CN102936349A - Production method of solid polycarboxylic acid water reducing agent - Google Patents
Production method of solid polycarboxylic acid water reducing agent Download PDFInfo
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- CN102936349A CN102936349A CN2012101789345A CN201210178934A CN102936349A CN 102936349 A CN102936349 A CN 102936349A CN 2012101789345 A CN2012101789345 A CN 2012101789345A CN 201210178934 A CN201210178934 A CN 201210178934A CN 102936349 A CN102936349 A CN 102936349A
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Abstract
The invention relates to a production method of a solid polycarboxylic acid water reducing agent. A liquid polycarboxylic acid water reducing agent is conveyed to a microwave drying oven via a conveyor belt and dried in the microwave drying oven; the used microwave frequency is 915 MHz or 2,450 MHz; irradiating energy is 3000-4000 kJ/kG; the microwave power is 1,500-2,500 kW; the thickness of the dried material is 8-10 cm; conveying speed of the conveyor belt is 0.5-0.8 m/min; a drying time is 12-18 min; and a drying temperature is 93-98 DEG C. With the production method, problems of high freight for long-distance transportation of the polycarboxylic acid water reducing agent and difficult package of the liquid product can be solved; and problems of large investment, product performance loss, low performance of the solid product, high energy consumption and the like in a conventional spray drying method can be prevented.
Description
Technical field
The present invention relates to the production method of water reducer, be specifically related to a kind of production method of solid polycarboxylic acids dehydragent.
Background technology
Water reducer refers to can reduce the mixing water amount under the constant condition of concrete workability and cement consumption, improves concrete strength, or under the constant condition of easily property and intensity, saves the admixture of cement consumption.
Polycarboxylate water-reducer is the cement dispersants a kind of commonly used during cement concrete uses, polycarboxylic acids dehydragent is comb type molecular structure, main chain is formed through radical polymerization by unsaturated monomer, side chain is comprised of oxyethane, the propylene oxide of different polymkeric substance, side chain is connected with ester bond or ehter bond mode with main chain, and wherein unsaturated monomer comprises: vinylformic acid (and ester), methacrylic acid (and ester), maleic anhydride, acrylamide, vinyl acetate, allylic monomers.Polycarboxylate water-reducer has the water-reducing rate height, volume is few, function of slump protection good, amount of air entrainment is moderate, and suitable configuration high strength, high workability, self-compacting concrete progressively obtain the approval in market, are used widely at national market.
The production normal operation aqueous solution polymerization of polycarboxylate water-reducer, the commodity polycarboxylate water-reducer that therefore obtains is solution morphology, solid content is generally 10～70%.Because the molecular weight of polycarboxylate water-reducer, its solids is softening with regard to occuring easily more than 80 ℃, as use conventional drying mode such as spraying drying etc. that water and material are heated simultaneously, must add auxiliary agent and could realize that drying obtains solid polycarboxylic acid water reducing agent, its drying is difficult, drying cost is high, the water reducer that drying obtains also has certain mass loss, adds that solid polycarboxylic acid water reducing agent performance that the auxiliary agent that wherein contains makes is well below the performance of identical solid content liquid polycarboxylate water-reducer; Therefore, generally use in the market all be solid content 10～70%(by percentage to the quality) aqueous solution liquid product, long-distance transportation is with high costs, the part solid phase prod only is applied to some special dimension such as dry-mixed mortar, self-compacting concrete etc.
Summary of the invention
The object of the present invention is to provide a kind of production method of solid polycarboxylic acid water reducing agent with low cost, the solid polycarboxylic acid water reducing agent that the method is produced is approaching with the liquid polycarboxylate water-reducer use properties of identical solid content.
Adopt following technical scheme for reaching above purpose the present invention:
A kind of production method of solid polycarboxylic acid water reducing agent is characterized in that: solid content is carried out drying for 10～70% liquid polycarboxylate water-reducers (commercially available prod) in mass concentration adopt microwave, and the control drying temperature is 90～100 ℃.
