CN102145985B - Preparation method of high-efficiency water reducing agent and early strength agent for concrete - Google Patents
Preparation method of high-efficiency water reducing agent and early strength agent for concrete Download PDFInfo
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- CN102145985B CN102145985B CN 201010107223 CN201010107223A CN102145985B CN 102145985 B CN102145985 B CN 102145985B CN 201010107223 CN201010107223 CN 201010107223 CN 201010107223 A CN201010107223 A CN 201010107223A CN 102145985 B CN102145985 B CN 102145985B
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Abstract
The invention provides a preparation method of a high-efficiency water reducing agent and an early strength agent for concrete. The preparation method comprises the following steps of: adding 1,200-1,400 kg of industrial naphthalene into a reaction kettle, heating for melting, raising the temperature to 110-120 DEG C, stirring uniformly, continually raising the temperature to 140-150 DEG C within 30 minutes and slowly adding 1,200-1,300 kg of sulfuric acid; raising the temperature to 155-160 DEG C, preserving heat for 3-4 hours and undergoing a sulfonation reaction; at the end of sulfonation, lowering the temperature to 120 DEG C and controlling the acid value at 31-32 percent; adding water to undergo a hydrolysis reaction, controlling the acid value at 28-28.5 percent and lowering the temperature to 90-100 DEG C when the acid value reaches a required level; adding 760-780 kg of formaldehyde within 2 hours and preserving heat for 4-5 hours; undergoing a condensation reaction and controlling the temperature at 100-120 DEG C; after condensation, adding 1,800-2,000 kg of carbide slag within 60 minutes for neutralizing until the pH value is between 8 and 9; separating by using a centrifuger with the rotating speed 10,000 revolutions per minute and drying the separated supernatant serving as a water reducing agent intermediate at the temperature of 380 DEG C to obtain the high-efficiency water reducing agent; separating a precipitate serving as an early strength agent intermediate, drying at the temperature between 140-150 DEG C, grinding, adding citric acid or 5-8 percent gluconic acid sodium salt, and stirring uniformly to obtain the early strength agent.
Description
Technical field
The present invention relates to the reasonable utilization of carbide slag, is that production technique is implemented to improve and optimization to traditional naphthalene, gets the preparation method of its high efficiency water reducing agent and hardening accelerator.
Background technology
The present invention utilizes the waste material of producing polyvinyl chloride, and namely carbide slag is raw material, by being the improvement of production technique to traditional naphthalene, the production method that is used for concrete high efficiency water reducing agent and hardening accelerator product of obtaining is still few in the pertinent literature retrieval report at home.The production technique that the present invention conceives the carbide slag of employing is diverse with adopting liquid caustic soda to produce technique, carbide slag is half wet solid, can't join in the reactor, N-process in the reaction must be put into separately another container carries out for this reason, the rotary conveyor that the neutralization reaction of scale production need adopt electronic scales with carbide slag through measuring uniform input, control the size of its reaction particles with specific rate of feeding, be beneficial to the separation of slag body, slag body after the separation, through composite, oven dry, obtain its product.This production method is brand-new, environmental protection, energy-conservation.
Summary of the invention
Purpose of the present invention: being used for the preparation method of concrete high efficiency water reducing agent and hardening accelerator, is to be optimization and the modification of production technique to traditional naphthalene, belongs to subtracting energy consumption, and energy saving and environment friendly production technique has higher using value.
The object of the present invention is achieved like this: a kind of preparation method for concrete high efficiency water reducing agent and hardening accelerator, NAPTHALENE FLAKES. (INDUSTRIAL GRADE） 1200-1400 kilogram is dropped in the reactor, heating is dissolved, being warming up to 110-120 ℃ stirs, when continuing 140-150 ℃ of intensification, slowly add sulfuric acid 1200-1300 kilogram, the time was controlled in 30 minutes; Be warming up to 155-160 ℃, constant temperature 3-4 hour, carry out sulfonation reaction; Sulfonation finishes, and temperature is down to 120 ℃, and acid number is controlled at 31%-32%; Add the water hydrolysis reaction, when acid number reached, namely acid number was controlled at 28%-28.5%, was cooled to 90-100 ℃; In 2 hours, add formaldehyde 760-780 kilogram, constant temperature 4-5 hour; Carry out condensation reaction, temperature is controlled at 100-120 ℃; After the condensation, with adding the neutralization of 1800-2000 kilogram carbide slag in 60 minutes, in and the pH value reach 8-9 and get final product, N-process is put into separately another container to carry out; The employing rotating speed is that 10000r/1 minute whizzer separates, and the supernatant liquor of separation is the water reducer intermediate, through the dry oven dry of 380 ℃ temperature, namely gets high efficiency water reducing agent; The paste throw out that separates is the hardening accelerator intermediate, through 140-150 ℃ temperature oven dry, pulverizes, and adding citric acid or Sunmorl N 60S 5-8% stir, and namely get hardening accelerator.
