CN104529222A - Retarding cement grinding aid and preparation method thereof - Google Patents
Retarding cement grinding aid and preparation method thereof Download PDFInfo
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- CN104529222A CN104529222A CN201410803354.XA CN201410803354A CN104529222A CN 104529222 A CN104529222 A CN 104529222A CN 201410803354 A CN201410803354 A CN 201410803354A CN 104529222 A CN104529222 A CN 104529222A
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- diethanolamine
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Abstract
The invention discloses a retarding cement grinding aid and a preparation method thereof. The retarding cement grinding aid is characterized by being prepared from the following raw materials in percentage by weight: 20%-30% of modified diethanol amine mother liquor, 1%-10% of glycerol, 5%-10% of sodium sulfate and the balance of water in a mixing manner; and the preparation method of the modified diethanol amine mother liquid comprises the following steps: weighing 21.1-25 parts of diethanol amine, 9.2 parts of epichlorohydrin and 10-12 parts of 40% sodium hydroxide aqueous solution; adding diethanol amine to a reaction container; dropwise adding epichlorohydrin and sodium hydroxide aqueous solution to the reaction container, stirring, and controlling the reaction temperature to be 40-50 DEG C; after dropwise adding, reacting for 1.0-2 hours; and evaporating a reaction product and removing the moisture, and taking supernatant liquid, namely the prepared modified diethanol amine mother liquor. The retarding cement grinding aid disclosed by the invention is easily adsorbed on the surfaces of cement granules; the aid-grinding and retarding effects are good; and the early and later strength of cement can be effectively improved.
Description
Technical field
The invention belongs to the admixture of cement, relate to a kind of retardation setting type cement grinding aid and preparation method thereof.The concrete of constructing under retardation setting type cement grinding aid of the present invention is specially adapted to hot climate, mass concrete and needing is parked or the cement concrete of long-distance transportation for a long time.
Background technology
Slow setting cement grinding aid is a kind of existing grind-aiding effect, can postpone again the cement additive of cement setting time; The concrete of constructing under being mainly used in hot climate, mass concrete and needing park for a long time or long-distance transportation cement concrete in.Slow setting cement grinding aid can improve the mill efficiency of cement clinker, optimizes cement granules grating, improves strength of cement; Concrete time of coagulation can be postponed, make fresh concrete keep plasticity in a long time, convenient construction; Owing to inhibit hydration heat speed, reduce the thermal discharge in concrete coagulation early stage, be therefore specially adapted to mass concrete engineering, early stage temperature can be prevented uneven and the phenomenon of cracking; The problem of constructing under can also solving concrete long-distance transportation and hot climate.The chemical composition of existing slow setting cement grinding aid mainly contains: molasses, sucrose, low molecular weight cellulose and derivative thereof, hydroxycarboxylic acid (salt) and inorganic salt etc.Complicated, too much interpolation inorganic salt improve reinforced effects, and effect is unstable.The absorption dispersion effect of glucide in cement is not good, is difficult to play good grinding-aid effect.And existing synthetic technology, generally need to use heating supercharging equipment, cost is higher.
Summary of the invention
Object of the present invention is intended to overcome deficiency of the prior art, provide that a kind of preparation technology is simple, delayed coagulation obviously and there is retardation setting type cement grinding aid of excellent grinding aid enhancement and preparation method thereof.
Content of the present invention is: a kind of retardation setting type cement grinding aid, is characterized in that: be the modification diethanolamine mother liquor of 20% ~ 30% by mass percent, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is water mixing composition;
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration is aqueous sodium hydroxide solution 10 ~ 12 mass parts of 40%, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) to be added dropwise in reaction vessel and to stir, controlling temperature of reaction is 40 ~ 50 DEG C, after dripping, then react 1.0 ~ 2 hours, pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor,
The chemical equation of described preparation modification diethanolamine mother liquor is:
In content of the present invention: describedly pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, be preferably and pour reaction product into container and be placed in vacuum drying oven, evaporation removing water wherein under the condition of temperature 70 ~ 90 DEG C, pressure 40 ~ 80Pa.