Be that 10～70% liquid polycarboxylate water-reducer carries out the solid polycarboxylic acid water reducing agent that microwave drying obtains to the solid content that adopts water solution polymerization process directly to obtain, its water content can be controlled in 5%(in the quality percentage composition) below, it is better that the solid polycarboxylic acid water reducing agent performance that obtains simultaneously reaches the liquid polycarboxylate water-reducer use properties of identical solid content; The contriver finds through long-term experiment, microwave has extremely strong selectivity heating to water, be at first to the moisture heating evaporation in institute's dried material and then the polycarboxylate water-reducer in the heated solution, so both guarantee the abundant drying to polycarboxylate water-reducer, guaranteed again the performance of gained solid polycarboxylic acid water reducing agent.
In order further to improve microwave drying effect and production efficiency, specifically adopt travelling belt to send into microwave drying oven the aforesaid liquid polycarboxylate water-reducer and transmit drying, the microwave frequency of using is 915MHZ or 2450MHZ, irradiation energy is 3000～4000KJ/KG, microwave power is 1500～2500KW, and the thickness of dried material is 8～10cm, and the travelling belt transfer rate is 0.5～0.8m/min, be 12～18min time of drying, and drying temperature is 93～98 ℃.The contriver finds in long-term experiment, if control bad also easily so that production efficiency does not lowly reach the requirement that large-scale industrialization is produced if thereby above parameter is controlled the performance that the solid polycarboxylic acid water reducing agent that local superheating impact makes appears in bad meeting, solid polycarboxylic acid water reducing agent performance obtained above reach identical solid content liquid polycarboxylate water-reducer use properties 88%～93%, water content below 4wt%, production efficiency is high, the solid polycarboxylic acid water reducing agent of gained can reach 100～140kg/h.
Further, the microwave frequency of above-mentioned employing is 2450MHZ, and irradiation energy is 3200～3600KJ/KG, and microwave power is 1900～2300KW, and the thickness of dried material is 9～10cm, and the travelling belt transfer rate is 0.6～0.7m/min, and be 12～15min time of drying.
The aforesaid liquid polycarboxylate water-reducer transmits drying at microwave drying oven, and more preferably, the microwave frequency of above-mentioned employing is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW; The thickness of control material on travelling belt is 9cm, and travelling belt speed is 0.7m/min, and drying temperature is 96 ℃, and be 13 minutes time of drying; The solid content of the solid polycarboxylic acid water reducing agent of dry gained is that 98～100%(is in the quality percentage composition), the solid polycarboxylic acid water reducing agent performance reach identical solid content liquid polycarboxylate water-reducer use properties 95%～100%.
In order to improve the drying efficiency in the microwave drying, also at the microwave drying upper box part vapor collection pipe is set, use blower fan that microwave steam is sent in the vapor collection pipe, make in the loft drier to be about the 0.9bar(absolute pressure for little negative pressure), greatly improved vaporization efficiency.
In order further to improve microwave drying efficient, before above-mentioned microwave drying, at first the liquid polycarboxylate water-reducer is carried out vacuum concentration, under vacuum condition, adopt fresh 1～10bar(absolute pressure) the 1bar(absolute pressure that produces of steam or microwave drying) steam carries out external source to the liquid polycarboxylate water-reducer and is heated to 85～90 ℃, makes its solid content be increased to 30～45%(in the quality percentage composition).When beginning first to carry out vacuum concentration without the microwave drying byproduct steam, just adopt fresh low-pressure steam, if carried out microwave drying, the low-pressure steam that then can utilize microwave drying to produce.
Most preferably, a kind of production method of solid polycarboxylic acid water reducing agent, it is characterized in that: be that 10～70%(is in the quality percentage composition to solid content at first) the liquid polycarboxylate water-reducer carries out vacuum concentration, in 0.01～1bar(absolute pressure) under, adopt fresh 1～10bar(absolute pressure) the 1bar(absolute pressure that produces of steam or microwave drying) steam carries out external source to the liquid polycarboxylate water-reducer and is heated to 88 ℃, makes its solid content be increased to 42%(in the quality percentage composition); Again the polycarboxylate water-reducer employing travelling belt of described vacuum concentration is sent into and carried out microwave drying in the microwave drying oven, at the microwave drying upper box part vapor collection pipe is set, use blower fan that microwave steam is sent in the vapor collection pipe, the microwave frequency that adopts is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW, the thickness of control material on travelling belt is 9cm, travelling belt speed is 0.7m/min, and drying temperature is 93～98 ℃, and be 13 clocks time of drying; The solid content of the solid polycarboxylic acid water reducing agent of dry gained is that 98～100%(is in the quality percentage composition), the solid polycarboxylic acid water reducing agent performance reach identical solid content liquid polycarboxylate water-reducer use properties 95%～100%.Send into pulverizer after the air cooling of dried solid polycarboxylic acid water reducing agent drying, broken rear pack namely obtains product; The production efficiency of solid polycarboxylic acid water reducing agent can reach 180～200kg/h.