The preparation method of described water reducer and hardening accelerator, the amount of water of hydrolysis reaction is that every mole of naphthalene hydrolysis adds 20 gram water.
The preparation method of described water reducer and hardening accelerator, the clean slurry value after the condensation reaches more than the 220mm.
The preparation method of described water reducer and hardening accelerator is characterized in that the concentration of the formaldehyde selected is more than 36%.
The preparation method of described water reducer and hardening accelerator selects the concentration of sulfuric acid more than 98%.
The preparation method of described water reducer and hardening accelerator, the fineness of gained high efficiency water reducing agent and hardening accelerator is≤13 granularities after the oven dry.
Design mechanism of the present invention:
The naphthalene series high-efficiency water-reducing agent of selecting is naphthalene sulfonic acidformaldehyde condensation product, can reduce mixing water content in the concrete, winter construction is without crystallization, can obviously increase concrete slump, improve concrete workability, save cement consumption, the reinforcing bar non-corroding is endangered, concrete shrinkage is had no adverse effects, improve largely the various mechanical properties of concrete and the endurance quality such as impervious, be fit to preparation early strong, high-strength, high impervious, self-compacting, pump concrete and gravitational grouting material, can be widely used in natural curing and steamed concrete engineering and goods.
The concrete early strength water-reducing agent of selecting belongs to non-chloride salt powdery concrete admixture, to the effect of reinforcing bar non-corroding, be suitable for temperature condition construction more than-5 ℃, reduce to some extent the mixing water consumption, increase slump, improve concrete strength, be applicable to the engineerings such as prefabricated components, prestressed concrete and common buildings, road, bridge, water conservancy, oil field and urban construction, this product is divided into I, II, three kinds of models of III, the III type is the composite highly effective early strength water-reducing agent, I, II type are applicable to the following concrete of C25, and the III type is applicable to C30, C40 concrete.
The present invention design is that production technique is implemented to improve to traditional naphthalene, and the method for utilizing carbide slag to produce water reducer, hardening accelerator is rational, feasible, and higher using value is arranged, and the not only energy-conservation but also environmental protection of this technique shows technical progress.
Description of drawings
Accompanying drawing is the process flow diagram that carbide slag is produced high efficiency water reducing agent, hardening accelerator.
Embodiment
Embodiment 1
In 1300 kilograms of input reactors of NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, heating is dissolved, and heats up 120 ℃ to stir; Heat up 140 ℃ the time, slowly add 1300 kilograms in sulfuric acid (concentration is more than 98%), the time was controlled in 30 minutes; Be warming up to 155 ℃, constant temperature 4 hours carries out sulfonation reaction; Sulfonation finishes, and temperature is down to 120 ℃, and acid number is controlled at 32%; Add water hydrolysis (amount adds 20 gram water for every mole of naphthalene hydrolysis) reaction, when acid number reached, acid number was controlled at 28%; Be cooled to 95 ℃; In 1.5 hours, add 780 kilograms in formaldehyde (concentration is more than 36%), constant temperature 4 hours; Carry out condensation reaction, temperature is controlled at 100 ℃; After the condensation (clean slurry value should reach more than the 220mm), with adding the neutralization of 1800-2000 kilogram carbide slag in 60 minutes, in reach 8-9 with the pH value and get final product, N-process is put into separately another container to carry out; The employing rotating speed is that 10000r/1 minute whizzer separates, and the supernatant liquor of separation is the water reducer intermediate, through the dry oven dry of 380 ℃ temperature (fineness is≤13 granularities), is high efficiency water reducing agent; The paste throw out that separates is the hardening accelerator intermediate, through 150 ℃ temperature oven dry, pulverizes (fineness is≤13 granularities), and adding citric acid 8% stirs, and namely gets hardening accelerator.