Another content of the present invention is: a kind of preparation method of retardation setting type cement grinding aid, it is characterized in that step is:
A, batching: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration be 40% aqueous sodium hydroxide solution 10 ~ 12 mass parts, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, for subsequent use;
B, preparation modification diethanolamine mother liquor: open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) being added dropwise in reaction vessel and stirring, control temperature of reaction is 40 ~ 50 DEG C; After dripping, then react 1.0 ~ 2 hours; Pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor;
C, prepare retardation setting type cement grinding aid: be the modification diethanolamine mother liquor of 20% ~ 30% by mass percentage, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is that water gets each component raw material; Modification diethanolamine mother liquor, glycerol, sodium sulfate and water are mixed, i.e. obtained retardation setting type cement grinding aid.
In another content of the present invention: pour reaction product into container described in step b and be placed in vacuum drying oven evaporation removing water wherein, be preferably and pour reaction product into container and be placed in vacuum drying oven, evaporation removing water wherein under the condition of temperature 70 ~ 90 DEG C, pressure 40 ~ 80Pa.
Compared with prior art, the present invention has features and beneficial effect:
(1) the present invention is adopted, the preparation process of slow setting cement grinding aid is without the need to any heating and pressurizing and vaccum-pumping equipment, can react at normal temperatures and pressures, synthesis cycle is short, operation is simple, and feasibility is high, and speed of reaction is fast, synthesis yield is high, and end product does not need through any separation or overanxious process;
(2) slow setting cement grinding aid provided by the invention, with the diethanolamine of modification for mother liquor, modified diethanolamine is small molecules polyhydroxy substance [(OHCH
2cH
2)
4n
2(CH
2)
2cH (OH)], easily form hydrogen bond, be conducive to being adsorbed on cement particle surface; This molecular structure polarity is large, the superfluous valency that can better balance on various material particles surface is good for, promote the infiltration of molecule in crackle, thus effectively improve the friability of material, weaken the reunion in mechanical milling process, stick with paste mill phenomenon, optimization grain composition can be played, improve the effect of strength of cement; When volume is 0.05%, and when keeping identical water cement ratio with control group, 28-day colloidal mortar compression strength of cement can improve 4.1Mpa; Because the functional groups point of modification diethanolamine is many, be very easily adsorbed on cement particle surface, form adsorption film, therefore effectively can delay the aquation of cement, postpone time of coagulation, and extend along with the increase of volume time of coagulation; When volume only 0.05% time, final setting time just can be made than contrast group leader more than 300min;
(3) adopt slow setting cement grinding aid provided by the invention, composite have a certain amount of glycerol, and object is to utilize the commissure effect forming hydrogen bond between polyhydroxy substance, improves the adsorptive power of grinding aid; The object of composite sodium sulfate is the intermiscibility regulating grinding aid, and sodium sulfate has certain enhancement; Glycerol and sodium sulfate mix the effect also serving and reduce product cost in right amount;
(4) retardation setting type cement grinding aid of the present invention has the following advantages: slow setting: grinding aid molecule of the present invention is polyhydroxy substance, easily forms hydrogen bond in cement particle surface absorption film-forming, thus delays hydrated cementitious; Grinding aid: the diethanolamine molecule polarity of modification is large, be adsorbed on the surperficial superfluous valency that can better balance on various material particles surface of cement clinker to be good for, promote the infiltration of molecule in crackle, thus effectively improve the friability of material, weaken the reunion in mechanical milling process, stick with paste mill phenomenon; Strengthen: after adding grinding aid of the present invention, cement macrobead content reduces, and specific surface area increases, and grain composition is optimized, thus serves the effect improving strength of cement; Therefore, after mixing slow setting grinding aid of the present invention, suitably can improve the consumption of mineral admixture, be conducive to energy-conserving profit waste;
(5) retardation setting type grinding aid provided by the invention also has the following advantages: diminishing: the cement of this slow setting of admixture grinding aid, standard consistency water requirement is lower than control group, mortar fluidity is greater than control group, and concrete workability is better than control group, is convenient to practice of construction; Delay heat release: early stage thermal discharge is low, avoid cement concrete inside and heat up too fast, temperature inequality causes the phenomenon of cracking, constructs under being specially adapted to mass concrete engineering and hot environment;
(6) product preparation process of the present invention is simple, and operation is easy, easily operates, practical.
Embodiment
The invention will be further described for embodiment plan given below; but can not be interpreted as it is limiting the scope of the invention; some nonessential improvement and adjustment that person skilled in art makes the present invention according to the content of the invention described above, still belong to protection scope of the present invention.
Described in embodiment 1 ~ 6, per-cent is mass percent.