The present invention has following beneficial effect:
1, the present invention has utilized the selectivity heating of microwave to water, rationally control simultaneously microwave drying process, the temperature that has guaranteed polycarboxylate water-reducer is unlikely too high and causes destruction to its performance, production obtains the solid polycarboxylic acid water reducing agent performance and reaches 95～100% of same amount liquid water reducer performance, the solid content of the solid polycarboxylic acid water reducing agent of dry gained is that 98～100%(is in the quality percentage composition), control moisture has significantly lowered transportation and packing cost at (in the quality percentage composition) below 2%.The inventive method production efficiency is high simultaneously, can reach 180～200kg/h, is suitable for large-scale industrial production.
2, utilized the low-pressure steam that reclaims the microwave generation in the inventive method, water reducer has been carried out vacuum concentration, significantly lowered power consumption while same apparatus and also improved production capacity, improved production efficiency, lowered production cost.
In a word, the problems such as the freight charges that the invention solves the polycarboxylate water-reducer long-distance transportation are high, liquid product packing cost difficulty, avoided also that conventionally spray-dried investment is large, the product performance loss, the solid phase prod performance is low, energy consumption is high, conventional microwave drying energy consumption is high, and byproduct steam does not add the problems such as utilization.
Description of drawings
Fig. 1: be the process flow sheet of preferred embodiment of the present invention.
Embodiment
Below by example the present invention is specifically described.Be necessary to be pointed out that at this; following instance only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the foregoing invention content.
Embodiment 1
A kind of production method of solid polycarboxylic acid water reducing agent, to be 40% polycarboxylate water-reducer stoste with 700kg/h quality percentage composition, the 1bar steam that utilizes microwave drying to obtain is 42% with polycarboxylate water-reducer vacuum concentration to quality percentage composition, material after will concentrating with toothed gear pump is sent on the travelling belt uniformly, keep travelling belt material thickness 9cm to enter in the tunnel type micro wave loft drier, at the microwave drying upper box part vapor collection pipe is set, use blower fan that microwave steam is sent in the vapor collection pipe, 20 of single microwave drying oven length 1m series connection, microwave drying oven total length 20m, total power is 2200kw, microwave drying time control 13min, the microwave frequency that adopts is 2450M HZ, irradiation energy is 3300KJ/KG, travelling belt speed is 0.7m/min, drying temperature is 96 ℃, form hard and the crisp and inner solid that contains a large amount of bubbles, after sending into solid the cooling of dry air cooling tank, travelling belt sends into pulverizer, obtain water content and be lower than 2% polycarboxylate water-reducer solid phase prod, this solid polycarboxylic acid water reducing agent can be consistent with same amount liquid water reducer performance after tested; Per hour can dry obtain the solid polycarboxylic acid water reducing agent of 200kg, be suitable for large-scale industrial production.
Embodiment 2
A kind of production method of solid polycarboxylic acid water reducing agent, be that 45%(is in the quality percentage composition with solid content) commodity liquid polycarboxylate water-reducer adopt volumetric pump that it is drawn on the travelling belt, send into microwave drying oven and transmit drying, the microwave frequency of described employing is 915MHZ, irradiation energy is 3000KJ/KG, and microwave power is 1500KW; The thickness of control material on travelling belt is 8cm, and travelling belt speed is 0.8m/min, and drying temperature is 100 ℃, and be 18 minutes time of drying; Send into pulverizer after the air cooling of dried solid polycarboxylic acid water reducing agent drying, broken rear pack namely obtains product.The solid content of the solid polycarboxylic acid water reducing agent of gained is that 96～97%(is in the quality percentage composition), the solid polycarboxylic acid water reducing agent performance reach identical solid content liquid polycarboxylate water-reducer use properties 97%.Production efficiency is high, the solid polycarboxylic acid water reducing agent of gained can reach 140kg/h.