Embodiment 2
In 1350 kilograms of input reactors of NAPTHALENE FLAKES. (INDUSTRIAL GRADE）, heating is dissolved, and heats up 110 ℃ to stir; When being warming up to 150 ℃, slowly add 1200 kilograms in sulfuric acid (concentration is more than 98%), the time was controlled in 30 minutes; Heat up 150 ℃, constant temperature 4 hours carries out sulfonation reaction; Sulfonation finishes, and temperature is down to 120 ℃, and acid number is controlled at 31%; Add water hydrolysis (amount adds 20 gram water for every mole of naphthalene hydrolysis) reaction, when acid number reached, acid number was controlled at 28.5%; Be cooled to 95 ℃; In 2 hours, add 760 kilograms in formaldehyde (concentration is more than 36%), constant temperature 4.5 hours; Carry out condensation reaction, temperature is controlled at 110 ℃; After the condensation (clean slurry value should reach more than the 220mm), with adding the neutralization of 1800-2000 kilogram carbide slag in 60 minutes, in reach 8-9 with the pH value and get final product, N-process is put into separately another container to carry out; The employing rotating speed is that 10000r/1 minute whizzer separates, and the supernatant liquor of separation is the water reducer intermediate, through the dry oven dry of 380 ℃ temperature (fineness is≤13 granularities), is high efficiency water reducing agent; The paste throw out that separates is the hardening accelerator intermediate, through 140 ℃ temperature oven dry, pulverizes (fineness is≤13 granularities), adds Sunmorl N 60S 7% and stirs, and namely gets hardening accelerator.
A, verify the performance of its high efficiency water reducing agent:
1. under the cement consumption condition identical with slump, use this water reducer, can reduce the 15-23% of mixing water amount; Its intensity of the 1st day can improve 40-50%, and intensity increased 30-40% again in the 3rd day, and intensity increased 10-20% again in the 28th day.
2. under the constant condition of identical cement consumption and water cement ratio, use this product, can obviously improve concrete workability, slump can increase 1.0-7.5 doubly.
3. in slump and the essentially identical situation of intensity, use this product, can save the 1.0-1.5% of cement consumption.
4. this product, has no adverse effects to concrete shrinkage without harm to reinforcing bar, can improve the various mechanical properties of concrete and the endurance quality such as impervious.
B, verify the performance of its concrete early strength agent:
1. at identical cement consumption, with the slump condition under, use this hardening accelerator, can reduce the mixing water amount, the I type be 7-10%, the II type be 10-15%, the III type be 15-20%.
2. at identical cement consumption, with the water cement ratio condition under, mixing this product slump can increase, more than the I type 3cm, more than the II type 5cm, more than the III type 8cm.
3. in same proportioning, under the slump condition, 3 days, 7 days, 28 days intensity is compared with common concrete and can be improved respectively I type 50%, 30%, 10%, II type 50%, 45%, 20%, III type 80%, 60%, 20%.
Claims (6)
1. preparation method who is used for concrete high efficiency water reducing agent and hardening accelerator, it is characterized in that: NAPTHALENE FLAKES. (INDUSTRIAL GRADE） 1200-1400 kilogram is dropped in the reactor, heating is dissolved, being warming up to 110-120 ℃ stirs, when continuing 140-150 ℃ of intensification, slowly add sulfuric acid 1200-1300 kilogram, the time was controlled in 30 minutes; Be warming up to 155-160 ℃, constant temperature 3-4 hour, carry out sulfonation reaction; Sulfonation finishes, and temperature is down to 120 ℃, and acid number is controlled at 31%-32%; Add the water hydrolysis reaction, when acid number reached, namely acid number was controlled at 28%-28.5%, was cooled to 90-100 ℃; In 2 hours, add formaldehyde 760-780 kilogram, constant temperature 4-5 hour; Carry out condensation reaction, temperature is controlled at 100-120 ℃; After the condensation, with adding the neutralization of 1800-2000 kilogram carbide slag in 60 minutes, in and the pH value reach 8-9 and get final product, N-process is put into separately another container to carry out; The employing rotating speed is that 10000r/1 minute whizzer separates, and the supernatant liquor of separation is the water reducer intermediate, through the dry oven dry of 380 ℃ temperature, namely gets high efficiency water reducing agent; The paste throw out that separates is the hardening accelerator intermediate, through 140-150 ℃ temperature oven dry, pulverizes, and adding citric acid or Sunmorl N 60S 5-8% stir, and namely get hardening accelerator.