Embodiment 1 (numbering DE-1):
A kind of retardation setting type cement grinding aid, consists of: the modification diethanolamine mother liquor of 20%, glycerol, the sodium sulfate of 5%, the water of 67% of 8%, total amount 100%.
The preparation process of this retardation setting type cement grinding aid has following steps:
A, take 21.1g diethanolamine, 9.2g epoxy chloropropane, added by diethanolamine in the there-necked flask of band whipping appts, epoxy chloropropane adds in constant pressure addition pipe for subsequent use; Take the NaOH aqueous solution of 10g 40%, add in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, slowly drip and stir, control temperature of reaction; Drip completely, then react 1.5 hours;
B, pour the reaction product of step a into beaker and be placed in vacuum drying oven, evaporating moisture content wherein, separate out NaCl, get supernatant liquid and namely obtain modification diethanolamine mother liquor;
The modification diethanolamine mother liquor of c, by mass percentage 20%, glycerol, the sodium sulfate of 5%, the water of 67% of 8%, get modification diethanolamine mother liquor, glycerol, sodium sulfate and water respectively and carry out composite mixing, i.e. obtained retardation setting type grinding aid.
Embodiment 2 ~ 6:
The proportioning of according to the form below 1, regulates the consumption of modification diethanolamine mother liquor, glycerol, sodium sulfate and water, prepares five kinds of retardation setting type grinding aids of embodiment numbering DE-2 ~ DE-6:
The proportioning raw materials of table 1 embodiment 1 ~ 6
| Numbering | Modification diethanolamine mother liquor % | Glycerol % | Sodium sulfate % | Water % |
| DE-1 | 20 | 8 | 5 | 67 |
| DE-2 | 22 | 8 | 5 | 65 |
| DE-3 | 24 | 4 | 7 | 65 |
| DE-4 | 26 | 4 | 7 | 63 |
| DE-5 | 28 | 2 | 9 | 61 |
| DE-6 | 30 | 2 | 9 | 59 |
The test of little mill is carried out to the slow setting grinding aid that embodiment 1 ~ 6 (numbering DE-1 ~ DE-6) obtains.
Test water mud grog and gypsum are all from Sichuan cement mill, and its chemical composition and mass percentage content see the following form 2 (total amounts 100%, remaining mass percentage content is loss on ignition):
Table 2 grog and gypsum chemical composition
| Composition | Loss on ignition | SiO 2 | Al 2O 3 | Fe 2O 3 | CaO | MgO | SO 3 |
| Grog % | 0.71 | 19.04 | 5.62 | 3.39 | 63.23 | 1.92 | 0.90 |
| Gypsum % | 8.65 | 1.70 | 0.30 | 0.20 | 38.41 | 0.80 | 48.63 |
Be that the grog of 95:5 and gypsum are crushed to below 5mm by mass ratio with jaw crusher, take 5kg raw material, the slow setting grinding aid taken evenly is dropped on raw material, then raw material is poured into φ 500mm × 500mm and test in little mill, grinding 25min, discharging 5min.Grinding aid volume is set to 0.05%, and arranges control group.
With reference to the regulation in GB/T17671-1999 " Test method for strength of hydraulic cement mortar ", strength test is carried out to the cement produced.Regulation according to GB/T1346-2011 " water quality standard denseness water consumption, time of coagulation, the stability method of inspection " carries out consumptive use of water normal consistence and time of coagulation measures.MalvernMastersizer 2000 laser particle analyzer is adopted to measure cement granularity.
Detected result is as table 3, table 4 and table 5:
Table 3 cement setting time detected result
| Slow setting grinding aid is numbered | Consumptive use of water normal consistence % | Presetting period min | Final setting time min |
| 0 | 25.6 | 107 | 172 |
| DE-1 | 25.5 | 440 | 515 |
| DE-2 | 25.5 | 450 | 526 |
| DE-3 | 25.4 | 433 | 561 |
| DE-4 | 25.3 | 452 | 540 |
| DE-5 | 25.2 | 465 | 545 |
| DE-6 | 25.0 | 447 | 510 |
Table 4 cement granularity detected result
Table 5 cement mortar detected result
From table 3, table 4 and table 5, retardation setting type grinding aid provided by the invention, has the following advantages: (1) slow setting: after mixing slow setting grinding aid of the present invention, cement setting time obviously extends; Early hydration heat release is slow, uses under being applicable to hot environment; For mass concrete engineering, the too fast phenomenon causing concrete cracking of early hydration heat release can be prevented; (2) grinding aid: laser particle size measurement result shows, slow setting grinding aid of the present invention can effectively reduce macrobead content, optimizes grain composition; (3) strengthen: as can be seen from Table 5,3 days of cement and the 28 days the highest amplification of folding strength are respectively 21.1%, 17.6%, and 3 days and the 28 days the highest amplification of ultimate compression strength are respectively 9.3%, 8.5%.Therefore, after mixing retardation setting type grinding aid provided by the invention, suitably can improve the consumption of mineral admixture, be conducive to energy-conserving profit waste.
