑞高分子材料有限公司 | Reduction and early strength polymer additive |
| CN102477160A (en) * | 2010-11-23 | 2012-05-30 | 浙江老虎山建材有限公司 | Method for preparing dry high-performance water reducer powder of polycarboxylic acid |
| EP2468696A1 (en) * | 2010-12-24 | 2012-06-27 | Sika Technology AG | Polymer comprising maleic acid, allylether and vinyl acetate, its process of production and use |
| CN102911320B (en) * | 2012-07-21 | 2015-01-07 | 北京工业大学 | Method for preparing powder polycarboxylic acid superplasticizer |
| CN103214208B (en) * | 2013-04-25 | 2015-05-20 | 山西凯迪建材有限公司 | Preparation method of powdery polycarboxylate superplasticizer |
| CN104446099A (en) * | 2014-11-06 | 2015-03-25 | 贵州恒一新材料有限公司 | Polycarboxylic acid water reducing agent and preparation method thereof |
| CN112225850A (en) * | 2020-10-20 | 2021-01-15 | 安徽森普新型材料发展有限公司 | Preparation method of high-stability powder polycarboxylate superplasticizer under strong mixing |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137263A (en) * | 1993-12-14 | 1996-12-04 | 花王株式会社 | Admixture for concrete |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137263A (en) * | 1993-12-14 | 1996-12-04 | 花王株式会社 | Admixture for concrete |
Non-Patent Citations (1)
| Title |
|---|
| VIVID-500聚羧酸超塑化剂性能评价. 季春伟等.混凝土，第4期. 2005 * |
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Effective date of registration: 20131227 Address after: 200232 Shanghai Xi Road No. 237 Building No. 17 Patentee after: Shanghai Sanrui Polymer Material Co., Ltd. Address before: 200233, 3 building, building 680, Guiping Road, Shanghai Patentee before: Shanghai Sanrui Chemistry Co., Ltd. |