Embodiment 3
A kind of production method of solid polycarboxylic acid water reducing agent, being that 30%(is in the quality percentage composition to solid content at first) the liquid polycarboxylate water-reducer carries out vacuum concentration, in 0.2～0.5bar(absolute pressure) under, the 1bar(absolute pressure that adopts microwave drying to produce) steam carries out external source to the liquid polycarboxylate water-reducer and is heated to 85 ℃, makes its solid content be increased to 40%(in the quality percentage composition); Again the polycarboxylate water-reducer employing travelling belt of described vacuum concentration is sent into and carried out microwave drying in the microwave drying oven, at the microwave drying upper box part vapor collection pipe is set, use blower fan that microwave steam is sent in the vapor collection pipe, the microwave frequency that adopts is 2450MHZ, and irradiation energy is 4000KJ/KG, and microwave power is 2500KW, the thickness of control material on travelling belt is 10cm, travelling belt speed is 0.5m/min, and drying temperature is 90 ℃, and be 12 minutes time of drying; Send into pulverizer after the air cooling of dried solid polycarboxylic acid water reducing agent drying, broken rear pack namely obtains product.The solid content of the solid polycarboxylic acid water reducing agent of gained is that 98～100%(is in the quality percentage composition), the solid polycarboxylic acid water reducing agent performance reach identical solid content liquid polycarboxylate water-reducer use properties 96%.Production efficiency is high, the solid polycarboxylic acid water reducing agent of gained can reach 100kg/h.
Embodiment 4～7: undertaken by following material and technique, all the other are with embodiment 3.
More than obtain the solid polycarboxylic acid water reducing agent performance and reach 95～100% of same amount liquid water reducer performance, the solid content of the solid polycarboxylic acid water reducing agent of dry gained is that 97～100%(is in the quality percentage composition), significantly lowered transportation and packing cost.Production efficiency is high, the solid polycarboxylic acid water reducing agent of gained can reach 100～160kg/h.
Embodiment 8
The contrast experiment: with the embodiment 1 gained polycarboxylate water-reducer solid phase prod aqueous solution that is made into the 20wt% solid content soluble in water, the liquid sample that alternative is got the polycarboxylate water-reducer of commodity 20wt% solid content compares test, and the test main project is as follows:
1, the flowing degree of net paste of cement simultaneous test of solid polycarboxylic acid water reducing agent
The cement paste fluidity measuring method: press GB8077-87 " concrete admixture uniformity test method " and measure flowing degree of net paste of cement, wherein cement takes by weighing 300g, and water takes by weighing 87g, and admixture dosage 1.3%, cement are standard cement.
| Dry sample | The aqueous solution | |
| Flowing degree of net paste of cement/mm | 230 | 220 |
2, solid polycarboxylic acid water reducing agent concrete simultaneous test
Raw material: standard cement, standard river sand, stone are 5～25mm continuous grading.
| Cement | Husky | Stone | Water | Water reducer |
| 360Kg | 860Kg | 105Kg | 180Kg | 5.4Kg |
Test result:
| Slump/expansion ratio | The 30min loss of slump | |
| Solid phase prod | 200/520mm | 20mm |
| Liquid product | 205/520mm | 20mm |
Conclusion: the solid polycarboxylic acid water reducing agent use properties that the present invention makes is consistent with the performance of commodity poly carboxylic acid liquid water reducer, and result of use is not affected because being processed into solid phase prod.
Claims (7)
1. the production method of a solid polycarboxylic acid water reducing agent is characterized in that: adopt microwave to carry out drying the liquid polycarboxylate water-reducer, the control drying temperature is 90～100 ℃.
2. production method as claimed in claim 1, it is characterized in that: adopt travelling belt to send into microwave drying oven described liquid polycarboxylate water-reducer and transmit drying, the microwave frequency of using is 915MHZ or 2450MHZ, irradiation energy is 3000～4000KJ/KG, microwave power is 1500～2500KW, and the thickness of dried material is 8～10cm, and the travelling belt transfer rate is 0.5～0.8m/min, be 12～18min time of drying, and drying temperature is 93～98 ℃.