Embodiment 7:
A kind of retardation setting type cement grinding aid is the modification diethanolamine mother liquor of 20% by mass percent, the glycerol of 1%, the sodium sulfate of 5%, and surplus 74% is water mixing composition;
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 21.1 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration is aqueous sodium hydroxide solution 10 mass parts of 40%, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) to be added dropwise in reaction vessel and to stir, controlling temperature of reaction is 40 DEG C, after dripping, then react 1.0 hours, pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor.
Embodiment 8:
A kind of retardation setting type cement grinding aid is the modification diethanolamine mother liquor of 30% by mass percent, the glycerol of 10%, the sodium sulfate of 10%, and surplus 50% is water mixing composition;
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration is aqueous sodium hydroxide solution 12 mass parts of 40%, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) to be added dropwise in reaction vessel and to stir, controlling temperature of reaction is 50 DEG C, after dripping, then react 2 hours, pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor.
Embodiment 9:
A kind of retardation setting type cement grinding aid is the modification diethanolamine mother liquor of 25% by mass percent, the glycerol of 6%, the sodium sulfate of 8%, and surplus 61% is water mixing composition;
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 22 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration is aqueous sodium hydroxide solution 11 mass parts of 40%, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) to be added dropwise in reaction vessel and to stir, controlling temperature of reaction is 45 DEG C, after dripping, then react 1.5 hours, pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor.
Embodiment 10 ~ 16:
A kind of retardation setting type cement grinding aid is the modification diethanolamine mother liquor of 20% ~ 30% by mass percent, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is water mixing composition;
In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration is aqueous sodium hydroxide solution 10 ~ 12 mass parts of 40%, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) to be added dropwise in reaction vessel and to stir, controlling temperature of reaction is 40 ~ 50 DEG C, after dripping, then react 1.0 ~ 2 hours, pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor.
In each embodiment, concrete mass parts (unit: gram) consumption of each component raw material sees the following form:
Embodiment 17:
A preparation method for retardation setting type cement grinding aid, step is:
A, batching: take diethanolamine 21.1 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration be 40% aqueous sodium hydroxide solution 10.2 mass parts, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, for subsequent use;
B, preparation modification diethanolamine mother liquor: open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) being added dropwise in reaction vessel and stirring, control temperature of reaction is 40 ~ 50 DEG C; After dripping, then react 1.5 hours; Pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor;
C, prepare retardation setting type cement grinding aid: be the modification diethanolamine mother liquor of 25%, the glycerol of 5%, the sodium sulfate of 7% and surplus 63% by mass percentage for water gets each component raw material; Modification diethanolamine mother liquor, glycerol, sodium sulfate and water are mixed, i.e. obtained retardation setting type cement grinding aid.
Embodiment 18:
A preparation method for retardation setting type cement grinding aid, step is:
A, batching: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration be 40% aqueous sodium hydroxide solution 10 ~ 12 mass parts, diethanolamine is added in the reaction vessel (such as there-necked flask) of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, for subsequent use;
The concrete mass parts consumption of each component raw material is arbitrary in embodiment 7 ~ 16, omits;
B, preparation modification diethanolamine mother liquor: open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution (slowly) being added dropwise in reaction vessel and stirring, control temperature of reaction is 40 ~ 50 DEG C; After dripping, then react 1.0 ~ 2 hours; Pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, separating out NaCl, get supernatant liquid and be obtained modification diethanolamine mother liquor;
C, prepare retardation setting type cement grinding aid: be the modification diethanolamine mother liquor of 20% ~ 30% by mass percentage, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is that water gets each component raw material; Modification diethanolamine mother liquor, glycerol, sodium sulfate and water are mixed, i.e. obtained retardation setting type cement grinding aid; The concrete mass percent consumption of each component raw material is arbitrary in embodiment 7 ~ 16, omits.