2. according to the preparation method of water reducer claimed in claim 1 and hardening accelerator, it is characterized in that: the amount of water of hydrolysis reaction is that every mole of naphthalene hydrolysis adds 20 gram water.
3. according to the preparation method of water reducer claimed in claim 1 and hardening accelerator, it is characterized in that: the clean slurry value after the condensation reaches more than the 220mm.
4. according to the preparation method of water reducer claimed in claim 1 and hardening accelerator, it is characterized in that: the concentration of the formaldehyde of selecting is more than 36%.
5. according to the preparation method of water reducer claimed in claim 1 and hardening accelerator, it is characterized in that: select the concentration of sulfuric acid more than 98%.
6. according to the preparation method of water reducer claimed in claim 1 and hardening accelerator, it is characterized in that: the fineness of gained high efficiency water reducing agent and hardening accelerator is≤13 granularities after the oven dry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204645A (en) * | 2013-04-24 | 2013-07-17 | 湖北恒利建材科技有限公司 | High-strength environmental-friendly high-efficiency water reducing admixture and preparation method thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271348A (en) * | 2015-10-11 | 2016-01-27 | 莱芜睿腾新型建材科技有限公司 | Preparation method of residue-free high-concentration water reducer |
| CN106630728A (en) * | 2016-09-07 | 2017-05-10 | 南京凯盛国际工程有限公司 | Blending method for early-strength water-reducing agent used for concrete |
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| CN1800075A (en) * | 2005-09-14 | 2006-07-12 | 中国建筑第三工程局商品混凝土公司 | Simplified method for preparing low alkaline naphthalene series concrete water reducing agent |
| CN101050082A (en) * | 2007-04-30 | 2007-10-10 | 江苏海润化工有限公司 | Water reducing agent for rare earth concrete and preparation method |
| CN101182167A (en) * | 2007-11-15 | 2008-05-21 | 武汉理工大学 | Wet-discharging fly ash composite carbide slag blending slurry and method for preparing the same |
| KR100847585B1 (en) * | 2007-05-22 | 2008-08-05 | 전남대학교산학협력단 | The preparation for concrete dispersion |
| CN101386587A (en) * | 2007-09-13 | 2009-03-18 | 浙江龙盛集团股份有限公司 | Production technology of methyl naphthalenesulfonic acid-methyl aldehyde condensation compound |
| CN101580352A (en) * | 2009-03-19 | 2009-11-18 | 四川吉龙化学建材有限公司 | Naphthalene water-reducing agent and processing technique of homologous dispersant thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1800075A (en) * | 2005-09-14 | 2006-07-12 | 中国建筑第三工程局商品混凝土公司 | Simplified method for preparing low alkaline naphthalene series concrete water reducing agent |
| CN101050082A (en) * | 2007-04-30 | 2007-10-10 | 江苏海润化工有限公司 | Water reducing agent for rare earth concrete and preparation method |
| KR100847585B1 (en) * | 2007-05-22 | 2008-08-05 | 전남대학교산학협력단 | The preparation for concrete dispersion |
| CN101386587A (en) * | 2007-09-13 | 2009-03-18 | 浙江龙盛集团股份有限公司 | Production technology of methyl naphthalenesulfonic acid-methyl aldehyde condensation compound |
| CN101182167A (en) * | 2007-11-15 | 2008-05-21 | 武汉理工大学 | Wet-discharging fly ash composite carbide slag blending slurry and method for preparing the same |
| CN101580352A (en) * | 2009-03-19 | 2009-11-18 | 四川吉龙化学建材有限公司 | Naphthalene water-reducing agent and processing technique of homologous dispersant thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103204645A (en) * | 2013-04-24 | 2013-07-17 | 湖北恒利建材科技有限公司 | High-strength environmental-friendly high-efficiency water reducing admixture and preparation method thereof |
| CN103204645B (en) * | 2013-04-24 | 2016-01-20 | 湖北恒利建材科技有限公司 | A kind of high-strength environment-friendly high-efficiency water reducer and preparation method thereof |
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