3. production method as claimed in claim 2, it is characterized in that: the microwave frequency of described employing is 2450MHZ, irradiation energy is 3200～3600KJ/KG, microwave power is 1900～2300KW, the thickness of dried material is 9～10cm, the travelling belt transfer rate is 0.6～0.7m/min, and be 12～15min time of drying.
4. production method as claimed in claim 1, it is characterized in that: adopt travelling belt to send into microwave drying oven described liquid polycarboxylate water-reducer and transmit drying, the microwave frequency of using is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW; The thickness of control material on travelling belt is 9cm, and travelling belt speed is 0.7m/min, and drying temperature is 96 ℃, and be 13 minutes time of drying.
5. such as each described production method of claim 1～4, it is characterized in that: also at the microwave drying upper box part vapor collection pipe is set, uses blower fan that microwave steam is sent in the vapor collection pipe, make in the loft drier to be about the 0.9bar(absolute pressure for little negative pressure).
6. production method as claimed in claim 5, it is characterized in that: before described microwave drying, at first the liquid polycarboxylate water-reducer is carried out vacuum concentration, under vacuum condition, adopt fresh 1～10bar(absolute pressure) the 1bar(absolute pressure that produces of steam or microwave drying) steam carries out external source to the liquid polycarboxylate water-reducer and is heated to 85～90 ℃, make its solid content be increased to 30～45%, in the quality percentage composition.
7. production method as claimed in claim 1, it is characterized in that: be that 10～70wt% liquid polycarboxylate water-reducer carries out vacuum concentration to solid content at first, in 0.01～1bar(absolute pressure) under, the 1bar(absolute pressure that adopts microwave drying to produce) steam carries out external source to the liquid polycarboxylate water-reducer and is heated to 88 ℃, make its solid content be increased to 42%, in the quality percentage composition; Again the polycarboxylate water-reducer employing travelling belt of described vacuum concentration is sent into and carried out microwave drying in the microwave drying oven, at the microwave drying upper box part vapor collection pipe is set, use blower fan that microwave steam is sent in the vapor collection pipe, the microwave frequency that adopts is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW, the thickness of control material on travelling belt is 9cm, travelling belt speed is 0.7m/min, and drying temperature is 93～98 ℃, and be 13 clocks time of drying.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104174178A (en) * | 2013-05-22 | 2014-12-03 | 宁阳瑞安工贸有限公司 | Drying method of flaky, strip-shaped or granular solid polycarboxylate superplasticizer |
| CN104501539A (en) * | 2014-12-01 | 2015-04-08 | 武汉理工大学 | Low-temperature drying method for polycarboxylate superplasticizer |
| CN110926116A (en) * | 2018-09-20 | 2020-03-27 | 天津金耀集团有限公司 | Drying method of solid material of steroid compound |
| CN116515045A (en) * | 2023-05-06 | 2023-08-01 | 上海宏韵新型建材有限公司 | Preparation method of slice type polycarboxylate superplasticizer |
-
2012
- 2012-06-01 CN CN201210178934.5A patent/CN102936349B/en active Active
Non-Patent Citations (2)
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| 《福建建筑》 20100701 方云辉 "固体聚羧酸减水剂的制备研究" 第145卷, 第7期 * |
| 方云辉: ""固体聚羧酸减水剂的制备研究"", 《福建建筑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104174178A (en) * | 2013-05-22 | 2014-12-03 | 宁阳瑞安工贸有限公司 | Drying method of flaky, strip-shaped or granular solid polycarboxylate superplasticizer |
| CN104501539A (en) * | 2014-12-01 | 2015-04-08 | 武汉理工大学 | Low-temperature drying method for polycarboxylate superplasticizer |
| CN110926116A (en) * | 2018-09-20 | 2020-03-27 | 天津金耀集团有限公司 | Drying method of solid material of steroid compound |
| CN116515045A (en) * | 2023-05-06 | 2023-08-01 | 上海宏韵新型建材有限公司 | Preparation method of slice type polycarboxylate superplasticizer |
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Address after: 408200 Chongqing Fengdu Industrial Park Zhenjiang Fine Chemical Park Patentee after: CHONGQING ZIGUANG HESHENG BUILDING MATERIAL Co.,Ltd. Address before: 408200 Zhenjiang fine chemical industry park, Fengdu County, Chongqing Patentee before: CHONGQING ZIGUANG HESHENG BUILDING MATERIAL Co.,Ltd. |