In above-described embodiment 7 ~ 18: describedly pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, be preferably and pour reaction product into container and be placed in vacuum drying oven, evaporation removing water wherein under the condition of temperature 70 ~ 90 DEG C, pressure 40 ~ 80Pa.
In above-described embodiment: each raw material adopted is commercially available prod.
In above-described embodiment: in the percentage adopted, do not indicate especially, be quality (weight) percentage or well known to a person skilled in the art percentage; Described quality (weight) part can be all gram or kilogram.
In above-described embodiment: the processing parameter (temperature, time, concentration etc.) in each step and each amounts of components numerical value etc. are scope, and any point is all applicable.
The concrete same prior art of technology contents described in content of the present invention and above-described embodiment.
The invention is not restricted to above-described embodiment, all can implement described in content of the present invention and there is described good result.
Claims (4)
1. a retardation setting type cement grinding aid, is characterized in that: be the modification diethanolamine mother liquor of 20% ~ 30% by mass percent, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is water mixing composition;
The preparation method of described modification diethanolamine mother liquor is: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration be 40% aqueous sodium hydroxide solution 10 ~ 12 mass parts, diethanolamine is added in the reaction vessel of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution being added dropwise in reaction vessel and stirring, controlling temperature of reaction is 40 ~ 50 DEG C; After dripping, then react 1.0 ~ 2 hours; Pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, getting supernatant liquid and be obtained modification diethanolamine mother liquor.
2. by retardation setting type cement grinding aid according to claim 1, it is characterized in that: describedly pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, pour reaction product into container and be placed in vacuum drying oven, evaporation removing water wherein under the condition of temperature 70 ~ 90 DEG C, pressure 40 ~ 80Pa.
3. a preparation method for retardation setting type cement grinding aid, is characterized in that step is:
A, batching: take diethanolamine 21.1 ~ 25 mass parts, epoxy chloropropane 9.2 mass parts, mass percent concentration be 40% aqueous sodium hydroxide solution 10 ~ 12 mass parts, diethanolamine is added in the reaction vessel of band whipping appts, epoxy chloropropane is added in constant pressure addition pipe, aqueous sodium hydroxide solution is added in another constant pressure addition pipe, for subsequent use;
B, preparation modification diethanolamine mother liquor: open two constant pressure addition pipes simultaneously, epoxy chloropropane and aqueous sodium hydroxide solution being added dropwise in reaction vessel and stirring, controlling temperature of reaction is 40 ~ 50 DEG C; After dripping, then react 1.0 ~ 2 hours; Pour reaction product into container and be placed in vacuum drying oven evaporation removing water wherein, getting supernatant liquid and be obtained modification diethanolamine mother liquor;
C, prepare retardation setting type cement grinding aid: be the modification diethanolamine mother liquor of 20% ~ 30% by mass percentage, the glycerol of 1% ~ 10%, the sodium sulfate of 5% ~ 10%, and surplus is that water gets each component raw material; Modification diethanolamine mother liquor, glycerol, sodium sulfate and water are mixed, i.e. obtained retardation setting type cement grinding aid.
4. by the preparation method of retardation setting type cement grinding aid described in claim 3, it is characterized in that: pour reaction product into container described in step b and be placed in vacuum drying oven evaporation removing water wherein, pour reaction product into container and be placed in vacuum drying oven, evaporation removing water wherein under the condition of temperature 70 ~ 90 DEG C, pressure 40 ~ 80Pa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109096127A (en) * | 2018-09-27 | 2018-12-28 | 湖北鑫统领万象科技有限公司 | Using silane coupling agent production by-product as the hydramine of raw material and preparation method and application |
| CN113445747A (en) * | 2021-06-28 | 2021-09-28 | 福建伯裕堡建筑科技发展有限公司 | Rigid composite waterproof structure containing FJT waterproof compacting agent and construction method thereof |
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| CN113445747A (en) * | 2021-06-28 | 2021-09-28 | 福建伯裕堡建筑科技发展有限公司 | Rigid composite waterproof structure containing FJT waterproof compacting agent and construction method thereof |
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|---|---|
| CN104529222B (en) | 2016-09-14 |
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