CN102936349B - 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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- CN102936349B CN102936349B CN201210178934.5A CN201210178934A CN102936349B CN 102936349 B CN102936349 B CN 102936349B CN 201210178934 A CN201210178934 A CN 201210178934A CN 102936349 B CN102936349 B CN 102936349B
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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 under concrete workability and the constant condition of cement consumption, can reduce mixing water amount, improves concrete strength, or under the constant condition of easily property and intensity, saves the admixture of cement consumption.
Polycarboxylate water-reducer is a kind of conventional cement dispersants 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 that water-reducing rate is high, volume is few, function of slump protection is good, amount of air entrainment is moderate, and suitable configuration high strength, high workability, self-compacting concrete progressively obtain the approval in market, at national market, are used widely.
Aqueous solution polymerization is generally used in the production of polycarboxylate water-reducer, and the commodity polycarboxylate water-reducer therefore obtaining is solution morphology, and solid content is generally 10～70%.Molecular weight due to polycarboxylate water-reducer, its solids is softened 80 ℃ of above just easily generations, as use conventional drying mode water and material to be heated simultaneously as dry grade of spraying, must add auxiliary agent could realize the dry solid polycarboxylic acid water reducing agent that obtains, it is dried difficulty, drying cost is high, the dry water reducer obtaining 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 be all solid content 10～70%(by percentage to the quality) aqueous solution liquid product, long-distance transportation is with high costs, part solid phase prod is only applied to some special dimension 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 approaches with the liquid polycarboxylate water-reducer use properties of identical solid content.
For reaching above object the present invention, adopt following technical scheme:
A production method for solid polycarboxylic acid water reducing agent, is characterized in that: solid content is dried for 10～70% liquid polycarboxylate water-reducers (commercially available prod) in mass concentration adopt microwave, and controlling drying temperature is 90～100 ℃.
The liquid polycarboxylate water-reducer that is 10～70% to the solid content that adopts water solution polymerization process directly to obtain carries out the solid polycarboxylic acid water reducing agent that microwave drying obtains, its water content can be controlled in 5%(in quality percentage composition) below, it is better that the solid polycarboxylic acid water reducing agent performance simultaneously obtaining reaches the liquid polycarboxylate water-reducer use properties of identical solid content; Contriver finds through long-term experiment, microwave has extremely strong selectivity heating to water, be first to the moisture heating evaporation in institute's dried material and then the polycarboxylate water-reducer in heated solution, so both guarantee the abundant of polycarboxylate water-reducer to be dried, guaranteed again the performance of gained solid polycarboxylic acid water reducing agent.
In order further to improve microwave drying effect and production efficiency, specifically aforesaid liquid polycarboxylate water-reducer being adopted travelling belt to send into microwave drying oven transmits dry, 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 travelling belt transfer rate is 0.5～0.8m/min, be 12～18min time of drying, and drying temperature is 93～98 ℃.Contriver finds in long-term experiment, if control the bad requirement that also easily makes production efficiency lowly not reach large-scale industrialization production if thereby above parameter is controlled the bad performance that there will be local superheating to affect the solid polycarboxylic acid water reducing agent making, 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 travelling belt transfer rate is 0.6～0.7m/min, and be 12～15min time of drying.
Aforesaid liquid polycarboxylate water-reducer transmits dry at microwave drying oven, more preferably, the microwave frequency of above-mentioned employing is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW; Controlling the thickness of 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 quality percentage composition), 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 microwave drying, also at microwave drying upper box part, vapor collection pipe is set, use blower fan that microwave steam is sent in vapor collection pipe, make for micro-negative pressure, to be about 0.9bar(absolute pressure in loft drier), greatly improved vaporization efficiency.
In order further to improve microwave drying efficiency, before above-mentioned microwave drying, first liquid polycarboxylate water-reducer is carried out to 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 liquid polycarboxylate water-reducer and is heated to 85～90 ℃, makes its solid content be increased to 30～45%(in quality percentage composition).While starting first to carry out vacuum concentration without microwave drying byproduct steam, just adopt fresh low-pressure steam, if carried out microwave drying, the low-pressure steam that 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: to solid content, be first that 10～70%(is in quality percentage composition) 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 liquid polycarboxylate water-reducer and is heated to 88 ℃, makes its solid content be increased to 42%(in quality percentage composition); To the polycarboxylate water-reducer of described vacuum concentration, adopt travelling belt to send into again and in microwave drying oven, carry out microwave drying, at microwave drying upper box part, vapor collection pipe is set, use blower fan that microwave steam is sent in vapor collection pipe, the microwave frequency adopting is 2450MHZ, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW, controlling the thickness of 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 quality percentage composition), solid polycarboxylic acid water reducing agent performance reach identical solid content liquid polycarboxylate water-reducer use properties 95%～100%.After the air cooling of dried solid polycarboxylic acid water reducing agent drying, send into pulverizer, broken rear pack 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 microwave drying process simultaneously, the temperature that has guaranteed polycarboxylate water-reducer is unlikely too high and causes the destruction to its performance, production obtains 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 quality percentage composition), control moisture at (in quality percentage composition) below 2%, significantly lowered transportation and packing cost.The inventive method production efficiency is high simultaneously, can reach 180～200kg/h, is suitable for large-scale industrial production.
2, in the inventive method, utilized and reclaimed the low-pressure steam that microwave produces, water reducer has been carried out to 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 polycarboxylate water-reducer long-distance transportation are high, liquid product packing cost difficulty, also avoided that conventionally spray-dried investment is large, product performance loss, 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.
Accompanying drawing explanation
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 is only used to further illustrate the present invention; 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 foregoing invention content.
Embodiment 1
A kind of production method of solid polycarboxylic acid water reducing agent, the polycarboxylate water-reducer stoste that is 40% by 700kg/h quality percentage composition, utilizing the 1bar steam that microwave drying obtains is 42% by polycarboxylate water-reducer vacuum concentration to quality percentage composition, with toothed gear pump, the material after concentrated is sent on travelling belt uniformly, keep travelling belt material thickness 9cm to enter in tunnel type micro wave loft drier, at microwave drying upper box part, vapor collection pipe is set, use blower fan that microwave steam is sent in vapor collection pipe, 20 of single microwave drying oven length 1m series connection, microwave drying oven total length 20m, total power is 2200kw, the microwave drying time is controlled 13min, the microwave frequency adopting 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, through travelling belt, solid is sent into dry air cooling tank and sent into pulverizer after cooling, obtain water content 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, the solid polycarboxylic acid water reducing agent that obtains 200kg that is dried per hour, is suitable for large-scale industrial production.
Embodiment 2
A kind of production method of solid polycarboxylic acid water reducing agent, by solid content, be that 45%(is in quality percentage composition) commodity liquid polycarboxylate water-reducer adopt volumetric pump to be drawn on travelling belt, sending into microwave drying oven transmits dry, the microwave frequency of described employing is 915MHZ, irradiation energy is 3000KJ/KG, and microwave power is 1500KW; Controlling the thickness of 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; After the air cooling of dried solid polycarboxylic acid water reducing agent drying, send into pulverizer, broken rear pack obtains product.The solid content of the solid polycarboxylic acid water reducing agent of gained is that 96～97%(is in quality percentage composition), 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, first to solid content, being that 30%(is in quality percentage composition) 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 liquid polycarboxylate water-reducer and is heated to 85 ℃, makes its solid content be increased to 40%(in quality percentage composition); To the polycarboxylate water-reducer of described vacuum concentration, adopt travelling belt to send into again and in microwave drying oven, carry out microwave drying, at microwave drying upper box part, vapor collection pipe is set, use blower fan that microwave steam is sent in vapor collection pipe, the microwave frequency adopting is 2450MHZ, and irradiation energy is 4000KJ/KG, and microwave power is 2500KW, controlling the thickness of 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; After the air cooling of dried solid polycarboxylic acid water reducing agent drying, send into pulverizer, broken rear pack obtains product.The solid content of the solid polycarboxylic acid water reducing agent of gained is that 98～100%(is in quality percentage composition), 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: by following material and technique, undertaken, all the other are with embodiment 3.
More than obtain 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 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
Contrast experiment: by the embodiment 1 gained polycarboxylate water-reducer solid phase prod aqueous solution that is made into 20wt% solid content soluble in water, the liquid sample that alternative is got the polycarboxylate water-reducer of commodity 20wt% solid content carries out simultaneous test, and test main project is as follows:
1, the flowing degree of net paste of cement simultaneous test of solid polycarboxylic acid water reducing agent
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 300g, and water takes 87g, admixture dosage 1.3%, cement is 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 is 5～25mm continuous grading.
| Cement | Husky | Stone | Water | Water reducer |
| 360Kg | 860Kg | 105Kg | 180Kg | 5.4Kg |
Test result:
| Slump/expansion ratio | 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, result of use is not affected because being processed into solid phase prod.
Claims (6)
1. a production method for solid polycarboxylic acid water reducing agent, is characterized in that: adopt microwave to be dried liquid polycarboxylate water-reducer; Adopting travelling belt to send into microwave drying oven described liquid polycarboxylate water-reducer transmits dry, the microwave frequency of using is 915MHz or 2450MHz, irradiation energy is 3000～4000KJ/KG, microwave power is 1500～2500KW, the thickness of dried material is 8～10cm, travelling belt transfer rate is 0.5～0.8m/min, and be 12～18min time of drying, and drying temperature is 93～98 ℃.
2. production method as claimed in claim 1, 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, travelling belt transfer rate is 0.6～0.7m/min, and be 12～15min time of drying.
3. 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 dry, the microwave frequency of using is 2450MHz, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW; Controlling the thickness of 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.
4. the production method as described in claim 1～3 any one, is characterized in that: also at microwave drying upper box part, vapor collection pipe is set, uses blower fan that microwave steam is sent in vapor collection pipe, make for micro-negative pressure, to be about 0.9bar absolute pressure in loft drier.
5. production method as claimed in claim 4, it is characterized in that: before described microwave drying, first liquid polycarboxylate water-reducer is carried out to vacuum concentration, under vacuum condition, the 1bar absolute pressure steam that adopts fresh 1～10bar absolute pressure steam or microwave drying to produce carries out external source to liquid polycarboxylate water-reducer and is heated to 85～90 ℃, make its solid content be increased to 30～45%, in quality percentage composition.
6. production method as claimed in claim 1, it is characterized in that: to solid content, be first that 10～70wt% liquid polycarboxylate water-reducer carries out vacuum concentration, under 0.01～1bar absolute pressure, the 1bar absolute pressure steam that adopts microwave drying to produce carries out external source to liquid polycarboxylate water-reducer and is heated to 88 ℃, make its solid content be increased to 42%, in quality percentage composition; To the polycarboxylate water-reducer of described vacuum concentration, adopt travelling belt to send into again and in microwave drying oven, carry out microwave drying, at microwave drying upper box part, vapor collection pipe is set, use blower fan that microwave steam is sent in vapor collection pipe, the microwave frequency adopting is 2450MHz, and irradiation energy is 3300KJ/KG, and microwave power is 2200KW, controlling the thickness of 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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| 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 |
| CN116515045B (en) * | 2023-05-06 | 2024-09-17 | 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. |